JP2010123977A - Chemical delivery system having purge system using complex purge technology - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a chemical delivery system having a purge system, with respect to a system or a manifold for delivering, transporting, supplying or feeding the chemical from a bulk delivery canister to a manufacturing process tool such as a chemical-vapor deposition device (CVD) and the like, more specifically to a process tool utilized in manufacturing an integrated circuit. <P>SOLUTION: The chemical delivery system (500) is disclosed based on the purge technology using various kinds of combinations of a medium-level vacuum source, a hard vacuum source, and/or a liquid flush system (506). Further, the delivery system is also equipped with a heater system for heating the chemical delivery system. <P>COPYRIGHT: (C)2010,JPO&INPIT

Description

  The present invention generally relates to a process tool, such as a chemical vapor deposition (or chemical vapor deposition) (CVD) device, and more particularly to a process utilized in the formation of integrated circuits. The present invention relates to systems and manifolds for delivering chemicals from a bulk delivery canister to a tool.

  For example, the manufacture of electronic devices such as integrated circuits is well known. In certain steps in such manufacturing, the chemical may be supplied to a predetermined process tool that uses the chemical. For example, CVD reactors are commonly used to form layers of a predetermined material such as a dielectric layer or a conductive layer. Historically, process chemicals were supplied to the CVD reactor through a bulk delivery cabinet. The chemicals used to form the integrated circuit must be ultra-pure to obtain a sufficient process yield. As the size of integrated circuits has decreased, the demand for maintaining the purity of the source chemical has increased in direct proportion. This is because impurities (contaminants, or contaminants) tend to adversely affect the electrical characteristics of the integrated circuit as the line spacing and intermediate dielectric layer thickness decreases. Increasing demand for chemical purity also affects chemical delivery systems.

  Thus, an improved chemical delivery system that prevents impurities from entering the process tool during chemical canister replacement or refill operations and other maintenance operations Is needed. Impurities in question can include particles, moisture and trace elements. There is a need for an improved manifold system to meet these demanding requirements.

  Furthermore, as the demand for chemical purity increases, the types of chemicals used in the manufacture of integrated circuits have increased. In addition, some chemicals for manufacturing integrated circuits exhibit more demanding physical properties and / or are more toxic than traditionally used chemicals, and thus chemical delivery systems. Imposes additional requirements on. For example, a very low vapor pressure chemical having a vapor pressure of 100 mT or less, or even 10 mT or less may be used in the manufacture of integrated circuits. One such chemical substance, TaEth (tantalum pentaethoxide), has a vapor pressure of 1 mT or less and can be used for CVD formation of dielectric layers. Another such chemical, TDEAT (tetrakis (diethylamido) titanium), has a vapor pressure of about 7 mT and could be used for CVD formation of titanium nitride layers. Yet another low vapor pressure chemical is TEASate (triethyl arsenate). Additional low vapor pressure chemicals may be those utilized to deposit (or deposit) a conductive layer comprising copper or TaN. Because the chemical vapor pressure is so low, traditional methods of purging the chemical delivery system manifold system are inadequate. Existing manifolds can adequately remove traditional compounds (compounds or blends) from lines and manifolds through repeated evacuation / gas purge cycles, whereas such evacuation / gas purge cycles can be Substances with very low pressure cannot be removed properly. Accordingly, there is a need for an improved method and apparatus for purging a manifold system so that very low vapor pressure chemicals can be adequately purged from various components of the chemical delivery system. It has been. In addition, materials such as TaEth may require heating of the chemical cabinet. Accordingly, it is desirable to have a chemical delivery system that efficiently incorporates a heating system into a gas cabinet.

  Other chemicals also impose increased requirements on the purge technology utilized. For example, chemicals that contain solid compounds in a solution with a liquid can also be used as reactants in the manufacture of integrated circuits. Solid chemicals are typically stored in chemical canisters in a dispersed state in an organic liquid. For example, a solid reactant such as a barium / strontium / titanate (BST) cocktail (solution) used to form the dielectric layer can be dispersed in a liquid such as tetrahydrofuran (THF) or triglyme. A wide variety of other solid materials can also be used in combination with other organic liquids, such as US Pat. No. 5,820,664, the disclosure of which is incorporated herein by reference. It is described in.

  When such solid compositions are sold and used in canisters, they are described in US Pat. Nos. 5,465,766, 5,562,132, and 5,607,002. As can be seen, canisters are often adapted to connect to a manifold for chemical distribution. However, as the canister changes, existing manifolds cannot adequately match the ability to clean (or clean) the manifolds and lines prior to replacement. Thus, when a vacuum / gas purge cycle is used on a solid / liquid composition, the liquid evaporates away and the solid compound remains in the line. This is unacceptable because the line is contaminated, especially when the canister is replaced with another compound. Particle contamination and chemical concentration changes cause severe process problems in process tools. There is a strong desire to solve this problem.

  Furthermore, it is desirable to improve the cleaning and purging process because the chemicals utilized are highly toxic and can be harmful. Accordingly, it is desirable to reduce the residual level of low vapor pressure chemicals (such as those described herein) in the chemical delivery system manifolds and lines.

  In addition, at least some of the chemicals that are contemplated for use in deposition systems have ambient temperature requirements that may require elevated temperatures to prevent solidification. Therefore, a chemical delivery system that addresses the above-mentioned problems while providing a controlled temperature environment efficiently and economically is desirable.

  The present invention provides a solution to one or more of the above disadvantages and needs. More particularly, a chemical delivery system is provided that employs complex technology to obtain an appropriate chemical purge of the chemical delivery system. The purge sequence functions to purge the chemical delivery system manifold and canister connection lines before removing an empty chemical supply canister or installing a new canister. More particularly, a purge technique is disclosed that may use at least one of various combinations of medium level vacuum sources, hard vacuum sources, and / or liquid flush systems. . By using multiple purge techniques, difficult-to-purge chemicals such as TaEth, TDEAT, BST, etc. can be efficiently purged from the chemical delivery system. The chemical delivery system may also include an efficient, conveniently arranged heater system for heating the chemical delivery system cabinet (or container). Advantageously, the manifold of the present invention allows for an improved purge effective against low vapor pressure (or low vapor pressure) materials and toxic chemicals.

  In one aspect, the present invention includes a method for purging low vapor pressure chemicals from a chemical delivery system having a plurality of valves and lines. The method uses a first purge technique to remove chemicals, gases, or impurities from at least some valves and lines; removes chemicals, gases, or impurities from at least some valves and lines; Using a second purge technique to remove; and using a third purge technique to remove chemicals, gases, or impurities from within at least some valves and lines. In this method, each of the first, second and third purge techniques can be different. The first purge technique may be a first vacuum (vacuum) process, the second purge technique may be a flowing purge process using an inert gas, The third purge technique may be a liquid flush (or liquid flush) process. Alternatively, the third purge technique is a second evacuation process, and the first and second evacuation processes may use different types of vacuum sources.

  Another method according to the present invention is a method of operating a chemical delivery system for delivering chemicals to a semiconductor process tool. The method includes supplying at least one liquid chemical from the chemical delivery system to the semiconductor process tool; purging gas, liquid chemical or impurities from at least a portion of the chemical delivery system. The purge includes the use of at least three different purge techniques; and changing (or replacing) at least one canister of the chemical delivery system, wherein the canister includes at least one type of canister Containing liquid chemicals.

  In yet another aspect of the invention, a method for purging a low vapor pressure liquid chemical from a chemical delivery system is provided. The method includes supplying a low vapor pressure liquid chemical to at least one line or valve of the chemical delivery system; and purging the low vapor pressure liquid chemical from the at least one line or valve. And the purge may include using at least three different purge techniques. The low vapor pressure liquid chemical may be TaEth, TDEAT or BST or other low vapor pressure chemicals.

  In another aspect, a method for forming a dielectric layer on a semiconductor substrate is provided. The method provides a semiconductor substrate having one or more layers; provides a deposition or deposition, deposition or deposition process tool; and a low vapor pressure liquid chemical. Connecting the chemical delivery system to the deposition process tool to feed the deposition process tool. The method includes periodically purging a low vapor pressure liquid chemical from at least a portion of a chemical delivery system, the purge including the use of at least three different purge techniques; and low Further comprising depositing a dielectric layer on the semiconductor substrate by using a vapor pressure liquid chemical in the deposition process tool. The low vapor pressure liquid chemical may be TaEth or BST.

  In yet another aspect, a method for forming a layer containing titanium on a semiconductor substrate is provided. The method includes providing a semiconductor substrate having one or more layers; providing a deposition process tool; and supplying a low vapor pressure liquid chemical to the deposition process tool. It may include connecting the substance delivery system to the deposition process tool. The method also includes periodically (or periodically) purging a low vapor pressure liquid chemical from at least a portion of the chemical delivery system, the purge using at least three different purge techniques. And depositing a layer containing titanium on the semiconductor substrate by using a low vapor pressure liquid chemical in the deposition process tool. The low vapor pressure liquid chemical may be TDEAT. The layer can include titanium nitride.

  In one aspect, the present invention may be a chemical delivery system. The chemical delivery system includes: at least one canister inlet and at least one canister outlet line; a plurality of manifold valves and lines; a first purge source connected to the plurality of manifold valves and lines; A first purge source inlet; a second purge source connected to the plurality of manifold valves and lines; a second purge source inlet; and a third purge source connected to the plurality of manifold valves and lines; A purge source inlet may be included, and each of the first, second and third purge sources may be a different type of purge source. The first purge source can be a first vacuum source, the second purge source can be a gas source (or gas supply), and the third purge source can be a liquid source (or liquid supply). . Alternatively, the third purge source can be a second vacuum source and the first and second vacuum sources can be different types of vacuum sources.

  In another aspect, a chemical delivery system is provided for delivering low vapor pressure liquid chemicals to a semiconductor process tool. The system is at least one chemical output line, connected to the manifold of the chemical delivery system and operable to supply a low vapor pressure liquid chemical to the semiconductor process tool An output line; at least three purge source inlet lines that connect at least three different purge sources to the manifold; and one or more refills connected to the manifold Can include refillable canisters. The one or more refillable canisters can include at least a first canister and a second canister. In addition, low vapor pressure liquid chemicals may be supplied from the second canister to the semiconductor process tool and the chemical delivery system may refill (refill) the second canister from the first canister. It can be done. Alternatively, the system may be able to supply liquid chemicals to the semiconductor process tool from both the first canister and the second canister.

  Another aspect disclosed herein may include a cabinet for housing a chemical delivery system. The cabinet is a plurality of cabinet walls forming an interior cabinet space, wherein at least one of the cabinet walls is a door; a cabinet wall; at least one heater element disposed within or adjacent to the door; And may include an air flow passage in close proximity to the at least one heater element. The cabinet may further include at least one heat exchange element in the air flow passage and thermally connected to the heater. The heat exchange element can be a plurality of fins. The air flow passage may be formed along the back side of the door and the heater element may be formed along the front side of the door. The cabinet door may have a cavity and an interface structure within the cavity that forms at least a portion of the door wall. The heater is provided in the recess of the door (or embedded in the door).

  Another aspect of the disclosed invention can include a temperature controlled cabinet for housing a liquid chemical delivery system. The cabinet may include at least one door; at least one heater element disposed in or on the door; an air vent in the door; and an air flow passage in close proximity to the at least one heater element. The air flow passage may be in thermal communication with or in communication with at least one heater element, and an air vent may provide (or supply) an air inlet to the air flow passage.

  In yet another aspect, a temperature controlled cabinet is provided for housing a liquid chemical delivery system. The cabinet may include a plurality of cabinet walls; and at least one heater element disposed within or on at least the first cabinet wall, the heater element being located outside the first cabinet wall, the heater Thermal energy from can be connected (or connected) to the interior of the cabinet through the first cabinet wall. The first cabinet wall may be at least part of a cabinet door. The cabinet may further include an air passage adjacent to the inside of the first cabinet wall.

  Yet another aspect of the present invention is a method for controlling the temperature of a cabinet containing a chemical delivery system. The method provides a plurality of cabinet walls forming an interior cabinet space; disposing at least one heater element within or in close proximity to at least the first cabinet wall; and Heat transfer from the heater to the internal cabinet space may be included using the cabinet wall as a heat transfer mechanism.

  In yet another aspect, a method for controlling the temperature of a cabinet containing a liquid chemical delivery system is provided. The method includes providing a plurality of cabinet walls forming an interior cabinet space; disposing at least one heater element outside at least a portion of the first cabinet wall; using the first cabinet wall as a heat transfer mechanism. Using heat to transfer heat from the heater to the inside of the first cabinet wall; and flowing air across the inside of the first cabinet to create side air in the interior cabinet space. ) May be heated to circulate the internal cabinet space.

  Yet another aspect of the present invention is a chemical delivery system manifold useful for delivering liquid chemicals from canisters. The manifold may include a vacuum supply valve connected to a vacuum generator; a pressure vent valve connected to the vacuum generator; and a carrier gas isolation valve connected to a carrier gas source. The manifold is a process line shutoff valve connected to a bypass valve and a canister outlet line, the canister outlet line being connectable to the canister outlet valve; a carrier gas shutoff valve and a bypass valve A flush inlet valve connected between and a liquid flush source; and a canister inlet line connectable between the canister inlet valve and the bypass valve.

  Also disclosed is a chemical delivery system manifold useful for delivering liquid chemicals from canisters. The system includes a first vacuum supply valve for connecting the manifold to a first vacuum source; a second vacuum supply valve for connecting the manifold to a second vacuum source, the first and second vacuum sources being of a type A second vacuum supply valve that is a different vacuum source; and a pressure vent valve connected to either or both of the first and second vacuum sources. The system also includes a carrier gas shutoff valve connected to a carrier gas source; a process line shutoff valve connected to a bypass valve and a canister outlet line, the canister outlet line connected to the canister outlet valve And can include a process line shutoff valve; and a canister inlet line that can be connected between the canister inlet valve and the bypass valve. The manifold may also include a flush inlet valve that is connected between the carrier gas shutoff valve and the bypass valve and that can be connected to a liquid flush source.

  In another aspect, a chemical delivery system is disclosed. The chemical delivery system includes (1) a vacuum supply valve; (2) a vacuum generator; (3) a carrier gas shutoff valve; (4) a bypass valve; (5) a process line shutoff valve; (6) Liquid flush inlet valve; (7) low pressure vent valve; (8) canister inlet valve; and (9) canister outlet valve. The system may be configured such that a vacuum supply valve is connected to a vacuum generator; a carrier gas shutoff valve is connected to a liquid flush inlet valve; and a liquid flush inlet valve is connected to a bypass valve. Also, a bypass valve is further connected to the process line shutoff valve; a low pressure vent valve is connected to the vacuum generator; a process line shutoff valve is also connected to the canister outlet valve; and a canister inlet valve is the canister Connected to outlet valve.

  Also disclosed is a method for purging low vapor pressure liquid chemicals from a chemical delivery system. The method can include providing a manifold. The manifold connects to a vacuum supply valve connected to a vacuum source, a pressure vent valve connected to a vacuum supply valve, a carrier gas shutoff valve connected to a carrier gas source, a bypass valve and a canister outlet line Process line shutoff valve (canister outlet line can be connected to canister outlet valve), flush inlet valve connected between carrier gas shutoff valve and bypass valve (flush inlet valve connected to liquid flush source) And a canister inlet line that can be connected between the canister inlet valve and the bypass valve. The method also supplies a low vapor pressure liquid chemical to at least one line or valve of the chemical delivery system; and purges the low vapor pressure liquid chemical from the at least one line or valve. Of course, the purge also includes the use of at least three different purge techniques.

In yet another aspect, a method for purging a low vapor pressure liquid chemical from a chemical delivery system is provided. The method can include providing a manifold. The manifold connects to a vacuum supply valve connected to a vacuum source, a pressure vent valve connected to a vacuum supply valve, a carrier gas shutoff valve connected to a carrier gas source, a bypass valve and a canister outlet line Process line shutoff valves (canister outlet lines can be connected to the canister outlet valves) and canister inlet lines that can be connected between the canister inlet valve and the bypass valve. The method includes supplying a low vapor pressure liquid chemical to at least one line or valve of the chemical delivery system; purging the low vapor pressure liquid chemical from the at least one line or valve; The purge may further comprise using at least three different purge techniques.
The present invention may include the following aspects.
Aspect 1 A method for purging a low vapor pressure chemical from a chemical delivery system having a plurality of valves and lines comprising:
Using a first purge technique to remove chemicals, gases, or impurities from within at least some valves and lines;
Using a second purge technique to remove chemicals, gases, or impurities from within at least some valves and lines; and
Use a third purge technique to remove chemicals, gases, or impurities from at least some valves and lines
Wherein each of the first, second and third purge techniques is different.
(Aspect 2) The method according to Aspect 1, wherein the first purge technique is a first evacuation process and the second purge technique is a flowing purge process using an inert gas.
(Aspect 3) The method of aspect 2, wherein the third purge technique is a liquid flush process.
(Aspect 4) The method according to Aspect 2, wherein the third purge technique is a second evacuation step, and the first and second evacuation steps use different types of vacuum sources.
(Aspect 5) The method according to Aspect 4, wherein the first evacuation step uses a Venturi vacuum source.
(Aspect 6) The method according to Aspect 5, wherein the second evacuation step uses a hard vacuum source.
Embodiment 7 The method of embodiment 6, wherein the hard vacuum source is provided from a process tool.
(Aspect 8) The method of aspect 1, further comprising a fourth purge technique.
(Aspect 9) The first purge technique is a first evacuation process, the second purge technique is a flowing purge process using an inert gas, the third purge technique is a liquid flush process, and the fourth purge technique. Is the second evacuation step, and the first and second evacuation steps use different types of vacuum sources.
(Aspect 10) The method according to aspect 9, wherein the first evacuation step uses a venturi vacuum source, and the second evacuation step uses a hard vacuum source.
Aspect 11 A method of operating a chemical delivery system for delivering chemicals to a semiconductor process tool comprising:
Supplying at least one liquid chemical from a chemical delivery system to a semiconductor process tool;
Purging gas, liquid chemicals or impurities from at least a portion of the chemical delivery system, the purge including the use of at least three different purge techniques; and
Modifying at least one canister of a chemical delivery system, the canister containing at least one liquid chemical
Including methods.
(Aspect 12) The method of aspect 11, wherein the chemical delivery system comprises at least a first canister and a second canister.
Aspect 13 The method of aspect 12, wherein at least one liquid chemical is supplied from the second canister to the semiconductor process tool and the chemical delivery system can replenish the second canister from the first canister. .
Embodiment 14: The method of embodiment 12, wherein the chemical delivery system is capable of supplying liquid chemicals from both the first canister and the second canister to the semiconductor process tool.
Embodiment 15: The method of embodiment 11, wherein the at least three different purge techniques comprise at least a first evacuation step and a flowing purge step using an inert gas.
Embodiment 16 The method of embodiment 15, wherein the at least three different purge techniques further comprise a liquid flush step.
Embodiment 17: The method of embodiment 16, wherein the chemical delivery system has at least a first canister and a second canister.
Embodiment 18: The method of embodiment 17, wherein at least one liquid chemical is supplied from the second canister to the semiconductor process tool and the chemical delivery system can replenish the second canister from the first canister. .
Embodiment 19 The method of embodiment 17, wherein the chemical delivery system is capable of supplying liquid chemicals to the semiconductor process tool from both the first canister and the second canister.
(Aspect 20) The method according to Aspect 15, wherein the first evacuation step uses a Venturi vacuum source.
(Aspect 21) The method according to Aspect 15, wherein the first evacuation step uses a hard vacuum source.
Embodiment 22 The method of embodiment 15, wherein the at least three different purge techniques further comprise a second evacuation step, wherein the first and second evacuation steps use different types of vacuum sources.
Embodiment 23 The method according to embodiment 22, wherein the chemical delivery system has at least a first canister and a second canister.
Embodiment 24 The method of embodiment 23, wherein at least one liquid chemical is supplied from the second canister to the semiconductor process tool and the chemical delivery system can replenish the second canister from the first canister. .
Embodiment 25 The method of embodiment 13, wherein the chemical delivery system is capable of supplying the liquid chemical from both the first canister and the second canister to the semiconductor process tool.
Embodiment 26 The method according to Embodiment 22, wherein the first evacuation step uses a Venturi vacuum source.
(Aspect 27) The method according to Aspect 22, wherein the second evacuation step uses a hard vacuum source.
Embodiment 28 The method of embodiment 27, wherein the hard vacuum source is provided from a semiconductor process tool.
Embodiment 29 The method of embodiment 11, wherein the purge comprises the use of a fourth purge technique.
(Aspect 30) The first purge technique is a first evacuation process, the second purge technique is a flowing purge process using an inert gas, the third purge technique is a liquid flush process, and the fourth purge technique. 30 is a second evacuation step, and the first and second evacuation steps use different types of vacuum sources.
Embodiment 31 The method of embodiment 30, wherein the chemical delivery system comprises at least a first canister and a second canister.
Aspect 32. The method of aspect 31, wherein at least one liquid chemical is provided from the second canister to the semiconductor process tool and the chemical delivery system can replenish the second canister from the first canister. .
Aspect 33. The method of aspect 31, wherein the chemical delivery system is capable of supplying liquid chemicals from both the first canister and the second canister to the semiconductor process tool.
(Aspect 34) The method according to aspect 30, wherein the first evacuation step uses a venturi vacuum source, and the second evacuation step uses a hard vacuum source.
Embodiment 35 The method of embodiment 34, wherein the hard vacuum source is provided from a semiconductor process tool.
Embodiment 36 The method of embodiment 35, wherein the chemical delivery system has at least a first canister and a second canister.
Embodiment 37 The method of embodiment 36, wherein at least one liquid chemical is supplied from the second canister to the semiconductor process tool and the chemical delivery system can replenish the second canister from the first canister. .
Embodiment 38 The method of embodiment 36, wherein the chemical delivery system is capable of supplying a liquid chemical to the semiconductor process tool from both the first canister and the second canister.
Embodiment 39 A method for purging a low vapor pressure liquid chemical from a chemical delivery system comprising:
Supplying low vapor pressure liquid chemicals to at least one line or valve of the chemical delivery system; and
Purging low vapor pressure liquid chemicals from at least one line or valve, the purge including the use of at least three different purge techniques;
Including methods.
Embodiment 40 The method according to embodiment 39, wherein the low vapor pressure liquid chemical is TaEth.
(Aspect 41) The chemical substance delivery system has at least a first canister and a second canister, a low vapor pressure liquid chemical substance is supplied from the second canister to the semiconductor process tool, and the chemical substance delivery system is a first chemical substance delivery system. 41. The method of aspect 40, wherein the second canister can be replenished from the canister.
(Aspect 42) The chemical delivery system has at least a first canister and a second canister, and the chemical delivery system has a low vapor pressure liquid chemical from both the first canister and the second canister to the semiconductor process tool. 41. The method of aspect 40, wherein
Embodiment 43 The method of embodiment 40, wherein the at least three different purge techniques comprise at least a first evacuation step and a flowing purge step using an inert gas.
Embodiment 44 The method of embodiment 43, wherein the at least three different purge techniques further comprise a liquid flush step.
Embodiment 45 The method according to embodiment 39, wherein the low vapor pressure liquid chemical is TDEAT.
(Aspect 46) The chemical substance delivery system has at least a first canister and a second canister, TDEAT is supplied from the second canister to the semiconductor process tool, and the chemical substance delivery system sends the second canister from the first canister. 46. The method of aspect 45, wherein the method can be replenished.
(Aspect 47) The chemical delivery system has at least a first canister and a second canister, and the chemical delivery system can supply TDEAT to the semiconductor process tool from both the first canister and the second canister. 46. A method according to embodiment 45.
Embodiment 48 The method of embodiment 45, wherein the at least three different purge techniques comprise at least a first evacuation step and a flowing purge step using an inert gas.
Embodiment 49 The method of embodiment 48, wherein the at least three different purge techniques further comprise a liquid flush step.
(Aspect 50) The method according to aspect 39, wherein the low vapor pressure liquid chemical is BST.
(Aspect 51) The chemical substance delivery system has at least a first canister and a second canister, the BST is supplied from the second canister to the semiconductor process tool, and the chemical substance delivery system sends the second canister from the first canister. 51. The method of aspect 50, wherein the method can be replenished.
(Aspect 52) The chemical substance delivery system has at least a first canister and a second canister, and the chemical substance delivery system can supply BST from both the first canister and the second canister to the semiconductor process tool. 51. A method according to aspect 50.
Embodiment 53 The method of embodiment 50, wherein the at least three different purge techniques comprise at least a first evacuation step and a flowing purge step using an inert gas.
Embodiment 54 The method of embodiment 53, wherein the at least three different purge techniques further comprise a liquid flush step.
(Aspect 55) A method for forming a dielectric layer on a semiconductor substrate, comprising:
Providing a semiconductor substrate having one or more layers;
Supplying deposition process tools;
Connecting a chemical delivery system to the deposition process tool to supply low vapor pressure liquid chemicals to the deposition process tool;
Periodically purging low vapor pressure liquid chemical from at least a portion of the chemical delivery system, the purge including the use of at least three different purge techniques; and
Deposit a dielectric layer on a semiconductor substrate by using a low vapor pressure liquid chemical in the deposition process tool
Including methods.
Embodiment 56 The method according to embodiment 55, wherein the low vapor pressure liquid chemical is TaEth or BST.
(Aspect 57) The chemical substance delivery system has at least a first canister and a second canister, and a low vapor pressure liquid chemical substance is supplied from the second canister to the semiconductor process tool, and the chemical substance delivery system is the first chemical substance delivery system. 57. The method of aspect 56, wherein the second canister can be replenished from the canister.
(Aspect 58) The chemical delivery system has at least a first canister and a second canister, and the chemical delivery system delivers a low vapor pressure chemical from both the first canister and the second canister to the semiconductor process tool. 57. The method according to aspect 56, which can be provided.
Embodiment 59 The method according to embodiment 56, wherein the at least three different purge techniques comprise at least a first evacuation step and a flowing purge step using an inert gas.
Embodiment 60 The method of embodiment 59, wherein the at least three different purge techniques further comprise a liquid flush step.
(Aspect 61) A method for forming a layer containing titanium on a semiconductor substrate, comprising:
Providing a semiconductor substrate having one or more layers;
Supplying deposition process tools;
Connecting a chemical delivery system to the deposition process tool to supply low vapor pressure liquid chemicals to the deposition process tool;
Periodically purging low vapor pressure liquid chemical from at least a portion of the chemical delivery system, the purge including the use of at least three different purge techniques; and
Deposit titanium-containing layers on semiconductor substrates by using low vapor pressure liquid chemicals in deposition process tools
Including methods.
Embodiment 62 The method according to embodiment 61, wherein the low vapor pressure liquid chemical is TDEAT.
Embodiment 63 The method of embodiment 62, wherein the layer comprises titanium nitride.
(Aspect 64) The chemical substance delivery system has at least a first canister and a second canister, the TDEAT is supplied from the second canister to the semiconductor process tool, and the chemical substance delivery system sends the second canister from the first canister. 63. A method according to aspect 62, which can be replenished.
(Aspect 65) The chemical substance delivery system has at least a first canister and a second canister, and the chemical substance delivery system can supply TaEth from both the first canister and the second canister to the semiconductor process tool. 63. A method according to aspect 62.
Embodiment 66 The method of embodiment 62, wherein the at least three different purge techniques comprise at least a first evacuation step and a flowing purge step using an inert gas.
Embodiment 67 The method of embodiment 66, wherein the at least three different purge techniques further comprise a liquid flush step.
(Aspect 68) A chemical delivery system comprising:
At least one canister inlet and at least one canister outlet line;
Multiple manifold valves and lines;
A first purge source inlet connecting the first purge source to a plurality of manifold valves and lines;
A second purge source inlet connecting the second purge source to the plurality of manifold valves and lines; and
Third purge source inlet connecting a third purge source to a plurality of manifold valves and lines
And wherein each of the first, second and third purge sources is a different type of purge source.
Embodiment 69 The system according to Embodiment 68, wherein the first purge source is a first vacuum source and the second purge source is a gas source.
Embodiment 70 The system according to embodiment 69, wherein the third purge source is a liquid source.
Embodiment 71 The system of embodiment 69, further comprising a liquid waste output line.
(Aspect 72) The system according to aspect 69, wherein the third purge source is a second vacuum source, and the first and second vacuum sources are different types of vacuum sources.
Embodiment 73 The system according to Embodiment 72, wherein the first vacuum source is a Venturi vacuum source.
(Aspect 74) The system according to aspect 73, wherein the second vacuum source is a hard vacuum source.
Embodiment 75 The system of embodiment 74, wherein the hard vacuum source is provided from a process tool.
Embodiment 76 The system of embodiment 68, further comprising a fourth purge source.
(Aspect 77) The first purge source is the first vacuum source, the second purge source is the inert gas source, the third purge source is the liquid source, and the fourth purge source is the second. The system according to aspect 76, wherein the system is a vacuum source and the first and second vacuum sources are different types of vacuum sources.
(Aspect 78) A system according to aspect 77, wherein the first vacuum source is a Venturi vacuum source and the second vacuum source is a hard vacuum source.
Embodiment 79 A chemical delivery system for delivering a low vapor pressure liquid chemical to a semiconductor process tool comprising:
At least one chemical output line that is connected to the chemical delivery system manifold and is operable to supply low vapor pressure liquid chemicals to semiconductor process tools ;
At least three purge source inlet lines connecting at least three different purge sources to the manifold; and
One or more refillable canisters connected to the manifold
Including system.
Embodiment 80: The system of Embodiment 79, wherein the one or more refillable canisters include at least a first canister and a second canister.
Embodiment 81 The liquid chemical of low vapor pressure is supplied from the second canister to the semiconductor process tool and the chemical delivery system can replenish the second canister from the first canister. system.
Embodiment 82 The system of embodiment 80, wherein the chemical delivery system is capable of supplying liquid chemicals from both the first canister and the second canister to the semiconductor process tool.
Embodiment 83 The system of Embodiment 79, wherein the at least three different purge sources comprise at least a first vacuum source and a gas source.
Embodiment 84: The system of embodiment 83, wherein the at least three different purge sources further comprise a liquid source.
Embodiment 85 The system of embodiment 84, wherein the chemical delivery system comprises at least a first canister and a second canister.
Embodiment 86: The system of embodiment 85, wherein the low vapor pressure liquid chemical is supplied from the second canister to the semiconductor process tool and the chemical delivery system can replenish the second canister from the first canister. .
Embodiment 87 The system of embodiment 85, wherein the chemical delivery system is capable of supplying liquid chemicals from both the first canister and the second canister to the semiconductor process tool.
(Aspect 88) The system according to aspect 83, wherein the first vacuum source is a Venturi vacuum source.
(Aspect 89) The system according to aspect 83, wherein the first vacuum source is a hard vacuum source.
Embodiment 90: The system of embodiment 83, wherein the at least three different purge sources further comprise a second vacuum source, wherein the first and second vacuum sources are different types of vacuum sources.
(Aspect 91) A system according to aspect 90, wherein the chemical delivery system has at least a first canister and a second canister.
Aspect 92. The system of aspect 91, wherein the low vapor pressure liquid chemical is supplied from the second canister to the semiconductor process tool and the chemical delivery system can replenish the second canister from the first canister. .
Embodiment 93 The system of embodiment 91, wherein the chemical delivery system is capable of supplying liquid chemicals from both the first canister and the second canister to the semiconductor process tool.
Embodiment 94: The system of Embodiment 90, wherein the first vacuum source is a Venturi vacuum source.
Embodiment 95 The system according to Embodiment 90, wherein the second vacuum source is a hard vacuum source.
Embodiment 96 The system of embodiment 95, wherein the hard vacuum source is provided from a semiconductor process tool.
(Aspect 97) The system of aspect 79, further comprising a fourth purge source inlet line, the fourth purge source inlet line connecting the fourth purge source to the manifold.
(Aspect 98) The first purge source is a first vacuum source, the second purge source is an inert gas source, the third purge source is a liquid source, and the fourth purge source is a second source. 98. The system of aspect 97, wherein the system is a vacuum source and the first and second vacuum sources are different types of vacuum sources.
Embodiment 99 The system of embodiment 98, wherein the chemical delivery system comprises at least a first canister and a second canister.
Embodiment 100: The system of embodiment 99, wherein the low vapor pressure liquid chemical is supplied from the second canister to the semiconductor process tool and the chemical delivery system can replenish the second canister from the first canister. .
Embodiment 101 The system of embodiment 99, wherein the chemical delivery system is capable of supplying liquid chemicals from both the first canister and the second canister to the semiconductor process tool.
(Aspect 102) The system according to aspect 98, wherein the first vacuum source is a Venturi vacuum source and the second vacuum source is a hard vacuum source.
Aspect 103. The system of aspect 102, wherein the hard vacuum source is provided from a semiconductor process tool.
(Aspect 104) The system according to aspect 103, wherein the chemical delivery system has at least a first canister and a second canister.
Aspect 105. The system of aspect 104, wherein the low vapor pressure liquid chemical is supplied from the second canister to the semiconductor process tool and the chemical delivery system can replenish the second canister from the first canister. .
Embodiment 106: The system of Embodiment 104, wherein the chemical delivery system is capable of supplying liquid chemicals from both the first canister and the second canister to the semiconductor process tool.
(Aspect 107) A cabinet for housing a chemical delivery system comprising:
A plurality of cabinet walls forming an internal cabinet space, wherein at least one of the cabinet walls is a door;
At least one heater element disposed within or adjacent to the door; and
Air flow passage in close proximity to at least one heater element
Including cabinet.
(Aspect 108) The cabinet of aspect 107, further comprising at least one heat exchange element in the air flow passage, wherein the heat exchange element is thermally connected to the heater.
(Aspect 109) The cabinet according to aspect 108, wherein the heat exchange element is a plurality of fins.
(Aspect 110) The cabinet according to aspect 107, further comprising at least one air vent in the door, wherein the air vent allows air to flow through the air flow passage.
(Aspect 111) The cabinet according to aspect 107, wherein the heater element is provided in the recess of the door.
(Aspect 112) A cabinet according to aspect 111, wherein the heater element is a flat silicon heater.
(Aspect 113) The cabinet of aspect 107, wherein the air flow passage is formed along the back side of the door wall and the heater element is formed along the front side of the door wall.
(Aspect 114) The cabinet of aspect 113, wherein the door has a cavity and an interface structure within the cavity, and the interface structure forms at least a portion of a wall of the door.
(Aspect 115) The cabinet according to aspect 114, wherein the heater element is provided in a recess of the interface structure.
(Aspect 116) A cabinet according to aspect 113, further comprising a heat exchange element in the air passage.
(Aspect 117) The cabinet according to aspect 116, wherein the heat exchange element is a fin.
(Aspect 118) The cabinet according to aspect 113, wherein the heater is provided in the recess of the door.
(Aspect 119) The cabinet according to aspect 113, further including at least one air vent in the door, wherein the air vent allows air to flow through the air flow passage.
Embodiment 120 A temperature controlled cabinet for housing a liquid chemical delivery system comprising:
At least one door;
At least one heater element disposed in or on the door;
An air vent in the door; and
Air flow passage in close proximity to at least one heater element
A cabinet in which the air flow passage is in thermal communication with at least one heater element and the air vent provides an air inlet to the air flow passage.
(Aspect 121) The cabinet of aspect 120, further comprising a plurality of heat exchange fins in the air flow passage, wherein the heat exchange fins are thermally connected to at least one heater element.
(Aspect 122) The cabinet according to aspect 120, wherein at least one heater element is provided in the recess of the door.
(Aspect 123) The cabinet of aspect 120, further comprising a door wall, wherein the heater element is disposed on one side of the wall and the air flow passage is disposed on the other side of the wall.
Aspect 124. The cabinet of aspect 120, further comprising at least one heat transfer element having an air flow passage, wherein the heat transfer element is thermally connected to the heater element through the door wall.
Embodiment 125 A temperature controlled cabinet for housing a liquid chemical delivery system comprising:
Multiple cabinet walls; and
At least one heater element disposed in or on at least the first cabinet wall
Wherein the heater element is located outside the first cabinet wall and the thermal energy from the heater is connected to the interior of the cabinet through the first cabinet wall.
(Aspect 126) A cabinet according to aspect 125, wherein the first cabinet wall is at least part of a cabinet door.
(Aspect 127) The cabinet according to aspect 125, further including an air passage adjacent to the inside of the first cabinet wall.
(Aspect 128) The cabinet of aspect 127, further comprising at least one heat exchange structure in the air passage.
(Aspect 129) A cabinet according to aspect 128, wherein the first cabinet wall is at least part of a cabinet door.
(Aspect 130) A method for controlling the temperature of a cabinet containing a chemical delivery system comprising:
Providing a plurality of cabinet walls forming an internal cabinet space;
Disposing at least one heater element at least within the first cabinet wall or in close proximity thereto; and
Heat transfer from the heater to the internal cabinet space using the first cabinet wall as a heat transfer mechanism
Including methods.
(Aspect 131) A method according to aspect 130, wherein the first cabinet wall is a cabinet door.
(Aspect 132) A method according to aspect 131, further comprising flowing air across the inside of the cabinet door.
Aspect 133. The aspect 131, further comprising forming an air passage adjacent to the inside of the door, wherein the heat transfer element is in the air passage and the heat transfer element is thermally connected to the cabinet door. Method.
(Aspect 134) The method of aspect 130, further comprising flowing air across the inside of the first cabinet wall.
Aspect 135. The aspect 134, further comprising forming an air passage adjacent to the inside of the door, wherein the heat transfer element is in the air passage and the heat transfer element is thermally connected to the cabinet door. Method.
Aspect 136 A method for controlling the temperature of a cabinet containing a liquid chemical delivery system comprising:
Providing a plurality of cabinet walls forming an internal cabinet space;
Disposing at least one heater element outside at least a portion of the first cabinet wall;
Heat transfer from the heater to the inside of the first cabinet wall using the first cabinet wall as a heat transfer mechanism; and
Heating the internal cabinet space by flowing air across the inside of the first cabinet and circulating side air in the internal cabinet space
Including methods.
Embodiment 137 The method of embodiment 136, wherein the air flows through the air passage.
Aspect 138. A method according to aspect 137, further comprising forming a heat transfer element in the air passage.
(Aspect 139) A method according to aspect 136, wherein the first cabinet wall is a cabinet door.
Embodiment 140 The method of embodiment 139, wherein air flows at least partially through the door vent and into the cabinet.
(Aspect 141) A method according to aspect 139, wherein the heater element is provided in the recess of the door.
Embodiment 142 A chemical delivery system manifold useful for delivery of liquid chemicals from a canister comprising:
A vacuum supply valve connected to the vacuum generator;
Pressure vent valve connected to the vacuum generator;
Carrier gas shutoff valve connected to carrier gas source;
A process line shut-off valve connected to the bypass valve and the canister outlet line, the canister outlet line being connectable to the canister outlet valve;
A flush inlet valve connected between the carrier gas shutoff valve and the bypass valve, the flush inlet valve being connectable to a liquid flush source; and
Canister inlet line connectable between canister inlet valve and bypass valve
Including manifold.
Aspect 143 The manifold of aspect 142 further comprising a liquid waste valve connected between the pressure vent valve and the canister inlet line.
(Aspect 144) The manifold according to aspect 142, further comprising a control valve connected between the canister inlet line and the liquid waste valve.
(Aspect 145) The manifold according to aspect 142, further comprising a critical orifice connected between the canister inlet line and the bypass valve.
(Aspect 146) The manifold according to aspect 142, further comprising a control valve connected between the canister inlet line and the bypass valve.
Aspect 147. The manifold of aspect 146, further comprising a liquid waste valve connected between the pressure vent valve and the control valve.
Aspect 148. The manifold according to aspect 142, wherein the pressure vent valve is connected to the vacuum generator via at least one additional valve.
Embodiment 149 The manifold of embodiment 148, wherein the additional valve is connected to the liquid waste canister.
(Aspect 150) The manifold according to aspect 148, wherein the additional valve is connected to a hard vacuum source.
(Aspect 151) A chemical delivery system manifold useful for delivering liquid chemicals from canisters:
A first vacuum supply valve for connecting the manifold to a first vacuum source;
A second vacuum supply valve for connecting the manifold to a second vacuum source, wherein the first and second vacuum sources are different types of vacuum sources;
A pressure vent valve connected to either or both of the first and second vacuum sources;
Carrier gas shutoff valve connected to carrier gas source;
A process line shutoff valve connected to the bypass valve and the canister outlet line, the canister outlet line being connectable to the canister outlet valve; and
Canister inlet line connectable between canister inlet valve and bypass valve
Including manifold.
(Aspect 152) The manifold according to aspect 151, further comprising a flash inlet valve connected between the carrier gas shutoff valve and the bypass valve, wherein the flash inlet valve can be connected to a liquid flash source.
(Aspect 153) A manifold according to aspect 142, further comprising a critical orifice connected between the canister inlet line and the bypass valve.
(Aspect 154) The manifold according to aspect 142, further comprising a control valve connected between the canister inlet line and the bypass valve.
(Aspect 155) A flush inlet valve connected between the carrier gas shutoff valve and the bypass valve, the flush inlet valve being connectable with a liquid flush source; and
Liquid waste valve connected between pressure vent valve and control valve
The manifold of aspect 154, further comprising:
(Aspect 156) A chemical delivery system comprising:
(1) Vacuum supply valve;
(2) Vacuum generator;
(3) Carrier gas shutoff valve;
(4) Bypass valve;
(5) Process line shutoff valve;
(6) Liquid flush inlet valve;
(7) Low pressure vent valve;
(8) Canister inlet valve;
(9) Canister outlet valve
Including:
A vacuum supply valve is connected to the vacuum generator;
A carrier gas shutoff valve is connected to the liquid flush inlet valve;
A liquid flush inlet valve is connected to the bypass valve;
A bypass valve is further connected to the process line shutoff valve;
A low pressure vent valve is connected to the vacuum generator;
A process line shutoff valve is also connected to the canister outlet valve; and
A system in which a canister inlet valve is connected to a canister outlet valve.
Aspect 157. The system according to aspect 156, further comprising a control valve, wherein the control valve is disposed between the canister inlet valve and the bypass valve.
Embodiment 158. The system of embodiment 157, further comprising a liquid waste output valve disposed between the control valve and the low pressure vent valve.
Embodiment 159. The system of embodiment 156, wherein the low pressure vent valve is connected to the vacuum generator via at least one additional valve.
(Aspect 160) The system according to aspect 159, wherein the additional valve is connected to the liquid waste canister.
Embodiment 161 A method for purging a low vapor pressure liquid chemical from a chemical delivery system comprising:
A manifold,
A vacuum supply valve connected to a vacuum source,
Pressure vent valve connected to the vacuum supply valve,
Carrier gas shutoff valve connected to carrier gas source,
A process line shut-off valve connected to the bypass valve and the canister outlet line, wherein the canister outlet line can be connected to the canister outlet valve;
A flush inlet valve connected between the carrier gas isolation valve and the bypass valve, the flush inlet valve being connectable to a liquid flush source; and
Canister inlet line connectable between canister inlet valve and bypass valve
Supplying a manifold containing
Supplying low vapor pressure liquid chemicals to at least one line or valve of the chemical delivery system; and
Purging low vapor pressure liquid chemicals from at least one line or valve, the purge including the use of at least three different purge techniques;
Including methods.
Aspect 162. The method of aspect 161, wherein the manifold further comprises a liquid waste valve connected between the pressure vent valve and the canister inlet line.
Embodiment 163 The method of embodiment 161, wherein the at least three different purge techniques include at least a first evacuation step, a flowing purge step using an inert gas, and a liquid flush step.
Embodiment 164 The method of embodiment 163, wherein the first evacuation step uses a Venturi vacuum source.
(Aspect 165) A method according to aspect 163, wherein the first evacuation step uses a hard vacuum source.
Embodiment 166. The method of embodiment 163, wherein the at least three different purge techniques further comprise a second evacuation step, wherein the first and second evacuation steps use different types of vacuum sources.
Embodiment 167 A method of purging a low vapor pressure liquid chemical from a chemical delivery system comprising:
A manifold,
A vacuum supply valve connected to a vacuum source,
Pressure vent valve connected to the vacuum supply valve,
Carrier gas shutoff valve connected to carrier gas source,
A process line shut-off valve connected to the bypass valve and the canister outlet line, wherein the canister outlet line can be connected to the canister outlet valve;
A canister inlet line that can be connected between a canister inlet valve and a bypass valve;
Supplying a manifold containing
Supplying low vapor pressure liquid chemicals to at least one line or valve of the chemical delivery system; and
Purging low vapor pressure liquid chemicals from at least one line or valve, the purge including the use of at least three different purge techniques;
Including methods.
(Aspect 168) At least three different purging techniques include at least a first evacuation step, a second evacuation step, and a flowing purge step using an inert gas, wherein the first and second evacuation steps are of the type 166. The method of embodiment 161, using a different vacuum source.
Embodiment 169 The method of embodiment 163, wherein the first evacuation step uses a Venturi vacuum source.
(Aspect 170) A method according to aspect 163, wherein the second evacuation step uses a hard vacuum source.
Embodiment 171 The method of embodiment 163, wherein the at least three different purge techniques further comprise a liquid flush step.

FIG. 2 illustrates an exemplary chemical delivery system of the present invention. FIG. 2 illustrates an exemplary chemical delivery system of the present invention. FIG. 6 shows another purge configuration according to the present invention. FIG. 6 shows another purge configuration according to the present invention. FIG. 6 shows another purge configuration according to the present invention. FIG. 6 shows another purge configuration according to the present invention. FIG. 6 shows another purge configuration according to the present invention. FIG. 6 shows another purge configuration according to the present invention. FIG. 3 shows a manifold system using a medium level vacuum, a flowing purge and a liquid flush. FIG. 3 shows a manifold system using a medium level vacuum, a flowing purge and a liquid flush. FIG. 3 shows a manifold system using a medium level vacuum, a flowing purge and a liquid flush. FIG. 3 shows a manifold system using a medium level vacuum, a flowing purge and a liquid flush. FIG. 3 shows a manifold system using a medium level vacuum, a flowing purge and a liquid flush. FIG. 3 shows a manifold system using a medium level vacuum, a flowing purge and a liquid flush. FIG. 3 shows a manifold system using a medium level vacuum, a flowing purge and a liquid flush. FIG. 3 shows a manifold system using a medium level vacuum, a flowing purge and a liquid flush. FIG. 3 shows a manifold system using a medium level vacuum, a flowing purge and a liquid flush. FIG. 3 shows a manifold system using a medium level vacuum, a flowing purge and a liquid flush. FIG. 3 shows a manifold system using a medium level vacuum, a flowing purge and a liquid flush. FIG. 3 shows a manifold system using a medium level vacuum, a flowing purge and a liquid flush. FIG. 3 shows a manifold system using a medium level vacuum, a flowing purge and a liquid flush. FIG. 3 shows a manifold system using a medium level vacuum, a flowing purge and a liquid flush. FIG. 3 shows a manifold system using a medium level vacuum, a flowing purge and a liquid flush. FIG. 3 shows a manifold system using a medium level vacuum, a flowing purge and a liquid flush. FIG. 3 shows a manifold system using a medium level vacuum, a flowing purge and a liquid flush. FIG. 3 shows a manifold system using a medium level vacuum, a flowing purge and a liquid flush. FIG. 2 illustrates a dual tank chemical delivery system with a medium level vacuum, a flowing purge and a flush liquid purge. FIG. 2 illustrates a dual tank chemical delivery system with a medium level vacuum, a flowing purge and a flush liquid purge. FIG. 2 illustrates a dual tank chemical delivery system with a medium level vacuum, a flowing purge and a flush liquid purge. FIG. 2 illustrates a dual tank chemical delivery system with a medium level vacuum, a flowing purge and a flush liquid purge. FIG. 2 illustrates a dual tank chemical delivery system with a medium level vacuum, a flowing purge and a flush liquid purge. FIG. 2 illustrates a dual tank chemical delivery system with a medium level vacuum, a flowing purge and a flush liquid purge. FIG. 2 illustrates a dual tank chemical delivery system with a medium level vacuum, a flowing purge and a flush liquid purge. FIG. 2 illustrates a dual tank chemical delivery system with a medium level vacuum, a flowing purge and a flush liquid purge. FIG. 2 illustrates a dual tank chemical delivery system with a medium level vacuum, a flowing purge and a flush liquid purge. FIG. 2 illustrates a dual tank chemical delivery system with a medium level vacuum, a flowing purge and a flush liquid purge. FIG. 2 illustrates a dual tank chemical delivery system with a medium level vacuum, a flowing purge and a flush liquid purge. FIG. 2 illustrates a dual tank chemical delivery system with a medium level vacuum, a flowing purge and a flush liquid purge. FIG. 2 illustrates a dual tank chemical delivery system with a medium level vacuum, a flowing purge and a flush liquid purge. FIG. 2 shows a dual tank refillable chemical delivery system with a medium level vacuum, a flowing purge and a hard vacuum. FIG. 2 shows a dual tank refillable chemical delivery system with a medium level vacuum, a flowing purge and a hard vacuum. FIG. 2 shows a dual tank refillable chemical delivery system with a medium level vacuum, a flowing purge and a hard vacuum. FIG. 2 shows a dual tank refillable chemical delivery system with a medium level vacuum, a flowing purge and a hard vacuum. FIG. 2 shows a dual tank refillable chemical delivery system with a medium level vacuum, a flowing purge and a hard vacuum. FIG. 2 shows a dual tank refillable chemical delivery system with a medium level vacuum, a flowing purge and a hard vacuum. FIG. 2 shows a dual tank refillable chemical delivery system with a medium level vacuum, a flowing purge and a hard vacuum. FIG. 2 shows a dual tank refillable chemical delivery system with a medium level vacuum, a flowing purge and a hard vacuum. FIG. 2 shows a dual tank refillable chemical delivery system with a medium level vacuum, a flowing purge and a hard vacuum. FIG. 2 shows a dual tank refillable chemical delivery system with a medium level vacuum, a flowing purge and a hard vacuum. FIG. 2 shows a dual tank refillable chemical delivery system with a medium level vacuum, a flowing purge and a hard vacuum. FIG. 2 shows a dual tank refillable chemical delivery system with a medium level vacuum, a flowing purge and a hard vacuum. FIG. 2 shows a dual tank refillable chemical delivery system with a medium level vacuum, a flowing purge and a hard vacuum. FIG. 2 shows a dual tank refillable chemical delivery system with a medium level vacuum, a flowing purge and a hard vacuum. FIG. 2 illustrates a dual tank chemical delivery system with a medium level vacuum, a flowing purge, a flush liquid purge and a hard vacuum. FIG. 2 illustrates a dual tank chemical delivery system with a medium level vacuum, a flowing purge, a flush liquid purge and a hard vacuum. FIG. 2 illustrates a dual tank chemical delivery system with a medium level vacuum, a flowing purge, a flush liquid purge and a hard vacuum. FIG. 2 illustrates a dual tank chemical delivery system with a medium level vacuum, a flowing purge, a flush liquid purge and a hard vacuum. FIG. 2 illustrates a dual tank chemical delivery system with a medium level vacuum, a flowing purge, a flush liquid purge and a hard vacuum. FIG. 2 illustrates a dual tank chemical delivery system with a medium level vacuum, a flowing purge, a flush liquid purge and a hard vacuum. FIG. 2 illustrates a dual tank chemical delivery system with a medium level vacuum, a flowing purge, a flush liquid purge and a hard vacuum. FIG. 2 illustrates a dual tank chemical delivery system with a medium level vacuum, a flowing purge, a flush liquid purge and a hard vacuum. FIG. 2 illustrates a dual tank chemical delivery system with a medium level vacuum, a flowing purge, a flush liquid purge and a hard vacuum. FIG. 2 illustrates a dual tank chemical delivery system with a medium level vacuum, a flowing purge, a flush liquid purge and a hard vacuum. FIG. 2 illustrates a dual tank chemical delivery system with a medium level vacuum, a flowing purge, a flush liquid purge and a hard vacuum. FIG. 2 illustrates a dual tank chemical delivery system with a medium level vacuum, a flowing purge, a flush liquid purge and a hard vacuum. FIG. 2 illustrates a dual tank chemical delivery system with a medium level vacuum, a flowing purge, a flush liquid purge and a hard vacuum. It is a figure which shows the cabinet for chemical substance delivery systems. FIG. 2 shows a door used with a chemical delivery system cabinet. FIG. 2 shows a door used with a chemical delivery system cabinet.

  The above and other problems are addressed by using a chemical delivery system that uses multiple technology to obtain an appropriate chemical purge of the chemical delivery system. The purge sequence acts to purge the chemical delivery system manifold and canister connection lines prior to removal of an empty chemical supply canister or after installation of a new canister.

  The types of chemicals that can be utilized in the present invention can vary widely depending on the type of process tool and the desired outcome. The techniques of the present invention are particularly advantageous when used with liquid chemical delivery systems that supply liquids for use in CVD systems such as those used in semiconductor manufacturing, for example. Examples of representative chemicals include TDEAT, tetraethylorthosilicate (“TEOS”), triethyl phosphate, trimethyl phosphite, trimethyl borate, titanium tetrachloride, and tantalum compounds (eg, TaEth); chlorinated hydrocarbons, ketones ( Solvents such as acetone and methyl ethyl ketone), esters (eg ethyl acetate), hydrocarbons, glycols, ethers, hexamethyldisilazane ("HMDS"); solids dispersed in liquids such as barium / strontium / titanate cocktails (mixtures) Examples include, but are not limited to, compounds. These examples of chemicals are not intended to be limiting in any way. Chemicals can have various purities and mixtures of chemicals can be used. In one embodiment, a single chemical is used. Certain chemicals advantageously have a purity of 99.999% or higher relative to trace metals (or trace metals). In one aspect of the invention, the canister 104 is at least partially filled with a chemical having a purity of at least 99.9999999999% based on the amount of trace metals in the chemical. The chemicals and delivery systems disclosed herein can be used in combination with any of a wide range of process tools such as, for example, LPCVD, PECVD, APCVD, MOCVD, and the like tools.

  More particularly, according to the present invention, the purge technique uses various combinations of some or all of the following purge techniques: first vacuum source, flowing purge (ie, process chemicals from the manifold line). A flow of inert gas to flash), a second vacuum source, and / or a liquid flash system. The first and second vacuum sources can generally be different vacuum sources having different vacuum levels. In one example, the first vacuum source can be at a degree of vacuum typically in the range of 100T or less, more typically in the range of 50-100T, such vacuum source being a “medium level vacuum”. vacuum) ”. Further, in such examples, the second vacuum source may be a degree of vacuum typically less than or equal to 100 mT, more typically in the range of 100 mT to 1 mT, such a vacuum source being a “hard vacuum ( hard vacuum, or high vacuum). However, it will be appreciated that the levels described herein are exemplary and other higher or lower vacuum levels may be utilized for the first and second vacuum sources. In one embodiment, the first (or medium level) vacuum source may be a Venturi vacuum source. By using multiple purge techniques, chemicals that are difficult to purge, such as TaEth, TDEAT, BST, can be efficiently purged from the chemical delivery system.

  FIG. 1A shows a chemical delivery system 100 configured using a combined purge technique. The chemical delivery system 100 shown in FIG. 1A shows a single tank (or single tank) chemical delivery system for illustrative purposes to illustrate the principles of the present invention. The system can be used in a number of different configurations, such as a dual tank or non-refillable system (two chemical canisters, one canister with the other canister). One that cannot be refilled), a dual tank refillable system (two chemical canisters, one canister can be refilled from the other canister), one of many process canisters Any bulk delivery system that utilizes a large bulk canister (within or away from the chemical delivery system) to replenish one, such as a system with three or more canisters It may be a thing. For illustration, FIG. 1B shows a chemical delivery system 100 using two chemical canisters.

  As illustrated in FIGS. 1A and 1B, the chemical delivery system 100 includes a manifold system 102. The manifold system includes chemical delivery system valves and lines. Although illustrated as a single block, the manifold system may be comprised of multiple manifold systems (or sub-manifold systems). Thus, it will be understood that the term manifold can refer to all valves and lines of the delivery system, and can also be used to refer to some parts of the valves and lines. The manifold may be in the form of a single chemical delivery system cabinet or may be distributed to multiple cabinets and located outside the cabinet. The system 100 includes a canister 104 (or canisters 104A and 104B shown in FIG. 1B) and a chemical outlet line 110 (also referred to as a process line) to supply chemicals to a process tool, such as a chemical vapor deposition tool. Can be included. Although one outlet line 110 is illustrated, the line 110 is comprised of two or more branch lines and associated branch interrupt and purge lines associated therewith or associated or connected. Can be done. The system 100 may also include a canister inlet 108 and outlet 106 (or inlets 108A and 108B and outlets 106A and 106B shown in FIG. 1B). Connected to the manifold system 102 are four inlet lines used for the purge operation, with a medium level vacuum line 112, a purge gas inlet 111, a hard vacuum line 114, and a liquid flush line 116. is there. A waste output line 118 is also provided. The waste output (or discharge) is connected to a waste output container (located inside or away from the delivery system) or connected to a dedicated waste line at the user's facility The The mid-level vacuum line 112 can be connected to a mid-level vacuum source, such as, for example, a Venturi vacuum generator. The purge gas inlet 111 may be connected to an inert gas line, such as a helium, nitrogen, or argon line, to form a flowing purge through the manifold. The hard vacuum line 114 can be connected to a hard vacuum source such as a stand alone vacuum pump. However, in a preferred embodiment, the hard vacuum source can be a process tool vacuum, described in more detail below. The liquid flush line 116 may be a source of flush (or flush) liquid such as, for example, a solvent such as tetrahydrofuran (THF) or triglyme. The given solvent used will vary depending on availability, cost, and the type of material being purged from the line. In general, solvents can be used to properly disperse solid chemicals (so that the chemical does not coagulate in the presence of the solvent), solubilize thick materials, and dilute chemicals with high vapor pressures. Adapted to allow. For example, when purging solid active chemicals dispersed in triglyme, triglyme is first used to wash the line and then treated with THF to remove traces of triglyme, if necessary. Alternatively, THF can be used alone if the environment allows. In another example, TaEth is washed away with ethanol or hexene. Another example may include using n-butyl acetate to wash away BST contained in the butyl acetate solution. The liquid flash line 116 may be connected to a dedicated flash liquid canister or else to a liquid supply line at the user's facility. Medium level vacuum line 112, purge gas line 111, hard vacuum line 114, and liquid flash line 116 provide purge from manifold system 102 where it is difficult to purge chemicals such as TaEth, TDEAT, BST, etc. Each can be used to assist. The present invention can also be used while using fewer than all four inlet lines. Thus, fewer than four inlet line combinations may be used, as shown in the exemplary embodiment shown in FIGS. 2A, 2B and 2C.

  By using multiple purge techniques (medium level vacuum, flowing purge, hard vacuum, or liquid flush) in combination, the advantages of each technique can be effectively utilized while minimizing the disadvantages of a particular technique. A hard vacuum is advantageous in that a lower pressure is obtained. However, free-standing hard vacuum sources are generally more expensive, require more maintenance, are larger, require more equipment, and produce more waste compared to venturi vacuum sources. However, the use of a venturi mid-level vacuum system eliminates the need for a free-standing hard vacuum source. Rather, a hard vacuum source typically present in a process tool can be utilized. The hard vacuum source of the process tool can be used to lower the pressure in the manifold system 102 by itself or following the use of a venturi vacuum. The hard vacuum from the process tool is then switched on to further reduce the pressure level in the manifold. By first using a medium level vacuum to lower the pressure, the load on the hard vacuum is reduced. By reducing the load on the hard vacuum, the hard vacuum source inherent in the process tool can be utilized without compromising the quality of any process performed in the process tool. Thus, the use of a Venturi vacuum makes it possible to use a readily available hard vacuum source without the additional costs associated with a free-standing hard vacuum source or a dedicated hard vacuum source.

  Similarly, flushing the manifold with liquid (or flushing) in combination with one or more vacuum sources is an advantageous purge technique. If the chemical being delivered is a solid suspended in an organic liquid, the manifold can liquid flush all lines to prevent the solid from accumulating in the line due to evaporation of the organic liquid. Can be configured as follows. When a dispersion is used, it is preferable to flush the line with a liquid solvent such as, for example, triglyme or tetrahydrofuran (THF) so that the compound does not precipitate in the line even when the line is depressurized. For example, a liquid flush prior to a vacuum purge (or vacuum purge) to remove solid residues (this occurs when vacuuming a manifold containing some solid-containing chemicals such as BST). Can be used. In addition, liquid flushes have the advantage of helping to remove very low vapor pressure chemicals from long and / or narrow tubes (even in situations where even a hard vacuum cannot adequately purge the manifold).

  When using a liquid flush, various methods of injecting and removing liquid from the manifold may be utilized. 3A, 3B and 3C show three examples of injecting and removing liquid from the manifold, other techniques may be used. Further, for purposes of illustration, FIGS. 3A, 3B and 3C illustrate a purge technique combined with a dual tank system having both a medium level vacuum inlet 112, a purge gas inlet 111 and a hard vacuum inlet 114. Show. The illustrated purge technique may be utilized with other system / canister configurations (or arrangements) described herein. As shown in FIG. 3A, a flash liquid inlet 116 may be provided. In some configurations, the flash liquid may be supplied from a dedicated chemical supply line 121 of the user's standard equipment line. Liquid waste generated by the liquid flush operation can be supplied to the waste container 120. Another configuration of the system of FIG. 3A may be a system without flash liquid inlet 116 and waste container 120. Such a system uses three purge techniques: a medium level vacuum purge, a hard vacuum purge, and a flowing gas purge. As shown in FIG. 3B, a combination of flash liquid source and waste container 122 may be used. In this configuration, liquid for flushing the manifold 102 is supplied from the container 122 through lines 123A and 123B and returned to the container 122 as waste. FIG. 3C shows yet another configuration in which a dedicated liquid source container 124 supplies flush liquid using lines 125A and 125B, and a dedicated liquid waste container collects liquid waste through lines 118A and 118B. Show. As will be described in more detail below, the waste container not only needs to recover the flush liquid, but also the process liquid drained (or drained) from at least a portion of the manifold line as part of the purge process Can also be recovered. The canisters 124, 122, and 120 (or other parts of the chemical delivery system) can be integrally placed inside one chemical delivery system housing or placed outside the chemical delivery system It will be appreciated that, in terms of functionality, and functionality, the system described herein operates equally well regardless of canister placement.

  For some embodiments of the invention described herein, the exact configuration of the manifold 102 is as long as it provides the capability to supply a stream of chemicals to the process tool and allow proper purging. It is not important in the practice of the present invention. The configuration of the valves in the manifold 102 can be modified so that individual lines can be purged and maintained separately.

  It will be appreciated that many manifold and canister configurations can be utilized in accordance with the present invention, including but not limited to the exemplary embodiments described in more detail below. For example, U.S. Pat. Nos. 5,465,766, 5,562,132, 5,590,695, 5,607,002 and 5,711,354 (these are the same) Additional manifold configurations such as those described in (incorporated herein by reference) may also be utilized with appropriate modifications to accommodate flow purge, liquid flush and / or hard vacuum.

  The manifold used in the present invention may advantageously be configured so that dead legs that are not purged are not present in the manifold, lines and fittings. In this regard, this configuration advantageously minimizes venting in tube crossing lines and bent (or flexible) lines by utilizing short straight tubes where possible. obtain. Furthermore, this configuration may advantageously utilize an SVCR joint (straight VCR joint). Generally, the pressure in the system is adjusted so that the pressure is higher on the upstream side than on the downstream side. A wide variety of valves may be used in the manifold, including but not limited to manually operated (or manually operated) valves, air operated valves, or other types of valves. The manifold valve can be controlled using process control equipment. The controller may manage the purge sequence and normal run mode (or operating mode). During the run mode, the system supplies chemicals to the process tool, which can be initiated after installation of the bulk chemical supply.

  Typically, process chemicals are removed or purged from the entire manifold system, after which the canisters are changed out (alternatively) or alternate flowing gas purges, vacuum (or evacuation) cycles, and / or Or it is stopped by a liquid purge. A brief overview of a typical cycle is first provided by the following more detailed example. When initiating a purge cycle, the chemical canister is typically first pressurized. The vacuum line is then dried down using a cycle purge. The cycle purge used here is a flowing gas purge followed by a vacuuming step. The cycle purge can be repeated any number of times until the desired drying or chemical removal is obtained. The vacuum line drying process removes moisture from the vacuum line resulting from the reaction with chemicals in the line between the canister outlet and the process line output 110. The vacuum can be a medium level vacuum with a venturi generator and / or a hard vacuum with a vacuum pump. After the line is dried, it comes into contact with (or is exposed to) process chemicals, drains the manifold line containing it and returns it to the canister (to canister output).

  After line drain, the general purge sequence can vary depending on whether a liquid flush or a hard vacuum is used. For example, if a liquid flush is used (without a hard vacuum), the manifold line in contact with the process chemistry is flushed (or flushed) with a liquid solvent. These lines are then subjected to a cycle purge of a medium level vacuum followed by an inert gas flowing purge to remove any residual solvent vapor. Thereafter, the canister is removed or replaced. During the canister replacement, the flowing purge may continue to prevent ambient air from entering the manifold and contaminating. After the new canister is attached to the manifold, a final cycle purge of the evacuation step and subsequent flowing gas purge may be performed to remove any traces of air from the new canister fitting.

  When using a hard vacuum with a liquid flush, a typical purge sequence after line drain is as follows. After line drain, the manifold line in contact with the process chemical is subjected to a medium level vacuum. These lines are then subjected to a hard vacuum. A medium level vacuum is initially used to minimize the load on the hard vacuum, as described above. Thereafter, a flowing purge may be initiated before and during canister replacement. After canister replacement, a cycle purge is initiated, after which the hard vacuum is finally pumped down (released).

  Examples of typical manifold structures are illustrated in FIGS. 4A-4I, but the invention is not limited thereto. 4A-4I illustrate one embodiment of a manifold system having a combined purge technique. For illustrative purposes, FIGS. 4A-4I illustrate the use of medium level vacuum, flowing purge, and liquid flush as multiple purge techniques. In addition, a single canister system is also shown for illustrative purposes, but the invention described herein is not limited to these particular embodiments. For each valve in the drawing, a white triangle indicates a line that is always open, and a black triangle indicates that the valve is closed until it is open.

  In FIG. 4A, a vacuum source 14, such as, for example, a Venturi vacuum generator, can be connected through line 12 to a vacuum supply valve (“VGS”) 10. VGS 10 functions to control the flow (or flow) of gas (eg, nitrogen, helium, or argon) through inert gas line 11 to vacuum source 14 when the vacuum source is a Venturi vacuum generator. To do. The vacuum source 14 may be attached to an exhaust line 13 that goes out to an exhaust pipe (exhaust or exhaust port). The vacuum source 14 may be connected to a low pressure vent valve (“LPV”) 60. In FIG. 4A, the vacuum source 14 is connected to the LPV 60 through lines 15 and 16. The check valve (or check valve) 33A in line 37 is closed as long as the manifold does not exceed a predetermined opening pressure. Line 37 is exhausted to the exhaust pipe of the cabinet. In general, the check valve 33A may be set to operate when the manifold pressure exceeds a preset level, for example, about 75 pounds per square inch. The check valve is connected to a carrier gas isolation valve (“CGI”) 30. CGI 30 may also be referred to as a carrier gas inlet valve. The check valve acts to evacuate the gas when the system pressure reaches a selected level. Line 31 may connect CGI 30 to regulator 32 that may supply a flow of pressurized inert gas. A delivery pressure gauge 36 is attached to the regulator 32 to monitor the regulator pressure and pressure during the entire operation.

  In FIG. 4A, a flush line inlet valve (“FLI”) 45 may be connected to CGI 30 through line 33. The FLI 45 is connected to the flash liquid inlet 116. Line 34 may connect FLI 45 to canister bypass valve (“CBV”) 40. Lines 41 and 42 may connect the CBV 40 to a process line isolation valve (“PLI”) 50 and a control valve (“CP2”) 70, respectively. PLI 50 is connected to process line output 110. The function of the PLI 50 is to control the flow of chemicals exiting the manifold. The CGI 30 functions to control the supply of pressurized gas (pressurized gas) to the manifold. The function of the CBV 40 controls the application of pressure or vacuum to the PLI 50 as well as to the line 71. Line 110 carries the chemical to either a process tool external to the delivery system or to another canister to be refilled in the dual tank refill system. The canister outlet line 52 functions to connect the PLI 50 to a canister outlet valve (“CO”) 92. Line 62 may connect CP2 70 to a liquid waste output valve (“LWO”) 61. LWO 61 is connected to a waste output line 118. LWO 61 is also connected to LPV 60 through line 63. The canister inlet line 71 may be routed from the control valve 70 to a canister inlet valve (“CI”) 90. The CI 90 functions to control canister pressurization and evacuation. The line 73 can connect the CO 92 and the CI 90. The CO 92 functions to control the flow of chemical from the canister 110 during chemical delivery, as well as the purge of the canister outlet junction during canister replacement. CI 90 and CO 92 function to connect the manifold to the corresponding structure of chemical canister 104, typically by joints such as male and female threaded joints. The coupling (coupler) connecting the manifold to the canister 104 is typically present in lines 71 and 52. CO 92 is a dual activator valve (dual activator valve or dual activator valve or double valve), and line 73 connects the dual actuated valve directly to CI 90. Alternatively, if the CO 92 is not a dual actuated valve, an additional valve is installed at the CO 92 and an additional line is installed from the additional valve to connect the additional valve to the line 71.

  The above-mentioned lines, also called conduits, tubes, pipes, and paths (or passages) etc., are composed of various types of materials such as 316L stainless steel tubes, Teflon® tubes, alloy steels such as Hastelloy. Each valve may be a conventional pneumatically actuated valve, such as, for example, a NUPRO 6L-M2D-111-P-III gas control valve. Similarly, the regulator can be of a standard type, such as an AP Tech 1806S 3PW F4-F4 V3 regulator. The system can be assembled by conventional methods, such as the use of pressure fitting valves or welding. The valves can be controlled using conventional process controls, such as an Omron programmable controller box connected to a touch screen control panel. Alternatively, the valve can be controlled using an ADCS APC ™ controller incorporating an embedded microprocessor for command sequence execution, along with software residing in the EPROM. The control unit may control the flow of pressurized gas, for example, to open or close the pneumatic valve.

  In use, the manifold of the present invention can be operated as follows. Valves in the manifold are properly opened and closed to allow pressurized gas to enter the system and to the canister in order to drive chemicals out of the canister 104 and into the delivery point. In FIG. 4B, dotted line 220 illustrates the path (or passage) of pressurized gas entering canister 104, and dotted line 221 is the liquid exiting canister 104 through dip tube 91. Indicates the route of chemical substances. Accordingly, pressurized gas from a source (or source) (not shown) is released (or opened) to line 31 by regulator 32. The gas then passes through the open CGI 30 and then enters the canister 104 through line 33, FLI 45, CBV 40, line 42, open CP2 70, line 71, and CI 90. Due to the pressure of the incoming gas, the liquid chemical rises up the dip tube and is routed through the CO 92, line 52, PLI 50 and outlet line 110 to the receiving location (eg, CVD process tool).

  If the supply canister is replaced (even a full canister), the line can be purged to remove residual chemicals from the manifold. The first process for removing residual chemicals from the manifold is a cycle purge process that includes a vacuum process and a flowing purge process. The cycle purge may include performing alternating evacuation and flowing purge. One evacuation process is described below with reference to FIG. 4C, and one flowing-purge process is described below with reference to FIG. 4D. The evacuation process can be implemented in a variety of ways, including through the configuration shown by dotted line 250 in FIG. 4C. Thus, in one embodiment, when gas enters the vacuum source 14 through lines 11 and 12 by opening the VGS 10, a vacuum is drawn down to the exhaust pipe through the line 13, thus the line. LPV 60 and CP2 70 are opened so that a vacuum is pulled on 15, 16, 63, 62, 42, 34, 33, 71, and 73.

  FIG. 4D illustrates the vacuum line dry down cycle purge flowing purge. In FIG. 4D, the pressurized gas is put into the line 31 by the regulator 32. When CGI 30, CP2 70 and LPV 60 are opened, the gases are shown in lines 31, 33, 34, 42, 71, 73, 62, 63, 16, 15, and 13 as shown by dotted line 260 in FIG. 4D. Flow through and thus purge the manifold. One advantage of this process is that it removes moisture and oxygen from lines such as lines 13, 15, and 16.

  Next, in order to remove the head pressure in the canister 104, a depressurization process is performed. For example, FIG. 4E shows a procedure that can cause decompression. In one depressurization method, gas is passed from line 11 through line 12 by opening VGS 10 so that a vacuum is created by the flow through line 13 to the exhaust pipe as shown by dotted line 230. Into the vacuum source 14. The vacuum generated at source 14 draws vacuum through line 15, line 16, open LPV 60, line 63, LWO 61, line 62, CP2 70, line 71, and open CI 90, As a result, the head space of the canister 104 is evacuated.

  After depressurization, a liquid drain is instituted to purify the liquid line (junction). Therefore, in FIG. 4F, gas is introduced into the line 31 through the regulator 32. CGI 30, CBV 40, and CO 92 are opened so that the liquid chemical is returned to canister 104 so that gas flows through lines 31, 33, 34, 41, and 52. The gas flow between line drains is indicated by dotted line 240. The depressurization and subsequent liquid drain sequence shown in FIGS. 4E and 4F can be performed iteratively to remove any liquid from the valves, tubes, and fittings.

  After the liquid drain, a flush liquid purge is performed. As shown in FIG. 4G, flash liquid is introduced from the flash liquid inlet 116. By opening portions of FLI 45, CBV 40, and CO 92, the flush liquid purges the entire wet surface area at the outlet of the manifold. Thus, the flush liquid flows through lines 34, 41, 52, 73, 71, and 62 as shown by dotted line 270. In addition, LWO 61 is opened and flush liquid exits manifold 102 through waste outlet 118. The combined line drain of the flash line is then opened with the CGI 30 open and purge gas line 34 using a configuration similar to that shown in FIG. 4G except that the FLI 45 is closed. , 41, 52, 73, 71, and 62, and can be carried out by repeating the cycle.

  After the flush line liquid purge and line drain, a canister removal cycle purge is performed, which includes a evacuation step and a flowing purge step, respectively. This cycle purge removes any residual solvent vapor remaining after the flush liquid purge step. The evacuation process is indicated by a dotted line 280 in FIG. 4H. Thus, in one embodiment, when gas enters the vacuum source 14 through lines 11 and 12 by opening VGS 10, a vacuum is drawn through line 13 to the exhaust pipe, thus lines 15, 16, LPV60, a part of CO92, and CBV40 are opened so that a vacuum is drawn in 63, 62, 71, 73, 52, 41, 34, and 33.

  In FIG. 4I, a flowing purge is performed as part of a canister removal cycle purge. In FIG. 4I, the pressurized gas is put into the line 31 by the regulator 32. By opening the CGI 30, CBV 40, a part of the CO 92, and the LPV 60, the gas flows into the lines 31, 33, 34, 41, 52, 73, 71, 62, 63 as shown by the dotted line 290 in FIG. 4I. , 16, 15 and 13 thus purging the manifold.

  After purging, the fitting is typically removed while maintaining a positive pressure on the manifold to keep moisture out of the manifold. For example, after removing the fitting, CGI 30, CBV 40, CO 92, CI 90, and CP2 70 are opened so that gas exits lines 52 and 71. After installing a new canister, a canister removal cycle purge as shown in FIGS. 4H and 4I may cause any water, trace air, or other impurities that may have entered the manifold, as well as new canister fittings and joints. It is typically repeated to remove any water, air, or impurities present in the.

  The embodiment of the present invention described with reference to FIGS. 4A-4I reduces the number of valves compared to a standard manifold (which can lower the cost of the manifold and reduce the number of locations where leakage can occur. As well as reducing the chance of valve failure in certain manifolds). This embodiment also reduces the number of dead legs in the system, thereby providing a more efficient flowing purge. With the increased ability to remove chemicals from the line during canister replacement, the manifold of this embodiment provides a system that can be used with harmful chemicals such as arsenic compounds. Similarly, the manifold of this embodiment can improve the use of dispersions, such as metals or solid compounds dispersed in organic carrier liquids such as diglyme and triglyme. When using a dispersion, it is preferable to flush the line with a liquid solvent such as, for example, triglyme or tetrahydrofuran (THF) so that the compound does not precipitate in the line when the line is decompressed. Furthermore, it is contemplated that for any embodiment of the present invention, the manifold can be heated to promote the evaporation of chemicals in the line. In this regard, the manifold is maintained in a heated environment and can be covered by a heating tape connected to a variac or the like. Alternatively, a heating element can be placed on the cabinet door as shown below with reference to FIGS. 10A and 10B. To facilitate evaporation during the flow purge, a heated gas such as heated argon, nitrogen, or other inert gas can be used instead. A combination of these techniques can also be used. For some types of chemicals, they can be purged with reactive chemicals that react with one or more compounds in the line to yield compounds that are more easily removed.

  The manifold of the present invention may include a sensor attached to line 15, for example, to determine whether the line of the manifold contains chemicals. Similarly, a sample port (or port) can be provided in line 15 and a sample of gas from the line can be withdrawn and examined using an analytical device to determine the presence (or presence) of a chemical.

  Another embodiment of the present invention, similar to the embodiment of FIGS. The embodiment of FIG. 4J is similar to the embodiment of FIG. 4A except that CP2 70 of FIG. 4A is removed. More specifically, as shown in FIG. 4J, CP2 is not used to connect lines 62, 71, and 42, but instead a tee fitting is used to connect lines 62, 71, and 42. Or a T-joint) 44 and a critical orifice 43. The critical orifice 43 functions as a flow restriction (restrictor) device to restrict (without impeding) gas flow from the line 42 to the tee fitting 44. The critical orifice 43 can be configured in a wide variety of ways. For example, the orifice 43 may be formed with a region having a narrowed inner diameter as compared to the inner diameter of other pipes, such as the line 42 and / or the tee joint 44. For this reason, a narrow area diverts the gas flow. For example, when the CBV 40 is opened, the gas flowing from the line 34 to the CBV 40 preferentially passes the CBV 40 in a larger amount than the flow through the line 42 and the orifice 43 due to the throttling action of the orifice 43. Exit and flow through line 41. As shown below, the use of the orifice 43 allows the formation of a gas flow pattern similar to that shown in FIGS. 4B-4I while using one fewer valve.

  In one embodiment, orifice 43 may be formed by using a VCR joint that connects line 42 and tee joint 44. The VCR joint may have a gasket inside the joint that has a narrower opening than the inner diameter of the line 42 and tee joint 44. For example, the line 42 may be composed of a 1/4 inch pipe having an inner diameter of 0.18 inches, whereas the orifice may have an opening diameter of 1/32 inch or 1/16 inch. Such a diameter ratio will restrict (or limit) the flow through the orifice as compared to other parts of the manifold system. As will be shown below, the gas flow through the orifice is used during the process of pressurizing the canister, for example, when the chemical exits the canister and is pushed to the delivery location of the chemical. Thus, the proper dimensions of the orifice may depend on the dimensions of the canister used with the manifold system and / or the desired chemical flow rate. In use, the manifold of the present invention can be operated as follows. Valves in the manifold are appropriately opened and closed to allow pressurized gas to enter the system and to the canister to force chemicals out of the canister 104 and into the delivery site. In FIG. 4B, dotted line 220 illustrates the path of pressurized gas entering canister 104, and dotted line 221 illustrates the path of liquid chemical that exits canister 104 through dip tube 91. Accordingly, pressurized gas from a source (not shown) is released to line 31 by regulator 32. The gas then passes through the open CGI 30 and then enters the canister 104 through line 33, FLI 45, CBV 40, line 42, open CP2 70, line 71, and CI 90. Due to the pressure of the incoming gas, the liquid chemical rises up the dip tube and is routed through the CO 92, line 52, PLI 50 and outlet line 110 to the receiving location (eg, CVD process tool).

  In use, the manifold of FIGS. 4J-4R can be operated as follows. Valves in the manifold are appropriately opened and closed to allow pressurized gas to enter the system and to the canister to force chemicals out of the canister 104 and into the delivery site. In FIG. 4K, dotted line 320 illustrates the path of pressurized gas entering canister 104 and dotted line 321 illustrates the path of liquid chemical that exits canister 104 through dip tube 91. Accordingly, pressurized gas from a source (not shown) is released to line 31 by regulator 32. The gas then passes through the open CGI 30 and then enters the canister 104 through line 33, FLI 45, CBV 40, line 42, orifice 43, tee fitting 44, line 71, and CI 90. Due to the pressure of the incoming gas, the liquid chemical rises up the dip tube and is routed through the CO 92, line 52, PLI 50 and outlet line 110 to the receiving location (eg, CVD process tool).

  If the supply canister is replaced (even a full canister), the line can be purged to remove residual chemicals from the manifold. The first process for removing residual chemicals from the manifold is a cycle purge process that includes a vacuuming process and a flowing purge process. The cycle purge may include performing alternating evacuation and flowing purge. One evacuation step will be described below with reference to FIG. 4L, and one flowing / purge step will be described below with reference to FIG. 4M. The evacuation process can be performed in a variety of ways, including through the arrangement shown by dotted line 350 in FIG. 4L. Thus, in one embodiment, when gas enters the vacuum source 14 through lines 11 and 12 by opening VGS 10, a vacuum is drawn through line 13 to the exhaust pipe, thus lines 15, 16, LPV 60 is opened so that a vacuum is drawn on 63, 62, 42, 34, 33, 71, and 73.

  In FIG. 4M, the flowing purge of the vacuum line drying cycle purge is illustrated. In FIG. 4M, the pressurized gas is put into the line 31 by the regulator 32. When CGI 30 and LPV 60 are opened, gas passes through lines 31, 33, 34, 42, 71, 73, 62, 63, 16, 15, and 13 as shown by dotted line 360 in FIG. 4M. Flow and thus purge the manifold.

  Next, in order to remove the head pressure in the canister 104, a pressure reducing process is performed. For example, FIG. 4N shows a procedure that can cause decompression. In one depressurization method, gas is passed from line 11 through line 12 by opening VGS 10 so that a vacuum is created by the flow through line 13 to the exhaust pipe as shown by dotted line 330. Into the vacuum source 14. The vacuum generated at the source 14 passes through the line 15, the line 16, the open LPV 60, the line 63, the LWO 61, the line 62, the tee joint 44, the orifice 43, the line 42, the line 34, the line 33, The line 71 and the open CI 90 are evacuated, thereby evacuating the canister 104 headspace.

  After depressurization, liquid draining is performed to purify the liquid line (joint). Therefore, in FIG. 4O, gas is introduced into the line 31 through the regulator 32. CGI 30, so that liquid chemicals are returned to canister 104 so that gas flows through lines 31, 33, 34, 41, 52, line 42, orifice 43, tee fitting 44, line 71, and line 73. CBV40 and CO92 are opened. Gas flow between line drains is indicated by dotted line 340.

  After the liquid drain, a flush liquid purge is performed. As shown in FIG. 4P, flash liquid is introduced from the flash liquid inlet 116. By opening portions of FLI 45, CBV 40, and CO 92, the flush liquid purges the entire wet surface area at the outlet of the manifold. Thus, the flush liquid flows through lines 34, 41, 52, 73, 71, 42, and 62 as indicated by dotted line 370. In addition, LWO 61 is opened and flush liquid exits manifold 102 through waste outlet 118.

  After the liquid purge, a canister removal cycle purge including an evacuation step and a flowing purge step is performed. This cycle purge removes any residual solvent vapor remaining after the flush liquid purge step. The evacuation process is indicated by a dotted line 380 in FIG. 4Q. Thus, in one embodiment, when gas enters the vacuum source 14 through lines 11 and 12 by opening VGS 10, a vacuum is drawn through line 13 to the exhaust pipe, thus lines 15, 16, The LPV 60, a part of the CO 92, and the CBV 40 are opened so that a vacuum is drawn on the 63, 62, 71, 73, 52, 41, 42, 34, and 33.

  In FIG. 4R, a flowing purge is performed as part of the canister removal cycle purge. In FIG. 4R, the pressurized gas is put into the line 31 by the regulator 32. By opening the CGI 30, CBV 40, part of the CO 92, and the LPV 60, the gas flows into the lines 31, 33, 34, 41, 42, 52, 73, 71, 62 as shown by the dotted line 390 in FIG. 4R. , 63, 16, 15 and 13 thus purging the manifold.

  5-7 illustrate various additional configurations that form a chemical delivery system that employs a combined purge technique. The techniques of FIGS. 5-7 may be used with manifold valve configurations (or arrangements) such as FIGS. 4A or 4J. 5A-5M illustrate a dual tank non-refillable delivery system using a medium level vacuum, a flowing purge, and a liquid flush purge. Such a configuration can be used for a wide variety of chemicals described herein. For example, in one embodiment, the configuration of FIGS. 5A-5M can be utilized in a liquid BST delivery system.

  An exemplary purge sequence for the system of FIG. 5A is shown in FIGS. Similar to FIGS. 4B-4I, dotted lines are used in FIGS. 5-7 to indicate vacuum, gas, or liquid flow. Similarly, for the valves common to FIGS. 5-7 such as FLI, VGS, LPV, CGI, CBV, PLI, CP2, CO, CI and LWO valves (if used), the same terms as FIGS. 4A-4I are used. It shall be attached. In addition, when additional canisters are used in a dual canister system, numbers 1 and 2 are added to the end of the valve reference terms to indicate parts of the manifold connected to the first and second canisters, respectively. It shall be. Thus, for example, as shown in FIG. 5A, two CO valves, CO1 and CO2, are provided connected to the first and second chemical canisters, respectively, and so on for the other valves. As shown in FIG. 5A, the chemical delivery system 500 may include a first chemical source canister 502 and a second chemical source canister 504. A liquid flash source 506 (eg, a canister containing a solvent) and a liquid flash waste container 508 (eg, a canister) are also provided. Associated with (or connected to) the first source canister 502 are valves FLI1, CGI1, CBV1, CP2-1, CI1, CO1, LWO1, LPV1, and PLI1, which are referred to FIG. 4A. Connected as described. Additional valves SPV1 and SVS1 are also associated with the source canister 502 as shown in FIG. 5A. A similar set of valves FLI2, CGI2, CBV2, CP2-2, CI2, CO2, LWO2, LPV2, PLI2, SPV2, and SVS2 are associated with the second source canister 504. The valves associated with each canister 502 and 504 may be included in two or more separate manifolds of the chemical delivery system 500, or may be included in a single (or single) manifold.

  Also, as shown in FIG. 5A, a liquid flash source 506 can be connected to valves SC1-SC6, and a liquid flash waste canister 508 can be connected to valves SW1-SW8. The chemical delivery system includes a regulator (REG) 512, a flow restrictor (or flow restrictor or flow restrictor) 510, a pressure transducer 514, and over pressure (as shown). An over-pressure check valve 516 may further be included.

  The operation of the chemical delivery system can be understood with reference to FIGS. FIG. 5B illustrates the chemical delivery run mode of the chemical delivery system 500. As shown in FIG. 5B, dotted line 522 indicates the flow of gas (eg, He gas) from gas source 518 to each canister 502 and 504. The gas is used to flush chemicals from canisters 502 and 504 to outlet 1 and outlet 2, respectively, as shown by dotted line 524.

  After stopping the run mode of FIG. 5B, a purge of the sequence of FIGS. 5C-5M may be performed. As shown, the purge sequence is illustrated with reference to the lines and valves associated with the first chemical source canister 502, but a similar sequence is used for the second chemical source canister. It will be understood that this can be done. After the run mode, a cycle purge process consisting of a venturi vacuum drying process and a flowing purge process may be performed. The Venturi vacuum drying process is indicated by the dotted line 530 in FIG. 5C and the flowing purge process is indicated by the dotted line 535 in FIG. 5D. The cycle purge can be performed repeatedly. Thereafter, by using a Venturi vacuum, canister decompression can be performed as shown by the dotted line 540 in FIG. 5E. Thereafter, an outlet line line drain may be performed as shown by the dotted line 545 in FIG. 5F. During line drain, a portion of the system can be maintained under vacuum, as shown by dotted line 547. Next, another canister decompression step may be performed as indicated by the dotted line 550 in FIG. 5G.

  Solvent flush is achieved by injecting gas from gas inlet 518 (as shown by dotted line 553) to drive solvent from liquid flush canister 506 to liquid waste container 508 as shown by dotted line 555 in FIG. 5H. Can be achieved. In this way, the source chemical remaining in the valves and lines of the chemical delivery system can be flushed (or washed away) with the solvent liquid. During this process, a portion of the system can be maintained under vacuum, as shown by dotted line 547. After the solvent flush, a liquid drain process may be performed to drain any solvent liquid remaining in the line to the liquid waste container, as shown by dotted line 560 in FIG. 5I. Also during this step, a portion of the system can be maintained under vacuum, as shown by dotted line 547. Thereafter, the liquid waste container 508 can be depressurized as indicated by the dotted line 565 in FIG. 5J. The liquid flush process of FIGS. 5H, 5I, and 5J can then be repeated to obtain a sufficient purge of source chemicals from the system valves and lines.

  After the liquid flush process, the system replaces the canister (the first source in the present embodiment described herein by a cycle purge consisting of a vacuuming process and a flowing purge process as shown in FIGS. 5K and 5L. The canister 502) can be prepared. As shown in FIG. 5K, dotted line 570 illustrates the evacuation process, and as illustrated in FIG. 5L, dotted line 575 illustrates the flowing purge process. A two-step (or two-stage) cycle purge process can be performed repeatedly. During the canister exchange, the canister is removed, but positive pressure and gas flow can be maintained in the lines connected to the canister inlet and outlet as shown by the dotted line 580 in FIG. 5M. After reconnecting another canister, a further cycle purge consisting of the evacuation step of FIG. 5K and the subsequent flow step of FIG. 5L can then be performed repeatedly.

  The embodiment described above with reference to FIGS. 5A-5M is a non-replenishable system (ie, no refill between the first chemical source canister 502 and the second chemical source canister 504). However, a refillable system can be configured similarly to the chemical delivery system 500 by adding a refill line between the outlet 1 and the inlet to the second canister 504. In this way, the techniques described herein can be utilized in a refillable dual canister system.

  Another embodiment of the present invention is shown in FIGS. The embodiment of FIGS. 6A-6N is a dual tank non-refillable chemical delivery system 600. The chemical delivery system 600 is configured to switch either one of the chemical source canisters 602 or 604 by a system that switches from one canister to the next when the chemical level in one canister goes low. Can be used so that one chemical can be fed from. The embodiment of FIGS. 6A-6N can be used to deliver liquid chemicals such as TDEAT or TaEth, for example. As shown in FIGS. 6A-6N, this embodiment includes the use of a combined purge technique. This technique includes a medium level vacuum (eg, a Venturi vacuum source), a flowing purge, a flush liquid purge, and / or a hard vacuum. A liquid flash source 606, such as a canister containing a solvent, is provided as shown. The liquid flash waste can be disposed in an empty chemical source canister 602 or 604 (ie, the canister being replaced). Alternatively, a dedicated liquid flash waste canister as shown in FIG. 5A can be used. Alternatively, the liquid waste can be flushed to a hard vacuum. As described in more detail below, a flush liquid purge may optionally be used to assist in draining the process line to the process line drain reservoir 608.

  Associated with the first source canister 602 are valves FLI1, CGI1, CBV1, CP2-1, CI1, CO1, LPV1, LWO1, SVS1, and PLI1, which were described with reference to FIG. 5A. Connected like the ones. A similar set of valves FLI 2, CGI 2, CBV 2, CP 2-2, CI 2, CO 2, LPV 2, PLI 2, LWO 2, and SVS 2 are associated with the second source canister 604. The valves associated with each canister 602 and 604 can be included in two or more separate manifolds of the chemical delivery system 600, or can be included in a single manifold.

  Also as shown in FIG. 6A, a liquid flash source 606 may be connected to valves SC1-SC5. The chemical delivery system may further include a regulator (REG) 612, a pressure transducer 614, an inert gas source 618 (eg, helium, etc.) and an over pressure check valve 616, as shown. A degas module 624 can be used to remove gas (eg, helium, etc.) from the liquid supplied to the process tool. Various parts of the chemical delivery system 600 can be connected to a hard vacuum, as indicated by the hard vacuum connection 620. An outlet is also provided for supplying liquid chemicals to the process tool. The flash line 622 between the valve SC1 and the valve 626 is not shown in its entirety to simplify the drawing, but the flash line 622 is one continuous connected line.

  The operation of the chemical delivery system can be understood with reference to FIGS. 6B-6N, which are the first when the second chemical source canister 604 is idle (idle or unused). FIG. 6 illustrates the steps performed when a chemical is supplied from a chemical source canister 602 and when the first chemical source canister 602 is replaced. FIG. 6B illustrates a chemical delivery run mode of the chemical delivery system 600. As shown in FIG. 6B, dotted line 628 shows the flow of gas (eg, He gas) from gas source 618 to canister 602. The gas is used to flush chemicals from the canister 602 to the outlet-1 and outlet-2 outlets, as shown by the dotted line 629. By using two or more outlets, chemicals can be supplied from a single chemical canister to two or more process tools. Thus, the chemical outlet is configured as a multi-branch outlet configuration. Furthermore, the chemical supply to outlet-1 and outlet-2 can be individually controlled by valves CC-1 and CC-2, respectively. Thus, chemicals can be fed from both outlets simultaneously, or only from outlet-1 or only from outlet-2. Valves O-1 and O-2 can be manual valves that are left open during normal operation.

  After stopping the run mode of FIG. 6B, a purge of the sequence of FIGS. 6C-6N may be performed. While purging the lines and valves associated with one canister, the other canister can be operated in run mode. As shown, the purge sequence is illustrated with reference to the lines and valves associated with the first chemical source canister 602, but a similar sequence is used for the second chemical source canister. It will be understood that this can be done. After stopping the run mode of the first chemical source canister 602, a cycle purge process comprising a venturi vacuum drying process and a flowing purge process may be performed. The Venturi vacuum drying process is indicated by the dotted line 630 in FIG. 6C, and the flowing purge process is indicated by the dotted line 635 in FIG. 6D. The cycle purge can be performed repeatedly. Thereafter, by using a Venturi vacuum, canister decompression can be performed as shown by the dotted line 640 in FIG. 6E. Thereafter, line drain of the exit line can be performed as shown by dotted line 645 in FIG. 6F. During line drain, a portion of the system can be maintained under vacuum, as shown by dotted line 647. Next, another canister decompression step may be performed as shown by the dotted line 650 in FIG. 6G.

  Solvent flush by injecting gas from gas inlet 618 (as indicated by dotted line 653) to drive solvent from liquid flash canister 606 to chemical source container 602 as indicated by dotted line 655 in FIG. 6H. Can be achieved. In this way, the source chemical remaining in the valves and lines of the chemical delivery system can be flushed with the solvent liquid. During this process, a portion of the system can be maintained under vacuum, as shown by dotted line 647. After the solvent flush, a liquid drain process may be performed to drain any solvent liquid remaining in the line to the liquid waste container, as shown by dotted line 660 in FIG. 6I. Also during this step, a portion of the system can be maintained under vacuum, as shown by dotted line 647. The steps of FIGS. 6G, 6H, and 6I can then be performed repeatedly to obtain a sufficient purge of source chemicals from the system valves and lines.

  Alternatively, rather than the steps of FIGS. 6H and 6I, the liquid waste can be flushed to a hard vacuum source. Therefore, the process of FIG. 6J can be used in place of the process of FIG. 6H. As indicated by the dotted line 656 in FIG. 6J, the solvent from the liquid flash canister 606 may be flushed to the hard vacuum connection 620 (rather than the chemical source canister as shown in FIG. 6H). After the solvent flush of FIG. 6J, a liquid drain process may be performed to drain any solvent liquid remaining in the line to the liquid waste container, as shown by the dotted line 661 in FIG. 6K. Also during this step, a portion of the system can be maintained under vacuum, as shown by dotted line 647. Thereafter, the steps of FIGS. 6G, 6K, and 6J may be repeated to obtain a sufficient purge of source chemicals from the valves and lines of the system.

  After the liquid flush process, the system replaces the canister (the first source in the present embodiment described herein by cycle purge consisting of a vacuuming process and a flowing purge process as shown in FIGS. 6L and 6M. The canister 602) can be prepared. As shown in FIG. 6L, dotted line 570 illustrates the evacuation process, and as illustrated in FIG. 6M, dotted line 575 illustrates the flowing purge process. A two-step cycle purge process can be performed repeatedly. During the canister exchange, the canister is removed, but positive pressure and gas flow can be maintained in the lines connected to the canister inlet and outlet as shown by dotted line 580 in FIG. 6N. After reconnecting another canister, a further cycle purge consisting of the evacuation step of FIG. 6L and the subsequent flow step of FIG. 6M can then be performed repeatedly.

  Flush line 622 can be used to provide a liquid flush for use in flushing the process lines connected between the outlets (outlet-1 and outlet-2) and the process tool. Accordingly, liquid solvent can be supplied from the liquid flash canister 606 through the valve 626 to the flash line 622, thereby allowing the other line in contact (or exposed) to the chemical supplied from the source chemical canister. To flush, the process line can be flushed with a liquid solvent, similar to the technique described above. Waste from the process line drain can be supplied to the process line drain reservoir 608. The reservoir 608 may or may not be stored in a cabinet that houses the chemical delivery system. In another embodiment, reservoir 608 may not be used, but liquid waste may be supplied to the hard vacuum connection in a manner similar to that described with reference to FIGS. 6J and 6K. Accordingly, liquid waste can be processed through a hard vacuum connection 620 disposed proximate to the valve 626. In either case, combined purge techniques, including evacuation, inert gas flow, and liquid flush techniques, can be used to purge the process line and associated valves.

  The process of draining and flushing the process line may be understood in more detail with reference to FIG. 6A. The draining and flushing process is described herein with reference to outlet-1 (thus, in this example, valve O-1 is opened), but between outlet-2 and the process tool. It will be appreciated that a similar process can be used to drain the process lines. Furthermore, the draining and flushing process described herein with reference to outlet-1 can be performed when supplying chemicals through outlet-2, and vice versa. Thus, one branch of the outlet can be purged when the other branch is still operating to supply chemicals to the process tool.

  To initialize the process line drain and flush, the process line drain reservoir 608 can be depressurized using the hard vacuum connection 620 and by opening the PV-ISO and CI-DR. . Thereafter, the process line drain reservoir outlet line can be opened by opening the CO-DR and MDV valves. Next, when valve MP-1 is opened, the line to the process tool is placed under vacuum and the liquid is drained to the reservoir. After the process line has been placed under vacuum, the next step is to pass the valve of outlet-1, CC-1, MP-1, MDV from the process tool and through the valve CO-DR to the process line drain. Flowing an inert gas (supplied by the process tool) into the reservoir. This flowing purge step pushes any fluid in the process line into the reservoir 608. A combined cycle of evacuation and inert gas extrusion processes can be performed.

  Next, the valve MP-1 is closed, and another canister is decompressed by opening the valves PV-ISO and CI-DR. After decompression, the valves PV-ISO and CI-DR can be closed. The valve P-ISO, PCR, MDV and CO-DR are then opened to drain any liquid in the line between valves MP-2 and MP-1 using an inert gas source. Can be swept into the reservoir

  The hard vacuum and subsequent liquid flush can then be performed repeatedly. First, the process line can be placed under a hard vacuum by opening valves PV-ISO, FP3-DR, MDV, and MP-1. After stopping the hard vacuum, the process line can be subjected to a liquid flush by opening valves PSV, PCR, and MP-1. This allows flush liquid to be pushed up to the process tool. The PSV valve can then be closed and the liquid in the process line can be drained to the drain reservoir 608 by opening the MDV and CO-DR valves. These hard vacuum and liquid flush steps can then be repeated (eg, 3-5 cycles).

  Thus, valves and lines associated with multi-branch outlets and reservoirs (valves O-1, O-2, CC-1, CC-2, MP-1, MP-2, PCR, MDV, HE-DR, P- ISO, PSV, PV-ISO and associated lines, which may be collectively referred to as distribution or outlet manifolds, may be purged using a combined purge technique. Thus, the use of the combined purge technique described with reference to the purge valve associated with the chemical supply canister is also beneficial for use to purge other valves of the chemical delivery system. It will be understood. When used with a valve associated with a supply canister, the combined purge technique may provide the advantage of limiting possible contamination during canister replacement, canister refill, and the like. When used with a valve associated with a multi-branch outlet (distribution manifold), the combined purge technique is used when the process line is removed from the line and / or during start-up (or start-up) of the use of the process line. Can provide the advantage of limiting possible contamination. Furthermore, a combined purge technique can be used for one branch of the outlet (eg outlet-1) and vice versa when the other branch (eg outlet-2) is still supplying chemicals. It is. Thus, using a combined purge technique that limits contamination is useful for canister manifolds (valves associated with a given canister) and distribution manifolds. Although described herein as separate manifolds, it is understood that the canister manifold and distribution manifold may be considered as a sub-part of a larger manifold that includes some or all of the valves of FIG. 6A. Let's be done.

  Yet another further embodiment of the present invention is shown in FIGS. The embodiment of FIGS. 7A-7M is a dual tank refill chemical delivery system 700. The embodiment of FIGS. 7A-7M can be used to deliver a liquid chemical such as, for example, TDEAT. As shown in FIGS. 7A-7M, this embodiment includes the use of a combined purge technique. This technique includes medium level vacuum, flowing purge, and hard vacuum. As will be described in more detail below, a liquid flush may optionally be used with this embodiment to assist in process line drainage. The optional liquid flash is a very low vapor pressure chemistry, such as TDEAT, when only medium level vacuum, flowing purge and hard vacuum can be used due to the long process line length and its dimensions. It can be advantageous when proper purging of such process lines for materials can be prevented. If the process line purge is inadequate, a flush liquid purge completes the purge process.

  The chemical delivery system 700 of FIG. 7A can be used to deliver a single chemical from a process canister 704 (eg, a 4 liter canister) to a process tool. The process canister 704 can be replenished from a bulk canister 702 (eg, a 5 gallon canister). The system is configured such that the bulk canister 702 can be removed and replaced when the bulk canister chemical level goes low. The system also includes a process line drain reservoir 708, a liquid flush inlet 705 (which can be connected to a user equipment solvent line, or a canister containing a solvent similar to that described above), and a hard vacuum. A hard vacuum connection 720 connected to a source (eg, a process tool hard vacuum) is also included. Associated with the bulk canister 702 are the valves CGI-L, CBV-L, CP2-L, CI-L, CO-L, LPV-L, and PLI-L, associated with the process canister 704. Included are valves CGI-R, CBV-R, CP2-R, CI-R, CO-R, LPV-R, and PLI-R (as used in FIGS. 7A-7M, “− L "indicates a valve associated with the bulk canister, and" -R "indicates a valve associated with the process canister). Valve HVI is connected to a hard vacuum 720 as shown, and valve VGI is connected to a VGS valve. The various valves can be included in two or more separate manifolds of chemical delivery system 700 or can be included in a single manifold. The chemical delivery system may further include a regulator (REG) 712, a pressure transducer 714, an inert gas source 718 (eg, helium) and an over pressure check valve 716, as shown. A degassing module 724 may be used to remove gas (eg, helium, etc.) from the liquid supplied to the process tool. Various parts of the chemical delivery system 700 may be connected to a hard vacuum, as indicated by the hard vacuum connection 720. Outlet 1 and outlet 2 supply liquid chemicals to the process tool in a multi-branch outlet configuration similar to that described above with reference to FIG. 6B.

  The replenishment process is illustrated in FIG. 7B. As illustrated in FIG. 7B, the gas flow indicated by dotted line 730 forces chemicals from bulk canister 702 to process canister 704 as indicated by dotted line 732. FIG. 7C illustrates a chemical delivery run mode of the chemical delivery system 700. As shown in FIG. 7C, dotted line 728 shows the flow of gas (eg, He gas) from gas source 718 to canister 704. The gas is used to flush chemicals from canister 704 to outlet-1 and outlet-2, as shown by dotted line 729.

  If replacement of the bulk canister 702 is desired, a purge of the sequence of FIGS. 7D-7M can be performed. The purge technique of FIGS. 7D-7M may be performed when the system is delivering chemicals from the process canister 704 to the process tool, as shown by dotted lines 728 and 729 in FIG. 7C. Thus, although not shown in FIGS. 7D-7M, gas and chemical flows shown by dotted lines 728 and 729 in FIG. 7C may exist at each step of the drawings. If purging is desired, a cycle purge process consisting of a Venturi vacuum drying process and a flowing purge process can be performed. The Venturi vacuum drying process is indicated by the dotted line 731 in FIG. 7D, and the flowing purge process is indicated by the dotted line 735 in FIG. 7E. The cycle purge can be performed repeatedly. Thereafter, by using a Venturi vacuum, canister decompression can be performed as shown by the dotted line 740 in FIG. 7F. Thereafter, a drain line on the exit line can be performed as shown by the dotted line 745 in FIG. 7G. During line drain, a portion of the system can be maintained under vacuum, as shown by dotted line 747. Next, another canister decompression step may be performed as indicated by the dotted line 750 in FIG. 7H.

  The system can then be prepared for a hard vacuum purge by first performing a venturi evacuation, as shown by dotted line 755 in FIG. 7I. A hard vacuum purge may then be performed as indicated by the dotted line 760 in FIG. 7J. After subjecting the system to a hard vacuum, positive pressure and gas flow can be maintained in lines connected to the canister inlet and outlet, as shown by the dotted line 780 in FIG. 7K, and the canister 702 is removed from the system. After reconnecting another canister 702, a Venturi evacuation step indicated by dotted line 782 in FIG. 7L may be followed by a pressurization step indicated by dotted line 784 in FIG. 7M. Thereafter, the evacuation and pressurization steps of FIGS. 7L and 7M can be performed repeatedly in a cycle that ends with a venturi evacuation step as shown in FIG. 7L. Eventually, a hard evacuation step indicated by dotted line 760 in FIG. 7J may be performed. At this point, the system is prepared to use the new bulk canister 702.

  Similar to that described above for system 600, flush inlet 705 is provided in system 700 of FIG. 7A to allow process line liquid purge. Waste from the process line liquid purge may be collected in the process line drain reservoir using techniques such as those described herein. The process line drain reservoir 708 may or may not be located in the same cabinet as the rest of the system 700. Further, similar to system 600, the outlet-1 drain and flush process may be performed while supplying chemicals through outlet-2, and vice versa. Thus, one branch of the outlet can be purged when the other branch is still operating to supply chemicals to the process tool. Further, similar to that described above with reference to FIG. 6A, the outlet purge provides the advantages of the combined technology purge of the present invention (eg, including vacuum purge, flowing gas purge, and liquid flush purge). can get.

  The cabinet containing the chemical delivery system of the present invention can be configured in a wide variety of ways. Exemplary cabinet configurations are shown in U.S. Pat. No. 5,711,354 and pending application number 09 / 141,865 filed Aug. 28, 1998, the disclosures of which are incorporated by reference Is expressly incorporated herein by reference. FIG. 8 shows a schematic chemical delivery system cabinet 1000. As shown in FIG. 8, the cabinet includes a plurality of cabinet walls. The walls can include sides, top and bottom that define the interior cabinet space. In one embodiment, the cabinet may be configured to be suitable for use in a hazardous explosive environment. Schematically, this is achieved by isolating all electronic components in an area covered with an inert gas. According to this method, the sparks emitted from the electronic components will be present in an essentially oxygen-free environment, thus significantly reducing the risk of explosion due to steam that may be present in the cabinet.

  Since some of the chemicals described above crystallize at or near room temperature, it is desirable to provide temperature control of the environment inside the cabinet 1000. Thus, for example, the desired cabinet temperature can be maintained at an internal temperature of about 30 degrees Celsius for TaEth. In addition, heating the cabinet may facilitate the evaporation of chemicals from the manifold line, thus improving the chemical purge in the manifold.

  In one embodiment, the cabinet may be heated by attaching a heating element to at least one door of the cabinet. A suitable door for use with a heating element is shown in FIGS. 9A and 9B. As shown in FIG. 9A, the door 1003 may include an air vent (or exhaust) 1004 and a heater interface (or heater connection) 1006. In general, by exhausting the exhaust line out of the cabinet for safety considerations, the positive flow of air entering the cabinet through a vent, such as the air vent 1004, for example (apart from using the heater). ) Maintained.

  As shown in more detail in FIG. 9B, the heater interface 1006 can be a concave (or recessed) cavity (or cavity) with a back wall 1008 provided in the recess of the door 1003. Within the heater interface 1006, a flat heater element (such as an 8 × 18 inch flat electrical silicon heater) may be attached to the heater interface rear wall 1008. The heater interface 1006 may be formed as an aluminum insert (or insert) placed in the door cavity. Heat is transferred from the heater interface to the inside of the cabinet, whether aluminum or any other material that can transfer heat. Arranging the heater elements in this manner allows easy access to the heater from the front of the cabinet and assists in isolating the heater from any explosive gases in the cabinet. Although not shown, a cover may be placed over the heater interface 1006 to protect the heater elements and the end user (or end user).

  Heat transfer from the heater element to the cabinet is also assisted by using an air vent 1004, fins 1010, and an air flow structure 1012 that serves to collect the air flow above the fins 1010 in one place. . Accordingly, the structure 1012 and the heater serve to form a restricted (or restricted) passage of air flow. Aluminum fins 1010 attached to the heater interface rear wall 1008 function to increase the metal surface area to improve heat transfer. Air flow structure 1012 provides a passage for air flowing into air vent 1004 through rear wall 1008 and fins 1010 (as indicated by air flow arrow 1014). Thereafter, warm air may enter the cabinet as indicated by air flow arrow 1014. According to this method, by using a heater element connected to the front door of the cabinet, the cabinet can be heated in an efficient and cost effective manner. Although the heater interface of FIGS. 9A and 9B is shown as a cavity provided in a recess in the door 1003, the heater interface may be configured in other manners. For example, the rear wall of the heater interface may be located on the outer panel of the door, so that the heater interface and heater element may protrude outside the door. Similarly, the rear wall of the heater interface may be located at the door opening so that the rear wall is flush with the door. In addition, the heater elements can be connected in a similar manner to other cabinet walls such as side, rear, top or bottom. Thus, heat can be conducted through the wall from elements external to the cabinet wall to the cabinet.

  Further modifications and alternative embodiments of the present invention will be apparent to those skilled in the art in view of the description herein. Accordingly, the description herein is to be construed as illustrative only and is for the purpose of teaching those skilled in the art the manner of carrying out the invention. It should be understood that the form of the invention shown and described herein is to be treated as the presently preferred embodiment. It will be apparent to those skilled in the art after having the advantages of this description of the invention that the elements shown and described herein may be replaced by equivalent elements, and certain features of the invention may be considered other It may be used independently of using features.

Claims (28)

(A) Vacuum supply valve connected to vacuum source, (b) Pressure vent valve connected to vacuum supply valve, (c) Carrier gas shutoff valve connected to carrier gas source, (d) Bypass A process line shutoff valve connected to the valve and canister outlet line, wherein the canister outlet line can be connected to the canister outlet valve; and (e) a canister inlet valve and a bypass valve Supplying low vapor pressure liquid chemical to at least one line or valve of the chemical delivery system including a manifold with a canister inlet line that can be connected therebetween, and low vapor pressure from the at least one line or valve Of the liquid chemical substance, and the purge is less Including at least the use of three different purge techniques.   The method of claim 1, wherein the manifold includes a flash inlet valve connected between a carrier gas isolation valve and a bypass valve, the flash inlet valve being connectable to a liquid flash source. The at least three different purge techniques include the following:
(I) flowing gas through at least one line or valve to push low vapor pressure liquid chemicals from the at least one line or valve to the source canister; (ii) at least one liquid solvent; Performing a liquid flush comprising flowing through a line or valve; (iii) applying a vacuum to the at least one line or valve; and (iv) flowing an inert gas through the at least one line or valve. The method of claim 1 or 2, comprising at least three of performing a flowing gas purge. The at least three different purge techniques are:
(I) flowing a gas through the at least one line or valve to push the low vapor pressure liquid chemical from the at least one line or valve to the source canister;
(Ii) after flowing the gas, performing a liquid flush comprising flowing a liquid solvent through at least one line or valve; and (iii) after performing the liquid flush, (a) vacuum Applying at least one line or valve, and (b) performing at least one of a flowing gas purge comprising flowing an inert gas through the at least one line or valve The method according to claim 1, comprising:   5. The method of claim 4, wherein after performing the liquid flush, the method includes applying a vacuum to at least one line or valve.   5. The method of claim 4, wherein after performing the liquid flush, the method includes performing a flowing gas purge that includes flowing an inert gas through at least one line or valve.   The method of claim 4, wherein the flowing gas purge is performed after applying a vacuum to at least one line or valve.   8. The method of claim 6 or 7, further comprising applying a vacuum to at least one line or valve after performing the flowing gas purge.   9. The method of any of claims 4-8, wherein performing the liquid flush comprises flowing liquid waste generated by the liquid flush into a waste container.   A low vapor pressure liquid chemical is supplied from the source canister to the chemical delivery system, and the source canister and the waste output container are located within a single chemical delivery system housing. Item 10. The method according to Item 9.   9. The method of any of claims 4-8, wherein performing the liquid flush comprises flowing liquid waste produced by the liquid flush into a low vapor pressure chemical supply canister.   12. A method according to any of claims 4 to 11, further comprising applying a vacuum to at least one line or valve prior to flowing the gas.   13. A method according to any of claims 4 to 12, further comprising applying a vacuum to at least one line or valve prior to performing the liquid flush.   14. A method according to any of claims 4 to 13, wherein applying a vacuum to at least one line or valve uses a Venturi vacuum source.   14. A method according to any of claims 4 to 13, wherein applying a vacuum to at least one line or valve uses a hard vacuum source.   14. A method according to any of claims 4 to 13, wherein applying a vacuum to the valves and lines includes using a Venturi vacuum source followed by a hard vacuum source. A chemical delivery system for low vapor pressure liquid chemicals:
A vacuum supply valve connected to a vacuum source;
Pressure vent valve connected to vacuum supply valve;
Carrier gas shutoff valve connected to carrier gas source;
A process line shut-off valve connected to the bypass valve and the canister outlet line, wherein the canister outlet line can be connected to the canister outlet valve; and between the canister inlet valve and the bypass valve A system that includes a manifold that includes canister inlet lines that can be connected.   The system of claim 17, further comprising a flush inlet valve connected between the carrier gas shutoff valve and the bypass valve, the flush inlet valve being connectable to a liquid flush source.   19. The system of claim 17 or 18, further comprising a source canister for the low vapor pressure liquid chemical configured to supply the low vapor pressure liquid chemical to the manifold.   20. The liquid of claim 17-19, wherein the liquid solvent is configured to flow liquid directly from a liquid flash source through at least a portion of the chemical delivery system and then to a waste output container. A system according to any of the above.   A low vapor pressure liquid chemical is supplied from the source canister to the chemical delivery system, and the source canister and the waste output container are located within a single chemical delivery system housing. Item 21. The system according to item 20.   The gas is configured to flow through at least a portion of the chemical delivery system to extrude a low vapor pressure liquid chemical from at least a portion of the chemical delivery system to the source canister. 19. The system according to 19.   The system of claim 19, wherein the system is configured for direct liquid disposal from a liquid flash source through at least a portion of the chemical delivery system and then directly to the source canister.   24. A system according to any of claims 17 to 23, wherein the vacuum source comprises a Venturi vacuum source.   24. A system according to any of claims 17 to 23, wherein the vacuum source comprises a hard vacuum source.   26. A system according to any of claims 17 to 25, operatively connected to deliver a low vapor pressure liquid chemical to a semiconductor process tool. A method of purging low vapor pressure chemicals from a chemical delivery system having a plurality of valves and lines and having a source canister for low vapor pressure liquid chemicals:
(I) flowing gas through the valve and line to push low vapor pressure liquid chemicals from the valve and line to the source canister;
(Ii) performing a liquid flush comprising flowing a liquid solvent through the valve and line after flowing the gas; and (iii) after performing the liquid flush, (a) applying a vacuum to the valve and Applying to the line; and (b) performing at least one of a flowing gas purge including flowing an inert gas through the valve and the line.   A chemical delivery system comprising a source canister for low vapor pressure liquid chemicals and a plurality of valves and lines for delivering low vapor pressure liquid chemicals to a point of use, wherein the valves and lines A system comprising a gas source configured to flow gas through valves and lines to push low vapor pressure liquid chemicals from a gas to a source canister.

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