KR20090108556A - Reagent dispensing apparatus and delivery method - Google Patents

Abstract

PURPOSE: A reactant distribution device and a transmitting method for evaporating the material in a semiconductor material are provided to reduce the waste and increase the utilization of the liquid or the solid bulb chemical substance by maintaining the liquid bulb chemical substance. CONSTITUTION: A reactant distribution device and a transmitting method for evaporating the material in a semiconductor material are as follows. The vapor reaction material distribution device is provided. The source chemical material is added to the vapor reaction material distribution device. The carrier gas is supplied to a vapor reaction material distribution device through a tube(103) and carrier gas supply line. The vapor reaction material and carrier gas are collected from the vapor reaction material distribution device through the vapor reaction material exhaust line.

Description

Reactant distribution device and delivery method {REAGENT DISPENSING APPARATUS AND DELIVERY METHOD}

The present invention relates to a gaseous or liquid reactant dispensing device that can be used to dispense gaseous or liquid reactants, such as precursors for the deposition of materials in the manufacture of semiconductor materials and devices.

High-purity chemicals used in the semiconductor and pharmaceutical industries require special packaging to maintain their purity during storage. This is especially true for chemicals that react with air and / or moisture in the air. Such high purity chemicals are typically supplied to containers such as bubblers or ampoules.

State-of-the-art chemical vapor deposition and atomic layer deposition tools use bubblers or empoules to deliver precursor chemicals into the deposition chamber. Such bubblers or empoules work by passing a carrier gas through a container of high purity liquid precursor chemical or by transporting precursor vapor with the gas to the deposition chamber.

The container is typically a one-part (ie, the top cover or lid cannot be removed from the base) container or two-part (ie the top cover or lid can be removed from the base and is It is made as a container (which can be attached with a bolt). Integral containers have a higher degree of integrity but are more difficult to clean than two-piece containers. Two-piece containers are easier to clean because the top cover or lid can be removed from the base, but more difficult to seal and reuse. Ease of cleaning allows for reuse of two-piece containers beyond what can be achieved with integral containers. Reuse of containers is important for cost minimization and for environmental issues.

As integrated circuits have become smaller in size, so have the dimensions of internal components or features. As their size decreases, the necessity of purer chemicals has increased to minimize the effects of impurities. Therefore, the manufacturer must not only be able to produce high purity chemicals, but also transfer them to containers that will be of high purity.

The standard materials that make up such containers were transformed from precision quartz containers into stainless steel in the late 1990s. See, for example, US Pat. No. 5,607,002. Such vessels are known in the industry as bubblers or empoules and today are routinely constructed of stainless steel, ie 316SS. See, for example, US Pat. Nos. 3,930,591, 6,029,717 and 7,077,388.

In addition, in most cases it is necessary to heat the empoules by some means to increase the vapor pressure of the precursor to increase the amount of chemicals in the carrier gas. It is important to monitor the temperature of the liquid precursor chemical inside the empoul to control the vapor pressure.

It is also important to know when the liquid precursor chemical inside the empoule is running out so that it can be changed at the end of the chemical vapor deposition or atomic layer deposition cycle. If the empoules dry out during the cycle, the entire batch of wafers will be lost, causing a potential loss of millions of dollars. Therefore, it is necessary to leave as little liquid precursor chemical inside the empoule as possible to avoid waste of expensive liquid precursor chemicals. As the cost of chemical precursors increases, it is more important to waste chemicals to the minimum possible.

It is necessary to develop more reliable seals for commercially acceptable two-part high purity chemical containers. U. S. Patent No. 6,905, 125 relates to metal gaskets, such as C-ring gaskets, for preventing the leakage of fluid in semiconductor manufacturing devices. High purity chemicals for the electronics industry require leaktight containers that can withstand high vacuums.

There is a need in the art for an easy-to-clean, two-phase gaseous or liquid reactant dispensing device that requires a reactant dispensing device that can maintain high purity of the pro- chemistry and reduce waste by increasing the use of pro- chemistry in the device.

Part of the invention relates to a gas phase reactant dispensing apparatus, wherein the dispensing apparatus

Courage,

With the adapter,

A fastening means,

The vessel comprises an upper wall member, a sidewall member and a lower wall member, configured to form an inner vessel compartment that maintains source chemical at a fill level and further form an interior gas space above the fill level,

The top wall member having a first end seal port opening, a second end seal port opening, and optionally one or more other end seal port openings,

A carrier gas supply inlet fitting is connected to the first end seal port opening;

The adapter includes a metal end seal gasket coupled to a tube extending through the first gas seal port opening and the internal gas space to the source chemical, through which the carrier gas bubbles into the source chemical. At least a portion of the source chemical vapor may be incorporated into the carrier gas to cause a flow of gaseous reactants into the interior gas space above the fill level, the tube having an inlet end and a lower wall member adjacent the first end seal port opening. Has an outlet end adjacent to

The first end seal port opening and the carrier gas supply inlet fitting have opposing surfaces, the opposing surfaces not contacting each other,

The metal end seal gasket is in contact with the first end seal port opening and opposing surfaces of the carrier gas supply inlet fitting,

The fastening means secures the carrier gas supply inlet fitting to the first end face seal port opening through the metal end face seal gasket and the opposing surfaces,

And a gaseous reactant outlet fitting connected to the second end face seal port opening, wherein the gaseous reactant can be dispensed from the device via the gaseous reactant outlet fitting.

In addition, some aspects of the invention relate to a method for delivering a vapor phase reactant to a deposition chamber,

Providing a gas phase reactant dispensing apparatus, the dispensing apparatus

Courage,

With the adapter,

Fastening means,

A carrier gas supply line,

A gaseous reactant discharge line,

The vessel comprises an upper wall member, a sidewall member and a lower wall member, configured to form an inner vessel compartment that maintains source chemical at a fill level and further form an internal gas space above the fill level,

The top wall member having a first end face seal port opening, a second end face seal port opening, and optionally one or more other end face seal port openings,

A carrier gas supply inlet fitting is connected to the first end seal port opening;

The adapter includes a first end seal port opening and a metal end seal gasket coupled to a tube extending through the internal gas space to the source chemical, through which the carrier gas bubbles and flows into the source chemical. At least a portion of the source chemical vapor may be incorporated into the carrier gas to cause a flow of gaseous reactants into the interior gas space above the fill level, the tube being connected to the inlet end and the bottom wall member adjacent the first end seal port opening. With an adjacent outlet end,

The first end seal port opening and the carrier gas supply inlet fitting have opposing surfaces, the opposing surfaces not contacting each other,

The metal end seal gasket is in contact with the first end seal port opening and opposing surfaces of the carrier gas supply inlet fitting,

The fastening means secures the carrier gas supply inlet fitting to the first end face seal port opening through the metal end face seal gasket and the opposing surfaces,

The carrier gas supply line extends outward from the carrier gas supply inlet fitting to deliver carrier gas to the source chemical, and at least one carrier gas flow control valve to control the flow of carrier gas through the carrier gas supply line. Inside,

A gaseous reactant outlet fitting is connected to the second end seal port opening, through which the gaseous reactant can be dispensed from the apparatus,

The gaseous reactant discharge line extends outward from the gaseous reactant outlet fitting to remove gaseous reactants from the internal gas space above the fill level, and the gaseous reactant discharge line controls the flow of gaseous reactants through the gaseous reactant discharge line. Providing a vapor phase reactant distribution device, optionally including one or more vapor phase reactant flow control valves therein, for

Adding a source chemical to the gas phase reactant distribution device;

Heating the source chemical in the gaseous reactant dispensing device to a temperature capable of evaporating the source chemical to provide a gaseous reactant;

Supplying a carrier gas to the gaseous reactant distribution device through the tube and the carrier gas supply line;

Recovering gaseous reactant and carrier gas from the gaseous reactant distribution device through the gaseous reactant discharge line;

It relates to a method for sending a gaseous reactant to the deposition chamber, comprising supplying a gaseous reactant and a carrier gas to the deposition chamber.

In addition, part of the invention relates to a liquid phase reactant dispensing apparatus, wherein the dispensing apparatus

Courage,

With the adapter,

A fastening means,

The vessel comprises an upper wall member, a sidewall member and a lower wall member, configured to form an inner vessel compartment that maintains source chemical at a fill level and further form an internal gas space above the fill level,

The top wall member having a first end face seal port opening, a second end face seal port opening, and optionally one or more other end face seal port openings,

An inert gas supply inlet fitting is connected to the first end seal port opening and an inert gas is supplied into the internal gas space above the fill level through the first end seal port opening to pressurize the internal gas space above the fill level. And

A liquid reactant outlet fitting is connected to the second end seal port opening;

The adapter includes a metal end seal gasket coupled to a tube extending through the second end seal port opening and the internal gas space to the source chemical, through which the liquid reactant can be dispensed from the device, and The tube has an outlet end adjacent the second end face seal port opening and an inlet end adjacent the bottom wall member,

The second end seal port opening and the liquid reactant outlet fitting have opposing surfaces, the opposing surfaces not contacting each other,

The metal end seal gasket is in contact with the second end seal port opening and opposing surfaces of the liquid reactant outlet fitting,

The fastening means relates to a liquid reactant dispensing device which secures a liquid reactant outlet fitting to the second end seal port opening through the metal end face seal gasket and opposing surfaces.

Part of the invention also relates to a method for delivering a vapor phase reactant to a deposition chamber,

Providing a liquid phase reagent dispensing apparatus, wherein the dispensing apparatus

Courage,

With the adapter,

Fastening means,

An inert gas supply line,

A liquid reactant discharge line,

The vessel comprises an upper wall member, a sidewall member and a lower wall member, configured to form an inner vessel compartment that maintains source chemical at a fill level and further form an internal gas space above the fill level,

The top wall member having a first end face seal port opening, a second end face seal port opening, and optionally one or more other end face seal port openings,

An inert gas supply inlet fitting is connected to the first end seal port opening and an inert gas is supplied into the internal gas space above the fill level through the first end seal port opening to pressurize the internal gas space above the fill level. And

A liquid reactant outlet fitting is connected to the second end seal port opening;

The adapter includes a metal end seal gasket coupled to a tube extending through the second end seal port opening and the internal gas space to the source chemical, through which the liquid reactant can be dispensed from the device, and The tube has an outlet end adjacent the second end face seal port opening and an inlet end adjacent the bottom wall member,

The second end seal port opening and the liquid reactant outlet fitting have opposing surfaces, the opposing surfaces not contacting each other,

The metal end seal gasket is in contact with the second end seal port opening and opposing surfaces of the liquid reactant outlet fitting,

The fastening means secures a liquid reactant outlet fitting to the second end seal port opening through the metal end face seal gasket and the opposing surfaces,

The inert gas supply line extends outward from the inert gas supply inlet fitting to deliver an inert gas to the internal gas space above the fill level and at least one inert to control the flow of inert gas through the inert gas supply line. It includes a gas flow control valve therein,

The liquid reactant discharge line extends outward from the liquid reactant outlet fitting to remove liquid reactant from the vessel, and the liquid reactant discharge line extends one or more liquid phases to control the flow of the liquid reactant through the liquid reactant discharge line. Providing a liquid phase reactant dispensing device, optionally including a reactant flow control valve therein;

Adding a liquid reactant to the liquid reactant distribution device;

Selectively heating the solid source chemical in the liquid reactant distribution device to a temperature capable of dissolving the solid source chemical to provide a liquid reactant;

Supplying an inert gas to the liquid reactant distribution device through the inert gas supply line;

Recovering a liquid reactant from the liquid reactant distribution device through the tube and the liquid reactant discharge line;

Providing a vaporization device, the vaporization device

Courage,

A carrier gas supply line,

A gaseous reactant discharge line,

The vessel is configured to form an inner vessel compartment for vaporizing the liquid reactant,

The liquid reactant discharge line connects a liquid reactant distribution device to the vaporization device,

A portion of the vaporization device has a carrier gas supply inlet opening, through which the carrier gas can be supplied to the vaporization device to produce vapor phase reactants by incorporating vapor of a liquid reactant into the carrier gas. ,

A portion of the vaporization device having a gaseous reactant outlet opening through which the gaseous reactant can be dispensed from the vaporization device,

The carrier gas supply line extends from the carrier gas supply inlet opening outwardly from the vaporization device to deliver carrier gas to the vaporization device, and at least one carrier gas flow to control the flow of carrier gas through the carrier gas supply line. Has a control valve inside,

The vapor phase reactant discharge line extends from the vapor phase reactant outward from the vapor phase reactant outlet opening to remove vapor phase reactant from the vaporization device to the deposition chamber, and the vapor phase reactant discharge line flows through the vapor phase reactant discharge line. Providing one or more vapor phase reactant flow control valves therein to selectively control the vaporization apparatus;

Supplying a liquid reactant to the vaporization apparatus;

Heating the liquid reactant in the vaporization apparatus to a temperature capable of evaporating the liquid reactant to provide a gaseous reactant;

Supplying a carrier gas to the vaporization apparatus through the carrier gas supply line;

Recovering gaseous reactant and carrier gas from the vaporization apparatus through the gaseous reactant discharge line;

A method of sending a gaseous reactant to a deposition chamber, comprising supplying a gaseous reactant and a carrier gas to the deposition chamber.

Part of the invention also relates to a gas phase reactant dispensing apparatus, wherein the dispensing apparatus

Courage,

End seal tee fitting,

With seal gasket at the end,

Fastening means for securing the end seal T-shaped fitting,

With the adapter,

Fastening means for securing the carrier gas supply inlet fitting,

Including annular space,

The vessel comprises an upper wall member, a sidewall member and a lower wall member, configured to form an inner vessel compartment that maintains source chemical at a fill level and further form an internal gas space above the fill level,

The top wall member has an end face seal port opening and optionally one or more other end face seal port openings,

The end seal T-shaped fitting has an end seal opening, a carrier gas supply inlet opening and a gaseous reactant outlet opening,

The end seal port opening has the end seal T-shaped fitting connected to the end seal port opening through an end seal opening, the end seal port opening and the end seal opening have opposing surfaces, the opposing surface They do not touch each other,

The end face seal gasket is in contact with the end surface seal port opening and opposing surfaces of the end face seal opening,

Fastening means for securing the end seal T-shaped fitting secures the end seal T-shaped fitting to the end seal port opening through opposing surfaces and the end seal gasket,

The adapter includes a carrier gas supply inlet opening, an end seal opening, an end seal port opening, and a metal end seal gasket coupled to a tube extending through the internal gas space to the source chemical, through which the carrier gas is introduced. Foaming into the source chemical may flow into the carrier gas such that at least a portion of the source chemical vapor is incorporated into the carrier gas to cause the flow of gaseous reactants into the internal gas space above the fill level, and the tube passes through the carrier gas supply inlet opening. Having an inlet end adjacent to and an outlet end adjacent to the lower wall member,

A carrier gas supply inlet fitting is attached to the carrier gas supply inlet opening,

The carrier gas supply inlet opening and the carrier gas supply inlet fitting have opposing surfaces, the opposing surfaces not contacting each other,

The metal end seal gasket is in contact with the carrier gas supply inlet opening and the opposing surfaces of the carrier gas supply inlet fitting,

The fastening means for securing the carrier gas supply inlet fitting secures the carrier gas supply inlet fitting to the carrier gas supply inlet opening via opposing surfaces and the metal end seal gasket,

The annular space is a space between the outer wall of the tube and the carrier gas supply inlet opening, the end face seal opening and the inner wall of the end face seal port opening, through which the gaseous reactant passes through the gas phase reactant outlet opening. A gas phase reactant dispensing apparatus, which may be dispensed from the apparatus.

In addition, part of the invention is a method for delivering a vapor phase reactant to a deposition chamber,

Providing a gas phase reactant dispensing apparatus, the dispensing apparatus

Courage,

End seal with T-type fittings,

With seal gasket at the end,

Fastening means for securing the end seal T-shaped fitting,

With the adapter,

Fastening means for securing the carrier gas supply inlet fitting,

Annular space,

A carrier gas supply line,

A gaseous reactant discharge line,

The vessel comprises an upper wall member, a sidewall member and a lower wall member, configured to form an inner vessel compartment that maintains source chemical at a fill level and further form an internal gas space above the fill level,

The top wall member has an end face seal port opening and optionally one or more other end face seal port openings,

The end seal T-shaped fitting has an end seal opening, a carrier gas supply inlet opening and a gaseous reactant outlet opening,

The end seal port opening has the end seal T-shaped fitting connected to the end seal port opening through an end seal opening, the end seal port opening and the end seal opening have opposing surfaces, and the opposing surfaces Do not touch each other,

The end face seal gasket is in contact with the end surface seal port opening and opposing surfaces of the end face seal opening,

Fastening means for securing the end seal T-shaped fitting secures the end seal T-shaped fitting to the end seal port opening through opposing surfaces and the end seal gasket,

The adapter includes a carrier gas supply inlet opening, an end seal opening, an end seal port opening, and a metal end seal gasket coupled to a tube extending through the internal gas space to the source chemical, through which the carrier gas is introduced. Foaming into the source chemical may flow into the carrier gas such that at least a portion of the source chemical vapor is incorporated into the carrier gas to cause the flow of gaseous reactants into the internal gas space above the fill level, and the tube passes through the carrier gas supply inlet opening. Having an inlet end adjacent to and an outlet end adjacent to the lower wall member,

A carrier gas supply inlet fitting is attached to the carrier gas supply inlet opening,

The carrier gas supply inlet opening and the carrier gas supply inlet fitting have opposing surfaces, the opposing surfaces not contacting each other,

The metal end seal gasket is in contact with the carrier gas supply inlet opening and the opposing surfaces of the carrier gas supply inlet fitting,

The fastening means for securing the carrier gas supply inlet fitting secures the carrier gas supply inlet fitting to the carrier gas supply inlet opening via opposing surfaces and the metal end seal gasket,

The annular space is a space between the outer wall of the tube and the carrier gas supply inlet opening, the end face seal opening and the inner wall of the end face seal port opening, through which the gaseous reactant passes through the gas phase reactant outlet opening. Can be dispensed from the device,

The carrier gas supply line extends outward from the carrier gas supply inlet fitting to deliver carrier gas to the source chemical, and at least one carrier gas flow control valve to control the flow of carrier gas through the carrier gas supply line. Inside,

The gaseous reactant discharge line extends outward from the gaseous reactant outlet opening to remove gaseous reactants from the internal gas space above the fill level, and the gaseous reactant discharge line flows through the gaseous reactant discharge line. Providing a gaseous reactant dispensing device, optionally including one or more gaseous reactant flow control valves therein for control;

Adding a source chemical to the gas phase reactant distribution device;

Heating the source chemical in the gaseous reactant dispensing device to a temperature capable of evaporating the source chemical to provide a gaseous reactant;

Supplying a carrier gas to the gaseous reactant distribution device through the tube and the carrier gas supply line;

Recovering gaseous reactant and carrier gas from the gaseous reactant distribution device through the gaseous reactant discharge line;

A method of sending a gaseous reactant to a deposition chamber, comprising supplying a gaseous reactant and a carrier gas to the deposition chamber.

In addition, part of the invention relates to a liquid phase reactant dispensing apparatus, wherein the dispensing apparatus

Courage,

End seal with T-type fittings,

With seal gasket at the end,

Fastening means for securing the end seal T-shaped fitting,

With the adapter,

Fastening means for securing the liquid reactant outlet fitting,

Including annular space,

The vessel comprises an upper wall member, a sidewall member and a lower wall member, configured to form an inner vessel compartment that maintains source chemical at a fill level and further form an internal gas space above the fill level,

The top wall member has an end face seal port opening and optionally one or more other end face seal port openings,

The end seal T-shaped fitting has an end seal opening, an inert gas supply inlet opening and a liquid reactant outlet opening,

The end seal port opening has the end seal T-shaped fitting connected to the end seal port opening through an end seal opening, the end seal port opening and the end seal opening have opposing surfaces, and the opposing surfaces Do not touch each other,

The end face seal gasket is in contact with the end surface seal port opening and opposing surfaces of the end face seal opening,

Fastening means for securing the end seal T-shaped fitting secures the end seal T-shaped fitting to the end seal port opening through opposing surfaces and the end seal gasket,

The adapter includes a liquid end reactant opening, an end seal opening, an end seal port opening, and a metal end seal gasket coupled to a tube extending through the internal gas space to the source chemical, through which the liquid reactant is formed. Wherein the tube has an outlet end adjacent to the liquid reactant outlet opening and an inlet end adjacent to the bottom wall member,

A liquid reactant outlet fitting is connected to the liquid reactant outlet opening,

The liquid reactant outlet opening and the liquid reactant outlet fitting have opposing surfaces, the opposing surfaces not contacting each other,

The metal end seal gasket is in contact with the opposing surfaces of the liquid reactant outlet opening and the liquid reactant outlet fitting,

The fastening means for securing the liquid reactant outlet fitting secures the liquid reactant outlet fitting to the liquid reactant outlet opening via opposing surfaces and the metal end seal gasket,

The annular space is a space between the outer wall of the tube and the liquid reactant outlet opening, the end seal opening and the inner wall of the end seal port opening, through which the inert gas pressurizes an internal gas space above the fill level. To an internal gas space above the fill level through an inert gas feed inlet opening.

In addition, the present invention is a method for sending a vapor phase reactant into a deposition chamber,

Providing a liquid phase reagent dispensing apparatus, wherein the dispensing apparatus

Courage,

End seal with T-type fittings,

With seal gasket at the end,

Fastening means for securing the end seal T-shaped fitting,

With the adapter,

Fastening means for securing the liquid reactant outlet fitting,

Annular space,

An inert gas supply line,

A liquid reactant discharge line,

The vessel comprises an upper wall member, a sidewall member and a lower wall member, configured to form an inner vessel compartment that maintains source chemical at a fill level and further form an internal gas space above the fill level,

The top wall member has an end face seal port opening and optionally one or more other end face seal port openings,

The end seal T-shaped fitting has an end seal opening, an inert gas supply inlet opening and a liquid reactant outlet opening,

The end seal port opening has the end seal T-shaped fitting connected to the end seal port opening through an end seal opening, the end seal port opening and the end seal opening have opposing surfaces, and the opposing surfaces Do not touch each other,

The end face seal gasket is in contact with the end surface seal port opening and opposing surfaces of the end face seal opening,

Fastening means for securing the end seal T-shaped fitting secures the end seal T-shaped fitting to the end seal port opening through opposing surfaces and the end seal gasket,

The adapter includes a liquid end reactant opening, an end seal opening, an end seal port opening, and a metal end seal gasket coupled to a tube extending through the internal gas space to the source chemical, through which the liquid reactant is formed. Wherein the tube has an outlet end adjacent to the liquid reactant outlet opening and an inlet end adjacent to the bottom wall member,

A liquid reactant outlet fitting is connected to the liquid reactant outlet opening,

The liquid reactant outlet opening and the liquid reactant outlet fitting have opposing surfaces, the opposing surfaces not contacting each other,

The metal end seal gasket is in contact with the opposing surfaces of the liquid reactant outlet opening and the liquid reactant outlet fitting,

The fastening means for securing the liquid reactant outlet fitting secures the liquid reactant outlet fitting to the liquid reactant outlet opening via opposing surfaces and the metal end seal gasket,

The annular space is a space between the outer wall of the tube and the liquid reactant outlet opening, the end seal opening and the inner wall of the end seal port opening, through which the inert gas pressurizes an internal gas space above the fill level. To the internal gas space above the filling level through an inert gas supply inlet opening,

The inert gas supply line extends outward from the inert gas supply inlet opening to deliver inert gas to the internal gas space above the fill level, and at least one to control the flow of inert gas through the inert gas supply line. An inert gas flow control valve therein;

The liquid reactant discharge line extends outward from the liquid reactant outlet fitting to remove the liquid reactant from the vessel, and the liquid reactant discharge line extends one or more liquid reactants to control the flow of the liquid reactant through the liquid reactant discharge line. Providing a liquid phase reactant dispensing device, optionally including a flow control valve therein;

Adding a liquid reactant to the liquid reactant distribution device;

Selectively heating the solid source chemical in the liquid reactant distribution device to a temperature capable of dissolving the solid source chemical to provide a liquid reactant;

Supplying an inert gas to the liquid reactant distribution device through the inert gas supply line;

Recovering a liquid reactant from the liquid reactant distribution device through the tube and the liquid reactant discharge line;

Providing a vaporization device, the vaporization device

Courage,

A carrier gas supply line,

A gaseous reactant discharge line,

The vessel is configured to form an inner vessel compartment for vaporizing the liquid reactant,

The liquid reactant discharge line connects a liquid reactant distribution device to the vaporization device,

A portion of the vaporization device has a carrier gas supply inlet opening, through which the carrier gas is supplied to the vaporization device to produce vapor phase reactants by incorporating vapor of a liquid reactant into the carrier gas. ,

A portion of the vaporization device having a gaseous reactant outlet opening through which the gaseous reactant can be dispensed from the vaporization device,

The carrier gas supply line extends from the carrier gas supply inlet opening outwardly from the vaporization device to deliver carrier gas to the vaporization device, and at least one carrier gas flow to control the flow of carrier gas through the carrier gas supply line. Has a control valve inside,

The vapor phase reactant discharge line extends from the vapor phase reactant outward from the vapor phase reactant outlet opening to remove vapor phase reactant from the vaporization device to the deposition chamber, and the vapor phase reactant discharge line flows through the vapor phase reactant discharge line. Providing one or more vapor phase reactant flow control valves therein to selectively control the vaporization apparatus;

Supplying a liquid reactant to the vaporization apparatus;

Heating the liquid reactant in the vaporization apparatus to a temperature capable of evaporating the liquid reactant to provide a gaseous reactant;

Supplying a carrier gas to the vaporization apparatus through the carrier gas supply line;

Recovering gaseous reactant and carrier gas from the vaporization apparatus through the gaseous reactant discharge line;

A method of sending a gaseous reactant to a deposition chamber, comprising supplying a gaseous reactant and a carrier gas to the deposition chamber.

The gaseous reactant distribution device or assembly of the present invention can be employed in a wide variety of process systems, for example, the gaseous reactants from a supply vessel may be chemically deposited to deposit a layer of material from a source vapor onto a substrate inside a chemical vapor deposition chamber. One of them is a chemical vapor deposition system that is passed through a vapor deposition chamber.

The gaseous or liquid reactant dispensing device or assembly of the present invention is easy to clean, maintains the purity of liquid precursor chemicals, and reduces waste by increasing the utilization of liquid or solid precursor chemicals.

Other aspects, features and examples of the present invention will become more apparent from the following description and appended claims.

The gaseous or liquid reactant dispensing device or assembly of the present invention is easy to clean, maintain the purity of liquid precursor chemicals, and reduce waste by increasing the utilization of liquid or solid precursor chemicals.

The present invention reduces the number of container designs required to support other applications. A standard two port container without a tube inserts a gasket / tube adapter between one of the ports and the corresponding valve, thereby providing a tube (ie a bubble tube for gas delivery or a dip tube for liquid delivery). Can be replaced with a container usable for applications requiring (see FIG. 1). The overall height of the container does not change. In contrast to the prior art, since the tube is not welded to the top of the container, it can be removed if modifications and / or replacements are needed. This results in increased flexibility.

In embodiments of the present invention, the length needed to add a tube to a container using an end seal port is not extended (ie the gasket is already used to seal the connection). With compression-fitted adapters, tubes can be added to ports using end seal fittings. The tube may be inserted to a predetermined length through the compression fitting, after which the compression fitting is fixed on the tube. In terms of leak tightness, compression fittings are generally less desirable than joining two parts with a (removable) end seal or (nonremovable) welding. Using opposite end seal parts with tubes to be welded, it is possible to add a tube to a port using an end seal fitting, the tube having a castle (male or female) opposite the port. In view of the foregoing, the present invention is universal (ie, the gasket / tube adapter will work with male or female end seal ports), and is preferred over welding tubes to fittings.

The present invention simplifies adding tubes by allowing the use of a standard set of gasket / tube adapters. The gasket / tube adapter can be retrofitted without exposing the vessel to contaminants (eg, particles from machine operation or welding) that are combined with the retrofit process. The length of the tube can be easily changed by short cutting or extension. The gasket / tube adapter can be leak tested independently of the container. Leakage at the junction of the dip tube directly welded to the container will be more expensive to repair compared to the gasket / tube adapter (ie, the value of the ampoule is much more expensive than the gasket / tube adapter).

Various modifications and variations of the present invention include the use of different materials (eg, copper, stainless steel, aluminum, nickel, Teflon, etc.) of structures for empoules and adapters; Different methods used to join gaskets to tubes in adapter formation (eg, welding, machine operation, shrinkage, fittings, etc.); Different end face seal gasket styles (e.g., flat or contoured) and different manufacturers (e.g., Parker, Hi-Tech, Swagelok, Fujikin, etc. ]; The use of gaskets and tubes of different sizes (eg, 1/8 inch (0.318 cm), 1/4 inch (0.635 cm), 1/2 inch (1.27 cm), etc.); Length of tube that can be varied; A tube that may optionally have holes along its length; It includes tubes that can vary in length (ie, of non-uniform cross section).

As described above with reference to FIG. 1, some of the present invention relates to a gaseous reactant distribution device,

Courage,

With the adapter,

A fastening means,

The vessel comprising an upper wall member, a side wall member and a lower wall member, configured to form an inner vessel compartment for maintaining source chemical at a fill level and to further form an inner gas space above the fill level,

The top wall member having a first end face seal port opening, a second end face seal port opening, and optionally one or more other end face seal port openings,

A container to which the carrier gas supply inlet fitting is connected, the first end seal port opening;

The adapter includes a first end seal port opening and a metal end seal gasket coupled to a tube extending through the internal gas space to the source chemical, through which the carrier gas can bubble into the source chemical. At least a portion of the source chemical vapor is incorporated into the carrier gas to cause a flow of gaseous reactants into the interior gas space above the fill level, the tube being adjacent to the inlet end and the bottom wall member adjacent the first end seal port opening. Having an outlet end,

The first end seal port opening and the carrier gas supply inlet fitting have opposing surfaces, the opposing surfaces not contacting each other,

The metal end seal gasket is in contact with the first end seal port opening and opposing surfaces of the carrier gas supply inlet fitting,

The fastening means secures the carrier gas supply inlet fitting to the first end face seal port opening through the metal end face seal gasket and the opposing surfaces,

And a gaseous reactant outlet fitting connected to the second end face seal port opening, wherein the gaseous reactant can be dispensed from the device via the gaseous reactant outlet fitting.

In addition, the gas phase reactant distribution device

A carrier gas supply line,

A gaseous reactant discharge line,

The carrier gas supply line extends outward from the carrier gas supply inlet fitting to deliver carrier gas to the source chemical, and at least one carrier gas flow control valve to control the flow of carrier gas through the carrier gas supply line. Inside,

The gaseous reactant discharge line extends outward from the gaseous reactant outlet fitting to remove gaseous reactants from the internal gas space above the fill level, and the gaseous reactant discharge line controls the flow of gaseous reactants through the gaseous reactant discharge line. Optionally includes one or more gas phase reactant flow control valves therein for the purpose.

The gas phase reactant distribution device also includes a gaseous reactant discharge line in the gaseous reactant in flow communication with the vapor delivery deposition system, wherein the deposition system is selected from chemical vapor deposition systems or atomic layer deposition systems.

In addition, as described above with reference to FIG. 1, the present invention relates to a liquid phase reactant distribution device,

Courage,

With the adapter,

Including fastening means,

The vessel comprises an upper wall member, a sidewall member and a lower wall member, configured to form an inner vessel compartment that maintains source chemical at a fill level and further form an internal gas space above the fill level,

The top wall member having a first end face seal port opening, a second end face seal port opening, and optionally one or more other end face seal port openings,

An inert gas supply inlet fitting is connected to the first end seal port opening and an inert gas is supplied into the internal gas space above the fill level through the first end seal port opening to pressurize the internal gas space above the fill level. And

A liquid reactant outlet fitting is connected to the second end seal port opening;

The adapter includes a metal end seal gasket coupled to a tube extending through the second end seal port opening and the internal gas space to the source chemical, through which the liquid reactant can be dispensed from the device, The tube having an outlet end adjacent the second end face seal port opening and an inlet end adjacent the bottom wall member,

The second end seal port opening and the liquid reactant outlet fitting have opposing surfaces, the opposing surfaces not contacting each other,

The metal end seal gasket is in contact with the second end seal port opening and opposing surfaces of the liquid reactant outlet fitting,

The fastening means relates to a liquid reactant dispensing device which secures a liquid reactant outlet fitting to the second end seal port opening through the metal end face seal gasket and opposing surfaces.

In addition, the liquid reactant distribution device,

An inert gas supply line,

A liquid reactant discharge line,

The inert gas supply line extends outward from the inert gas supply inlet fitting to deliver an inert gas to the internal gas space above the fill level and at least one inert to control the flow of inert gas through the inert gas supply line. It includes a gas flow control valve therein,

The liquid reactant discharge line extends outward from the liquid reactant outlet fitting to remove the liquid reactant from the vessel, and the liquid reactant discharge line extends one or more liquid reactants to control the flow of the liquid reactant through the liquid reactant discharge line. Optionally include a flow control valve therein.

The liquid phase reactant distribution device also includes a liquid reactant discharge line in fluid communication with the vaporization device, the vaporization device in flow communication with the vapor delivery deposition system, wherein the deposition system is a chemical vapor deposition system and an atomic layer deposition system. Is selected from.

The vessel or empoul is typically processed into stainless steel, for example 316L, and is electropolished to prevent contamination of precursor liquid or solid source chemicals. Adapters are also typically machined from stainless steel. The cover or top wall member may optionally be removed to facilitate cleaning and reuse. The container may include a cylindrically shaped sidewall member or a sidewall member forming a non-cylindrical shape.

The fastening means is used to secure the carrier gas supply inlet fitting to the first end seal port opening through the opposing surfaces and the metal end seal gasket of the adapter. Suitable fastening means include, for example, the engagement of a male nut or body hex with a female nut.

The fastening means is used to secure the liquid reactant outlet fitting to the second end seal port opening through the opposing surfaces and the metal end seal gasket of the adapter. Suitable fastening means include, for example, the engagement of a male nut or body hex with a female nut.

In an embodiment of the present invention, the gasket / tube assembly (ie, the adapter) affects the flow pattern of the fluid through the combined vessel and / or tubing. Orientation of the flow pattern of the gas or liquid has been used to transport precursors for depositing thin films. Containers should be made using materials that do not react with the precursors. As mentioned above, stainless steel is typically selected as the material for constructing the container of the precursor. The gasket tube assembly may be constructed of similar material (eg, stainless steel or nickel).

The invention may also be used to redirect the flow pattern of reactants (gas and / or liquid) to the reaction vessel. This example is used for the simultaneous injection of reactants used for thin film deposition. Separation of reactants that can be gas phase reacted just before contacting the substrate surface can reduce the likelihood of particle formation and increase film deposition rate.

In an embodiment of the invention, the gasket / tube adapter is prefabricated and inserted into the desired port. The end face seal connection will then be sealed in a conventional manner (eg, by tightening the connection using a male nut and a female nut). By way of example, there are VCR components (eg, Swagelok) as the end seal connections, but other types may be used.

As discussed above, FIG. 4 is a cross-sectional view of a part that may be used to assemble a metal gasket end face seal connection 150 without a gasket / tube assembly (see Swagelok catalog MS-01-24). Metal gasket 120 is used for seal end fittings (eg, Swagelok's VCR). It is a disk with a hole in the center. Reference numeral 121 is a surface of the metal gasket 120 in contact with the beads 101 of the end seal fitting 100 upon sealing. Reference numeral 122 is the surface of the metal gasket 120 in contact with the beads 111 of the end face seal fitting 110 upon sealing. Reference numeral 100 denotes an end seal fitting (eg, VCR of Swagelok) that uses a metal gasket 120 to connect to the end seal fitting 110. Reference numeral 101 is a bead that forms the seal face of the end face seal fitting 100 with the surface 121 of the metal gasket 120. 102 is the inner surface of the end seal fitting 100 in contact with the processing fluid (liquid or gas). 103 is the end of the end face seal fitting 100, opposite the sealing bead 101. End 103 of end face seal fitting 100 is coupled to (eg, welded to) another processing component (eg, a tube, valve, container, etc.). Depending on the pressure gradient, fluid enters or exits the end seal fitting 100 through the end 103.

End seal fitting 110 uses metal gasket 120 to connect to end seal fitting 100. The beads 111 form the seal face of the end face seal fitting 110 with the surface 122 of the metal gasket 120. Reference numeral 112 is an inner surface of the end seal fitting 110 in contact with the processing fluid (liquid or gas). Reference numeral 113 is an end of the end face seal fitting 110 that faces the sealing bead 111. The end 113 of the end seal fitting 110 is coupled to (eg, welded to) another processing component (eg, a tube, a valve, a container, etc.). Depending on the pressure gradient, fluid enters or exits the end face seal fitting 110 through the end 113. The male nut 130 is tight against the female nut 140 to form an assembled connection 150.

As discussed above, Figure 5 is a cross-sectional view of a part that can be used to assemble a metal gasket end face seal connection using a gasket / tube adapter used in the present invention. Metal gasket / tube adapter 220 consists of a metal gasket coupled to the tube. Reference numeral 221 denotes the surface of the gasket / tube adapter 220 in contact with the beads 201 of the end seal fitting 200 upon sealing. Reference numeral 222 is the surface of the gasket / tube adapter 220 in contact with the beads 211 of the end seal fitting 210 upon sealing. Reference numeral 223 is the inner surface of the gasket / tube adapter 220 in contact with the processing fluid (liquid or gas). Reference numeral 224 is the end of the gasket / tube adapter 220, opposite the ends where the surfaces 221, 222 contact the beads 201, 211, respectively. End seal fitting 200 (eg, Swagelok's VCR) uses metal gasket / tube adapter 220 to connect with end seal fitting 210. Bead 201 forms a sealing face of end seal fitting 200 with surface 221 of gasket / tube adapter 220. Reference numeral 202 denotes the inner surface of the end seal fitting 200 in contact with the processing fluid (liquid or gas).

 Reference numeral 203 is an end of the end face seal fitting 200 opposite the sealing bead 201. End 203 of end seal fitting 200 is coupled to (eg, welded to) another processing component (eg, a tube, valve, container, etc.). Depending on the pressure gradient, fluid enters or exits the end seal fitting 200 through the end 203.

 End seal fitting 210 uses a metal gasket / tube adapter 220 to connect with end seal fitting 200. Bead 211 forms the sealing face of end seal fitting 210 with surface 222 of gasket / tube adapter 220. Reference numeral 212 denotes an inner surface of the end seal fitting 200 in contact with the processing fluid (liquid or gas). Reference numeral 213 is an end of the end face seal fitting 210, opposite the sealing bead 211. End 213 of end face seal fitting 210 is coupled to (eg, welded to) another processing component (eg, a tube, valve, container, etc.). Since the connection is made using the gasket / tube adapter 220, the fluid does not flow through the end 213. Instead, fluid flows through the end 224 of the gasket / tube adapter 220. The male nut 230 is tight against the female nut 240 to form an assembled connection 250. When assembling the connector 250, the fluid does not flow through the end 213 of the end face seal fitting 210. Fluid entering or exiting the end seal fitting 200 through the end 203 flows in or out of the gasket / tube adapter 220 via the end 224.

6 shows an example of a flow passage through assemblies 150 and 250. Arrows in FIG. 6 indicate the direction and passage of fluid flow. Because of the use of the gasket / tube adapter 220 in the assembly 250, the passage of fluid flow in the assembly 250 is different than in the assembly 150.

The empoules may include inlet and outlet valves that allow chemicals to be sent to end use equipment. Optional empoul equipment includes a source chemical level sensor and a fill port to determine when the empoule is nearly empty. The material in the vessel is conveyed at low vapor pressure in vacuum or using an inert gas to withdraw the vapor. The material can be alternately delivered to the end use equipment as liquid through the dip tube, and the end use equipment can be vaporized or dispensed as needed.

The temperature sensor is preferably included in the empoule to ensure uniform thermal conduction. The source chemical level sensor is preferably included in the empoule to ensure effective use of the source chemical. Valve and source chemical level sensors are attached through the end seal connection to ensure a clean, leak proof seal. Once assembled in the sterile chamber, the empoules are adjusted to remove leaks and adsorbed water which are inspected with a helium leak detector. Empoul is designed to be used at low torque pressures, slightly higher than the atmosphere.

In an embodiment of the invention, the temperature sensor extends generally vertically downward from the outside of the upper end of the vessel through a portion of the upper wall member and into the interior space of the vessel, the lower end of the temperature sensor being located in the non-interfering vicinity of the lower wall surface. . The source chemical level sensor extends generally vertically downward from the outside of the upper end of the vessel through a portion of the top wall member to the interior space of the vessel, and the lower end of the source chemical level sensor is located in the non-interfering vicinity of the bottom wall surface. The temperature sensor is operatively placed in the vessel to determine the temperature of the source chemical of the vessel, the source chemical level sensor is operatively placed in the vessel to determine the level of the source chemical of the vessel, the temperature sensor and The source chemical level sensor is located in non-interfering proximity to each other in the vessel, and the lower end of the temperature sensor is located at or near the surface of the vessel relative to the lower end of the source chemical level sensor, Sensors and source chemical level sensors are located in source chemicals in flow communication within the vessel. The source chemical level sensor is selected from an ultrasonic sensor, an optical sensor, a capacitive sensor, and a float-type sensor, the temperature sensor including a thermowell and a thermocouple. do.

In an embodiment of the present invention, the bottom wall member provides a sump cavity, and at the bottom of the sump cavity, a temperature sensor, a source chemical level sensor, a dip tube and / or a bubble tube may be disposed. Such a structure may allow a high volume percentage of the initially supplied liquid or solid source chemicals used when used to selectively distribute the source chemicals. For example, 95 volume% or more, preferably 98 volume% or more can be tolerated. In addition, this structure can improve the economics of the process in which the dispensed source chemicals are used, the distribution system, and the source chemical source.

The present invention enables the minimum amount of precursor chemical for semiconductors to remain in the empoule or bubbler when the source chemical level sensor indicates exhaustion of the contents. This is very important as the complexity and cost of precursors for semiconductors increases. To minimize costs, semiconductor manufacturers hope to minimize the consumption of precursors as much as possible. Also, in the present invention, the temperature sensor is located in the recessed sump cavity as well as the source chemical level sensor. This ensures the reading of the actual temperature of the precursor for the source chemical semiconductor while the source chemical level sensor indicates the presence of the precursor. This is important in terms of safety. If the temperature sensor is outside the semiconductor precursor, it will send a false low temperature signal to the heating device. This can cause overheating of the empoules, which can lead to decomposition and instability of precursors for semiconductors.

Referring back to the vessel or empoule, the vessel may be equipped with a source chemical level sensor, which is close to the surface of the sump cavity of the vessel from the top outside the vessel, through the non-central position of the top wall member of the vessel. Thereby extending downward to a lower end non-centrically located in the bottom member, thereby enabling the use of at least 95% of the source chemical reactant when the source chemical is contained in the vessel. The top of the source chemical level sensor can be connected to the central processing unit by a source chemical level sensor signaling line, thereby centralizing the source chemical level signal sensed during operation of the system from the source chemical level sensor. Can be delivered to the unit.

At the same time, the vessel may be equipped with temperature sensors, i.e. thermowells and thermocouples, the thermowells and thermocouples penetrating downward from the top of the vessel outside the center located in the upper wall member of the vessel, It extends very close to the surface of the sump cavity to a lower end located in the center of the bottom wall member. The top of the temperature sensor may be connected to the central processing unit by a temperature sensing signal transmission line, thereby transferring the sensed temperature signal from the temperature sensor to the central processing unit while the system is operating.

The central processing unit, which may include a microprocessor, computer or other suitable control means, may be connected to the flow control valve by means of a control signal transmission line (eg, via an appropriate valve actuator element), thereby connecting the flow control valve. It can optionally be controlled and control the flow of carrier gas towards the vessel. In addition, the central processing unit may be connected to the second flow control valve by a control signal transmission line (eg, via an appropriate valve actuator element), thereby selectively regulating the flow control valve and by gas or liquid phase from the vessel. The release of reactants can be controlled. For the purposes of the present invention, the flow control valve may comprise an isolation valve, a metering valve, or the like.

The present invention enables semiconductor manufacturers to use the maximum amount of precursor while consuming very little before the change-out of empoules. This minimizes consumption in certain applications and maximizes the recovery of the input for semiconductor precursors.

Source chemicals useful in the present invention can vary widely and include, for example, Groups 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, Liquid or solid precursors for metals selected from the Group 12, 13, 14, 15, 16, and Lanthanide families. Exemplary source chemicals include, for example, ruthenium, hafnium, tantalum, molybdenum, platinum, gold, titanium, lead, Solid or liquid precursors for metals selected from palladium, zirconium, bismuth, strontium, barium, calcium, antimony and thallium, or Precursors for metalloids selected from silicon, germanium and tellurium. Preferred organometallic precursor compounds include ruthenium containing organometallic precursor compounds, hafnium containing organometallic precursor compounds, tantalum containing organometallic precursor compounds and / or molybdenum containing organometallic precursor compounds.

Solid source chemicals that sublime and solid source chemicals that are melted by heat can be used in the present invention. For example, subliming solid source chemicals can be used in the gas phase reactant distribution device shown in FIG. Thermally melted solid source chemicals may be used in the gas phase reactant distribution device shown in FIG. 1 and the liquid phase reactant distribution device shown in FIG. 1. Similarly, liquid source chemicals may be used in the gas phase reactant distribution device shown in FIG. 1 and the liquid phase reactant distribution device shown in FIG. 1. If subliming solid source chemicals are used, it is necessary to use dust capture equipment.

The gaseous or liquid reactants useful in the present invention may vary widely, for example, Groups 2, 3, 4, 5, 6, 7, 8, 9, 10, 11 of the periodic table. Liquid or solid precursors for metals selected from the Group, Group 12, 13, 14, 15, 16, and Lanthanon families. Exemplary precursors are, for example, metal precursors selected from ruthenium, hafnium, tantalum, molybdenum, platinum, gold, titanium, lead, palladium, zirconium, bismuth, strontium, barium, calcium, antimony and thallium, or silicon, germanium And precursors for metalloids selected from tellurium. Preferred organometallic precursor compounds include ruthenium containing organometallic precursor compounds, hafnium containing organometallic precursor compounds, tantalum containing organometallic precursor compounds and / or molybdenum containing organometallic precursor compounds.

The gaseous reactant distribution device may further comprise a carrier gas source connected to the carrier gas supply line. Likewise, the liquid reactant distribution device may further comprise an inert gas source connected to the inert gas supply line.

In addition, the gas phase reactant distribution device

A deposition chamber,

A gaseous reactant discharge line,

An optional heatable susceptor,

May include a waste discharge line,

The deposition chamber is selected from a chemical vapor deposition chamber or an atomic layer deposition chamber,

Said vapor reactant discharge line connects a vapor reactant distribution device to a deposition chamber,

The selectively heatable susceptor is embedded in a deposition chamber and located in a receiving relationship in a vapor reactant discharge line,

The waste discharge line is connected to the deposition chamber,

Accordingly, the gaseous reactant enters the deposition chamber via the gaseous reactant discharge line and contacts the substrate on a selectively heatable susceptor, and the remaining waste is discharged through the waste discharge line.

The substrate is comprised of a metal selected from metals, metal silicides, metal carbides, metal nitrides, semiconductors, insulators and barrier materials. The substrate is preferably a pattern wafer.

In addition, the liquid reactant distribution device

A deposition chamber,

Liquid reactant discharge line,

A portion of the vaporization apparatus having a carrier gas supply inlet,

Part of the vaporization apparatus having a gaseous reactant outlet,

A carrier gas supply line,

A gaseous reactant discharge line,

An optional heatable susceptor,

May include a waste discharge line,

The deposition chamber is selected from a chemical vapor deposition chamber and an atomic layer deposition chamber,

The liquid reactant discharge line connects the liquid reactant distribution device to a vaporization device,

A carrier gas is supplied to the vaporization apparatus through the carrier gas supply inlet, and vapor of the liquid reactant is incorporated into the carrier gas to produce a gaseous reactant,

The gaseous reactant may be withdrawn from the vaporization device through the gaseous reactant outlet,

The carrier gas supply line extends from the carrier gas supply inlet outwardly from the vaporization device to deliver carrier gas to the vaporization device, and the carrier gas supply line has a carrier gas therein to control the flow of carrier gas therethrough. Built-in flow control valve,

The vapor phase reactant discharge line extends from the vaporizer to the vapor phase reactant outlet from outside the vaporizer to remove the vapor phase reactant from the vaporizer and the vapor phase reactant discharge line passes through the vapor phase reactant to control the flow of vapor reactant therethrough. Built-in reactant flow control valve,

The selectively heatable susceptor is embedded in a deposition chamber and located in a receiving relationship in a vaporization apparatus,

The waste discharge line is connected to the deposition chamber,

Accordingly, the gaseous reactant enters the deposition chamber via the gaseous reactant discharge line and contacts the substrate on a selectively heatable susceptor, and the remaining waste is discharged through the waste discharge line.

The substrate is composed of a metal selected from metals, metal silicides, metal carbides, metal nitrides, semiconductors, insulators and barrier materials. The substrate is preferably a pattern wafer.

In another embodiment, a portion of the invention relates to a gas phase reactant distribution device, wherein the gas phase reactant distribution device is

Courage,

End seal with T-type fittings,

With seal gasket at the end,

Fastening means,

With the adapter,

Including annular space,

The vessel comprises an upper wall member, a sidewall member and a lower wall member, configured to form an inner vessel compartment for maintaining source chemical at a fill level and further form an internal gas space for the fill level,

The top wall member has an end face seal port opening and optionally one or more other end face seal port openings,

The end seal T-shaped fitting has an end seal opening, a carrier gas supply inlet, and a gaseous reactant outlet,

The end seal port opening has an end seal T-shaped fitting connected to an end seal opening, the end seal port opening and the end seal opening have opposing surfaces, the opposing surfaces not contacting each other,

The end face seal gasket, such as metal, is in contact with the end face seal port opening and opposing surfaces of the end face seal opening,

The fastening means secures an end seal T-shaped fitting to the end seal port opening through the end seal gasket and the opposing surfaces,

The adapter includes a carrier gas supply inlet opening, an end seal opening, an end seal port opening, and a metal end seal gasket coupled to a tube extending through the internal gas space to the source chemical, through which the carrier gas is introduced. Foaming into the source chemical may flow into the carrier gas such that at least a portion of the source chemical vapor is incorporated into the carrier gas to cause the flow of gaseous reactants into the internal gas space above the fill level, and the tube passes through the carrier gas supply inlet opening. Having an inlet end adjacent to and an outlet end adjacent to the lower wall member,

The carrier gas supply inlet opening has a carrier gas supply inlet fitting attached thereto;

The carrier gas supply inlet opening and the carrier gas supply inlet fitting have opposing surfaces, the opposing surfaces not contacting each other,

The metal end seal gasket is in contact with the carrier gas inlet fitting and opposing surfaces of the carrier gas supply inlet opening,

The fastening means secures the carrier gas supply inlet fitting to the carrier gas supply inlet opening through the metal seal gasket and the opposing surfaces,

The annular space is located between the carrier gas supply inlet opening, the end seal opening and the inner wall of the end seal port opening and the outside of the tube, wherein the gaseous reactant can be dispensed from the device through the gaseous reactant outlet opening. have.

In addition, the gas phase reactant distribution device,

A carrier gas supply line,

A gaseous reactant discharge line,

The carrier gas supply line extends outward from the carrier gas supply inlet fitting to deliver carrier gas to the source chemical, and at least one carrier gas flow control valve to control the flow of carrier gas through the carrier gas supply line. Inside,

The gaseous reactant discharge line extends outward from the gaseous reactant outlet opening to remove gaseous reactants from the internal gas space above the fill level and at least one therein to control the flow of gaseous reactants through the gaseous reactant discharge line. And optionally a gaseous reactant flow control valve.

The vapor phase reactant distribution device also includes a vapor phase reactant discharge line in flow communication with the vapor phase vapor deposition system, the vapor deposition system being selected from a chemical vapor deposition system or an atomic layer deposition system.

In addition, the gas phase reactant distribution device,

A deposition chamber,

A gaseous reactant discharge line,

An optional heatable susceptor,

A waste discharge line,

The deposition chamber is selected from a chemical vapor deposition chamber or an atomic layer deposition chamber,

The vapor reactant discharge line connects the vapor reactant distribution device to the deposition chamber,

The selectively heatable susceptor is contained within a deposition chamber and located in a receiving relationship in a gaseous reactant discharge line,

The waste discharge line is connected to the deposition chamber,

Accordingly, the gaseous reactants enter the deposition chamber via the gaseous reactant discharge line and contact the substrate on a selectively heatable susceptor, and the remaining waste is discharged through the waste discharge line.

The substrate is composed of a metal selected from metals, metal silicides, metal carbides, metal nitrides, semiconductors, insulators and barrier materials. The substrate is preferably a pattern wafer.

In another embodiment, a portion of the invention relates to a liquid reactant distribution device, wherein the liquid reactant distribution device is

Courage,

End seal with T-type fittings,

With seal gasket at the end,

With the adapter,

Fastening means,

Including annular space,

The vessel comprises an upper wall member, a sidewall member and a lower wall member, configured to form an inner vessel compartment that maintains source chemical at a fill level and further form an internal gas space above the fill level,

The top wall member has an end face seal port opening and one or more other end face port openings,

The end seal T-shaped fitting has an end seal opening, an inert feed inlet opening and a liquid reactant outlet opening,

The end seal port opening has an end seal T-shaped fitting to which an end seal opening is connected, the end seal port opening and the end seal opening have opposing surfaces, and the opposing surfaces do not contact each other,

The end seal gasket, for example a metal end seal gasket, is in contact with the end seal port opening and in opposing surfaces of the end seal opening,

The fastening means secures an end seal T-shaped fitting to the end seal port opening through the end seal gasket and opposing surfaces,

The adapter includes a metal end seal gasket coupled to a tube extending into the source chemical through the liquid reactant outlet opening, the end seal opening, the end seal port opening, and the internal gas space, through which the liquid reactant is deposited. Wherein the tube has an outlet end adjacent to the liquid reactant outlet opening and an inlet end adjacent to the bottom wall member,

A liquid reactant outlet fitting is connected to the liquid reactant outlet opening,

The liquid reactant outlet opening and the liquid reactant outlet fitting have opposing surfaces, the opposing surfaces not contacting each other,

The metal end seal gasket is in contact with the opposing surfaces of the liquid reactant outlet opening and the liquid reactant outlet fitting,

Said fastening means secures a liquid reactant outlet fitting to said liquid reactant outlet opening through said metal end face seal gasket and opposing surfaces,

The annular space exists between the outer wall of the tube and the inner wall of the liquid reactant outlet opening, the end face seal opening and the end face seal port opening, through which an inert gas is introduced above the fill level through an inert gas supply inlet opening. It is fed into the gas space to pressurize the internal gas space above the fill level.

In addition, the liquid reactant distribution device,

An inert gas supply line,

A liquid reactant discharge line,

The inert gas supply line extends outward from the inert gas supply inlet opening to deliver the inert gas to the internal gas space above the fill level, and the inert gas supply line is internally configured to control the flow of the inert gas therethrough. One or more inert gas flow control valves,

The liquid reactant discharge line extends outward from the liquid reactant outlet fitting to remove liquid reactant from the vessel, and the liquid reactant discharge line controls one or more liquid reactant flows therein to control the flow of liquid reactant therethrough. Optionally embed valve.

The liquid phase reactant distribution device also includes a liquid phase reactant discharge line in fluid communication with the vaporization device, the vaporization device in flow communication with the vapor phase deposition system, and the deposition system in atomic layer deposition with the chemical vapor deposition system. Is selected from the system.

In addition, the liquid reactant distribution device,

A deposition chamber,

Liquid reactant discharge line,

A carrier gas supply line,

A gaseous reactant discharge line,

Heatable susceptor,

A waste discharge line,

The deposition chamber is selected from a chemical vapor deposition chamber and an atomic layer deposition chamber,

The liquid reactant discharge line connects a liquid reactant distribution device to the vaporization device,

A portion of the vaporization device has a carrier gas supply inlet opening, through which the carrier gas is supplied to the vaporization device to produce vapor phase reactants by incorporating vapor of a liquid reactant into the carrier gas. ,

A portion of the vaporization device has a gaseous reactant outlet opening through which the gaseous reactant can be discharged from the vaporization device,

The carrier gas supply line extends from the carrier gas supply inlet opening outwardly from the vaporization device to deliver carrier gas to the vaporizer, and a carrier gas flow control valve to control the flow of carrier gas through the carrier gas supply line. Inside,

The vapor phase reactant discharge line extends from the vapor phase reactant outward from the vapor phase reactant outlet opening to remove vapor phase reactant from the vaporization device to the deposition chamber, and the vapor phase reactant discharge line flows through the vapor phase reactant discharge line. A gaseous reactant flow control valve therein to control the

The heatable susceptor is included in a deposition chamber and located in a receiving relationship with the vaporization apparatus,

The waste discharge line is connected to the deposition chamber,

Accordingly, the gaseous reactant enters the deposition chamber via the gaseous reactant discharge line and contacts the substrate on the heatable susceptor, and the remaining waste is discharged through the waste discharge line.

 The substrate is composed of a metal selected from metals, metal silicides, metal carbides, metal nitrides, semiconductors, insulators and barrier materials. The substrate is preferably a pattern wafer.

As mentioned above, the present invention relates to a method for delivering a vapor phase reactant to a deposition chamber,

Providing a gas phase reactant dispensing apparatus, the dispensing apparatus

Courage,

With the adapter,

Fastening means,

A carrier gas supply line,

A gaseous reactant discharge line,

The vessel comprises an upper wall member, a sidewall member and a lower wall member, configured to form an inner vessel compartment that maintains source chemical at a fill level and further form an internal gas space above the fill level,

The top wall member having a first end face seal port opening, a second end face seal port opening, and optionally one or more other end face seal port openings,

A carrier gas supply inlet fitting is connected to the first end seal port opening;

The adapter includes a first end seal port opening and a metal end seal gasket coupled to a tube extending through the internal gas space to the source chemical, through which the carrier gas bubbles and flows into the source chemical. At least a portion of the source chemical vapor may be incorporated into the carrier gas to cause a flow of gaseous reactants into the interior gas space above the fill level, the tube being connected to the inlet end and the bottom wall member adjacent the first end seal port opening. With an adjacent outlet end,

The first end seal port opening and the carrier gas supply inlet fitting have opposing surfaces, the opposing surfaces not contacting each other,

The metal end seal gasket is in contact with the first end seal port opening and opposing surfaces of the carrier gas supply inlet fitting,

The fastening means secures the carrier gas supply inlet fitting to the first end face seal port opening through the metal end face seal gasket and the opposing surfaces,

The carrier gas supply line extends outward from the carrier gas supply inlet fitting to deliver carrier gas to the source chemical, and at least one carrier gas flow control valve to control the flow of carrier gas through the carrier gas supply line. Inside,

A gaseous reactant outlet fitting is connected to the second end seal port opening, through which the gaseous reactant can be dispensed from the apparatus,

The gaseous reactant discharge line extends outward from the gaseous reactant outlet fitting to remove gaseous reactants from the internal gas space above the fill level, and the gaseous reactant discharge line controls the flow of gaseous reactants through the gaseous reactant discharge line. Providing a vapor phase reactant distribution device, optionally including one or more vapor phase reactant flow control valves therein, for

Adding a source chemical to the gas phase reactant distribution device;

Heating the source chemical in the gaseous reactant dispensing device to a temperature capable of evaporating the source chemical to provide a gaseous reactant;

Supplying a carrier gas to the gaseous reactant distribution device through the tube and the carrier gas supply line;

Recovering gaseous reactant and carrier gas from the gaseous reactant distribution device through the gaseous reactant discharge line;

Supplying a gaseous reactant and a carrier gas to the deposition chamber.

In addition, the method,

Contacting the vapor phase reactant with the substrate in a deposition chamber, on a selectively heatable susceptor,

And discharging all residual waste through a waste discharge line connected to the deposition chamber. The deposition chamber may be selected from chemical vapor deposition chambers and atomic layer deposition chambers.

In operation of the system described above, the source chemical is placed in a vessel and heated to a sufficient temperature, whereby the source chemical is evaporated. The carrier gas flows through the carrier gas supply line and the bubble tube to the carrier gas inlet opening, from which the carrier gas bubbles into the source chemical. The carrier gas flow control valve controls the flow of carrier gas exiting the source chemical. Vapor from the source chemical is incorporated into the carrier gas to produce a gaseous reactant.

The gaseous reactant exits the internal gas space through the gaseous reactant outlet opening and the gaseous reactant discharge line. The gaseous reactant flows from the gaseous reactant discharge line to the deposition chamber. The gas phase reactant flow control valve controls the flow of gaseous reactants flowing into the deposition chamber. In the deposition chamber vapor phase reactants are deposited on a wafer or other substrate element mounted to a heatable substrate or other mounting structure. It is discharged from the waste discharge line from the deposition chamber. Waste vapors can be moved to recycling, recovery, waste treatment, disposal, or other deposition means.

During this operation, the source chemical fill level in the vessel is sensed by the source chemical level sensor. At the end of a chemical vapor deposition or atomic layer deposition cycle, it is important to know when the liquid precursor chemical in the vessel is running out to change. The source chemical level is gradually attenuated and consequently lowered into the sump cavity to the minimum liquid head (liquid height in the sump cavity), at which point the central processing unit senses the source chemical level signal correspondingly to the sensed source chemical level signal. Receive via signal transmission line. In response, the central processing unit transmits a control signal from the control signal transmission line to the carrier gas flow control valve to close the valve and block the flow of the carrier gas into the vessel, and simultaneously control signal from the control signal transmission line. Transfer to close the gaseous reactant flow control valve and block the flow of gaseous reactant from the vessel.

In addition, the temperature of the source chemical in the vessel during this operation is sensed by the temperature sensor. It is important to sense the temperature of the liquid precursor chemical in the vessel to control the vapor pressure. If the temperature of the source chemical of the vessel is too high, the central processing unit receives the correspondingly sensed temperature signal via a temperature sensing signal transmission line. The central processing unit transmits the control signal to the heating means in the control signal transmission line to correspondingly lower the temperature.

The gaseous reactant distribution device, i.e., the bubbler, of the present invention may be useful for vaporizing liquid and solid materials, i.e., the body and solid source reactants used in chemical vapor deposition, atomic layer deposition, and ion implantation processes. have. See, eg, US Pat. No. 7,077,388 B2.

As mentioned above, part of the present invention relates to a method for delivering a vapor phase reactant to a deposition chamber,

Providing a liquid phase reagent dispensing apparatus, wherein the dispensing apparatus

Courage,

With the adapter,

Fastening means,

An inert gas supply line,

A liquid reactant discharge line,

The vessel comprises an upper wall member, a sidewall member and a lower wall member, configured to form an inner vessel compartment that maintains source chemical at a fill level and further form an internal gas space above the fill level,

The top wall member having a first end face seal port opening, a second end face seal port opening, and optionally one or more other end face seal port openings,

An inert gas supply inlet fitting is connected to the first end seal port opening and an inert gas is supplied into the internal gas space above the fill level through the first end seal port opening to pressurize the internal gas space above the fill level. And

A liquid reactant outlet fitting is connected to the second end seal port opening;

The adapter includes a metal end seal gasket coupled to a tube extending through the second end seal port opening and the internal gas space to the source chemical, through which the liquid reactant can be dispensed from the device, and The tube has an outlet end adjacent the second end face seal port opening and an inlet end adjacent the bottom wall member,

The second end seal port opening and the liquid reactant outlet fitting have opposing surfaces, the opposing surfaces not contacting each other,

The metal end seal gasket is in contact with the second end seal port opening and opposing surfaces of the liquid reactant outlet fitting,

The fastening means secures a liquid reactant outlet fitting to the second end seal port opening through the metal end face seal gasket and the opposing surfaces,

The inert gas supply line extends outward from the inert gas supply inlet fitting to deliver an inert gas to the internal gas space above the fill level and at least one inert to control the flow of inert gas through the inert gas supply line. It includes a gas flow control valve therein,

The liquid reactant discharge line extends outward from the liquid reactant outlet fitting to remove the liquid reactant from the vessel, and the liquid reactant discharge line extends one or more liquid reactants to control the flow of the liquid reactant through the liquid reactant discharge line. Providing a liquid phase reactant dispensing device, optionally including a flow control valve therein;

Adding a liquid reactant to the liquid reactant distribution device;

Selectively heating the solid source chemical in the liquid reactant distribution device to a temperature capable of dissolving the solid source chemical to provide a liquid reactant;

Supplying an inert gas to the liquid reactant distribution device through the inert gas supply line;

Recovering a liquid reactant from the liquid reactant distribution device through the tube and the liquid reactant discharge line;

Providing a vaporization device, the vaporization device

Courage,

A carrier gas supply line,

A gaseous reactant discharge line,

The vessel is configured to form an inner vessel compartment for vaporizing the liquid reactant,

The liquid reactant discharge line connects a liquid reactant distribution device to the vaporization device,

A portion of the vaporization device has a carrier gas supply inlet opening, through which the carrier gas is supplied to the vaporization device to produce vapor phase reactants by incorporating vapor of a liquid reactant into the carrier gas. ,

A portion of the vaporization device having a gaseous reactant outlet opening through which the gaseous reactant can be dispensed from the vaporization device,

The carrier gas supply line extends from the carrier gas supply inlet opening outwardly from the vaporization device to deliver carrier gas to the vaporization device, and at least one carrier gas flow to control the flow of carrier gas through the carrier gas supply line. Has a control valve inside,

The vapor phase reactant discharge line extends from the vapor phase reactant outward from the vapor phase reactant outlet opening to remove vapor phase reactant from the vaporization device to the deposition chamber, and the vapor phase reactant discharge line flows through the vapor phase reactant discharge line. Providing one or more vapor phase reactant flow control valves therein to selectively control the vaporization apparatus;

Supplying a liquid reactant to the vaporization apparatus;

Heating the liquid reactant in the vaporization apparatus to a temperature capable of evaporating the liquid reactant to provide a gaseous reactant;

Supplying a carrier gas to the vaporization apparatus through the carrier gas supply line;

Recovering gaseous reactant and carrier gas from the vaporization apparatus through the gaseous reactant discharge line;

A method of sending a gaseous reactant to a deposition chamber, comprising supplying a gaseous reactant and a carrier gas to the deposition chamber.

In addition, the method,

Contacting a vapor phase reactant with a substrate in a deposition chamber, optionally on said heatable susceptor,

And discharging all residual waste through a waste discharge line connected to the deposition chamber. The deposition chamber may be selected from chemical vapor deposition chambers and atomic layer deposition chambers.

In operation of the system described above, the source chemical is located in the vessel and the inert gas flows through the inert gas supply line to the inert gas supply inlet opening and into the internal gas space above the fill level to pressurize the internal gas space above the fill level. Will flow. An inert gas flow control valve controls the flow of inert gas discharged into the internal gas space above the fill level.

The liquid reactant exits the vessel through the liquid reactant outlet opening (ie, dip tube) and the liquid reactant discharge line. The liquid reactant flows from the liquid reactant discharge line to the vaporization apparatus. The liquid phase reactant flow control valve controls the flow of the liquid phase reactant flowing to the vaporization device.

In the vaporization apparatus, the liquid phase reactant is vaporized to form source vapors for subsequent vapor deposition operations. The vaporization apparatus may also contain a carrier gas that binds or shrouds with the source vapors produced by vaporization of the liquid phase reactants. Alternatively, the source vapor may flow in downstream form in a downstream vapor deposition operation. In all cases the source vapors from the vaporization apparatus flow through the vapor phase reactant discharge line to the deposition chamber. In the deposition chamber, vapor phase reactants are deposited on a wafer or other substrate element that is mounted to a heatable substrate or other mounting structure. Waste steam from the deposition chamber is discharged in the waste discharge line. Waste may be moved to recycling, recovery, waste disposal, disposal or other deposition means.

During this operation, the source chemical fill level in the vessel is sensed by the source chemical level sensor. At the end of the chemical vapor deposition or atomic layer deposition cycle, it is important to know when the liquid precursor chemical in the vessel is being exhausted to change. The source chemical level is gradually attenuated and consequently lowered into the sump cavity to the minimum liquid head (liquid height in the sump cavity), at which point the central processing unit senses the source chemical level signal correspondingly to the sensed source chemical level signal. Receive via signal transmission line. In response, the central processing unit transmits a control signal from the control signal transmission line to the carrier gas flow control valve to close the valve and block the flow of the carrier gas to the vessel, and simultaneously transmits the control signal from the control signal transmission line. Thereby closing the liquid reactant flow control valve and blocking the flow of liquid reactant from the vessel.

In addition, the temperature of the source chemical in the vessel during this operation is sensed by the temperature sensor. It is important to monitor the temperature of the liquid precursor chemical in the vessel to control the vapor pressure. If the temperature of the source chemical of the vessel is too high, the central processing unit receives the correspondingly sensed temperature signal via a temperature sensing signal transmission line. The central processing unit transmits the control signal to the heating means in the control signal transmission line to correspondingly lower the temperature.

The liquid reactant dispensing apparatus of the present invention may be useful for dispensing reactants such as precursors used in chemical vapor deposition, atomic layer deposition, and ion implantation processes, and achieve high levels of recovery of liquid reactants from the vessel. . See, for example, US Pat. No. 6,077,356.

In another embodiment, part of the invention is a method for delivering a vapor phase reactant to a deposition chamber,

Providing a gas phase reactant dispensing apparatus, the dispensing apparatus

Courage,

End seal with T-type fittings,

With seal gasket at the end,

Fastening means for securing the end seal T-shaped fitting,

With the adapter,

Fastening means for securing the carrier gas supply inlet fitting,

Annular space,

A carrier gas supply line,

A gaseous reactant discharge line,

The vessel comprises an upper wall member, a sidewall member and a lower wall member, configured to form an inner vessel compartment that maintains source chemical at a fill level and further form an internal gas space above the fill level,

The top wall member has an end face seal port opening and optionally one or more other end face seal port openings,

The end seal T-shaped fitting has an end seal opening, a carrier gas supply inlet opening and a gaseous reactant outlet opening,

The end seal port opening has the end seal T-shaped fitting connected to the end seal port opening through an end seal opening, the end seal port opening and the end seal opening have opposing surfaces, and the opposing surfaces Do not touch each other,

The end seal gasket, for example the end seal gasket of metal, is in contact with and aligned with the opposing surfaces of the end seal port opening and the end seal opening,

Fastening means for securing the end seal T-shaped fitting secures the end seal T-shaped fitting to the end seal port opening through opposing surfaces and the end seal gasket,

The adapter includes a carrier gas supply inlet opening, an end seal opening, an end seal port opening, and a metal end seal gasket coupled to a tube extending through the internal gas space to the source chemical, through which the carrier gas is introduced. Foaming into the source chemical may flow into the carrier gas such that at least a portion of the source chemical vapor is incorporated into the carrier gas to cause the flow of gaseous reactants into the internal gas space above the fill level, and the tube passes through the carrier gas supply inlet opening. Having an inlet end adjacent to and an outlet end adjacent to the lower wall member,

A carrier gas supply inlet fitting is attached to the carrier gas supply inlet opening,

The carrier gas supply inlet opening and the carrier gas supply inlet fitting have opposing surfaces, the opposing surfaces not contacting each other,

The metal end seal gasket is in contact with the carrier gas supply inlet opening and the opposing surfaces of the carrier gas supply inlet fitting,

The fastening means for securing the carrier gas supply inlet fitting secures the carrier gas supply inlet fitting to the carrier gas supply inlet opening via opposing surfaces and the metal end seal gasket,

The annular space is a space between the outer wall of the tube and the carrier gas supply inlet opening, the end face seal opening and the inner wall of the end face seal port opening, through which the gaseous reactant passes through the gas phase reactant outlet opening. Can be dispensed from the device,

The carrier gas supply line extends outward from the carrier gas supply inlet fitting to deliver carrier gas to the source chemical, and at least one carrier gas flow control valve to control the flow of carrier gas through the carrier gas supply line. Inside,

The gaseous reactant discharge line extends outward from the gaseous reactant outlet opening to remove gaseous reactants from the internal gas space above the fill level, and the gaseous reactant discharge line controls the flow of gaseous reactants through the gaseous reactant discharge line. Providing a vapor phase reactant distribution device, optionally including one or more vapor phase reactant flow control valves therein, for

Adding a source chemical to the gas phase reactant distribution device;

Heating the source chemical in the gaseous reactant dispensing device to a temperature capable of evaporating the source chemical to provide a gaseous reactant;

Supplying a carrier gas to the gaseous reactant distribution device through the tube and the carrier gas supply line;

Recovering gaseous reactant and carrier gas from the gaseous reactant distribution device through the gaseous reactant discharge line;

It relates to a method for sending a gaseous reactant to the deposition chamber, comprising supplying a gaseous reactant and a carrier gas to the deposition chamber.

In addition, this method,

Contacting a vapor phase reactant with a substrate in a deposition chamber, optionally on said heatable susceptor,

And discharging all residual waste through a waste discharge line connected to the deposition chamber.

In addition, the gas phase reactant distribution device in the above method includes a gaseous reactant discharge line in flow communication with the gaseous reactant deposition system, wherein the deposition system is selected from a chemical vapor deposition system or an atomic layer deposition system.

In another embodiment, part of the invention is directed to a method for delivering a vapor phase reactant to a deposition chamber,

Providing a liquid phase reagent dispensing apparatus, wherein the dispensing apparatus

Courage,

End seal with T-type fittings,

With seal gasket at the end,

Fastening means for securing the end seal T-shaped fitting,

With the adapter,

Fastening means for securing the liquid reactant outlet fitting,

Annular space,

An inert gas supply line,

A liquid reactant discharge line,

The vessel comprises an upper wall member, a sidewall member and a lower wall member, configured to form an inner vessel compartment that maintains source chemical at a fill level and further form an internal gas space above the fill level,

The top wall member has an end face seal port opening and optionally one or more other end face seal port openings,

The end seal T-shaped fitting has an end seal opening, an inert gas supply inlet opening and a liquid reactant outlet opening,

The end seal port opening has the end seal T-shaped fitting connected through an end seal opening, the end seal port opening and the end seal opening have opposing surfaces, the opposing surfaces not contacting each other,

The end face seal gasket, for example an end face gasket of metal, is in contact with the end seal port opening and in opposing surfaces of the end face seal opening,

Fastening means for securing the end seal T-shaped fitting secures the end seal T-shaped fitting to the end seal port opening through the end seal gasket and opposing surfaces,

The adapter includes a metal end seal gasket coupled to a tube extending into the source chemical through the liquid reactant outlet opening, the end seal opening, the end seal port opening, and the internal gas space, through which the liquid reactant is deposited. Wherein the tube has an outlet end adjacent to the liquid reactant outlet opening and an inlet end adjacent to the bottom wall member,

The liquid phase reactant outlet opening is connected to a liquid phase reactant outlet fitting,

The liquid reactant outlet opening and the liquid reactant outlet fitting have opposing surfaces, the opposing surfaces not contacting each other,

The metal end seal gasket is in contact with the opposing surfaces of the liquid reactant outlet opening and the liquid reactant outlet fitting,

Fastening means for securing the liquid reactant outlet fitting secures the liquid reactant outlet fitting to the liquid reactant outlet opening through the metal end face gasket and opposing surfaces,

The annular space is a space between the outer wall of the tube and the liquid reactant outlet opening, the end seal opening and the inner wall of the end seal port opening, through which the inert gas flows into an internal gas space above the fill level. Can be fed through a feed inlet opening to pressurize the internal gas space above the fill level,

The inert gas supply line extends outward from the inert gas supply inlet opening to deliver an inert gas to the internal gas space above the fill level and at least one inert to control the flow of inert gas through the inert gas supply line. It includes a gas flow control valve therein,

The liquid reactant discharge line extends outward from the liquid reactant outlet fitting to remove liquid reactant from the vessel, and the liquid reactant discharge line extends one or more liquid phases to control the flow of the liquid reactant through the liquid reactant discharge line. Providing a liquid phase reactant dispensing device, optionally including a reactant flow control valve therein;

Adding a liquid reactant to the liquid reactant distribution device;

Selectively heating the solid source chemical in the liquid reactant distribution device to a temperature capable of dissolving the solid source chemical to provide a liquid reactant;

Supplying an inert gas to the liquid reactant distribution device through the inert gas supply line;

Recovering a liquid reactant from the liquid reactant distribution device through the tube and the liquid reactant discharge line;

Providing a vaporization device, the vaporization device

Courage,

A carrier gas supply line,

A gaseous reactant discharge line,

The vessel is configured to form an inner vessel compartment for vaporizing the liquid reactant,

The liquid reactant discharge line connects a liquid reactant distribution device to the vaporization device,

A portion of the vaporization device has a carrier gas supply inlet opening, through which the carrier gas can be supplied to the vaporization device to produce vapor phase reactants by incorporating vapor of a liquid reactant into the carrier gas. ,

A portion of the vaporization device having a gaseous reactant outlet opening through which the gaseous reactant can be dispensed from the vaporization device,

The carrier gas supply line extends from the carrier gas supply inlet opening outwardly from the vaporization device to deliver carrier gas to the vaporization device, and at least one carrier gas flow to control the flow of carrier gas through the carrier gas supply line. Has a control valve inside,

The vapor phase reactant discharge line extends from the vapor phase reactant outward from the vapor phase reactant outlet opening to remove vapor phase reactant from the vaporization device to the deposition chamber, and the vapor phase reactant discharge line flows through the vapor phase reactant discharge line. Providing one or more vapor phase reactant flow control valves therein to selectively control the vaporization apparatus;

Supplying a liquid reactant to the vaporization apparatus;

Heating the liquid reactant in the vaporization apparatus to a temperature capable of evaporating the liquid reactant to provide a gaseous reactant;

Supplying a carrier gas to the vaporization apparatus through the carrier gas supply line;

Recovering gaseous reactant and carrier gas from the vaporization apparatus through the gaseous reactant discharge line;

Supplying a gaseous reactant and a carrier gas to the deposition chamber.

In addition, the method,

Contacting the vapor phase reactant with the substrate in a deposition chamber, on a selectively heatable susceptor,

Exhausting all residual waste through a waste discharge line connected to the deposition chamber.

In the method, the liquid reactant distribution device further comprises a liquid reactant discharge line in fluid communication with the vaporization device, wherein the vaporization device is in gaseous reactant flow communication with the vapor delivery deposition system, the deposition system being Chemical vapor deposition systems and atomic layer deposition systems.

In one embodiment of the invention, organometallic compounds are used in vapor deposition techniques to form powders, films or coatings. The compound may be used as a single source precursor or may be used with steam generated by heating one or more other precursors, such as one or more other organometallic compounds or metal complexes.

Deposition can be performed when other gas phase components are present. In one embodiment of the invention, film deposition is performed when one or more inert carrier gases are present. Examples of inert gases include inert gases such as nitrogen, argon, helium as well as other gases that do not react with the organometallic compound precursor under process conditions. In another embodiment, film deposition is performed when one or more reactive gases are present. Some of the reactive gases that can be used include, but are not limited to, hydrazine, oxygen, hydrogen, air, oxygen rich air, ozone (O ₃ ), nitrous oxide (N ₂ O), water vapor, organic vapors, ammonia, and the like. It doesn't work. As is known in the art, the presence of oxidizing gases such as, for example, air, oxygen, oxygen rich air, O ₃ , N ₂ O, or vapors of oxidized organic compounds, promotes the formation of metal oxide films.

The deposition method described in the present invention may be performed to form a film, powder, or coating comprising a single metal, or a film, powder, or coating comprising a single metal oxide. In addition, mixed films, powders or coatings may be deposited, for example, with mixed metal oxide films. Mixed metal oxide films can be formed, for example, by using various organometallic precursors, at least one of which is selected from the organometallic compounds described above.

Vapor film deposition can be performed, for example, to form a film layer of a predetermined thickness in the range of 1 nm or less to 1 mm or more. The precursors described herein are particularly useful for producing thin films, such as films having a thickness in the range of about 10 nm to about 100 nm. For example, the films of the present invention may be considered to produce metal electrodes, such as capacitor electrodes and dielectric materials, particularly in n-channel metal electrodes in logic, DRAM (DRAM) applications.

In addition, the deposition method is suitable for producing a layered film, wherein two or more layers differ in state or composition. Examples of layered films include metal-insulator-semiconductor and metal-insulator-metal.

Organometallic compound precursors may be used in atomic layer deposition, chemical vapor deposition, or more particularly metalorganic chemical vapor deposition processes known in the art. For example, the aforementioned organometallic compound precursors can be used in chemical vapor deposition processes in the atmosphere, as well as chemical vapor deposition processes at low pressures. The compounds can be used in cold wall or warm wall type chemical vapor deposition, a technique in which only the substrate is heated, as well as hot wall chemical vapor deposition in which the entire reaction chamber is heated.

In addition, the aforementioned organometallic compound precursors may be used in a plasma or light assisted chemical vapor deposition process where energy from the plasma or electromagnetic energy is used to activate the chemical vapor deposition precursor, respectively. In addition, the compounds may be used in ion beam, electron beam assisted chemical vapor deposition processes, in which an ion beam or electron beam is directed to a substrate, respectively, to supply energy for decomposing a chemical vapor deposition precursor. In addition, a laser assisted chemical vapor deposition process may be used in which laser light is directed to a substrate to affect the photolysis reaction of the chemical vapor deposition precursor.

The deposition method can be performed with various chemical vapor deposition reactors, such as, for example, hot wall or cold wall reactors, plasma assisted, light assisted or laser assisted reactors as known in the art.

Exemplary substrates useful in deposition chambers include, for example, materials selected from metals, metal silicides, semiconductors, insulators, and barrier materials. Preferred substrates are pattern wafers. Examples of substrates that can be coated using the deposition method include metal substrates such as Al, Ni, Ti, Co, Pt, Ta; Metal silicides such as TiSi ₂ , CoSi ₂ , NiSi ₂ ; Semiconductor materials such as Si, SiGe, GaAs, InP, diamond, GaN, SiC; Insulators such as SiO ₂ , Si ₃ N ₄ , HfO ₂ , Ta ₂ O ₅ , Al ₂ O ₃ , barium strontium titanate (BST); Barrier materials such as solid substrates such as TiN, TaN; Or a substrate comprising a combination of these materials. In addition, films or coatings may be formed on glass, ceramics, plastics, thermoset polymer materials, and other coating or film layers. In a preferred embodiment, film deposition is on a substrate used in the manufacture or processing of electronic components. In another embodiment, the substrate is used to supply a low resistivity conductor deposition or optical transfer film that is stable when oxidant is present at high temperatures.

The deposition method can be performed to deposit a film on a substrate having a smooth flat surface. In one embodiment, the method is performed to deposit a film on a substrate used in wafer fabrication or processing. For example, it may be performed to deposit a film on a patterned substrate that includes features such as trenches, holes, or vias. In addition, the deposition method may be incorporated into other steps of wafer fabrication or processing, such as masking, etching, and the like.

The chemical vapor deposition film may be deposited to a predetermined thickness. For example, the film formed may be 1 micrometer thick or less, preferably 500 nanometers or less, more preferably 200 nanometers or less. Films up to 50 nanometers thick, such as films having a thickness between about 0.1 nanometers and 20 nanometers, can also be made.

In addition, the aforementioned organometallic compound precursors may be used in the method of the present invention to form films by atomic layer deposition or atomic layer nucleation techniques while the substrate is exposed to alternating pulses of precursors, oxidants and inert gas streams. Can be. Continuous layer deposition techniques are described, for example, in US Pat. No. 6,287,965 and US Pat. No. 6,342,277. The entire disclosure of both patents is incorporated herein by reference.

For example, in one atomic layer deposition cycle, the substrate is exposed in a sequential manner to a) an inert gas, b) an inert gas carrying a precursor vapor, c) an inert gas, d) an oxidant, alone or in combination with an inert gas. In general, each step can be as short as the equipment allows (eg, one thousandth of a second) and as long as the process requires (eg, a few seconds or minutes). The duration of one cycle can be as short as a thousandth of a second and as long as a few minutes. The cycle repeats a cycle that can range from several minutes to several hours. The film produced can be as thin as a few nanometers or as thick as, for example, one millimeter (mm).

Thus, the means and methods of the present invention provide a system for supplying and dispensing gaseous or liquid phase reactants, wherein from 95% to 98% of the volume of source chemicals originally supplied allows for use in an apparatus in which the gaseous or liquid phase reactants are selectively dispensed. Substantial advances in prior art solutions are achieved. Ease of cleaning of the two-part empoul allows for reuse of two-part empouls, superior to that obtainable in one-part empouls.

Thus, in operations such as semiconductor and superconductor production, the means and methods of the present invention reduce waste of source chemicals to levels as low as 2% to 5% of the volume originally filled into the dispensing vessel and reuse the empoules several times. To make it possible.

Thus, the process of the present invention significantly improves the economics of source chemical feed and gaseous or liquid phase reactant distribution systems, and the process in which the gaseous or liquid phase reactants being dispensed are used. In various instances, the present invention may allow for cost effective use of source chemicals, which has been a substantial problem excluded by the waste level nature of the prior art methods.

Various modifications and variations of the present invention will be apparent to those skilled in the art, and such variations and modifications may be included within the spirit and scope of the present application.

1 is a schematic diagram showing a partial cross section of a gaseous reactant dispensing device without a dip tube, a gaseous reactant dispensing device with a bubble tube, and a liquid phase reactant dispensing device with a dip tube.

2 is a schematic representation of a cross section of an adapter (ie, metal end seal gasket and tube).

3 is a schematic view showing a cross section of a single port vessel transformed into a dual port vessel with a tube.

4 is a schematic diagram illustrating a cross section of a component that may be used to assemble a metal end seal gasket connection without an adapter.

5 is a schematic diagram showing a cross section of a component that may be used to assemble a metal end face seal gasket connection using an adapter.

6 is a schematic diagram showing a cross section of a flow path through a metal end seal gasket connection without an adapter and a flow path through a metal end seal gasket connection using an adapter.

<Explanation of symbols for the main parts of the drawings>

100: end seal fitting

101: sealing bead

110: end seal fitting

111: sealing bead

120: gasket

130: male nut

140: female nut

150: connection assembly

200: end face seal fitting

201: sealing bead

210: end seal fitting

211: sealing bead

220: adapter

230: male nut

240: female nut

250: connection assembly

Claims (10)

A method for sending a vapor phase reactant into a deposition chamber, (a) providing a gaseous reactant dispensing apparatus, wherein the dispensing apparatus Courage, With the adapter, Fastening means, A carrier gas supply line, A gaseous reactant discharge line, The vessel comprises an upper wall member, a sidewall member and a lower wall member, configured to form an inner vessel compartment that maintains source chemical at a fill level and further form an internal gas space above the fill level, The top wall member having a first end face seal port opening, a second end face seal port opening, and optionally one or more other end face seal port openings, A carrier gas supply inlet fitting is connected to the first end seal port opening; The adapter includes a first end seal port opening and a metal end seal gasket coupled to a tube extending through the internal gas space to the source chemical, through which the carrier gas bubbles and flows into the source chemical. At least a portion of the source chemical vapor may be incorporated into the carrier gas to cause a flow of gaseous reactants into the interior gas space above the fill level, the tube being connected to the inlet end and the bottom wall member adjacent the first end seal port opening. With an adjacent outlet end, The first end seal port opening and the carrier gas supply inlet fitting have opposing surfaces, the opposing surfaces not contacting each other, The metal end seal gasket is in contact with the first end seal port opening and opposing surfaces of the carrier gas supply inlet fitting, The fastening means secures the carrier gas supply inlet fitting to the first end face seal port opening through the metal end face seal gasket and the opposing surfaces, The carrier gas supply line extends outward from the carrier gas supply inlet fitting to deliver carrier gas to the source chemical, and at least one carrier gas flow control valve to control the flow of carrier gas through the carrier gas supply line. Inside, A gaseous reactant outlet fitting is connected to the second end seal port opening, through which the gaseous reactant can be dispensed from the apparatus, The gaseous reactant discharge line extends outward from the gaseous reactant outlet fitting to remove gaseous reactants from the internal gas space above the fill level, and the gaseous reactant discharge line controls the flow of gaseous reactants through the gaseous reactant discharge line. Providing a vapor phase reactant distribution device, optionally including one or more vapor phase reactant flow control valves therein, for (b) adding a source chemical to the gaseous reactant distribution device, (c) heating the source chemical in the gaseous reactant distribution device to a temperature capable of evaporating the source chemical to provide a gaseous reactant, (d) supplying carrier gas to the gaseous reactant distribution device through the tube and the carrier gas supply line; (e) recovering gaseous reactant and carrier gas from the gaseous reactant distribution device via the gaseous reactant discharge line; (f) supplying a gaseous reactant and a carrier gas to the deposition chamber. A method of delivering a vapor phase reactant to a deposition chamber. The method of claim 1, (g) contacting a vapor phase reactant with a substrate in a deposition chamber, optionally on said heatable susceptor, (h) further discharging all residual waste through a waste discharge line connected to the deposition chamber; A method of delivering a vapor phase reactant to a deposition chamber. The method of claim 1, The deposition chamber is selected from a chemical vapor deposition chamber and an atomic layer deposition chamber. A method of delivering a vapor phase reactant to a deposition chamber. The method of claim 2, The substrate is comprised of a material selected from metals, metal silicides, metal carbides, metal nitrides, semiconductors, insulators and barrier materials A method of delivering a vapor phase reactant to a deposition chamber. The method of claim 2, The substrate is a pattern wafer A method of delivering a vapor phase reactant to a deposition chamber. The method of claim 1, In the gas phase reactant distribution device the vessel is made of stainless steel. A method of delivering a vapor phase reactant to a deposition chamber. The method of claim 1, The tube comprises a bubble tube and is made of stainless steel A method of delivering a vapor phase reactant to a deposition chamber. The method of claim 1, The fastening means in the gas phase reactant dispensing device comprises a coupling of a male nut or body hex to a female nut. A method of delivering a vapor phase reactant to a deposition chamber. The method of claim 1, The lower wall member has a sump cavity extending therefrom extending downward from the surface of the lower wall member. A method of delivering a vapor phase reactant to a deposition chamber. The method of claim 9, The gas phase reactant distribution device, A temperature sensor extending substantially vertically downward from the top wall member through the internal gas space to the source chemical, the lower end being incoherently located proximate to the surface of the sump cavity; And further comprising a source chemical level sensor extending from the third end seal port opening of the top wall member through the internal gas space generally vertically downwards, the lower end being incoherently adjacent to the surface of the sump cavity. , The temperature sensor is operatively disposed in the vessel to measure the temperature of the source chemical in the vessel, the source chemical level sensor is operatively disposed in the vessel to measure the level of the source chemical in the vessel, The temperature sensor and the source chemical level sensor are incoherently and incoherently adjacent to each other in the vessel, the lower end of the temperature sensor being close to the surface of the sump cavity equally or closer to the lower end of the source chemical level sensor. And the temperature sensor and source chemical level sensor are in source chemical flow communication within the vessel. A method of delivering a vapor phase reactant to a deposition chamber.

Images