CN1924086A - Liquid-conveying metallorganics chemical vapour deposition apparatus - Google Patents

Liquid-conveying metallorganics chemical vapour deposition apparatus Download PDF

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CN1924086A
CN1924086A CN 200610104630 CN200610104630A CN1924086A CN 1924086 A CN1924086 A CN 1924086A CN 200610104630 CN200610104630 CN 200610104630 CN 200610104630 A CN200610104630 A CN 200610104630A CN 1924086 A CN1924086 A CN 1924086A
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liquid
gas
valve
reaction chamber
assembly
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CN100482858C (en
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刘卫国
周顺
高爱华
张伟
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Xian Technological University
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Xian Technological University
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Abstract

The invention discloses a metal organic chemical gas-phase sedimentary equipment transmitted by liquid, which comprises the following parts: multi-element gasifying component, reacting chamber, RF discharge plasmid, vacuum component, operational prevention and draining disposing component and electric control component, wherein the multi-element gasifying component is composed of multi-path liquid transmission channels, two-path gas transmission channel, atomizer, carburetor, valve and pipe; the liquid is atomized and carbureted, which is transmitted into reacting chamber to react with gas to produce needed oxide; the sediment forms film on the substrate, whose temperature is controllable; the electric control component realizes self-control of whole technology through programmable controller PLC.

Description

Liquid-conveying metallorganics chemical vapour deposition apparatus
Technical field
The invention belongs to chemical vapor deposition growing technology field, specifically is a kind of liquid-conveying metallorganics chemical vapour deposition apparatus.
Background technology
Metal organic-matter chemical gas deposition (Metal Organic Chemical Vapor Deposition, be called for short MOCVD), it is a technology of preparation high quality epitaxial film, prepared epitaxial film is mainly used in photoelectricity, semi-conductor and microwave device, and also the technology with the preparation VLSI (very large scale integrated circuit) chip is relevant.Since 20th century, proposed the sixties first, development through the seventies to the eighties, become the core growth technology of photoelectron material epitaxial wafer preparations such as gallium arsenide, indium phosphide the nineties, particularly prepared the main stream approach of gallium nitride light-emitting diode and laser apparatus epitaxial wafer.Up to the present, also there is not other method can be by comparison from the gallium nitride epitaxial slice of growth and leading indicators such as the performance of device and production cost.Simultaneously, the MOCVD technology also is widely used in the preparation of function metal oxide film, as superconducting thin film, ferroelectric membranc etc.The MOCVD deposition that contains lead ferroelectric film has progressively become one of main flow direction of preparation of industrialization ferroelectric membranc from now on.
With mocvd method deposited iron conductive film, has high stability of molecule under the vapour pressure of selected metallorganics Ying Zaigao, to avoid the decomposition in the course of conveying.In the MOCVD of function metal oxide technology, the MO source of component elder generation body is different from hydride and first, the ethyl organic compound in the semi-conductor MOCVD technology, adopts metal alkoxide and metal-liquid state and solid matters such as diketone inner complex usually.
Because the component complexity of some function metal oxides, the liquid MO source material that respective element is difficult to synthesize gaseous state MO source and higher vapor pressure is arranged, and steam forces down, the MO source of poor heat stability elder generation body, can not be transported to reaction chamber by gas of carrier gas by bubbler (bubbler).This just makes traditional MOCVD technology can not prepare above-mentioned metal oxide film, more can not prepare the film of differing materials simultaneously.Be example with traditional gaseous source MOCVD equipment deposition pzt thin film now, first body commonly used is Pb (TMHD) 2, Ti[OCH (CH 3) 2] 4, Zr[OC (CH 3) 3] 4, its vapour pressure is respectively 6.65Pa, 665Pa, 133Pa, and as seen their vapour pressure deficit is bigger, and this just makes the obstacle that equipment is restive and cause conveying.
Source material is required harshness, and this has restricted the development of the MOCVD technology of metal oxide to a great extent.
The application for a patent for invention communication type multi-reaction chamber high temperature mocvd device of Chinese patent 200410065874.1, though having overcome same MOCVD equipment, it can only be used for growing with a kind of defective of thin-film material of series, but this equipment remains a kind of traditional gaseous source MOCVD equipment, it is had relatively high expectations to source material, needs MO source elder generation body to have higher vapour pressure, good thermostability.
Publication number is that the patent application of CN1377991A is ZnO film growth MOCVD equipment and a technology thereof, can improve ZnO film growth quality and homogeneity and help the P type or the adulterated advantage of high resistant though have, this equipment equally to the requirement of source material than higher.
Why saying that above background technology is traditional gaseous source MOCVD equipment, is that what carry in the transport pipe is gas because they all are that the source is transported to reaction chamber in the gasiform mode, and flow control also is the flow of the gas of control.This mode just makes MO source elder generation body must possess vapour pressure height, the good characteristics of thermostability, is the thing of comparison difficulty and prepare for desire that some function metal oxide films go to seek suitable MO source elder generation body.
Project team of the present invention finds report or the document closely related and the same with the present invention more as yet to domestic and international patent documentation and the journal article retrieval of publishing.
Summary of the invention
The objective of the invention is to overcome the shortcoming of above-mentioned technology or equipment existence, having solved traditional MOCVD equipment exists vapour pressure deficit between the gaseous source MOCVD differing materials to be difficult to greatly to control and the problem of the obstacle carried, source material is required to reduce, be convenient to realize the alternating deposit of multiple film in the metal oxide film.Provide a kind of film, the acquisition accurate film of component and multi-component film that can obtain superstructure, the film quality height; Can realize the deposition of ferroelectric membranc, superconducting thin film and oxide electrode film, the liquid-conveying metallorganics chemical vapour deposition apparatus of automation degree of equipment height, compact construction.
Below technical scheme of the present invention is elaborated
Realization of the present invention is liquid-conveying metallorganics chemical vapour deposition apparatus, include reaction chamber assembly, the rf (discharge) plasma assembly, vacuum subassembly, operation protection and emission treatment assembly, electrically-controlled component, the rf (discharge) plasma assembly is connected on the electrode of reaction chamber assembly gas distribution box by output electrode, the gas output tube road of reaction chamber assembly is connected on the operated pneumatic valve of vacuum subassembly, the waste gas output channel of vacuum subassembly is directly connected to the emission-control equipment of operation protection and emission treatment assembly, it is characterized in that: total equipment also includes polynary vaporization component, polynary vaporization component is removable integration assembly, mainly by multichannel liquid source transfer passage, the two-way gas delivery channels, spraying gun, vaporizer, valve and pipeline constitute, spraying gun wherein is in the vaporizer top, the sealing of employing sealing-ring, carburetor structure is cylindric, be welded with pipe fitting on the sidewall of cylinder middle and upper part, the pipe fitting that passes through of the mixed gas of carrier gas and reactant gases enters vaporizer; The formation of liquid source transfer passage is identical, liquid source is the MO source, the liquid transfer passage of single channel is equipped with the MO source container successively by the liquid input direction, magnetic valve, transferpump, back pressure valve, electromagnet cut off valve, the output of the end electromagnet cut off valve of the transfer passage of each road liquid source is divided into two-way again after merging by adaptor, the electromagnet cut off valve of leading up to is received operation protection and emission treatment assembly, spraying gun is received by electromagnet cut off valve in another road, and the liquid that is transferred is transported to reaction chamber assembly with carrier gas and the mixed total gas of reactant gases by corrugated tube after atomizing and vaporization; Vaporizer has well heater, and pipe fitting has well heater, and the electrically-controlled component that has programmable touch screen is connected with each construction components circuit, adopts programmable logic controller PLC to constitute the core of system's control, and whole technological processs are controlled automatically.
The present invention is directed to traditional MOCVD equipment exists vapour pressure deficit between the gaseous source MOCVD differing materials to be difficult to greatly to control and the problem of the obstacle carried, be provided with polynary vaporization component, the design of the transfer passage of the multichannel liquid source of polynary vaporization component, two-way gas delivery channels, spraying gun, vaporizer etc. has fundamentally solved the complete conveying of gas-liquid attitude component and effectively control, realized deposition, can obtain accurate film of component and multi-component film high-quality ferroelectric membranc, superconducting thin film and oxide electrode film.Polynary vaporization component is vaporized certain density liquid source, utilize carrier gas to be sent to reaction chamber, in between two plate electrodes, producing plasma discharge under the electric field excitation that the rf (discharge) plasma assembly provides, generate needed oxide compound with reactant gases, be deposited on the substrate of Controllable Temperature, waste gas and unreacted matters be via vacuum system, and by operation protection and the discharging of emission treatment assembly.Vaporizer and pipe fitting have well heater.Vaporization component be made as black box conveniently replaced, clean and maintenance, realize the deposition of different thin-film materials, bigger range of application can be arranged.
Liquid source is contained in the container, and liquid supplying passage also comprises the pipeline of transferpump, valve and corresponding specification.Under the cooperation of valve, transferpump can be transported to the certain density liquid source that has that is contained in the liquid source container in the spraying gun by certain mode and speed and atomize, vaporization formation source steam in vaporizer utilizes carrier gas that source steam is sent into reaction chamber then.
Can select to allow one road liquid source passage work carry out the film preparation of accurate component, also can select to allow multichannel liquid source passage work simultaneously simultaneously and carry out the preparation of multi-component film.
Gas delivery channels is respectively carrier gas passage and reaction gas passage, and by gas meter control, the magnetic valve in the gas delivery channels is used for controlling the through and off of gas circuit respectively for carrier gas and reaction gas flow.By adaptor carrier gas path and reactant gas passage are combined into one tunnel gas passage.
Realization of the present invention is that also the vacuum subassembly of liquid-conveying metallorganics chemical vapour deposition apparatus also includes the powder catcher, the powder catcher is made up of catcher top and catcher lower section that can be for convenience detach, catcher lower section and one section stainless steel tube welding constitute an integral body, by clamp two portions about the catcher are tightened up and loose Ji, the powder catcher is a tubular structure, drum outer wall is installed with refrigerating unit, powder art catcher upper end is connected with reaction chamber assembly by gas receiver, powder catcher lower end is divided into two-way, the angle valve of leading up to is connected to dried pump, and another road is connected with lobe pump by angle valve.
The gas that comes out from reaction chamber enters from the inlet of powder catcher, after gas is run into cold wall, forms powder or liquid and falls, and residual gas is taken away by the pump group by stainless steel tube.Solved the instant discharging of unreacting substance effectively.
Realization of the present invention also is liquid-conveying metallorganics chemical vapour deposition apparatus, upper/lower electrode in the reaction chamber assembly is the adjustable distance electrode, promptly the top electrode flat board that links to each other with the rf (discharge) plasma assembly is served as by gas distribution box, the gas distribution box bottom is evenly distributed with aperture, lower electrode is made of substrate table, spacing between this two electrode adopts and increases or reduce backing plate quantity and regulates, backing plate closely contact with top electrode and thickness certain.
Interelectrode distance is made as adjustable,, can regulates the rf (discharge) plasma parameter with regard to the many links that can control.
Realization of the present invention also is: in the reaction chamber of reaction chamber assembly, the resistance heater that is imbedded in the substrate table is designed to the multiple tracks circular concentric.
Be imbedded in the resistance heater in the substrate table, resistive arrangement becomes the multiple tracks circular concentric.To guarantee the homogeneity of heating.
Realization of the present invention also is: set up butterfly valve between angle valve in the air extractor of vacuum subassembly and lobe pump inlet, gas receiver is connected with film rule and gamut rule respectively by angle valve and angle valve.
The device of setting up all is for the ease of monitoring and control.
Because the present invention has designed the liquid supplying way of liquid-conveying metallorganics chemical vapour deposition apparatus, avoided many sources of the gas to carry the complexity problem that faces, alternative method has been proposed; The transfer passage and the two-way gas delivery channels of the multichannel liquid source that is provided with, by polynary vaporization component certain density liquid source is vaporized, utilize carrier gas to be sent to the technical scheme of reaction chamber, solved the difficult problem that vapour pressure deficit is difficult to control and carry obstacle greatly between traditional gaseous source MOCVD differing materials effectively, source material is required also therefore to reduce, and can be convenient to realize the alternating deposit of multiple film.The present invention also designed polynary vaporization component structure and with the combination of whole metal organic-matter chemical vapor deposition apparatus, design and improved the structure of reaction chamber assembly, set up the powder catcher, especially the setting of spraying gun and vaporizer finished the atomizing of liquid and vaporization and with the mixing of carrier gas and reactant gases.Utilize the present invention can carry out the alternating deposit of multiple film, can realize the deposition of ferroelectric membranc, superconducting thin film and oxide electrode film, can obtain superstructure metallorganics.Can obtain accurate film of component and multi-component film.The film quality height requires to reduce to source material, total automation degree of equipment height, compact construction.
Description of drawings:
Fig. 1 is a composition synoptic diagram of the present invention;
Fig. 2 is the structural representation of present device;
Fig. 3 is a reaction chamber structure synoptic diagram of the present invention;
Fig. 4 is the structural representation of spraying gun of the present invention, vaporizer combination;
Fig. 5 is a powder catcher structure drawing of device of the present invention;
Fig. 6 is the vertical view of Fig. 5.
Embodiment:
Describe in detail below in conjunction with accompanying drawing
Embodiment 1: referring to Fig. 1, liquid-conveying metallorganics chemical vapour deposition apparatus, include reaction chamber assembly, rf (discharge) plasma assembly, vacuum subassembly, operation protection and emission treatment assembly, electrically-controlled component, the rf (discharge) plasma assembly is connected on the electrode of reaction chamber assembly gas distribution box by output electrode, the gas output tube road of reaction chamber assembly is connected on the operated pneumatic valve of vacuum subassembly, and the waste gas output channel of vacuum subassembly is directly connected to the emission-control equipment of operation protection and emission treatment assembly.Total equipment also includes polynary vaporization component 1, polynary vaporization component 1 is removable integration assembly, mainly constitute by multichannel liquid source transfer passage, two-way gas delivery channels, spraying gun 19, vaporizer 20, valve and pipeline, spraying gun 19 wherein is in vaporizer 20 tops, adopt sealing-ring 56 sealings, carburetor structure is cylindric, and the vaporizer material is a stainless steel, be welded with pipe fitting 51 on the sidewall of cylinder middle and upper part, pipe fitting 51 adopts the stainless steel polishing pipe fitting.The mixed gas 52 of carrier gas and reactant gases enters vaporizer 20 by this section pipe fitting 51; The formation of the transfer passage of liquid source is identical, liquid source is the MO source, the liquid transfer passage of single channel is equipped with MO source container, magnetic valve, transferpump, back pressure valve, electromagnet cut off valve successively by the liquid input direction, the output of the end electromagnet cut off valve of the transfer passage of each road liquid source is divided into two-way again after merging by adaptor, the electromagnet cut off valve 17 of leading up to is received operation protection and emission treatment assembly 5, and spraying gun 19 is received by electromagnet cut off valve 18 in another road; The liquid that is transferred is transported to reaction chamber assembly 2 with carrier gas and the mixed total gas 40 of reactant gases by corrugated tube after atomizing and vaporization, vaporizer 20 has well heater 54, well heater 54 is made of on every side the cylindrical wall that the heating zone is wrapped in vaporizer 20, also be wound with heating zone 50 around the stainless steel polishing pipe fitting 51, the heating zone terminals link to each other with the PLC temperature control input terminus of electrically-controlled component 6, measure temperature value and show on touch-screen; By transferpump and cooperate magnetic valve and electromagnet cut off valve carries out the conveying of liquid source and blended control.The gas delivery channels of two-way constitutes identical, one the tunnel is the carrier gas input channel, another road is the reactant gases input channel, gas passage is connected under meter 38,39, magnetic valve 36,37 successively by gas input direction, the output of magnetic valve 36,37 is combined into one road gas passage by adaptor with carrier gas passage and reaction gas passage and receives on the stainless steel polishing pipe fitting 51 of 1 li vaporizer 20 of polynary vaporization component, by gas meter 38,39 controls, magnetic valve 36,37 is used for controlling the through and off of gas circuit respectively for carrier gas and reaction gas flow.
The electrically-controlled component 6 that has programmable touch screen is connected with each construction components circuit, adopts programmable logic controller PLC to constitute the core of system's control, and whole technological processs are controlled automatically.
Whole vaporization component 1 is designed to the integration assembly, can integral replacing, realize the deposition of different thin-film materials.
With respect to traditional gaseous source MOCVD equipment, all be that the source is transported to reaction chamber in the gasiform mode, present device is that liquid source is delivered directly to reaction chamber, design has liquid to atomize to handle and the device of vaporization process, what carry in the transport pipe is liquid, and flow control also is the flow of the liquid of control.The method of utilizing liquid to carry can reduce the requirement to source material, thus the alternating deposit of the multiple film of easier realization, the deposition of realization ferroelectric membranc, superconducting thin film and oxide electrode film.
Embodiment 2: overall device is with embodiment 1, vacuum subassembly 4 of the present invention also includes powder catcher 32, powder catcher 32 is made up of catcher top 58 and catcher lower section 63 that can be for convenience detach, by 60 pairs of catchers of clamp up and down two portions tighten up and unclamp, powder catcher 32 is a tubular structure, drum outer wall is installed with refrigerating unit 66, powder catcher 32 upper ends are connected with reaction chamber assembly 2 by gas receiver 24, powder catcher 32 lower ends are divided into two-way, the DN25 angle valve 27 of leading up to is connected to dried pump 28, and another road is connected with lobe pump 29 by DN50 angle valve 31.
Refrigerating unit 66 is to be close to the drum outer wall uniform winding by stainless steel tube to be welded on the drum outer wall, injects liquid nitrogen and form cold-trap in catcher top 58 is cylinder external wall of upper portion stainless steel tube; Pipe inner cylinder bottom 63 and one section stainless steel tube 65 formations one integral body connect two portions by clamp 60, thereby easy powder with collection for convenience detach takes out, and sealing-ring 64 is used for sealing.The gas 45 that comes out from reaction chamber enters from the inlet 59 of powder catcher 32, after gas 45 is run into cold wall, forms powder or liquid and falls, and residual gas will be taken away from the lower end by the pump group through stainless steel tube 65 from the upper end of stainless steel tube 65.
Embodiment 3: overall device is with embodiment 2, referring to Fig. 3, upper/lower electrode in the reaction chamber assembly 2 is the adjustable distance electrode, promptly the top electrode flat board that links to each other with rf (discharge) plasma assembly 3 is served as by gas distribution box 47, gas distribution box 47 bottoms are evenly distributed with aperture, lower electrode is made of substrate table 44, and spacing between this two electrode adopts and increases or reduce backing plate quantity and regulates, backing plate closely contact with top electrode and thickness certain.
Embodiment 4: referring to accompanying drawing 4, source of the present invention steam 55, carrier gas and reactant gases 52 thorough mixing in vaporizer, mixing total gas 40 enters from the reaction chamber upper end, referring to accompanying drawing 3, entered reaction chamber 23 through gas distribution box 47 after 43 heating of gas distribution box well heater, plasma body 46 adopts RF-wise to produce, and electrode is served as by gas distribution box, and the substrate with certain temperature that plasma body 46 arrives on the substrate table 44 forms film.Spacing between two electrodes of the dull and stereotyped lower electrode that constitutes with substrate table 44 of the top electrode that links to each other with radio-frequency match box 22 can be regulated, and the mode of adjusting is for increasing or minimizing backing plate quantity, these backing plates closely contact with top electrode and thickness certain.PTFE dead ring 41 is used for making reaction chamber and the dull and stereotyped insulation of top electrode, and water-cooled screen 42 is used for heat insulation.
The heating of substrate is to adopt the resistance heater be imbedded in the substrate table to heat and control, and resistance heater is that indium scandium alloy resistive arrangement becomes the multiple tracks circular concentric, helps improving the homogeneity of substrate table 44 surface temperatures.
Embodiment 5: specific embodiment is with embodiment 4, set up butterfly valve 30 between DN50 angle valve 31 in the air extractor of vacuum subassembly 4 and lobe pump inlet, gas receiver 24 is connected with film rule 26 and gamut rule 34 respectively by DN25 angle valve 25 and DN25 angle valve 33.
Embodiment 6:
Referring to Fig. 2, work of the present invention is at first to be handle or liquid, or it is solid-state, or the first body of liquid state and solid-state blended MO source is dissolved in certain density solution of formation or suspension liquid in the organic solvent by stoichiometric ratio, then by realizing that the transferpump that flow is accurately controlled is transported to spraying gun 19 to this solution or suspension liquid, vaporization in vaporizer 20 again after atomizing, carrier gas by preheating at last is transported to reaction chamber 23, under the rf electric field excitation, between two plate electrodes, produce plasma body, generate needed oxide compound with reactant gases, be deposited on the substrate of Controllable Temperature and form film.
Embodiment 7:
Specific embodiment adopts the present invention to prepare PZT (Pb (Zr with embodiment 5 xTi 1-x) O 3) film
Reaction chamber 23 of the present invention adopts columnar structured, and the bottom links to each other with gas receiver 24 by 4 flanges of symmetrical placement, referring to accompanying drawing 2, can guarantee the homogeneity of reaction chamber air-flow like this, uncaps in reaction chamber top, and the open and close of pneumatics control loam cake are arranged.
The fluid passage parallel arranged and the installed device of multichannel liquid supplying passage are identical.Referring to accompanying drawing 2, come the relative position relation of devices illustrated with installed device on the paths, container 8, magnetic valve 10, transferpump 12, back pressure valve 14, the electromagnet cut off valve 16 in splendid attire MO source are installed successively by the liquid input direction on fluid passage, wherein transferpump is a piston pump, it has continuously and pulse is carried liquid mode, liquid transfer rate 0-10ml/h for two kinds; Delivery precision 0.01ml/h.Back pressure valve 14 is to install because of the job requirement of piston pump, electromagnet cut off valve 16 is used for the through and off of controlled liq, the two-way fluid passage is combined as one road fluid passage by adaptor, open at electromagnet cut off valve 18, when magnetic valve 17 cuts out, mixed source enters ultrasonic atomizer 19 atomizings and vaporization in vaporizer 20, wherein the vaporization temperature of the atomizing power of spraying gun and vaporizer can be regulated, the design of electromagnet cut off valve 17 is in order to realize pipeline, the cleaning of piston pump and valve is when at MO source container 7, pack in 8 cleaning solvent and close at electromagnet cut off valve 18, can realize under the state that valve 17 is opened pipeline, the cleaning of piston pump and valve.
The present invention's design has two gas circuit paths, referring to accompanying drawing 2, the one tunnel is carrier gas argon gas path, and another road is a reactant gases oxygen path, by gas meter 38,39 controls, magnetic valve 36,37 is used for controlling the through and off of gas circuit respectively for carrier gas and reaction gas flow.By adaptor carrier gas path and reactant gas passage are combined into one tunnel gas passage, be transported in the vaporizer 20 through pipe fitting 51, referring to accompanying drawing 4, stainless steel polishing pipe fitting 51 outer walls are tied with the heating zone, and can realize can be 0~280 ℃ of adjusting to the heating and the Heating temperature of gas.
Source steam, carrier gas and reactant gases thorough mixing, the total gas 40 of mixing in vaporizer 20 enter from reaction chamber 23 upper ends, referring to accompanying drawing 3, entered reaction chamber 23 through gas distribution chamber 47 after 43 heating of gas distribution box well heater, plasma body adopts RF-wise to produce, provide radiofrequency signal by radio-frequency power supply 21, radio-frequency match box 22 is used for carrying out impedance matching, and electrode is served as by gas distribution box, mixed gas produces plasma body 46 through RF-wise, and plasma body is the formation of deposits film on substrate.Gamut rule 26, film rule 34 are used for monitoring reaction indoor base vacuum and working vacuum respectively, and gamut rule 26, film rule 34 link to each other with gas receiver 24 by angle valve 25,33 separately, referring to accompanying drawing 2.
Referring to accompanying drawing 2, air extractor is made up of dried pump 28 and lobe pump 29, reaction chamber 23 is given when taking out, angle valve 27 is opened, and angle valve 31 is in closing condition, realizes giving of reaction chamber 23 taken out by dried pump 28, when gamut rule 34 are shown as 5Pa, close angle valve 27, open butterfly valve 30 and angle valve 31, make up by dried pump and lobe pump reaction chamber is bled.When reaction chamber 23 vacuum tightnesss that show when gamut rule 26 meet the demands, close angle valve 25, open angle valve 33, after mixing total gas 40 and entering, the pressure that the closed loop system of being made up of film rule 26 and butterfly valve 30 is controlled reaction chamber satisfies set(ting)value.The air outlet of dried pump 28 links to each other with exhaust gas processing device, and the residual gas after vent gas treatment enters atmosphere.
When multichannel liquid supplying passage of the present invention is a two-way, when two-way is different liquid source, can realize the alternating deposit of two kinds of films, as obtaining gradient film PbZrO 3/ PbTiO 3, PZT/BaTiO 3With BaTiO 3/ SrTiO 3Deng, wherein at BaTiO 3/ SrTiO 3In the gradient film, suitable if processing parameter is selected, can obtain superstructure.
Utilize the present invention that the source material requirement is reduced, can obtain high-quality thin film and multi-component film.Can be used to obtain superconducting thin film equally, as ybco film etc.
By the touch-screen select operating mode, (manually, automatically), now being example automatically, processing parameter is set in menu, after configuring processing parameter, sets working routine again, automatically perform after can setting according to processing requirement, can work out simultaneously user program and preserve, get final product working procedure after having set the work program, the general of system finish the technology whole process as requested automatically.
Embodiment 8:
Specific embodiment is with embodiment 7, and difference is that the fluid passage of multichannel liquid supplying passage is three the tunnel, the road fluid passage that is promptly increased for contain lanthanum (La) liquid source, can deposit have that gradient concentration distributes mix lanthanum (La) pzt thin film etc.By increasing the method for liquid supplying passage number, realize more complex oxide depositing of thin film.。
Compare with traditional gaseous source MOCVD equipment deposition pzt thin film, the present invention adopts PZT source elder generation liquid solution to be delivered directly to reaction chamber and deposits pzt thin film, thereby has avoided many gaseous source to carry the complexity problem that faces, and source material is required to reduce.MO source elder generation liquid solution is to form after being dissolved in ethylene glycol monomethyl ether by the solid-state first body of PZT powdery, and the solid-state first body of PZT powdery is after lead acetate, titanium isopropylate and acetylpropyl alcohol zirconium are closed processing through the acetylpropyl alcohol huge legendary turtle, is obtaining through drying under reduced pressure.

Claims (5)

1. liquid-conveying metallorganics chemical vapour deposition apparatus, include reaction chamber assembly, the rf (discharge) plasma assembly, vacuum subassembly, operation protection and emission treatment assembly, electrically-controlled component, the rf (discharge) plasma assembly is connected on the electrode of reaction chamber assembly gas distribution box by output electrode, the gas output tube road of reaction chamber assembly is connected on the operated pneumatic valve of vacuum subassembly, the waste gas output channel of vacuum subassembly is directly connected to the emission-control equipment of operation protection and emission treatment assembly, it is characterized in that: total equipment also includes polynary vaporization component (1), polynary vaporization component (1) is removable integration assembly, mainly by multichannel liquid source transfer passage, the two-way gas delivery channels, spraying gun (19), vaporizer (20), valve and pipeline constitute, spraying gun wherein (19) is in vaporizer (20) top, adopt sealing-ring (56) sealing, carburetor structure is cylindric, be welded with pipe fitting (51) on the sidewall of cylinder middle and upper part, the pipe fitting (51) that passes through of the mixed gas of carrier gas and reactant gases (52) enters vaporizer (20); The formation of liquid source transfer passage is identical, liquid source is the MO source, the liquid transfer passage of single channel is equipped with the MO source container successively by the liquid input direction, magnetic valve, transferpump, back pressure valve, electromagnet cut off valve, the output of the end electromagnet cut off valve of the transfer passage of each road liquid source is divided into two-way again after merging by adaptor, the electromagnet cut off valve of leading up to is received operation protection and emission treatment assembly (5), spraying gun (19) is received by electromagnet cut off valve in another road, and the liquid that is transferred is transported to reaction chamber assembly (2) with carrier gas and the mixed total gas of reactant gases (40) by corrugated tube after atomizing and vaporization; Vaporizer (20) has well heater (54), and pipe fitting (51) has well heater (50), and the electrically-controlled component (6) that has programmable touch screen is connected with each construction components circuit, adopts programmable logic controller PLC to constitute, and whole technological processs are controlled automatically.
2. liquid-conveying metallorganics chemical vapour deposition apparatus according to claim 1, it is characterized in that: described vacuum subassembly (4) also includes powder catcher (32), powder catcher (32) is made up of catcher top (58) and catcher lower section (63) that can be for convenience detach, catcher lower section (63) constitutes an integral body with one section stainless steel tube (65) welding, by clamp (60) to catcher up and down two portions tighten up and unclamp, powder catcher (32) is a tubular structure, drum outer wall is installed with refrigerating unit (66), powder catcher (32) upper end is connected with reaction chamber assembly (2) by gas receiver (24), powder catcher (32) lower end is divided into two-way, the angle valve (27) of leading up to is connected to dried pump (28), and another road is connected with lobe pump (29) by angle valve (31).
3. liquid-conveying metallorganics chemical vapour deposition apparatus according to claim 2, it is characterized in that: the upper/lower electrode in the described reaction chamber assembly (2) is the adjustable distance electrode, promptly the top electrode flat board that links to each other with rf (discharge) plasma assembly (3) is served as by gas distribution box (47), gas distribution box (47) bottom is evenly distributed with aperture, lower electrode is made of substrate table (44), spacing between this two electrode adopts and increases or reduce backing plate quantity and regulates, backing plate closely contact with top electrode and thickness certain.
4. liquid-conveying metallorganics chemical vapour deposition apparatus according to claim 3 is characterized in that: reaction chamber (23) lining of described reaction chamber assembly (2), the resistance heater that is imbedded in the substrate table is designed to the multiple tracks circular concentric.
5. liquid-conveying metallorganics chemical vapour deposition apparatus according to claim 4, it is characterized in that: set up butterfly valve (30) between angle valve (31) in the air extractor of described vacuum subassembly (4) and lobe pump (29) inlet, gas receiver (24) is connected with film rule (26) and gamut rule (34) respectively by angle valve (25) and angle valve (33).
CNB2006101046309A 2006-09-22 2006-09-22 Liquid-conveying metallorganics chemical vapour deposition apparatus Expired - Fee Related CN100482858C (en)

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CN102220565A (en) * 2011-06-13 2011-10-19 南开大学 Chemical vapor deposition equipment used for studying light trapping structure of silicon thin-film cell
WO2012079467A1 (en) * 2010-12-13 2012-06-21 北京北方微电子基地设备工艺研究中心有限责任公司 Cavity component and metal-organic chemical vapor deposition device with same
CN102560418A (en) * 2010-12-29 2012-07-11 理想能源设备有限公司 Chemical vapor deposition device
CN101730373B (en) * 2008-11-03 2012-09-05 北京坚润表面材料研究所 Method and device for forming new materials by discharge of fog gas
CN102744024A (en) * 2011-04-22 2012-10-24 苏州市奥普斯等离子体科技有限公司 Low temperature plasma grafting vaporization method and apparatus
CN103372405A (en) * 2012-04-30 2013-10-30 韩国能源技术研究院 Method and apparatus for synthetizing composite using simultaneous vaporization, vaporizer for composite synthesis apparatus, vaporizer heater, and composite
CN105202309A (en) * 2014-06-24 2015-12-30 北大方正集团有限公司 Pipeline stirring device and plasma chemical vapor deposition equipment
CN106362423B (en) * 2016-09-26 2019-04-16 中国电子科技集团公司第四十八研究所 A kind of liquid source vaporising device
CN110965026A (en) * 2018-09-30 2020-04-07 深圳市引擎门科技有限公司 Steam continuous supply system and method
CN112813406A (en) * 2020-12-30 2021-05-18 武汉工程大学 Equipment and method for preparing three-dimensional metal simple substance film on surface of special-shaped piece based on CVD technology
CN114121590A (en) * 2021-11-19 2022-03-01 北京北方华创微电子装备有限公司 Process chamber
CN115161617A (en) * 2022-09-08 2022-10-11 拓荆科技(上海)有限公司 Gas distribution structure and vapor deposition equipment
CN115613005A (en) * 2021-07-16 2023-01-17 长鑫存储技术有限公司 Atomization device and thin film deposition system
CN114121590B (en) * 2021-11-19 2024-05-17 北京北方华创微电子装备有限公司 Process chamber

Cited By (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101730373B (en) * 2008-11-03 2012-09-05 北京坚润表面材料研究所 Method and device for forming new materials by discharge of fog gas
WO2012079467A1 (en) * 2010-12-13 2012-06-21 北京北方微电子基地设备工艺研究中心有限责任公司 Cavity component and metal-organic chemical vapor deposition device with same
CN102560418A (en) * 2010-12-29 2012-07-11 理想能源设备有限公司 Chemical vapor deposition device
CN102744024A (en) * 2011-04-22 2012-10-24 苏州市奥普斯等离子体科技有限公司 Low temperature plasma grafting vaporization method and apparatus
CN102220565A (en) * 2011-06-13 2011-10-19 南开大学 Chemical vapor deposition equipment used for studying light trapping structure of silicon thin-film cell
CN102220565B (en) * 2011-06-13 2012-08-29 南开大学 Chemical vapor deposition equipment used for studying light trapping structure of silicon thin-film cell
CN103372405A (en) * 2012-04-30 2013-10-30 韩国能源技术研究院 Method and apparatus for synthetizing composite using simultaneous vaporization, vaporizer for composite synthesis apparatus, vaporizer heater, and composite
CN103372405B (en) * 2012-04-30 2015-09-09 韩国能源技术研究院 Apply the compound synthesizer of simultaneously vaporizing and method, the vaporizer of described device, vaporizer heater and compound
CN105202309A (en) * 2014-06-24 2015-12-30 北大方正集团有限公司 Pipeline stirring device and plasma chemical vapor deposition equipment
CN105202309B (en) * 2014-06-24 2017-09-26 北大方正集团有限公司 Pipeline mixing device and plasma chemical vapor deposition equipment
CN106362423B (en) * 2016-09-26 2019-04-16 中国电子科技集团公司第四十八研究所 A kind of liquid source vaporising device
CN110965026A (en) * 2018-09-30 2020-04-07 深圳市引擎门科技有限公司 Steam continuous supply system and method
CN112813406A (en) * 2020-12-30 2021-05-18 武汉工程大学 Equipment and method for preparing three-dimensional metal simple substance film on surface of special-shaped piece based on CVD technology
CN115613005A (en) * 2021-07-16 2023-01-17 长鑫存储技术有限公司 Atomization device and thin film deposition system
CN114121590A (en) * 2021-11-19 2022-03-01 北京北方华创微电子装备有限公司 Process chamber
CN114121590B (en) * 2021-11-19 2024-05-17 北京北方华创微电子装备有限公司 Process chamber
CN115161617A (en) * 2022-09-08 2022-10-11 拓荆科技(上海)有限公司 Gas distribution structure and vapor deposition equipment
CN115161617B (en) * 2022-09-08 2023-01-13 拓荆科技(上海)有限公司 Gas distribution structure and vapor deposition equipment

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