CN104445986A - Method for coating carbon on quartz ampoule for growing crystals - Google Patents
Method for coating carbon on quartz ampoule for growing crystals Download PDFInfo
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- CN104445986A CN104445986A CN201410669839.4A CN201410669839A CN104445986A CN 104445986 A CN104445986 A CN 104445986A CN 201410669839 A CN201410669839 A CN 201410669839A CN 104445986 A CN104445986 A CN 104445986A
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- quartz ampoule
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/15—Deposition methods from the vapour phase
- C03C2218/152—Deposition methods from the vapour phase by cvd
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- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
The invention discloses a method for coating carbon on a quartz ampoule for growing crystals. The method comprises the following steps: putting a to-be-coated quartz ampoule by carbon into a tube furnace, increasing the temperature of the tube furnace to the temperature for coating carbon, and exhausting air in the tube furnace; then introducing acetylene which serves as a carbon source into the tube furnace, pyrolyzing the acetylene at a high temperature, and depositing a layer of carbon film on the inner wall of the quartz ampoule; and finally post-processsing the carbon film. By adopting the method disclosed by the invention, a gas way device can be simplified, no vacuum device and exhaust pipe needs to be installed, and the efficiency of coating carbon can be improved significantly. In addition, the method can meet the carbon coating requirements of quartz ampoules of various sizes and shapes.
Description
Technical field
Embodiments of the present invention relate to technical field of crystal growth, and more specifically, embodiments of the present invention relate to a kind of plating carbon method of the quartz ampoule for crystal growth.
Background technology
Growing method is mainly divided into melt method for growing, solution growth, vapor phase growth and solid state growth according to its parent phase type, wherein, melt method for growing is modal a kind of monocrystalline acquisition technology, this method is positioned in quartz ampoule by polycrystal raw material, and be warming up to more than fusing point, then Slow cooling generates monocrystalline.
Mineral crystal generally all has higher fusing point, and in process of growth under the high temperature conditions, high-temperature fusant easily and quartz ampoule adhesion, cause heterogeneous nucleation, affect crystal quality, meeting tearing quartz ampoule when adhesion is serious, ampoule inner high voltage gas is sprayed, causes bursting of quartz ampoule.In order to prevent the adhesion of high-temperature fusant and quartz ampoule, usually plating one deck and the nonwettable carbon film of high-temperature fusant at quartz ampoule, ensureing carrying out smoothly and monocrystalline quality of crystal growth.
Current plating carbon method mainly contains two kinds: one adopts ethanol as carbon source, in high vacuum environment, passed into by ethanol in High Temperature Furnaces Heating Apparatus, ethanol generation cracking, at quartz ampoule internal surface depositing carbon film, this method needs to be equipped with high-vacuum installation and ethanol evaporating device, and airshed controls more complicated; The second is using methane as carbon source, and shove charge also vacuumizes, and is warming up to more than 1000 DEG C, makes methane cracking and at quartz crucible inner surface depositing carbon film, this method needs comparatively high decomposition temperature and comparatively atmospheric flow.Mainly there are following problems in existing technique: plating carbon device is more complicated, needs to configure multiple valve and gas circuit; Schedule of operation is more complicated, and is difficult to the plating carbon requirement of the quartz ampoule of simultaneous adaptation plurality of specifications; The carbon content of carbon source is not high, generally needs comparatively air volume and longer aeration time; Cooling time is longer, and at least need within more than ten hour, just can complete, efficiency is lower.
Summary of the invention
Instant invention overcomes the deficiencies in the prior art, a kind of embodiment of plating carbon method of the quartz ampoule for crystal growth is provided, with expect to solve plating carbon device be equipped with require high, schedule of operation is complicated, be difficult to the plating carbon of the quartz ampoule adapting to plurality of specifications requires and the carbon content of carbon source is not high causes the problems such as plating carbon time long, plating carbon weak effect.
For solving above-mentioned technical problem, one embodiment of the present invention by the following technical solutions:
For a plating carbon method for the quartz ampoule of crystal growth, it comprises the following steps:
(1) quartz ampoule of carbon to be plated is positioned in tube furnace
First the quartz ampoule of carbon to be plated is placed in quartz socket tube, then quartz socket tube is put into the plating carbon humidity province of tube furnace, then the air outlet of the ventpipe of air feeder is placed in quartz ampoule; Optimum position is that the ventpipe mouth of pipe is positioned at apart from quartz ampoule afterbody 30 millimeters of places;
(2) tube furnace heats up and exhausted air
First at ambient pressure tube furnace is risen to 900 ~ 1000 DEG C, then keep homo(io)thermism and with air feeder pass in described quartz ampoule purity be more than 99.99% rare gas element eliminating quartz ampoule in air;
(3) pass into carbon-source gas and plating carbon is carried out to quartz ampoule
The flow of rare gas element is adjusted to 30 ~ 70mL/min, then in quartz ampoule, pass into acetylene by the speed that air feeder take flow as 2 ~ 5mL/min and carry out plating carbon to quartz ampoule, the time passing into acetylene when the ventpipe of described air feeder is in a fixed position in quartz ampoule is 5 ~ 10 minutes;
Preferably, the depositing time that ventpipe is located quartz ampoule afterbody 30 millimeters is 5 minutes; Then ventpipe is moved 50 millimeters outside boiler tube, depositing time is 5 minutes; Finally ventpipe is moved 50 millimeters again outside boiler tube, depositing time is 5 minutes.According to the model of quartz ampoule, can increase or reduce above-mentioned mobile ventpipe and the number of times of deposition.According to the needs of quartz ampoule to carbon film thickness, also can extend or shorten the time of each deposition, the present invention is conducive to controlling carbon film thickness, adapts to the plating carbon of Multiple Type quartz ampoule.Depositing time refers to that ventpipe passes into the time of acetylene when being in some fixed positions in quartz ampoule, namely in the time passing into acetylene process Center Vent tube and be in some fixed positions in quartz ampoule.
(4) aftertreatment is carried out to the quartz ampoule of plating carbon
After plating carbon terminates, close air feeder, take out the quartz socket tube in tube furnace and in quartz socket tube, pass into the rare gas element that purity is more than 99.99%, under ensureing that quartz ampoule keeps inert environments, make it at room temperature cool, namely obtain the quartz ampoule of plating carbon.
The temperature impact plating carbon effect of tube furnace, tube furnace is warming up to 900 ~ 1000 DEG C by the present invention, and in this temperature range, acetylene is effectively decomposed, and is conducive to improving plating carbon effect.Plating carbon method of the present invention do not adopt 900 DEG C under temperature, because cannot carry out plating carbon lower than acetylene when 900 DEG C is difficult to be decomposed, meanwhile, the present invention does not adopt the temperature of more than 1000 DEG C yet, because the too high oxidation accelerating carbon film of temperature, and meeting acceleration equipment is aging.
Present invention uses the air in highly purified rare gas element eliminating quartz ampoule, its object is to prevent acetylene and air mixed from blasting, prevent atmospheric oxidation carbon film from causing the failure of plating carbon simultaneously.The plating carbon mode adopted due to the present invention is open plating carbon, does not adopt airtight vacuum environment, therefore needs to adopt rare gas element to prevent air to the interference of plating carbon process.The present invention is not only front-seat except the air in quartz ampoule at plating carbon, in plating carbon process, also use rare gas element to carry out excluding air.By flow be rare gas element and the flow of 30 ~ 70mL/min be 2 ~ 5mL/min acetylene together with pass in quartz ampoule, both can ensure good plating carbon effect, can prevent again acetylene and air mixed from blasting; If inert gas flow is too high or the too low carbon film that all can cause of acetylene flow is oxidizable, and inert gas flow is too low or the too high meeting of acetylene flow causes acetylene accounting too high, makes explosion hazard greatly increase.It is too short that acetylene passes into the time, and carbon film layer covers not exclusively, and acetylene passes into overlong time and then causes carbon film blocked up, easily comes off.
The present invention is not oxidized when taking out in order to ensure to plate the quartz ampoule that completes of carbon, thus continuing to pass into high purity inert gas when cooling, preventing air from entering.High purity inert gas of the present invention refers to that purity is the rare gas element of more than 99.99%.
Further technical scheme is, after described plating carbon humidity province refers to tube furnace intensification, in-furnace temperature is the region of 900 ~ 1000 DEG C.Described in-furnace temperature is obtained by warm field test in stove.
Further technical scheme is, passing into purity described in step (2) is that the flow of the rare gas element of more than 99.99% is not less than 70mL/min, and the time of passing into is no less than 10min.Rare gas element should get rid of the air in quartz ampoule completely, and very few flow and the too short time that passes into cannot reach this object.
Further technical scheme is, passing into inert gas flow when carbon-source gas carries out plating carbon to quartz ampoule described in step (3) is 50mL/min, and acetylene flow is 5mL/min.The inert gas flow of 50mL/min and the acetylene flow of 5mL/min can either reach best plating carbon effect, explosion hazard can be dropped to again minimum, and can save time, raise the efficiency.
Further technical scheme is, described rare gas element is nitrogen or argon gas.
Further technical scheme is, described air feeder comprises rare gas element controller, acetylene controller, ventpipe, described rare gas element controller is communicated with ventpipe, acetylene controller is communicated with ventpipe, and the gas outlet of rare gas element controller and acetylene controller arranges the valve for controlling gas conveying respectively.This air feeder can provide rare gas element and acetylene respectively for the present invention, and can also control the flow of various gas, also gas and vapor permeation can be provided.
The SY-9312D type controller that rare gas element controller and acetylene controller can use Beijing limited control of holy industry science and technology to manufacture, but be not limited in this.
Why existing plating carbon technique configures complicated vacuum system and exhaust system, major cause is to ensure that carbon film sedimentation rate is greater than the oxidation consumption speed of carbon film, in order to optimize plating carbon device, then demand fulfillment carbon film sedimentation rate under normal pressure opens wide system is greater than the oxidation consumption speed of carbon film, found through experiments and can realize above object using acetylene as carbon source, acetylene carbon content ratio is high, decomposition temperature is lower, sedimentation rate is very fast, the deposition of carbon film can be realized under normal pressure opens wide system, thus save vacuum unit and gas barrier, and under this unlimited system, ventilation position can be adjusted easily, realize the plating carbon requirement of different size and shape ampoule.In addition, acetylene effectively can shorten the plating carbon time as carbon source and reduce air flow, without the need to also can realize effective combination of carbon film and ampoule interior wall through long cooling after plating carbon, there will not be stripping phenomenon, meet crystal growth requirement, thus can shorten cooling time by technological method of the present invention, significantly improve plating carbon efficiencies.
Compared with prior art, one of beneficial effect of the present invention is: do not need configuration vacuum unit and exhaust line, simplify gas path device; The plating carbon that can meet the quartz ampoule of plurality of specifications requires and simple to operate, is easy to regulate; The plating carbon deadline is foreshortened to 1 ~ 2 hour from 10 ~ 24 hours, significantly improves plating carbon efficiencies.
Accompanying drawing explanation
Fig. 1 is plating carbon device structure schematic diagram of the present invention.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
Accompanying drawing 1 is plating carbon device structure schematic diagram of the present invention.In figure, 1 is tube furnace boiler tube, and 2 is heating zone, and 3 is quartz ampoule, and 4 is ventpipe, and 5 is rare gas element controller, and 6 is inert gas piping valve, and 7 is acetylene pipe valve, and 8 is acetylene controller.Specific embodiments of the invention are as follows:
Embodiment 1
The quartz ampoule of carbon to be plated is positioned in tube furnace: the quartz ampoule 3 of carbon to be plated is put into tube furnace boiler tube 1 plating carbon humidity province (tube furnace heat up after in-furnace temperature be the region of 900 ~ 1000 DEG C, this temperature is obtained by warm field test in stove), after determining plating carbon location, ventpipe 4 is put into quartz ampoule 3, and the ventpipe mouth of pipe is positioned at apart from quartz ampoule afterbody 30 millimeters of places.
Tube furnace heats up and exhausted air: with the speed of 5 DEG C/min, furnace temperature is risen to 900 DEG C at ambient pressure, insulation 30 minutes after temperature, and open rare gas element controller 5, open the nitrogen eliminating residual air that inert gas piping valve 6 logical purity in quartz ampoule 3 is more than 99.99%, gas flow is 70 ml/min, and the time of logical nitrogen is 10 minutes.
Pass into carbon-source gas and carry out plating carbon to quartz ampoule: open acetylene controller 8, open acetylene pipe valve 7, regulate acetylene flow to be 2 ml/min, and regulate nitrogen flow to be 30 ml/min, depositing time is 5 minutes; Then ventpipe is moved 50 millimeters outside boiler tube, depositing time is 5 minutes; Finally ventpipe is moved 50 millimeters again outside boiler tube, depositing time is 5 minutes.Depositing time refers to that ventpipe passes into the time of acetylene when being in some fixed positions in quartz ampoule, namely in the time passing into acetylene process Center Vent tube and be in some fixed positions in quartz ampoule.
Aftertreatment is carried out to the quartz ampoule of plating carbon: after carbon film deposition terminates, close acetylene pipe valve 7, acetylene controller 8, inert gas piping valve 6, rare gas element controller 5 successively, take out ventpipe and quartz socket tube, quartz socket tube to be positioned under room temperature and continue logical purity be more than 99.99% nitrogen make its naturally cooling, namely obtain the quartz ampoule of plating carbon.
Embodiment 2
The quartz ampoule of carbon to be plated is positioned in tube furnace: the quartz ampoule 3 of carbon to be plated is put into tube furnace boiler tube 1 plating carbon humidity province (tube furnace heat up after in-furnace temperature be the region of 900 ~ 1000 DEG C, this temperature is obtained by warm field test in stove), after determining plating carbon location, ventpipe 4 is put into quartz ampoule 3, and the ventpipe mouth of pipe is positioned at apart from quartz ampoule afterbody 30 millimeters of places.
Tube furnace heats up and exhausted air: with the speed of 6 DEG C/min, furnace temperature is risen to 950 DEG C at ambient pressure, insulation 30 minutes after temperature, and open rare gas element controller 5, open the argon gas eliminating residual air that inert gas piping valve 6 logical purity in quartz ampoule 3 is more than 99.99%, gas flow is 70 ml/min, and the time of logical argon gas is 10 minutes.
Pass into carbon-source gas and carry out plating carbon to quartz ampoule: open acetylene controller 8, open acetylene pipe valve 7, regulate acetylene flow to be 5 ml/min, and regulate argon flow amount to be 50 ml/min, depositing time is 5 minutes; Then ventpipe is moved 50 millimeters outside boiler tube, depositing time is 5 minutes; Finally ventpipe is moved 50 millimeters again outside boiler tube, depositing time is 5 minutes.
Aftertreatment is carried out to the quartz ampoule of plating carbon: after carbon film deposition terminates, close acetylene pipe valve 7, acetylene controller 8, inert gas piping valve 6, rare gas element controller 5 successively, take out ventpipe and quartz socket tube, quartz socket tube to be positioned under room temperature and the nitrogen that logical purity is more than 99.99% makes its naturally cooling, namely to obtain the quartz ampoule of plating carbon.
Embodiment 3
The quartz ampoule of carbon to be plated is positioned in tube furnace: the quartz ampoule 3 of carbon to be plated is put into tube furnace boiler tube 1 plating carbon humidity province (tube furnace heat up after in-furnace temperature be the region of 900 ~ 1000 DEG C, this temperature is obtained by warm field test in stove), after determining plating carbon location, ventpipe 4 is put into quartz ampoule 3, and the ventpipe mouth of pipe is positioned at apart from quartz ampoule afterbody 30 millimeters of places.
Tube furnace heats up and exhausted air: with the speed of 8 DEG C/min, furnace temperature is risen to 1000 DEG C at ambient pressure, insulation 30 minutes after temperature, and open rare gas element controller 5, open the nitrogen eliminating residual air that inert gas piping valve 6 logical purity in quartz ampoule 3 is more than 99.99%, gas flow is 70 ml/min, and the time of logical nitrogen is 10 minutes.
Pass into carbon-source gas and carry out plating carbon to quartz ampoule: open acetylene controller 8, open acetylene pipe valve 7, regulate acetylene flow to be 5 ml/min, and regulate nitrogen flow to be 65 ml/min, depositing time is 10 minutes; Then ventpipe is moved 50 millimeters outside boiler tube, depositing time is 10 minutes; Finally ventpipe is moved 50 millimeters again outside boiler tube, depositing time is 10 minutes.
Aftertreatment is carried out to the quartz ampoule of plating carbon: after carbon film deposition terminates, close acetylene pipe valve 7, acetylene controller 8, inert gas piping valve 6, rare gas element controller 5 successively, take out ventpipe and quartz socket tube, quartz socket tube to be positioned under room temperature and the nitrogen that logical purity is more than 99.99% makes its naturally cooling, namely to obtain the quartz ampoule of plating carbon.
Although with reference to multiple explanatory embodiment of the present invention, invention has been described here, but, should be appreciated that, those skilled in the art can design a lot of other amendment and embodiment, these amendments and embodiment will drop within spirit disclosed in the present application and spirit.More particularly, in the scope of, accompanying drawing open in the application and claim, multiple modification and improvement can be carried out to the building block of subject combination layout and/or layout.Except the modification of carrying out building block and/or layout is with except improvement, to those skilled in the art, other purposes also will be obvious.
Claims (7)
1., for a plating carbon method for the quartz ampoule of crystal growth, it is characterized in that it comprises the following steps:
(1) quartz ampoule of carbon to be plated is positioned in tube furnace
First the quartz ampoule of carbon to be plated is placed in quartz socket tube, then quartz socket tube is put into the plating carbon humidity province of tube furnace, then the air outlet of the ventpipe of air feeder is placed in quartz ampoule;
(2) tube furnace heats up and exhausted air
First at ambient pressure tube furnace is risen to 900 ~ 1000 DEG C, then keep homo(io)thermism and with air feeder pass in described quartz ampoule purity be more than 99.99% rare gas element eliminating quartz ampoule in air;
(3) pass into carbon-source gas and plating carbon is carried out to quartz ampoule
The flow of rare gas element is adjusted to 30 ~ 70mL/min, then in quartz ampoule, pass into acetylene by the speed that air feeder take flow as 2 ~ 5mL/min and carry out plating carbon to quartz ampoule, the time passing into acetylene when the ventpipe of described air feeder is in a fixed position in quartz ampoule is 5 ~ 10 minutes;
(4) aftertreatment is carried out to the quartz ampoule of plating carbon
After plating carbon terminates, close air feeder, take out the quartz socket tube in tube furnace and in quartz socket tube, pass into the rare gas element that purity is more than 99.99%, making it at room temperature cool, namely obtain the quartz ampoule of plating carbon.
2. the plating carbon method of the quartz ampoule for crystal growth according to claim 1, is characterized in that described plating carbon humidity province refers to that the rear in-furnace temperature of tube furnace intensification is the region of 900 ~ 1000 DEG C.
3. the plating carbon method of the quartz ampoule for crystal growth according to claim 2, is characterized in that described in-furnace temperature is obtained by warm field test in stove.
4. the plating carbon method of the quartz ampoule for crystal growth according to claim 1, it is characterized in that passing into described in step (2) purity is that the flow of the rare gas element of more than 99.99% is not less than 70mL/min, and the time of passing into is no less than 10min.
5. the plating carbon method of the quartz ampoule for crystal growth according to claim 1, it is characterized in that passing into described in step (3) inert gas flow when carbon-source gas carries out plating carbon to quartz ampoule is 50mL/min, and acetylene flow is 5mL/min.
6. the plating carbon method of the quartz ampoule for crystal growth according to claim 1, is characterized in that described rare gas element is nitrogen or argon gas.
7. the plating carbon method of the quartz ampoule for crystal growth according to claim 1, it is characterized in that described air feeder comprises rare gas element controller, acetylene controller, ventpipe, described rare gas element controller is communicated with ventpipe, acetylene controller is communicated with ventpipe, and the gas outlet of rare gas element controller and acetylene controller arranges the valve for controlling gas conveying respectively.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105483825A (en) * | 2015-12-11 | 2016-04-13 | 华中科技大学 | Preparation method of bromine-lead-cesium single crystals |
| CN106591797A (en) * | 2016-11-23 | 2017-04-26 | 东莞劲胜精密组件股份有限公司 | Method for quickly coating carbon film |
| CN107268070A (en) * | 2017-06-10 | 2017-10-20 | 中国科学院合肥物质科学研究院 | A kind of method of low absorption phosphorus germanium zinc crystal growth |
| CN108996916A (en) * | 2018-09-05 | 2018-12-14 | 成都中建材光电材料有限公司 | A kind of method of quartz inside pipe wall plated film |
| CN112851138A (en) * | 2020-12-26 | 2021-05-28 | 云南农业大学 | Smoked carbon device of quartz ampoule wall |
| CN115259684A (en) * | 2022-08-02 | 2022-11-01 | 安徽光智科技有限公司 | Carbon plating method for quartz device |
| CN115928010A (en) * | 2022-11-18 | 2023-04-07 | 有研国晶辉新材料有限公司 | Quartz container carbon fumigating device and carbon fumigating method |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105483825A (en) * | 2015-12-11 | 2016-04-13 | 华中科技大学 | Preparation method of bromine-lead-cesium single crystals |
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| CN106591797A (en) * | 2016-11-23 | 2017-04-26 | 东莞劲胜精密组件股份有限公司 | Method for quickly coating carbon film |
| CN107268070A (en) * | 2017-06-10 | 2017-10-20 | 中国科学院合肥物质科学研究院 | A kind of method of low absorption phosphorus germanium zinc crystal growth |
| CN108996916A (en) * | 2018-09-05 | 2018-12-14 | 成都中建材光电材料有限公司 | A kind of method of quartz inside pipe wall plated film |
| CN108996916B (en) * | 2018-09-05 | 2021-06-08 | 成都中建材光电材料有限公司 | Method for coating inner wall of quartz tube |
| CN112851138A (en) * | 2020-12-26 | 2021-05-28 | 云南农业大学 | Smoked carbon device of quartz ampoule wall |
| CN112851138B (en) * | 2020-12-26 | 2021-07-23 | 云南农业大学 | Smoked carbon device of quartz ampoule wall |
| CN115259684A (en) * | 2022-08-02 | 2022-11-01 | 安徽光智科技有限公司 | Carbon plating method for quartz device |
| CN115259684B (en) * | 2022-08-02 | 2024-03-08 | 安徽光智科技有限公司 | Carbon plating method for quartz device |
| CN115928010A (en) * | 2022-11-18 | 2023-04-07 | 有研国晶辉新材料有限公司 | Quartz container carbon fumigating device and carbon fumigating method |
| CN115928010B (en) * | 2022-11-18 | 2023-08-18 | 有研国晶辉新材料有限公司 | Carbon fumigating device and carbon fumigating method for quartz container |
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