CN104445986B - A kind of plating carbon method of the quartz ampoule for crystal growth - Google Patents
A kind of plating carbon method of the quartz ampoule for crystal growth Download PDFInfo
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- CN104445986B CN104445986B CN201410669839.4A CN201410669839A CN104445986B CN 104445986 B CN104445986 B CN 104445986B CN 201410669839 A CN201410669839 A CN 201410669839A CN 104445986 B CN104445986 B CN 104445986B
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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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- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
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- Organic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
The invention discloses a kind of plating carbon method of quartz ampoule for crystal growth, the quartz ampoule of carbon to be plated is positioned in tube furnace, tube furnace is warming up to plating carbon temperature air-out, then pass to acetylene as carbon source, at high temperature acetylene cracking also deposits one layer of carbon film at ampoule interior wall, finally carbon film is carried out post processing. The method of the invention can simplify gas path device, it is not necessary to configuration vacuum equipment and gas exhaust piping, can significantly improve plating carbon efficiencies, and can meet the plating carbon requirement of various sizes and shape quartz ampoule.
Description
Technical field
The present invention relates to technical field of crystal growth, more particularly it relates to an the plating carbon method of the quartz ampoule for crystal growth.
Background technology
Growing method is broadly 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, the method is to be positioned in quartz ampoule by polycrystal raw material, and it is warming up to more than fusing point, then Slow cooling generates monocrystalline.
Mineral crystal generally all has higher fusing point, and in growth course under the high temperature conditions, high-temperature fusant is easily and quartz ampoule adhesion, cause heterogeneous nucleation, affect crystal quality, meeting tearing quartz ampoule when adhesion is serious, make ampoule inner high voltage gas spray, cause bursting of quartz ampoule. In order to prevent the adhesion of high-temperature fusant and quartz ampoule, generally plate last layer and the nonwettable carbon film of high-temperature fusant at quartz ampoule, it is ensured that being smoothed out and monocrystalline quality of crystal growth.
Current plating carbon method mainly has two kinds: one is to adopt ethanol as carbon source, in high vacuum environment, is passed into by ethanol in high temperature furnace, ethanol cracks, at quartz ampoule inner surface depositing carbon film, the method needs to be equipped with high-vacuum installation and ethanol evaporating device, and throughput controls more complicated; The second is as carbon source, shove charge evacuation using methane, is warming up to more than 1000 DEG C, makes methane cracking and at quartz crucible inner surface depositing carbon film, and the method needs relatively high decomposition temperature and relatively atmospheric flow. Existing technique is primarily present following problems: plating carbon device is more complicated, it is necessary to configure multiple valve and gas circuit; Operation sequence 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, it is generally required to relatively air volume and longer duration of ventilation; Cool time is longer, at least needs within more than ten hour, just can complete, inefficient.
Summary of the invention
Instant invention overcomes the deficiencies in the prior art, the embodiment of a kind of plating carbon method of quartz ampoule for crystal growth is provided, with expectation can solve plating carbon device be equipped with require high, operation sequence complicated, is difficult in adapt to the plating carbon of the quartz ampoule of plurality of specifications requires and the carbon content of carbon source is not high causes the problem such as plating carbon time length, plating carbon weak effect.
For solving above-mentioned technical problem, one embodiment of the present invention by the following technical solutions:
A kind of plating carbon method of the quartz ampoule for 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 gas outlet of the breather of feeder is placed in quartz ampoule;Optimum position is that the breather mouth of pipe is positioned at from quartz ampoule afterbody 30 millimeters place;
(2) tube furnace heats up and air-out
First at ambient pressure tube furnace is risen to 900��1000 DEG C, then keep temperature constant and in described quartz ampoule, pass into the air in the noble gas eliminating quartz ampoule that purity is 99.99% more than with feeder;
(3) pass into carbon-source gas and quartz ampoule is carried out plating carbon
The flow of noble gas is adjusted to 30��70mL/min, then to passing into acetylene in quartz ampoule, quartz ampoule carrying out plating carbon with the speed that flow is 2��5mL/min with feeder, the time passing into acetylene when the breather of described feeder is in quartz ampoule a fixed position is 5��10 minutes;
Preferably, the sedimentation time that breather is located quartz ampoule afterbody 30 millimeters is 5 minutes; Then outside boiler tube, breather being moved 50 millimeters, sedimentation time is 5 minutes; Finally outside boiler tube, breather being moved 50 millimeters again, sedimentation time is 5 minutes. Model according to quartz ampoule, it is possible to increase or reduce above-mentioned mobile breather the number of times deposited. According to the quartz ampoule needs to carbon film thickness, it is also possible to extend or shorten the time of deposition every time, the present invention is conducive to controlling carbon film thickness, adapts to the plating carbon of Multiple Type quartz ampoule. Sedimentation time refers to that breather passes into the time of acetylene when being in quartz ampoule some fixed position, namely passing into the time that acetylene process Center Vent tube is in quartz ampoule some fixed position.
(4) quartz ampoule of plating carbon is carried out post processing
After plating carbon terminates, close feeder, take out the quartz socket tube in tube furnace and in quartz socket tube, pass into the noble gas that purity is more than 99.99%, it is ensured that quartz ampoule keeps under inert environments, make it at room temperature cool down, 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. The plating carbon method of the present invention does not adopt 900 DEG C of temperature below, because acetylene is difficult to be decomposed and cannot be carried out plating carbon during lower than 900 DEG C, meanwhile, the present invention does not adopt the temperature of more than 1000 DEG C yet, because the too high oxidation that can accelerate carbon film of temperature, and meeting acceleration equipment is aging.
Present invention uses highly purified noble gas and get rid of the air in quartz ampoule, its object is to prevent acetylene and air mixing from blasting, prevent air oxidation carbon film from causing plating carbon failure simultaneously. The plating carbon mode adopted due to the present invention is open plating carbon, does not adopt airtight vacuum environment, it is therefore desirable to adopt noble gas to prevent the air interference to plating carbon process. The present invention is not only front-seat except the air in quartz ampoule at plating carbon, also uses noble gas to get rid of air in plating carbon process. The noble gas that flow is 30��70mL/min is passed in quartz ampoule together with the acetylene that flow is 2��5mL/min, both can ensure that good plating carbon effect, be prevented from again acetylene and air mixing is blasted; If inert gas flow is too high or acetylene flow is too low all can cause that carbon film is oxidizable, and inert gas flow is too low or the too high meeting of acetylene flow causes that acetylene accounting is too high so that explosion danger is greatly increased. 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 that carbon film is blocked up, it is easy to come off.
The quartz ampoule that the present invention completes to ensure plating carbon is not oxidized when taking out, thus continues to pass into high purity inert gas when cooling, it is prevented that air enters. High purity inert gas of the present invention refers to the noble gas that purity is more than 99.99%.
Further technical scheme is, described plating carbon humidity province refer to tube furnace heat up after in-furnace temperature be the region of 900��1000 DEG C. Described in-furnace temperature is obtained by temperature field test in stove.
Further technical scheme is, the flow passing into the noble gas that purity is more than 99.99% described in step (2) is not less than 70mL/min, and the time that passes into is no less than 10min. Noble gas should be got rid of the air in quartz ampoule, very few flow and the too short time that passes into completely and be unable to reach this purpose.
Further technical scheme is, pass into described in step (3) carbon-source gas quartz ampoule is carried out plating carbon time inert gas flow be 50mL/min, 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, can be preferably minimized by explosion danger again, and can save the time, improve efficiency.
Further technical scheme is, described noble gas is nitrogen or argon.
Further technical scheme is, described feeder includes noble gas controller, acetylene controller, breather, described noble gas controller connects with breather, acetylene controller connects with breather, and the gas outlet of noble gas controller and acetylene controller is respectively arranged to control the valve of gas conveying. This feeder can provide noble gas and acetylene respectively for the present invention, and can also control the flow of various gas, it is also possible to gas mixing is provided.
Noble gas controller and acetylene controller can use the SY-9312D type controller that Beijing sage's industry limited control of science and technology manufactures, it is not limited to this.
Why existing plating carbon technique configures vacuum system and the gas extraction system of complexity, main reason is that the oxidation consumption speed ensureing carbon film sedimentation rate more than carbon film, in order to optimize plating carbon device, then need to meet and open wide under system carbon film sedimentation rate more than the oxidation consumption speed of carbon film at normal pressure, it is found through experiments and can realize object above using acetylene as carbon source, acetylene carbon content ratio is high, decomposition temperature is relatively low, sedimentation rate is very fast, the deposition realizing carbon film under system can be opened wide at normal pressure, thus saving vacuum equipment and exhaust apparatus, and under this unlimited system, ventilation position can be adjusted easily, realize the plating carbon requirement of different size and shape ampoule. additionally, acetylene can effectively shorten the plating carbon time as carbon source and reduce ventilation, need not move through long cooling after plating carbon and also can realize effective combination of carbon film and ampoule interior wall, do not have stripping phenomenon, meet crystal growth requirement, technical method thereby through the present invention can shorten cool time, and plating carbon efficiencies is greatly improved.
Compared with prior art, the invention has the beneficial effects as follows: vacuum equipment and gas exhaust piping need not be configured, simplify gas path device; The plating carbon of the quartz ampoule that can meet plurality of specifications requires and simple to operate, it is easy to regulate; The plating carbon deadline was 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.
Detailed description of the invention
In order to make the purpose 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 is only in order to explain the present invention, is 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 the thermal treatment zone, and 3 is quartz ampoule, and 4 is breather, and 5 is noble gas 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 the plating carbon humidity province of tube furnace boiler tube 1, and (after tube furnace heats up, in-furnace temperature is the region of 900��1000 DEG C, this temperature is obtained by temperature field test in stove), after determining plating carbon location, breather 4 is put into quartz ampoule 3, and the breather mouth of pipe is positioned at from quartz ampoule afterbody 30 millimeters place.
Tube furnace heats up and air-out: with the speed of 5 DEG C/min, furnace temperature is risen to 900 DEG C at ambient pressure, it is incubated 30 minutes after temperature, and open noble gas controller 5, open the nitrogen that inert gas piping valve 6 logical purity in quartz ampoule 3 is more than 99.99% and get rid of residual air, gas flow is 70 ml/min, and the time of logical nitrogen is 10 minutes.
Passing into carbon-source gas and quartz ampoule carries out plating carbon: open acetylene controller 8, open acetylene pipe valve 7, regulating acetylene flow is 2 ml/min, and to regulate nitrogen flow be 30 ml/min, and sedimentation time is 5 minutes; Then outside boiler tube, breather being moved 50 millimeters, sedimentation time is 5 minutes; Finally outside boiler tube, breather being moved 50 millimeters again, sedimentation time is 5 minutes. Sedimentation time refers to that breather passes into the time of acetylene when being in quartz ampoule some fixed position, namely passing into the time that acetylene process Center Vent tube is in quartz ampoule some fixed position.
The quartz ampoule of plating carbon is carried out post processing: after carbon film deposition terminates, close acetylene pipe valve 7, acetylene controller 8, inert gas piping valve 6, noble gas controller 5 successively, take out breather and quartz socket tube, quartz socket tube is positioned under room temperature and continues the nitrogen that logical purity is more than 99.99% and make its natural 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 the plating carbon humidity province of tube furnace boiler tube 1, and (after tube furnace heats up, in-furnace temperature is the region of 900��1000 DEG C, this temperature is obtained by temperature field test in stove), after determining plating carbon location, breather 4 is put into quartz ampoule 3, and the breather mouth of pipe is positioned at from quartz ampoule afterbody 30 millimeters place.
Tube furnace heats up and air-out: with the speed of 6 DEG C/min, furnace temperature is risen to 950 DEG C at ambient pressure, it is incubated 30 minutes after temperature, and open noble gas controller 5, open the argon that inert gas piping valve 6 logical purity in quartz ampoule 3 is more than 99.99% and get rid of residual air, gas flow is 70 ml/min, and the time of logical argon is 10 minutes.
Passing into carbon-source gas and quartz ampoule carries out plating carbon: open acetylene controller 8, open acetylene pipe valve 7, regulating acetylene flow is 5 ml/min, and to regulate argon flow amount be 50 ml/min, and sedimentation time is 5 minutes; Then outside boiler tube, breather being moved 50 millimeters, sedimentation time is 5 minutes; Finally outside boiler tube, breather being moved 50 millimeters again, sedimentation time is 5 minutes.
The quartz ampoule of plating carbon is carried out post processing: after carbon film deposition terminates, close acetylene pipe valve 7, acetylene controller 8, inert gas piping valve 6, noble gas controller 5 successively, take out breather and quartz socket tube, quartz socket tube is positioned under room temperature and nitrogen that logical purity is more than 99.99% makes its natural cooling, namely 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 the plating carbon humidity province of tube furnace boiler tube 1, and (after tube furnace heats up, in-furnace temperature is the region of 900��1000 DEG C, this temperature is obtained by temperature field test in stove), after determining plating carbon location, breather 4 is put into quartz ampoule 3, and the breather mouth of pipe is positioned at from quartz ampoule afterbody 30 millimeters place.
Tube furnace heats up and air-out: with the speed of 8 DEG C/min, furnace temperature is risen to 1000 DEG C at ambient pressure, it is incubated 30 minutes after temperature, and open noble gas controller 5, open the nitrogen that inert gas piping valve 6 logical purity in quartz ampoule 3 is more than 99.99% and get rid of residual air, gas flow is 70 ml/min, and the time of logical nitrogen is 10 minutes.
Passing into carbon-source gas and quartz ampoule carries out plating carbon: open acetylene controller 8, open acetylene pipe valve 7, regulating acetylene flow is 5 ml/min, and to regulate nitrogen flow be 65 ml/min, and sedimentation time is 10 minutes; Then outside boiler tube, breather being moved 50 millimeters, sedimentation time is 10 minutes; Finally outside boiler tube, breather being moved 50 millimeters again, sedimentation time is 10 minutes.
The quartz ampoule of plating carbon is carried out post processing: after carbon film deposition terminates, close acetylene pipe valve 7, acetylene controller 8, inert gas piping valve 6, noble gas controller 5 successively, take out breather and quartz socket tube, quartz socket tube is positioned under room temperature and nitrogen that logical purity is more than 99.99% makes its natural cooling, namely obtain the quartz ampoule of plating carbon.
Although reference be made herein to invention has been described for the multiple explanatory embodiment of the present invention, but, it should be understood that those skilled in the art can be designed that a lot of other amendments and embodiment, these amendments and embodiment will drop within spirit disclosed in the present application and spirit. More specifically, disclosure, drawings and claims scope in, it is possible to building block and/or layout to theme composite configuration carry out multiple modification and improvement. Except the modification that building block and/or layout are carried out and improvement, to those skilled in the art, other purposes also will be apparent from.
Claims (7)
1. the plating carbon method for the quartz ampoule of crystal growth, it is characterised 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 gas outlet of the breather of feeder is placed in quartz ampoule;
(2) tube furnace heats up and air-out
First at ambient pressure tube furnace is risen to 900��1000 DEG C, then keep temperature constant and in described quartz ampoule, pass into the air in the noble gas eliminating quartz ampoule that purity is 99.99% more than with feeder;
(3) pass into carbon-source gas and quartz ampoule is carried out plating carbon
The flow of noble gas is adjusted to 30��70mL/min, then to passing into acetylene in quartz ampoule, quartz ampoule carrying out plating carbon with the speed that flow is 2��5mL/min with feeder, the time passing into acetylene when the breather of described feeder is in quartz ampoule a fixed position is 5��10 minutes;
(4) quartz ampoule of plating carbon is carried out post processing
Plating carbon closes feeder after terminating, and takes out the quartz socket tube in tube furnace and passes into the noble gas that purity is more than 99.99% in quartz socket tube so that it is at room temperature cooling down, and namely obtains the quartz ampoule of plating carbon.
2. the plating carbon method of the quartz ampoule for crystal growth according to claim 1, it is characterised in that described plating carbon humidity province refer to tube furnace heat up after in-furnace temperature be the region of 900��1000 DEG C.
3. the plating carbon method of the quartz ampoule for crystal growth according to claim 2, it is characterised in that described in-furnace temperature is obtained by temperature field test in stove.
4. the plating carbon method of the quartz ampoule for crystal growth according to claim 1, it is characterised in that the flow passing into the noble gas that purity is more than 99.99% described in step (2) is not less than 70mL/min, and the time that passes into is no less than 10min.
5. the plating carbon method of the quartz ampoule for crystal growth according to claim 1, it is characterised in that pass into described in step (3) carbon-source gas quartz ampoule is carried out plating carbon time inert gas flow be 50mL/min, acetylene flow is 5mL/min.
6. the plating carbon method of the quartz ampoule for crystal growth according to claim 1, it is characterised in that described noble gas is nitrogen or argon.
7. the plating carbon method of the quartz ampoule for crystal growth according to claim 1, it is characterized in that described feeder includes noble gas controller, acetylene controller, breather, described noble gas controller connects with breather, acetylene controller connects with breather, and the gas outlet of noble gas controller and acetylene controller is respectively arranged to control the valve of gas conveying.
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| CN105483825B (en) * | 2015-12-11 | 2018-09-25 | 华中科技大学 | A kind of bromine lead caesium method for preparing single crystal |
| 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 |
| 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 |
| CN112851138B (en) * | 2020-12-26 | 2021-07-23 | 云南农业大学 | Smoked carbon device of quartz ampoule wall |
| CN115259684B (en) * | 2022-08-02 | 2024-03-08 | 安徽光智科技有限公司 | Carbon plating method for quartz device |
| 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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| CN101109077A (en) * | 2007-08-21 | 2008-01-23 | 西安电子科技大学 | Method of plasma chemistry vapor depositing fluoridation amorphous carbon membrane and membrane layer structure thereof |
| CN202829838U (en) * | 2012-11-06 | 2013-03-27 | 马天慧 | Device for plating cracked carbon on quartz tubes or graphite crucibles |
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| TWI434949B (en) * | 2012-03-14 | 2014-04-21 | Nat Univ Tsing Hua | Chemical vapor deposition of graphene on dielectrics |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101109077A (en) * | 2007-08-21 | 2008-01-23 | 西安电子科技大学 | Method of plasma chemistry vapor depositing fluoridation amorphous carbon membrane and membrane layer structure thereof |
| CN202829838U (en) * | 2012-11-06 | 2013-03-27 | 马天慧 | Device for plating cracked carbon on quartz tubes or graphite crucibles |
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