CN116102239A - Film coating process and preparation method of quartz large-caliber diffusion furnace tube for single crystal - Google Patents
Film coating process and preparation method of quartz large-caliber diffusion furnace tube for single crystal Download PDFInfo
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- CN116102239A CN116102239A CN202211732059.0A CN202211732059A CN116102239A CN 116102239 A CN116102239 A CN 116102239A CN 202211732059 A CN202211732059 A CN 202211732059A CN 116102239 A CN116102239 A CN 116102239A
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 170
- 239000010453 quartz Substances 0.000 title claims abstract description 152
- 238000002360 preparation method Methods 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 37
- 238000009792 diffusion process Methods 0.000 title claims abstract description 28
- 230000008569 process Effects 0.000 title claims abstract description 23
- 239000013078 crystal Substances 0.000 title claims abstract description 22
- 239000007888 film coating Substances 0.000 title description 2
- 238000009501 film coating Methods 0.000 title description 2
- 238000001704 evaporation Methods 0.000 claims abstract description 28
- 238000000576 coating method Methods 0.000 claims abstract description 22
- 230000008020 evaporation Effects 0.000 claims abstract description 20
- 239000002994 raw material Substances 0.000 claims abstract description 20
- 238000007740 vapor deposition Methods 0.000 claims abstract description 18
- 239000011248 coating agent Substances 0.000 claims abstract description 17
- 238000005906 dihydroxylation reaction Methods 0.000 claims abstract description 14
- 239000004576 sand Substances 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 238000000227 grinding Methods 0.000 claims abstract description 8
- 239000012943 hotmelt Substances 0.000 claims abstract description 7
- 239000000463 material Substances 0.000 claims description 28
- 238000004140 cleaning Methods 0.000 claims description 24
- 238000007747 plating Methods 0.000 claims description 22
- 238000010438 heat treatment Methods 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 14
- 229910018487 Ni—Cr Inorganic materials 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 230000001276 controlling effect Effects 0.000 claims description 10
- 239000007789 gas Substances 0.000 claims description 10
- 230000001105 regulatory effect Effects 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 239000003599 detergent Substances 0.000 claims description 8
- 238000002844 melting Methods 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 239000011812 mixed powder Substances 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 5
- 238000011010 flushing procedure Methods 0.000 claims description 5
- 238000010849 ion bombardment Methods 0.000 claims description 5
- 230000008018 melting Effects 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 238000005086 pumping Methods 0.000 claims description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 3
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 claims description 3
- 238000009835 boiling Methods 0.000 claims description 3
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 3
- 239000000292 calcium oxide Substances 0.000 claims description 3
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 3
- 230000008859 change Effects 0.000 claims description 3
- ZHPNWZCWUUJAJC-UHFFFAOYSA-N fluorosilicon Chemical compound [Si]F ZHPNWZCWUUJAJC-UHFFFAOYSA-N 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 3
- 150000002500 ions Chemical class 0.000 claims description 3
- 239000005543 nano-size silicon particle Substances 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 3
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 claims description 3
- 229910001950 potassium oxide Inorganic materials 0.000 claims description 3
- 238000010926 purge Methods 0.000 claims description 3
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims description 3
- 238000005201 scrubbing Methods 0.000 claims description 3
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims description 3
- 229910001948 sodium oxide Inorganic materials 0.000 claims description 3
- 238000005507 spraying Methods 0.000 claims description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 3
- 238000004804 winding Methods 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 238000011068 loading method Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 5
- 238000010407 vacuum cleaning Methods 0.000 abstract description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 107
- 230000000052 comparative effect Effects 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 230000029936 alkylation Effects 0.000 description 2
- 238000005804 alkylation reaction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000007689 inspection Methods 0.000 description 2
- 238000007737 ion beam deposition Methods 0.000 description 2
- 238000001755 magnetron sputter deposition Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000007738 vacuum evaporation Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000009751 slip forming Methods 0.000 description 1
- 239000011043 treated quartz Substances 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B20/00—Processes specially adapted for the production of quartz or fused silica articles, not otherwise provided for
-
- 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
- C03C17/001—General methods for coating; Devices therefor
- C03C17/003—General methods for coating; Devices therefor for hollow ware, e.g. containers
- C03C17/004—Coating the inside
-
- 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
- C03C17/06—Surface treatment of glass, not in the form of fibres or filaments, by coating with metals
- C03C17/09—Surface treatment of glass, not in the form of fibres or filaments, by coating with metals by deposition from the vapour phase
-
- 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
- C03C23/00—Other surface treatment of glass not in the form of fibres or filaments
- C03C23/0075—Cleaning of glass
-
- 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
- C03C23/00—Other surface treatment of glass not in the form of fibres or filaments
- C03C23/0085—Drying; Dehydroxylation
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a coating process and a preparation method of a quartz large-caliber diffusion furnace tube for single crystals, wherein the coating process comprises the following steps: s1, sequentially carrying out pretreatment, grinding and mixing, sand baking treatment, hot melt drawing and vacuum dehydroxylation treatment on the preparation raw materials of the quartz tube to obtain the quartz tube, and S2, preparing the pretreated quartz tube. The preparation method has reasonable process arrangement, simple preparation process and low pollution, the prepared quartz tube has excellent comprehensive performance, the service life and performance of electronic equipment can be effectively improved, the quartz tube is cleaned by a vacuum cleaning device consisting of a mechanical pump and a molecular pump air suction system, and the lower end of an evaporation wire is fixed with a heavy hammer to ensure that the evaporation wire is vertically fixed on quartzThe center of the tube is used as a vacuum chamber, the temperature of the quartz tube is maintained above 150deg.C, and the vacuum degree during vapor deposition is better than 1×10 ‑ 3 Pa, so that the coating film on the inner surface of the quartz tube is a simple and feasible method, so that the inner surface of the quartz tube with a larger aperture can be uniformly coated.
Description
Technical Field
The invention relates to the technical field of quartz products, in particular to a coating process and a preparation method of a quartz large-caliber diffusion furnace tube for single crystals.
Background
The quartz glass tube is special industrial technical glass manufactured by silicon dioxide, is a very excellent base material, and has a series of excellent physical and chemical properties and high temperature resistance: the softening point temperature of the quartz glass is about 1730 ℃, the quartz glass can be used for a long time at 1100 ℃, and the highest use temperature in a short time can reach 1450 ℃; corrosion resistance: apart from hydrofluoric acid, quartz glass hardly reacts chemically with other acids, in particular chemical stability at high temperatures; the heat stability is good: the thermal expansion coefficient of the quartz glass is extremely small, and the quartz glass can bear severe temperature change, and can not crack when being placed in the water of about 1100 ℃.
In the prior art, for example, the Chinese patent number is: the method for coating the inner wall of the quartz tube comprises five steps of cleaning the inner wall of the quartz tube, deionizing, amino silane alkylation, organifying and high-temperature carbon plating film forming, wherein the amino silane alkylation on the inner wall of the quartz tube is used for modifying the inner surface of the quartz tube, changing the hydrophilicity into hydrophobicity and improving the affinity with an organic reagent, so that the inner wall of the quartz tube is coated with the organic reagent, the organic reagent is dehydrated and carbonized at high temperature to form a layer of in-situ carbon film on the inner wall of the quartz tube, then the organic gas is carbonized at high temperature to provide a mobile carbon source, the film is continuously formed, and the film forming quality and thickness are controlled by controlling the film forming temperature and time, so that the film forming on the inner wall of the quartz tube is completed.
However, in the prior art, the defects of difficult processing, easy oxidation, poor filtering performance and the like of the quartz tube are caused by unreasonable preparation process links of the quartz tube; the existing common quartz tube coating methods comprise vacuum evaporation coating, ion beam deposition, magnetron sputtering coating and the like, but under the vacuum condition, molecules move into linear motion, and metal molecules cannot be deep into a quartz tube with a large length-diameter ratio, so that the methods are difficult to uniformly coat a conductive film in the quartz tube with a large diameter.
Therefore, we propose a quartz large-caliber diffusion furnace tube film plating process for single crystals and a preparation method thereof so as to solve the problems set forth in the above.
Disclosure of Invention
The invention aims to provide a quartz large-caliber diffusion furnace tube film plating process for single crystals and a preparation method thereof, so as to solve the defects that in the prior art, the quartz tube is difficult to process, easy to oxidize, poor in filtering performance and the like due to unreasonable preparation process links of the quartz tube; the existing common quartz tube coating methods comprise vacuum evaporation coating, ion beam deposition, magnetron sputtering coating and the like, but under the vacuum condition, molecules move into linear motion, and metal molecules cannot be deep into a quartz tube with a large length-diameter ratio, so that the methods have the problem that a conductive film is difficult to uniformly coat in the quartz tube with a large diameter.
In order to achieve the above purpose, the present invention provides the following technical solutions: a quartz large-caliber diffusion furnace tube film plating process for single crystals and a preparation method thereof comprise the following steps:
s1, sequentially carrying out pretreatment, grinding and mixing, sand baking treatment, hot melt drawing and vacuum dehydroxylation treatment on the preparation raw materials of the quartz tube to obtain the quartz tube.
S2, preparing a pretreated quartz tube.
S3, washing the quartz tube with a detergent and performing ion bombardment cleaning treatment.
S4, carrying out vapor deposition treatment on the quartz tube.
Preferably, in step S1, the preparation raw materials of the quartz tube are sequentially subjected to pretreatment, grinding and mixing, sand baking treatment, hot-melt drawing and vacuum dehydroxylation treatment, and the method comprises the following steps:
s11, treating the main material in the preparation raw material with hydrofluoric acid with the concentration of 12% for 15-20 minutes, then flushing with clean water and drying, adding a proper amount of deionized water into the auxiliary material, mixing and stirring to prepare viscous liquid with the concentration of 85%;
s12, adding the pretreated main materials and auxiliary materials into a ball mill, treating for 3-5 hours, controlling the temperature of the ball mill at 55-60 ℃, then sending the prepared mixed powder into a sand baking machine, controlling the temperature at 850-900 ℃, and continuously stirring and treating for 2-4 hours;
s13, controlling the temperature of the continuous melting furnace to be 2000-2200 ℃, and hot-melting the mixture at the temperature for 1-2 hours and drawing the mixture into a tube;
and S14, finally, carrying out vacuum dehydroxylation treatment on the formed quartz tube, wherein the temperature of the dehydroxylation treatment is controlled to be 900-1200 ℃, and the treatment time is 2.5-4 hours, so as to obtain the final quartz tube.
Preferably, in step S11, the main material in the raw material for preparing the quartz tube is nano silicon powder, and the auxiliary materials in the raw material for preparing the quartz tube include sodium oxide, potassium oxide, aluminum oxide, calcium oxide, titanium oxide and rare earth oxide.
Preferably, in step S2, a step of preparing a pre-treated quartz tube includes:
s21, placing the quartz tube into an ethanol aqueous solution, ultrasonically cleaning for 15-30min, and drying to obtain a clean quartz tube;
s22, coating a fluorine-silicon liquid film on the inner wall of the quartz tube, standing for 10-20S, and then rapidly cleaning to obtain a pretreated quartz tube;
s23, placing the quartz tube in the step S22 in a reaction kettle, spraying an aluminum isopropoxide solution into the reaction kettle, standing at a constant temperature for 20-30min, and purging with nitrogen for 30-50min;
s24, heating for 30-50min, and taking out the quartz tube to obtain the pretreated quartz tube.
Preferably, in step S3, the quartz tube is subjected to a detergent washing and ion bombardment cleaning treatment, comprising:
s31, placing the pretreated quartz tube in deionized water added with a detergent, boiling for 15-20min, then fully flushing with flowing water, scrubbing with acetone and ethanol, and finally drying with a drying device;
s32, loading the quartz tube into a cleaning device, and pumping the quartz tube into the device to 1 multiplied by 10 -5 Pa；
S33、Starting mechanical pump and molecular pump to pump air when vacuum degree is better than 1×10 -3 Stopping the molecular pump after Pa, regulating the discharge voltage to about 1700V, slowly charging Ar gas, carefully regulating the gas supply valve to ensure that the Ar gas is stably discharged in the quartz tube, cleaning the inner surface of the quartz tube by ions, and finally stopping discharging.
Preferably, in step S32, the cleaning device is composed of a mechanical pump and a molecular pump pumping system, and a weight is fixed to the lower end of the vapor deposition wire, so as to ensure that the vapor deposition wire is vertically fixed to the center of the quartz tube.
Preferably, in step S33, the discharge power source is used to provide a high voltage required for discharging in the quartz tube, and the energy required for evaporation of the vapor deposition wire is provided by the evaporation power source.
Preferably, in step S4, the vapor deposition treatment is performed on the quartz tube, including:
s41, restarting the molecular pump after discharge cleaning, baking the quartz tube, and when the temperature of the quartz tube is more than 200 ℃, the vacuum degree is better than 1 multiplied by 10 -3 After Pa, starting evaporation;
s42, the vapor plating wire is formed by winding nine Ni-Cr wires with the diameter of 0.2mm, and the Ni-Cr wires are slowly heated before formal vapor plating so that impurities on the surface of the vapor plating wire are thoroughly evaporated;
s43, heating current is gradually increased from 1A to 6A, each integral gear stays for 10min, and the evaporating wires gradually change from dark red to orange red along with the continuous increase of the heating current;
s44, in the state of 6A, the color of the pipe wall is found to be gradually deepened, which means that the Ni-Cr wires start to evaporate at the moment, the heating current of the evaporating wires is regulated to 6.1A so as to improve the evaporation rate, and after the evaporating is continuously carried out for 0.5h, the Ni-Cr wires are observed to be dark red in the pipe, and the pipe is opaque, which proves that the film is basically plated at the moment.
Compared with the prior art, the invention has the beneficial effects that:
1. the preparation method has the advantages that the quartz tube is obtained by sequentially carrying out pretreatment, grinding and mixing, sand baking treatment, hot melting and drawing and vacuum dehydroxylation treatment on the preparation raw materials of the quartz tube, the preparation method has reasonable process arrangement, simple and convenient preparation process, low pollution and moderate cost, and the prepared quartz tube has excellent comprehensive performance and can effectively improve the service life and performance of electronic equipment;
2. the invention cleans the quartz tube by a vacuum cleaning device composed of a mechanical pump and a molecular pump air suction system, and a heavy hammer is fixed at the lower end of the vapor plating wire, which ensures that the vapor plating wire is vertically fixed in the center of the quartz tube as a vacuum chamber, the temperature of the quartz tube must be kept above 150 ℃ and the vacuum degree during vapor plating is better than 1 multiplied by 10 -3 Pa, so that the film plating on the inner surface of the quartz tube is a simple and feasible method, thus a uniform and firm conductive film can be obtained on the inner surface of the quartz tube, and meanwhile, the inner surface of the quartz tube with larger aperture can be uniformly plated, thereby avoiding the problems of high cost and low efficiency caused by evaporation plating on a large vacuum system.
Drawings
FIG. 1 is a flow chart of a process for coating a quartz large-caliber diffusion furnace tube for single crystals and a preparation method thereof.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
Referring to fig. 1, the present invention provides a technical solution: a quartz large-caliber diffusion furnace tube film plating process for single crystals and a preparation method thereof comprise the following steps:
step one, preparing a quartz tube by sequentially carrying out pretreatment, grinding and mixing, sand baking treatment, hot melt drawing and vacuum dehydroxylation treatment on the preparation raw materials of the quartz tube.
11 Treating the main material in the preparation raw material with hydrofluoric acid with the concentration of 12 percent for 15-20 minutes, then flushing with clean water and drying, adding a proper amount of deionized water into the auxiliary material, mixing and stirring to prepare viscous liquid with the concentration of 85 percent; the main material in the raw material for preparing the quartz tube is nano silicon powder, and the auxiliary materials in the raw material for preparing the quartz tube comprise sodium oxide, potassium oxide, aluminum oxide, calcium oxide, titanium oxide and rare earth oxide.
12 Adding the pretreated main material and auxiliary material into a ball mill for treatment for 3-5 hours, controlling the temperature of the ball mill to be 55-60 ℃, then sending the prepared mixed powder into a sand baking machine, controlling the temperature to be 850-900 ℃, and continuously stirring for 2-4 hours.
13 Controlling the temperature of the continuous melting furnace to be 2000-2200 ℃, and drawing the mixture into a tube after hot melting for 1-2 hours at the temperature.
14 Finally, carrying out vacuum dehydroxylation treatment on the formed quartz tube, wherein the temperature of the dehydroxylation treatment is controlled to be 900-1200 ℃ and the treatment time is 2.5-4 hours, thus obtaining the final quartz tube.
And step two, preparing a pretreated quartz tube.
21 Placing the quartz tube into ethanol water solution, ultrasonically cleaning for 15-30min, and drying to obtain the clean quartz tube.
22 Coating the inner wall of the quartz tube with a fluorine-silicon liquid film, standing for 10-20s, and then rapidly cleaning to obtain the pretreated quartz tube.
23 Placing the quartz tube in the step S22 in a reaction kettle, spraying aluminum isopropoxide solution into the reaction kettle, standing at constant temperature for 20-30min, and purging with nitrogen for 30-50min.
24 Then heating for 30-50min, and taking out the quartz tube to obtain the pretreated quartz tube.
And thirdly, washing the quartz tube with a detergent and performing ion bombardment cleaning treatment.
31 Placing the pretreated quartz tube in deionized water with detergent, boiling for 15-20min, then washing with flowing water, scrubbing with acetone and ethanol, and finally drying with drying equipment.
32 The quartz tube is then placed in a cleaning apparatus and the apparatus is evacuated to 1X 10 -5 Pa; the cleaning device consists of a mechanical pump and a molecular pumpThe air extraction system is composed, and a heavy hammer is fixed at the lower end of the vapor deposition wire, so that the vapor deposition wire is ensured to be vertically fixed at the center of the quartz tube.
33 Opening mechanical pump and molecular pump to exhaust air when vacuum degree is better than 1 x 10 -3 Stopping the molecular pump after Pa, regulating the discharge voltage to about 1700V, slowly filling Ar gas, carefully regulating the gas supply valve to ensure that the Ar gas is stably discharged in the quartz tube, cleaning the inner surface of the quartz tube by ions, and stopping discharging finally; the discharge power supply is used for providing high voltage required by discharge in the quartz tube, and the energy required by evaporation of the vapor deposition wire is provided by the evaporation power supply.
And fourthly, carrying out evaporation treatment on the quartz tube.
41 After discharge cleaning, restarting the molecular pump, baking the quartz tube, when the temperature of the quartz tube is more than 200 ℃, the vacuum degree is better than 1 multiplied by 10 -3 After Pa, vapor deposition was started.
42 The vapor plating wire is formed by winding nine Ni-Cr wires with the diameter of 0.2mm, and the Ni-Cr wires are slowly heated before formal vapor plating so that impurities on the surface of the vapor plating wire are thoroughly evaporated.
43 The heating current is gradually increased from 1A to 6A, each integral gear stays for 10min, and the evaporation wire gradually changes from dark red to orange red along with the continuous increase of the heating current.
44 Under the condition of 6A, the color of the pipe wall is found to be gradually deepened, which means that the Ni-Cr wire is evaporated at the moment, the heating current of the evaporating wire is regulated to 6.1A to improve the evaporation rate, and after the continuous evaporation for 0.5h, the Ni-Cr wire is observed to be dark red in the pipe, and the pipe is opaque, which proves that the film is basically plated at the moment.
Example 2
The process and the preparation method for coating a quartz large-caliber diffusion furnace tube for single crystals provided by the embodiment are approximately the same as those of the embodiment 1, and the main differences are that:
in step S11, the main material in the preparation raw material is treated with hydrofluoric acid having a concentration of 10% for 15 minutes, and then washed with clean water and dried.
In the step S12, the pretreated main materials and auxiliary materials are added into a ball mill for treatment for 3-5 hours, the temperature of the ball mill is controlled at 55 ℃, and then the prepared mixed powder is sent into a sand baking machine, the temperature is controlled at 850-900 ℃, and the stirring treatment is continuously carried out for 2 hours.
In step S43, the heating current is gradually increased from 1A-6A, each integral gear stays for 10min, and the evaporation wire gradually changes from dark red to orange red along with the continuous increase of the heating current.
Example 3
The process and the preparation method for coating a quartz large-caliber diffusion furnace tube for single crystals provided by the embodiment are approximately the same as those of the embodiment 1, and the main differences are that:
in step S11, the main material in the preparation raw material is treated with hydrofluoric acid having a concentration of 12% for 20 minutes, and then washed with clean water and dried.
In the step S12, the pretreated main materials and auxiliary materials are added into a ball mill for treatment for 3-5 hours, the temperature of the ball mill is controlled at 60 ℃, and then the prepared mixed powder is sent into a sand baking machine, the temperature is controlled at 850-900 ℃, and the stirring treatment is continuously carried out for 3 hours.
In step S43, the heating current is gradually increased from 1A-4A, each integral gear stays for 10min, and the evaporation wire gradually changes from dark red to orange red along with the continuous increase of the heating current.
Comparative example 1
The process and the preparation method for coating a quartz large-caliber diffusion furnace tube for single crystals provided by the embodiment are approximately the same as those of the embodiment 1, and the main differences are that: in step S11, the main material in the preparation raw material is treated with hydrofluoric acid having a concentration of 10% for 20 minutes, and then washed with clean water and dried.
Comparative example 2
The process and the preparation method for coating a quartz large-caliber diffusion furnace tube for single crystals provided by the embodiment are approximately the same as those of the embodiment 1, and the main differences are that: in the step S12, the pretreated main materials and auxiliary materials are added into a ball mill for treatment for 3-5 hours, the temperature of the ball mill is controlled at 60 ℃, and then the prepared mixed powder is sent into a sand baking machine, the temperature is controlled at 850-900 ℃, and the stirring treatment is continuously carried out for 3 hours.
Comparative example 3
The process and the preparation method for coating a quartz large-caliber diffusion furnace tube for single crystals provided by the embodiment are approximately the same as those of the embodiment 1, and the main differences are that: in step S43, the heating current is gradually increased from 1A-4A, each integral gear stays for 10min, and the evaporation wire gradually changes from dark red to orange red along with the continuous increase of the heating current.
Inspection and analysis
The quartz large-caliber diffusion furnace tubes prepared in examples 1 to 3 and comparative examples 1 to 3 were taken, and the relevant performances of the prepared quartz large-caliber diffusion furnace tubes were examined, and the examination method is as follows:
the thermal stability of each quartz large-caliber diffusion furnace tube is respectively checked according to the detection standard GB/T10701-2008, the hydroxyl content of each quartz large-caliber diffusion furnace tube is respectively checked according to the detection standard GB/T12442-1990, the film-based binding force of each quartz large-caliber diffusion furnace tube is respectively checked according to the detection standard GB/T1732, and the obtained test results are recorded in Table 1;
table 1 quartz large diameter diffusion furnace tube inspection table
By analyzing the related data in the table, the quartz tube is obtained by sequentially carrying out pretreatment, grinding and mixing, sand baking treatment, hot melt drawing and vacuum dehydroxylation treatment on the preparation raw materials of the quartz tube, and the preparation method has reasonable procedure arrangement, simple and convenient preparation process, low pollution and moderate cost, and the prepared quartz tube has excellent comprehensive performance and can effectively improve the service life and performance of electronic equipment; the quartz tube is cleaned by a vacuum cleaning device consisting of a mechanical pump and a molecular pump air suction system, and the lower end of the vapor deposition wireA heavy hammer is fixed to ensure that the vapor deposition wire is vertically fixed in the center of the quartz tube as a vacuum chamber, the temperature of the quartz tube is maintained above 150 ℃ and the vacuum degree during vapor deposition is better than 1 multiplied by 10 -3 Pa, so that the film plating on the inner surface of the quartz tube is a simple and feasible method, thus a uniform and firm conductive film can be obtained on the inner surface of the quartz tube, and meanwhile, the inner surface of the quartz tube with larger aperture can be uniformly plated, thereby avoiding the problems of high cost and low efficiency caused by evaporation plating on a large vacuum system.
Although the present invention has been described with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments described, or equivalents may be substituted for elements thereof, and any modifications, equivalents, improvements and changes may be made without departing from the spirit and principles of the present invention.
Claims (8)
1. A quartz large-caliber diffusion furnace tube film plating process for single crystals and a preparation method thereof are characterized by comprising the following steps:
s1, sequentially carrying out pretreatment, grinding and mixing, sand baking treatment, hot melt drawing and vacuum dehydroxylation treatment on preparation raw materials of a quartz tube to obtain the quartz tube;
s2, preparing a pretreated quartz tube;
s3, washing the quartz tube with a detergent and performing ion bombardment cleaning treatment;
s4, carrying out vapor deposition treatment on the quartz tube.
2. The process and method for manufacturing a large diameter diffusion furnace tube of quartz for single crystal according to claim 1, wherein in step S1, the preparation raw material of the quartz tube is sequentially subjected to pretreatment, grinding and mixing, sand baking treatment, hot melt drawing and vacuum dehydroxylation, comprising the steps of:
s11, treating the main material in the preparation raw material with hydrofluoric acid with the concentration of 12% for 15-20 minutes, then flushing with clean water and drying, adding a proper amount of deionized water into the auxiliary material, mixing and stirring to prepare viscous liquid with the concentration of 85%;
s12, adding the pretreated main materials and auxiliary materials into a ball mill, treating for 3-5 hours, controlling the temperature of the ball mill at 55-60 ℃, then sending the prepared mixed powder into a sand baking machine, controlling the temperature at 850-900 ℃, and continuously stirring and treating for 2-4 hours;
s13, controlling the temperature of the continuous melting furnace to be 2000-2200 ℃, and hot-melting the mixture at the temperature for 1-2 hours and drawing the mixture into a tube;
and S14, finally, carrying out vacuum dehydroxylation treatment on the formed quartz tube, wherein the temperature of the dehydroxylation treatment is controlled to be 900-1200 ℃, and the treatment time is 2.5-4 hours, so as to obtain the final quartz tube.
3. The process and method for preparing a large-caliber diffusion furnace tube for single crystals according to claim 2, wherein in step S11, the main material in the raw material for preparing the quartz tube is nano silicon powder, and the auxiliary materials in the raw material for preparing the quartz tube include sodium oxide, potassium oxide, aluminum oxide, calcium oxide, titanium oxide and rare earth oxide.
4. The process and method for manufacturing a large diameter diffusion furnace tube of quartz for single crystal according to claim 1, wherein in step S2, the step of manufacturing a pretreated quartz tube comprises:
s21, placing the quartz tube into an ethanol aqueous solution, ultrasonically cleaning for 15-30min, and drying to obtain a clean quartz tube;
s22, coating a fluorine-silicon liquid film on the inner wall of the quartz tube, standing for 10-20S, and then rapidly cleaning to obtain a pretreated quartz tube;
s23, placing the quartz tube in the step S22 in a reaction kettle, spraying an aluminum isopropoxide solution into the reaction kettle, standing at a constant temperature for 20-30min, and purging with nitrogen for 30-50min;
s24, heating for 30-50min, and taking out the quartz tube to obtain the pretreated quartz tube.
5. The process and method for manufacturing a large diameter diffusion furnace tube of quartz for single crystal according to claim 1, wherein in step S3, the quartz tube is subjected to a detergent washing and ion bombardment cleaning treatment, comprising:
s31, placing the pretreated quartz tube in deionized water added with a detergent, boiling for 15-20min, then fully flushing with flowing water, scrubbing with acetone and ethanol, and finally drying with a drying device;
s32, loading the quartz tube into a cleaning device, and pumping the quartz tube into the device to 1 multiplied by 10 -5 Pa；
S33, starting a mechanical pump and a molecular pump for pumping, when the vacuum degree is better than 1 multiplied by 10 -3 Stopping the molecular pump after Pa, regulating the discharge voltage to about 1700V, slowly charging Ar gas, carefully regulating the gas supply valve to ensure that the Ar gas is stably discharged in the quartz tube, cleaning the inner surface of the quartz tube by ions, and finally stopping discharging.
6. The process for coating a film on a large diameter diffusion furnace tube of quartz for single crystal according to claim 5, wherein in step S32, the cleaning device comprises a mechanical pump and a molecular pump pumping system, and a weight is fixed at the lower end of the vapor deposition wire to ensure that the vapor deposition wire is vertically fixed at the center of the quartz tube.
7. The process and method for manufacturing a large diameter diffusion furnace tube of quartz for single crystal according to claim 5, wherein in step S33, the discharge power source is used to provide high voltage required for discharging in the quartz tube, and the energy required for evaporating the vapor deposition wire is provided by the evaporation power source.
8. The process for coating a large diameter diffusion furnace tube of quartz for single crystal according to claim 1, wherein in step S4, the vapor deposition treatment is performed on the quartz tube, comprising:
s41, restarting the molecular pump after discharge cleaning, baking the quartz tube, and when the temperature of the quartz tube is more than 200 ℃, the vacuum degree is better than 1 multiplied by 10 -3 After Pa, starting evaporation;
s42, the vapor plating wire is formed by winding nine Ni-Cr wires with the diameter of 0.2mm, and the Ni-Cr wires are slowly heated before formal vapor plating so that impurities on the surface of the vapor plating wire are thoroughly evaporated;
s43, heating current is gradually increased from 1A to 6A, each integral gear stays for 10min, and the evaporating wires gradually change from dark red to orange red along with the continuous increase of the heating current;
s44, in the state of 6A, the color of the pipe wall is found to be gradually deepened, which means that the Ni-Cr wires start to evaporate at the moment, the heating current of the evaporating wires is regulated to 6.1A so as to improve the evaporation rate, and after the evaporating is continuously carried out for 0.5h, the Ni-Cr wires are observed to be dark red in the pipe, and the pipe is opaque, which proves that the film is basically plated at the moment.
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