CN114105682B - Improved method and device for prolonging service life of graphite crucible - Google Patents
Improved method and device for prolonging service life of graphite crucible Download PDFInfo
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- CN114105682B CN114105682B CN202111419330.0A CN202111419330A CN114105682B CN 114105682 B CN114105682 B CN 114105682B CN 202111419330 A CN202111419330 A CN 202111419330A CN 114105682 B CN114105682 B CN 114105682B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 124
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 106
- 239000010439 graphite Substances 0.000 title claims abstract description 106
- 238000000034 method Methods 0.000 title claims abstract description 42
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 68
- 239000011248 coating agent Substances 0.000 claims abstract description 57
- 238000000576 coating method Methods 0.000 claims abstract description 57
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 38
- 239000010937 tungsten Substances 0.000 claims abstract description 38
- 238000005507 spraying Methods 0.000 claims abstract description 29
- 238000005087 graphitization Methods 0.000 claims abstract description 27
- 239000000843 powder Substances 0.000 claims abstract description 27
- 239000011812 mixed powder Substances 0.000 claims abstract description 26
- 229910052751 metal Inorganic materials 0.000 claims abstract description 25
- 239000002184 metal Substances 0.000 claims abstract description 25
- 239000000758 substrate Substances 0.000 claims abstract description 22
- 238000007750 plasma spraying Methods 0.000 claims abstract description 16
- 238000005498 polishing Methods 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 9
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 8
- 229910001930 tungsten oxide Inorganic materials 0.000 claims abstract description 8
- 150000003841 chloride salts Chemical class 0.000 claims abstract description 7
- 239000000243 solution Substances 0.000 claims description 16
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 10
- 238000001354 calcination Methods 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 9
- 238000004140 cleaning Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 5
- 230000001681 protective effect Effects 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 4
- UYJXRRSPUVSSMN-UHFFFAOYSA-P ammonium sulfide Chemical compound [NH4+].[NH4+].[S-2] UYJXRRSPUVSSMN-UHFFFAOYSA-P 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 3
- 238000000605 extraction Methods 0.000 claims description 3
- 238000005342 ion exchange Methods 0.000 claims description 3
- 238000001694 spray drying Methods 0.000 claims description 3
- 238000004073 vulcanization Methods 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 230000008569 process Effects 0.000 abstract description 21
- 230000002035 prolonged effect Effects 0.000 abstract description 6
- 230000007246 mechanism Effects 0.000 description 20
- 238000003825 pressing Methods 0.000 description 16
- 238000010438 heat treatment Methods 0.000 description 10
- 239000000463 material Substances 0.000 description 10
- 238000007789 sealing Methods 0.000 description 10
- 230000000694 effects Effects 0.000 description 9
- 238000001514 detection method Methods 0.000 description 8
- 238000004321 preservation Methods 0.000 description 7
- 239000011159 matrix material Substances 0.000 description 5
- 238000002844 melting Methods 0.000 description 5
- 230000008018 melting Effects 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- 238000005299 abrasion Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000003870 refractory metal Substances 0.000 description 4
- 239000002699 waste material Substances 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000010720 hydraulic oil Substances 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 229920000049 Carbon (fiber) Polymers 0.000 description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000004917 carbon fiber Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000011800 void material Substances 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000002679 ablation Methods 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 229910052735 hafnium Inorganic materials 0.000 description 1
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 239000010955 niobium Substances 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
- C04B41/88—Metals
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/51—Metallising, e.g. infiltration of sintered ceramic preforms with molten metal
- C04B41/5133—Metallising, e.g. infiltration of sintered ceramic preforms with molten metal with a composition mainly composed of one or more of the refractory metals
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/02—Pretreatment of the material to be coated, e.g. for coating on selected surface areas
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
- C23C4/06—Metallic material
- C23C4/067—Metallic material containing free particles of non-metal elements, e.g. carbon, silicon, boron, phosphorus or arsenic
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
- C23C4/134—Plasma spraying
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
- F27B17/00—Furnaces of a kind not covered by any preceding group
- F27B17/0016—Chamber type furnaces
- F27B17/0041—Chamber type furnaces specially adapted for burning bricks or pottery
- F27B17/005—Chamber type furnaces specially adapted for burning bricks or pottery with cylindrical chambers
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
- F27B17/00—Furnaces of a kind not covered by any preceding group
- F27B17/0016—Chamber type furnaces
- F27B17/0041—Chamber type furnaces specially adapted for burning bricks or pottery
- F27B17/0075—Heating devices therefor
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- 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
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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Abstract
The invention relates to the technical field of graphitizing furnaces, in particular to an improved method and device for prolonging the service life of a graphite crucible. The improved method for prolonging the service life of the graphite crucible comprises the following steps: preparing mixed powder: tungsten oxide, Si powder, C powder and chloride salt are mixed according to the mass ratio of 45-60: 15-30: 10-25: 5-30, mixing uniformly to obtain mixed powder; pretreatment: polishing a graphite crucible substrate, and carrying out pretreatment to obtain an activated graphite crucible; primary bath: carrying out primary bath on the activated graphite crucible in the mixed powder to obtain a graphite crucible with a primary tungsten coating; secondary spraying: and carrying out plasma spraying on the surface of the graphite crucible with the primary tungsten coating by using the spraying powder containing the metal tungsten powder to obtain the graphite crucible with the gradient tungsten coating. The method can prevent the graphite crucible from being oxidized and even broken in the graphitization process; the service life is prolonged.
Description
Technical Field
The invention relates to the technical field of graphitization furnaces, in particular to an improved method and device for prolonging the service life of a graphite crucible.
Background
The graphitization furnace is mainly used for high-temperature treatment of sintering and graphitization of carbon materials, graphitization of PI films, graphitization of heat conduction materials, sintering of carbon fiber ropes, sintering graphitization of carbon fiber filaments, purification of graphite powder, other materials capable of being graphitized in a carbon environment and the like. Its use temperature is up to 3000 deg.C. High production efficiency, energy saving and electricity saving.
The main heating furnace type of the prior industrial graphitization production of carbon is an Acheson furnace, and the principle of the Acheson furnace graphitization heating is that the resistance material between products is heated firstly, then the products in the resistance material are heated, and finally the products and the resistance material are heated together to reach the preset temperature. Because the heating process is achieved through self-heating of the resistance materials and products, the heating condition in the whole furnace is difficult to predict and control, so that the temperature difference of each heating point in the Acheson furnace is generally large, and the temperature difference of each position in the furnace is large after power transmission is finished.
The current Acheson furnace temperature measuring means mainly uses a graphite crucible to be directly inserted into a furnace core part and obtains temperature data of each part through an infrared temperature measuring instrument. Because of the high graphitization final temperature, many graphite crucibles oxidize or even break before reaching the final temperature, and the final temperature cannot be measured.
Disclosure of Invention
In view of the deficiencies of the prior art, it is a first technical object of the present invention to provide an improved method for increasing the service life of a graphite crucible.
In view of the deficiencies of the prior art, a second technical object of the present invention is to provide an improved apparatus for increasing the service life of a graphite crucible.
The first technical object of the present invention is achieved by the following technical solutions:
an improved method for increasing the service life of a graphite crucible, comprising the steps of:
(1) preparing mixed powder: tungsten oxide, Si powder, C powder and chloride salt are mixed according to the mass ratio of 45-60: 15-30: 10-25: 5-30, mixing uniformly to obtain mixed powder;
(2) pretreatment: polishing a graphite crucible substrate, and carrying out pretreatment to obtain an activated graphite crucible;
(3) primary bath: carrying out primary bath on the activated graphite crucible in the mixed powder to obtain a graphite crucible with a primary tungsten coating;
(4) secondary spraying: and carrying out plasma spraying on the surface of the graphite crucible with the primary tungsten coating by using spraying powder containing metal tungsten powder to obtain the graphite crucible with the gradient tungsten coating.
The method adopts three steps of pretreatment, primary bath and secondary spraying to prepare the graphite crucible base material, improves the physical and chemical compatibility of the metal tungsten, improves the spraying effect by increasing the powder fluidity through granulating and spheroidizing the metal tungsten powder, improves the bonding strength of the plasma spraying outer coating and the matrix, and prevents the graphite crucible from being oxidized and even broken in the graphitization process; and finally, preparing the graphite crucible with the gradient tungsten coating, wherein the whole coating is well combined with the graphite crucible substrate, and the graphite crucible has the excellent performance of metal tungsten while maintaining the excellent performance of the graphite crucible such as strength.
Tungsten is the highest melting refractory metal. Metals having a melting point above 1650 ℃ and a certain reserve, as well as metals having a melting point above the melting point of zirconium (1852 ℃), are generally referred to as refractory metals. Typical refractory metals are tungsten, tantalum, molybdenum, niobium, hafnium, chromium, vanadium, zirconium and titanium. The most important advantages of tungsten, a refractory metal, are its good high temperature strength, good corrosion resistance to molten alkali metals and vapors, and its oxide volatilization and liquid phase oxide only at temperatures above 1000 c. However, it also has the disadvantage of a high plastic-brittle transition temperature and difficulty in plastic working at room temperature.
The metal tungsten (W) is the metal with the highest known melting point at present, has the characteristics of high strength, high elastic modulus, low thermal expansion coefficient and the like, and is a good ablation-resistant material.
The graphite crucible coating prepared by the invention has excellent performance, and has the advantages of low cost, small pollution and easy realization of large-scale efficient production.
Preferably, the pretreatment of step (2) comprises polishing the graphite crucible substrate to roughen the surface, then ultrasonically cleaning the graphite crucible substrate in absolute ethyl alcohol, then soaking the graphite crucible substrate in a sodium carbonate solution, then soaking the graphite crucible substrate in a nitric acid solution, then washing the graphite crucible substrate with water, and finally airing the graphite crucible substrate in air or drying the graphite crucible substrate in an oven.
The specific pretreatment process can improve the bonding strength of the subsequent plasma spraying outer coating and the matrix, and prevent the graphite crucible from being oxidized and even broken in the graphitization process.
Preferably, the preliminary bath in the step (3) includes burying the activated graphite crucible in the mixed powder, putting the whole into a high-temperature vacuum graphitization furnace, preserving the heat for 1-1.5h at 3000-3500 ℃ in an argon protective atmosphere, polishing with abrasive paper to flatten the surface of the coating, cleaning and drying to obtain the graphite crucible with the primary tungsten coating.
The specific initial bath process can improve the bonding strength of the subsequent plasma spraying outer coating and the matrix and prevent the graphite crucible from being oxidized and even broken in the graphitization process.
Preferably, the plasma spraying process in the step (4) is as follows: 70-80KW of spraying power, 90-100L/min of main air flow, 1.5-2.5r/min of powder feeding amount and 6-9cm of distance between the top end of the nozzle and the surface of the sample.
The specific plasma spraying process parameters of the invention can improve the bonding strength of the plasma spraying outer coating and the matrix and prevent the graphite crucible from being oxidized and even broken in the graphitization process.
Preferably, the preparation method of the spraying powder containing the metal tungsten powder in the step (4) comprises the following steps:
s1, adding metal tungsten powder into an ammonium tungstate aqueous solution, then adding ammonium sulfide for vulcanization, and then carrying out countercurrent exchange through an ion exchange column to collect the residual solution;
s2, extracting the residual liquid through an extraction system, standing for layering, and collecting an extract liquid;
s3, evaporating and crystallizing the extract, and then preparing spherical ammonium tungstate particles by adopting a spray drying method;
s4, microwave calcination: and calcining the spherical ammonium tungstate particles in a microwave calcining furnace to prepare the spraying powder containing the metal tungsten powder, wherein the obtained tungsten powder is spherical and has the particle size of 0.1-3 mu m.
The invention improves the spraying effect by performing granulation and spheroidization treatment on the metal tungsten powder to increase the powder fluidity.
The second technical object of the present invention is achieved by the following technical solutions:
a graphitization furnace, which is a high-temperature vacuum graphitization furnace used in the primary bath process in the step (3),
the furnace cover sealing mechanism is arranged on one side of the furnace mechanism;
the furnace mechanism comprises a furnace cover, a furnace body, a support frame and a vacuum pump, wherein a first fixing ring is fixedly connected to the top of the outer side of the furnace body, a second fixing ring is fixedly connected to the bottom of the outer side of the furnace cover, the support frame is installed at the bottom of the furnace body, and the air suction end of the vacuum pump is communicated with the furnace body through a pipeline;
the capping mechanism comprises a side frame, a first motor, a rotating shaft, a driving gear, a driven wheel, a hydraulic oil cylinder, a hydraulic rod, a lifting plate, a second motor, a screw rod, a pressing block and a pressing rod, wherein the first motor is fixedly connected to the side frame through a bolt, the rotating shaft is welded with an output shaft of the first motor, the driving gear is welded to the rotating shaft, the top of the side frame is rotatably connected with the driven wheel, the driving gear is meshed with the driven wheel, the driven wheel is fixedly connected with the bottom of the hydraulic oil cylinder through a bolt, an output shaft of the hydraulic oil cylinder is fixedly connected with the hydraulic rod, one end of the lifting plate is welded to the hydraulic rod, the second motor is installed on the lifting plate through a bolt, an output shaft of the second motor penetrates through the lifting plate and is welded with the screw rod, and the screw rod is in threaded connection with the pressing block, the pressure rod is welded on the pressure block.
The sealing mechanism of a general graphitizing furnace is used for pressing and sealing a furnace cover by manually screwing a sealing element on the periphery of the furnace cover, so that the operation is complicated, and the abrasion degree is increased during use, so that the service life is shortened; and the different pressure degrees around the furnace cover are easily caused, which is not beneficial to the use of the graphite crucible primary bath process in the step (3); the invention overcomes the defects of the prior art, the cover sealing mechanism compresses and seals the furnace mechanism through a mechanical automation structure, the automatic operation is simple and convenient, and the pressure of each point on the edge of the furnace cover is the same because the pressure point of the furnace cover is positioned at the center right above the furnace cover, thereby effectively reducing the abrasion degree of each point on the edge of the furnace cover when in use and prolonging the service life; the primary bath effect of the graphite crucible in the step (3) can be improved, so that the secondary spraying effect of the graphite crucible is improved, and the graphite crucible is prevented from being oxidized and even broken in the graphitization process; and the graphitizing furnace and the graphitizing crucible with prolonged service life can be mutually combined and matched in the graphitizing process, so that the service lives of the graphitizing crucible and the graphitizing furnace are further prolonged, and the effects of synergy and service life increase are achieved.
As a preferable technical scheme of the invention, the number of the pressure levers is four, the four pressure levers are distributed in a rectangular shape, and the bottom ends of the pressure levers are welded with the top of the furnace cover.
As a preferable technical scheme of the invention, a limiting rod is welded at the top of the furnace cover, and the top end of the limiting rod penetrates through the lifting plate and is in sliding connection with the lifting plate.
As a preferred technical scheme of the present invention, a sealing ring is bonded to the bottom of the second fixing ring, a positioning column is welded to the bottom of the second fixing ring, a positioning hole is formed in the first fixing ring, and the positioning column is matched with the positioning hole.
As a preferable technical scheme of the invention, the bottom of the furnace body is communicated with a waste discharge pipe, and the top of the furnace cover is communicated with an air inlet pipe.
As a preferred technical scheme of the invention, the inner side wall of the furnace body is fixedly connected with a heat preservation shell through a bottom plate, the inner side of the heat preservation shell is provided with a graphite crucible, and the outer side wall of the heat preservation shell is provided with a heating coil.
In conclusion, the invention has the following beneficial effects:
1. the method adopts three steps of pretreatment, primary bath and secondary spraying to prepare the graphite crucible base material, improves the physical and chemical compatibility of the metal tungsten, improves the spraying effect by increasing the powder fluidity through granulating and spheroidizing the metal tungsten powder, improves the bonding strength of the plasma spraying outer coating and the matrix, and prevents the graphite crucible from being oxidized and even broken in the graphitization process; finally, preparing the graphite crucible with the gradient tungsten coating, wherein the whole coating is well combined with the graphite crucible substrate, and the graphite crucible has excellent properties of metal tungsten while maintaining the excellent properties of the graphite crucible such as strength and the like;
2. the graphite crucible coating prepared by the method has excellent performance, and has the advantages of low cost, small pollution and easy realization of large-scale efficient production;
3. the sealing mechanism of a general graphitizing furnace is used for pressing and sealing a furnace cover by manually screwing a sealing element on the periphery of the furnace cover, so that the operation is complicated, and the abrasion degree is increased during use, so that the service life is shortened; and the different pressure degrees around the furnace cover are easily caused, which is not beneficial to the use of the graphite crucible primary bath process in the step (3); the invention overcomes the defects of the prior art, the cover sealing mechanism compresses and seals the furnace mechanism through a mechanical automation structure, the automatic operation is simple and convenient, and the pressure of each point on the edge of the furnace cover is the same because the pressure point of the furnace cover is positioned at the center right above the furnace cover, thereby effectively reducing the abrasion degree of each point on the edge of the furnace cover when in use and prolonging the service life; the primary bath effect of the graphite crucible in the step (3) can be improved, so that the secondary spraying effect of the graphite crucible is improved, and the graphite crucible is prevented from being oxidized and even broken in the graphitization process; and the graphitizing furnace and the graphitizing crucible with prolonged service life can be mutually combined and matched in the graphitizing process, so that the service lives of the graphitizing crucible and the graphitizing furnace are further prolonged, and the effects of synergy and service life increase are achieved.
Drawings
FIG. 1 is a schematic structural view of a graphitization furnace of the present invention;
FIG. 2 is an enlarged structural view of the region A of FIG. 1 according to the present invention;
FIG. 3 is an enlarged structural view of the region B shown in FIG. 1.
In the figure: 10. a furnace cover; 11. a furnace body; 12. a heat preservation shell; 13. a graphite crucible; 14. a heating coil; 15. a waste discharge pipe; 16. a support frame; 17. a vacuum pump; 18. an air inlet pipe; 111. a first retaining ring; 112. positioning holes; 121. a second fixing ring; 122. a seal ring; 123. a positioning column; 21. a side frame; 22. a first motor; 23. a rotating shaft; 24. a driving gear; 25. a driven wheel; 26. a hydraulic cylinder; 27. a hydraulic lever; 28. a lifting plate; 29. a limiting rod; 210. a second motor; 211. a screw rod; 212. briquetting; 213. a pressure lever.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
Example 1
An improved method for increasing the service life of a graphite crucible, comprising the steps of:
(1) preparing mixed powder: tungsten oxide, Si powder, C powder and chloride salt are mixed according to the mass ratio of 45: 15: 10: 30, uniformly mixing to obtain mixed powder;
(2) pretreatment: specifically, a graphite crucible substrate is polished to roughen the surface, then is ultrasonically cleaned in absolute ethyl alcohol, then is soaked in a sodium carbonate solution, then is soaked in a nitric acid solution, then is washed, and finally is placed in the air to be dried or is dried in an oven;
(3) primary bath: carrying out primary bath on the activated graphite crucible in the mixed powder to obtain a graphite crucible with a primary tungsten coating; embedding an activated graphite crucible in mixed powder, putting the whole body into a high-temperature vacuum graphitization furnace, preserving heat for 1h at 3000 ℃ under the protection of argon gas, polishing with abrasive paper to flatten the surface of a coating, cleaning and drying to obtain the graphite crucible with a primary tungsten coating;
(4) secondary spraying: carrying out plasma spraying on the surface of a graphite crucible with a primary tungsten coating by using spraying powder containing metal tungsten powder; the plasma spraying process comprises the following steps: spraying power of 70KW, main gas flow of 90L/min, powder delivery amount of 1.5r/min, and distance from the top end of the nozzle to the surface of the sample of 9 cm; obtaining the graphite crucible with the gradient tungsten coating.
Through detection, the graphite crucible outer coating with the gradient tungsten coating prepared by the invention is compact, the porosity of the outer coating is less than or equal to 1%, and the service life of the graphite crucible is 150% of the original service life.
Example 2
An improved method for increasing the service life of a graphite crucible, comprising the steps of:
(1) preparing mixed powder: mixing tungsten oxide, Si powder, C powder and chloride salt according to the mass ratio of 60: 30: 25: 5, uniformly mixing to obtain mixed powder;
(2) pretreatment: specifically, a graphite crucible substrate is polished to roughen the surface, then is ultrasonically cleaned in absolute ethyl alcohol, then is soaked in a sodium carbonate solution, then is soaked in a nitric acid solution, then is washed, and finally is placed in the air to be dried or is dried in an oven;
(3) primary bath: carrying out primary bath on the activated graphite crucible in the mixed powder to obtain a graphite crucible with a primary tungsten coating; embedding an activated graphite crucible in mixed powder, putting the whole into a high-temperature vacuum graphitization furnace, preserving heat for 1.5h at 3500 ℃ in an argon protective atmosphere, then polishing with abrasive paper to flatten the surface of a coating, cleaning and drying to obtain the graphite crucible with a primary tungsten coating;
(4) secondary spraying: carrying out plasma spraying on the surface of a graphite crucible with a primary tungsten coating by using spraying powder containing metal tungsten powder; the plasma spraying process comprises the following steps: the spraying power is 80KW, the main airflow is 100L/min, the powder feeding amount is 2.5r/min, and the distance from the top end of the nozzle to the surface of the sample is 6 cm; obtaining the graphite crucible with the gradient tungsten coating.
The detection proves that the graphite crucible outer coating with the gradient tungsten coating prepared by the invention is compact, the porosity of the outer coating is less than or equal to 1 percent, and the service life of the graphite crucible is 152 percent of the original service life.
Example 3
An improved method for increasing the service life of a graphite crucible, comprising the steps of:
(1) preparing mixed powder: mixing tungsten oxide, Si powder, C powder and chloride salt according to the mass ratio of 50: 20: 15: 20, uniformly mixing to obtain mixed powder;
(2) pretreatment: specifically, a graphite crucible substrate is polished to roughen the surface, then is ultrasonically cleaned in absolute ethyl alcohol, then is soaked in a sodium carbonate solution, then is soaked in a nitric acid solution, then is washed, and finally is placed in the air to be dried or is dried in an oven;
(3) primary bath: carrying out primary bath on the activated graphite crucible in the mixed powder to obtain a graphite crucible with a primary tungsten coating; embedding an activated graphite crucible in mixed powder, putting the whole body into a high-temperature vacuum graphitization furnace, preserving heat for 1.2h at 3200 ℃ under the argon protective atmosphere, then polishing by using abrasive paper to flatten the surface of a coating, cleaning and drying to obtain the graphite crucible with a primary tungsten coating;
(4) secondary spraying: carrying out plasma spraying on the surface of a graphite crucible with a primary tungsten coating by using spraying powder containing metal tungsten powder; the plasma spraying process comprises the following steps: the spraying power is 75KW, the main airflow is 95L/min, the powder feeding amount is 2r/min, and the distance from the top end of the nozzle to the surface of the sample is 8 cm; obtaining the graphite crucible with the gradient tungsten coating.
Through detection, the graphite crucible outer coating with the gradient tungsten coating prepared by the invention is compact, the void ratio of the outer coating is less than or equal to 1%, and the service life of the graphite crucible is 160% of the original service life.
Example 4
The same as example 1, except that the method for preparing the powder for spraying containing metallic tungsten powder comprises:
s1, adding metal tungsten powder into an ammonium tungstate aqueous solution, then adding ammonium sulfide for vulcanization, and then carrying out countercurrent exchange through an ion exchange column to collect the residual solution;
s2, extracting the residual liquid through an extraction system, standing and layering, and collecting extract liquor;
s3, evaporating and crystallizing the extract, and then preparing spherical ammonium tungstate particles by adopting a spray drying method;
s4, microwave calcination: and calcining the spherical ammonium tungstate particles in a microwave calcining furnace to prepare the spraying powder containing the metal tungsten powder, wherein the obtained tungsten powder is spherical and has the particle size of 0.1-3 mu m.
The detection proves that the graphite crucible outer coating with the gradient tungsten coating prepared by the invention is compact, the porosity of the outer coating is less than or equal to 1 percent, and the service life of the graphite crucible is 170 percent of the original service life.
Example 5
The same as example 4, except that a specific high-temperature vacuum graphitization furnace is used in the primary bath process of step (3), referring to fig. 1-3, the graphitization furnace includes a furnace mechanism and a capping mechanism, the capping mechanism is disposed at one side of the furnace mechanism; the capping mechanism compresses and seals the furnace mechanism through a mechanical automation structure.
Referring to fig. 1 and 3, the furnace mechanism includes a furnace cover 10, a furnace body 11, a support frame 16 and a vacuum pump 17, the top of the outer side of the furnace body 11 is fixedly connected with a first fixing ring 111, the bottom of the outer side of the furnace cover 10 is fixedly connected with a second fixing ring 121, the support frame 16 is installed at the bottom of the furnace body 11, and the suction end of the vacuum pump 17 is communicated with the furnace body 11 through a pipeline; first solid fixed ring 111 and the laminating of the solid fixed ring 121 of second compress tightly the back, can make bell 10 compress tightly the top of furnace body 11, the bottom of the solid fixed ring 121 of second bonds and has sealed circle 122, sealed circle 122 is used for improving the leakproofness, the bottom welding of the solid fixed ring 121 of second has reference column 123, has seted up locating hole 112 on the solid fixed ring 111 of first, reference column 123 and locating hole 112 phase-match for the position of location bell 10 prevents bell 10 skew center.
Referring to fig. 1 and 2, the capping mechanism includes a side frame 21, a first motor 22, a rotating shaft 23, a driving gear 24, a driven wheel 25, a hydraulic cylinder 26, a hydraulic rod 27, a lifting plate 28, a second motor 210, a screw rod 211, a pressing block 212 and a pressing rod 213, the first motor 22 is fixedly connected to the side frame 21 through a bolt, the rotating shaft 23 is welded to an output shaft of the first motor 22, the driving gear 24 is welded to the rotating shaft 23, the top of the side frame 21 is rotatably connected to the driven wheel 25, the driving gear 24 is engaged with the driven wheel 25, the first motor 22 drives the rotating shaft 23 to rotate, and further drives the driving gear 24 to rotate, the driven wheel 25 drives the hydraulic cylinder 26 to rotate, the furnace cover 10 is driven to rotate, the driven wheel 25 is fixedly connected to the bottom of the hydraulic cylinder 26 through a bolt, an output shaft of the hydraulic cylinder 26 is fixedly connected to the hydraulic rod 27, and the hydraulic cylinder 26 drives the hydraulic rod 27 to ascend or descend, and then the furnace cover 10 is driven to ascend or descend, one end of the lifting plate 28 is welded on the hydraulic rod 27, the second motor 210 is installed on the lifting plate 28 through a bolt, an output shaft of the second motor 210 penetrates through the lifting plate 28 and is welded with the screw rod 211, the screw rod 211 is in threaded connection with the pressing block 212, the pressing rod 213 is welded on the pressing block 212, and the second motor 210 drives the screw rod 211 to rotate, so that the pressing block 212 moves up and down, and further the furnace cover 10 is pressed tightly through the pressing rod 213. The number of the pressing rods 213 is four, the four pressing rods 213 are distributed in a rectangular shape, and the bottom ends of the pressing rods 213 are welded with the top of the furnace cover 10, so that the firmness of connection between the furnace cover 10 and the pressing block 212 is improved.
Specifically, referring to fig. 1, a limiting rod 29 is welded to the top of the furnace cover 10, and the top end of the limiting rod 29 penetrates through the lifting plate 28 and is slidably connected with the lifting plate 28 for guiding the furnace cover 10 to move.
Specifically, referring to fig. 1, the bottom of the furnace body 11 is connected to a waste discharge pipe 15, and the top of the furnace cover 10 is connected to an air inlet pipe 18. The waste discharge pipe 15 is used for discharging impurities and waste gas in the furnace body 11, the inner side wall of the furnace body 11 is fixedly connected with a heat preservation shell 12 through a bottom plate, a graphite crucible 13 is arranged on the inner side of the heat preservation shell 12, a heating coil 14 is arranged on the outer side wall of the heat preservation shell 12, and the heating coil 14 heats the graphite crucible 13.
The working principle is as follows: the capping mechanism compresses and seals the furnace mechanism through a mechanical automation structure. After the material drops into and accomplishes, first motor 22 drives pivot 23 and rotates, and then drive driving gear 24 and rotate, drive hydraulic cylinder 26 through following driving wheel 25 and rotate, it rotates to drive bell 10, make bell 10 be located directly over the furnace body 11, hydraulic cylinder 26 drives hydraulic stem 27 and rises or descends, tentatively drive bell 10 and cover furnace body 11, second motor 210 drives lead screw 211 and rotates, make briquetting 212 reciprocate, make briquetting 212 drive bell 10 push down furnace body 11, further compress tightly bell 10, automatic operation, and is simple and convenient, bell 10 edge each point pressure is the same, reduce the degree of wear of bell 10 edge each point, and service life is prolonged.
The detection shows that the service life of the graphite furnace is 155 percent of the original service life; the graphite crucible with the gradient tungsten coating prepared by the invention has compact outer coating, the void ratio of the outer coating is less than or equal to 1 percent, and the service life of the graphite crucible is 175 percent of the original service life.
Comparative example 1
The same as example 1, except that the mixed powder contained no tungsten oxide. Through detection, the porosity of the outer coating of the graphite crucible prepared by the embodiment is more than 8%, and the service life of the graphite crucible is 105% of the original service life.
Comparative example 2
The same as example 1, except that the mixed powder contained no Si powder and no C powder. Through detection, the porosity of the outer coating of the graphite crucible prepared by the embodiment is more than 6%, and the service life of the graphite crucible is 110% of the original service life.
Comparative example 3
The same as example 1, except that the mass ratio of the mixed powder is: tungsten oxide, Si powder, C powder and chloride salt are mixed according to the mass ratio of 30: 40: 25: 5, mixing the components. Through detection, the porosity of the outer coating of the graphite crucible prepared by the embodiment is more than 4%, and the service life of the graphite crucible is 115% of the original service life.
Finally, it should be noted that: in the description of the present invention, it should be noted that the terms "vertical", "upper", "lower", "horizontal", and the like indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience of describing the present invention and simplifying the description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present invention.
In the description of the present invention, it should also be noted that, unless otherwise explicitly specified or limited, the terms "disposed," "mounted," "connected," and "connected" are to be construed broadly and may, for example, be fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (3)
1. An improved method for prolonging the service life of a graphite crucible is characterized by comprising the following steps:
(1) preparing mixed powder: tungsten oxide, Si powder, C powder and chloride salt are mixed according to the mass ratio of 45-60: 15-30: 10-25: 5-30, mixing uniformly to obtain mixed powder;
(2) pretreatment: polishing a graphite crucible substrate, and carrying out pretreatment to obtain an activated graphite crucible;
(3) primary bath: carrying out primary bath on the activated graphite crucible in the mixed powder to obtain a graphite crucible with a primary tungsten coating; the preliminary bath in the step (3) comprises the steps of burying the activated graphite crucible in the mixed powder, then putting the activated graphite crucible into a high-temperature vacuum graphitization furnace integrally, preserving heat for 1-1.5h at 3000-3500 ℃ in an argon protective atmosphere, then polishing with abrasive paper to flatten the surface of the coating, cleaning and drying to obtain the graphite crucible with the primary tungsten coating;
(4) secondary spraying: and carrying out plasma spraying on the surface of the graphite crucible with the primary tungsten coating by using spraying powder containing metal tungsten powder to obtain the graphite crucible with the gradient tungsten coating.
2. An improved method of increasing the service life of a graphite crucible as claimed in claim 1, wherein: and (2) the pretreatment comprises the steps of polishing the graphite crucible substrate to roughen the surface, then ultrasonically cleaning the graphite crucible substrate in absolute ethyl alcohol, then soaking the graphite crucible substrate in a sodium carbonate solution, then soaking the graphite crucible substrate in a nitric acid solution, then washing the graphite crucible substrate with water, and finally airing the graphite crucible substrate in the air or drying the graphite crucible substrate in an oven.
3. An improved method of increasing the service life of a graphite crucible as claimed in claim 2, wherein: the preparation method of the spraying powder containing the metal tungsten powder in the step (4) comprises the following steps:
s1, adding metal tungsten powder into an ammonium tungstate aqueous solution, then adding ammonium sulfide for vulcanization, and then carrying out countercurrent exchange through an ion exchange column to collect the residual solution;
s2, extracting the residual liquid through an extraction system, standing for layering, and collecting an extract liquid;
s3, evaporating and crystallizing the extract, and then preparing spherical ammonium tungstate particles by adopting a spray drying method;
s4, microwave calcination: and calcining the spherical ammonium tungstate particles in a microwave calcining furnace to prepare the spraying powder containing the metal tungsten powder, wherein the obtained tungsten powder is spherical and has the particle size of 0.1-3 mu m.
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| US20090183995A1 (en) * | 2004-01-09 | 2009-07-23 | Nguyen Thinh T | Ceramic material for use at elevated temperature |
| CN101493284A (en) * | 2009-02-24 | 2009-07-29 | 上海大学 | Crucible for fusing titan and method of preparation thereof |
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