CN115072732A - Preparation method of titanium diboride ultrafine powder - Google Patents
Preparation method of titanium diboride ultrafine powder Download PDFInfo
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- CN115072732A CN115072732A CN202210668142.XA CN202210668142A CN115072732A CN 115072732 A CN115072732 A CN 115072732A CN 202210668142 A CN202210668142 A CN 202210668142A CN 115072732 A CN115072732 A CN 115072732A
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- QYEXBYZXHDUPRC-UHFFFAOYSA-N B#[Ti]#B Chemical compound B#[Ti]#B QYEXBYZXHDUPRC-UHFFFAOYSA-N 0.000 title claims abstract description 67
- 229910033181 TiB2 Inorganic materials 0.000 title claims abstract description 67
- 239000000843 powder Substances 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000000126 substance Substances 0.000 claims abstract description 92
- 239000000047 product Substances 0.000 claims abstract description 56
- 150000003839 salts Chemical class 0.000 claims abstract description 53
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 50
- 239000002131 composite material Substances 0.000 claims abstract description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000008367 deionised water Substances 0.000 claims abstract description 29
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 29
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 28
- 239000010431 corundum Substances 0.000 claims abstract description 28
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 25
- 238000001035 drying Methods 0.000 claims abstract description 24
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000006227 byproduct Substances 0.000 claims abstract description 16
- 238000001816 cooling Methods 0.000 claims abstract description 15
- 238000002156 mixing Methods 0.000 claims abstract description 15
- 238000001914 filtration Methods 0.000 claims abstract description 14
- 239000000203 mixture Substances 0.000 claims abstract description 14
- 238000000227 grinding Methods 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- 238000001354 calcination Methods 0.000 claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000001291 vacuum drying Methods 0.000 claims abstract description 10
- 239000012300 argon atmosphere Substances 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims description 30
- 238000012360 testing method Methods 0.000 claims description 28
- 239000002245 particle Substances 0.000 claims description 22
- 238000004140 cleaning Methods 0.000 claims description 10
- BUKHSQBUKZIMLB-UHFFFAOYSA-L potassium;sodium;dichloride Chemical group [Na+].[Cl-].[Cl-].[K+] BUKHSQBUKZIMLB-UHFFFAOYSA-L 0.000 claims description 10
- 238000013329 compounding Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 11
- 238000005406 washing Methods 0.000 abstract description 6
- 239000002994 raw material Substances 0.000 abstract description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 24
- 239000010936 titanium Substances 0.000 description 22
- 229910052719 titanium Inorganic materials 0.000 description 21
- OMOVVBIIQSXZSZ-UHFFFAOYSA-N [6-(4-acetyloxy-5,9a-dimethyl-2,7-dioxo-4,5a,6,9-tetrahydro-3h-pyrano[3,4-b]oxepin-5-yl)-5-formyloxy-3-(furan-3-yl)-3a-methyl-7-methylidene-1a,2,3,4,5,6-hexahydroindeno[1,7a-b]oxiren-4-yl] 2-hydroxy-3-methylpentanoate Chemical compound CC12C(OC(=O)C(O)C(C)CC)C(OC=O)C(C3(C)C(CC(=O)OC4(C)COC(=O)CC43)OC(C)=O)C(=C)C32OC3CC1C=1C=COC=1 OMOVVBIIQSXZSZ-UHFFFAOYSA-N 0.000 description 15
- 239000012071 phase Substances 0.000 description 13
- 238000002474 experimental method Methods 0.000 description 12
- 239000000463 material Substances 0.000 description 11
- 238000006243 chemical reaction Methods 0.000 description 10
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- 239000000919 ceramic Substances 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 7
- 239000007788 liquid Substances 0.000 description 7
- 238000005054 agglomeration Methods 0.000 description 6
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical group O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
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- 239000012429 reaction media Substances 0.000 description 2
- 230000003014 reinforcing effect Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 229910010271 silicon carbide Inorganic materials 0.000 description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 102100023904 Nuclear autoantigenic sperm protein Human genes 0.000 description 1
- 101710149564 Nuclear autoantigenic sperm protein Proteins 0.000 description 1
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- UQZIWOQVLUASCR-UHFFFAOYSA-N alumane;titanium Chemical compound [AlH3].[Ti] UQZIWOQVLUASCR-UHFFFAOYSA-N 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000011362 coarse particle Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
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- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
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- 230000008020 evaporation Effects 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000005242 forging Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 235000000396 iron Nutrition 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229910052575 non-oxide ceramic Inorganic materials 0.000 description 1
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- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052574 oxide ceramic Inorganic materials 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000010587 phase diagram Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
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- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000005488 sandblasting Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 description 1
- 238000005491 wire drawing Methods 0.000 description 1
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
- C01B35/02—Boron; Borides
- C01B35/04—Metal borides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- 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
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/5805—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on borides
- C04B35/58064—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on borides based on refractory borides
- C04B35/58071—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on borides based on refractory borides based on titanium borides
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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Abstract
The invention relates to a preparation method of titanium diboride ultrafine powder, which comprises the following steps: putting the composite molten salt into a vacuum drying oven for drying to remove moisture, so as to obtain a first substance; mixing titanium dioxide and boron powder to obtain a second substance; mixing the first and second substances, manually grinding to uniformly mix the first and second substances, and placing the mixture into a corundum crucible; putting the corundum crucible into a tubular furnace for calcination, heating and keeping the temperature for a period of time under the protection of argon atmosphere, and then cooling to obtain a third substance; taking out the third substance cooled to room temperature, dissolving the third substance in deionized water, and removing residual salt and byproducts to obtain a fourth substance; and filtering the fourth substance, repeatedly washing with deionized water and absolute ethyl alcohol, and drying a product obtained by filtering to obtain the required product. The production process is simple, environment-friendly, and free of generation and residue of high-risk substances in the production process and after delivery; the product of the invention has relatively low raw material price and good product performance.
Description
Technical Field
The invention relates to a preparation technology of high-end ceramic powder, and more particularly relates to a preparation method of titanium diboride ultrafine powder.
Background
The titanium-based composite material has good room-temperature mechanical properties, and has good strength, hardness, wear resistance, firmness and the like under the condition of not high temperature (generally below 600 ℃). Until now, research on the discontinuous reinforced titanium-based composite material has achieved certain achievement, and some research achievements have been applied to the fields of aerospace, automobile manufacturing, heavy machinery and the like. On the basis of a matrix, the strength and hardness of the titanium-based composite material are greatly improved by adding the reinforcing phase, and the types of the reinforcing phase mainly comprise TiC and TiB at present 2 、SiC、B 4 C. TiB, and the like. Wherein TiB 2 Has the characteristics of stable structure, high hardness, small difference of thermal expansion coefficients between titanium matrixes, mutual solubility and the like which are incomparable with other reinforced phases, thereby becoming the titanium matrix composite material reinforcement which is most widely applied at present. Further, titanium diboride (TiB) 2 ) The ceramic powder is more suitable for being used under the working conditions of high temperature and high erosion than tungsten carbide (WC) ceramic powder. Titanium diboride powder is gray (or grayish black) with the sixth highest melting point material ranking in the world currently known. The oxidation resistance temperature in the air can reach 1100 ℃, and the ceramic material has excellent physical and chemical properties, high hardness except a high melting point, excellent chemical stability, excellent electrical and thermal conductivity and excellent mechanical properties at high temperature.
The titanium diboride and the composite material thereof can be compounded with other metals and ceramic-based polymers to form a series of novel materials with commercial application values. The application range of the titanium diboride is wider, and specifically: (1) the titanium diboride can be used as a grain refining and particle strengthening additive and is doped into aluminum-based, copper-based titanium-aluminum alloys and iron-based materials, so that the mechanical mechanics and physical and chemical properties of the materials can be greatly improved. This grain refinement and grain strengthening effect will increase with the increase in purity and fineness of the titanium diboride powder; (2) titanium diboride can be compounded with non-oxide ceramics such as silicon carbide, aluminum nitride, boron nitride, titanium carbide and the like, and can also be compounded with oxide ceramic materials such as aluminum oxide and the like, and a large number of experimental studies show that the prepared novel composite material has more excellent mechanical strength and fracture toughness resistance, and can be used for manufacturing one of excellent materials of armor protection materials; (3) the titanium diboride particles are doped with high-performance resin to be prepared into PTC heating ceramics and head type PTC materials, so that the PTC heating ceramics and head type PTC materials have the characteristics of safety, electricity saving, reliability, easy processing and forming and the like, and are a key high-tech technology for updating household appliances such as electric irons, electric blankets, electric ovens, air conditioner hot air greenhouses and the like; (4) the titanium diboride has excellent conductivity and excellent erosion resistance to molten metal, and can be used for manufacturing evaporation vessels, molten metal crucibles, aluminum electrolysis bath cathodes, spark plugs and other electrode and contact starting materials; (5) because of good wettability of titanium diboride and molten metal aluminum, the titanium diboride is used as the cathode coating material of the aluminum electrolytic cell, so that the power consumption of the aluminum electrolytic cell can be reduced, and the service life of the aluminum electrolytic cell is prolonged; (6) titanium diboride can be used to make ceramic cutting tools and dies, and can be used to make finishing tools, wire drawing dies, extrusion dies, sand blasting nozzles, sealing elements, etc.
Research on titanium-based composites originated in the 70 s, and at the mid-80 s, it has been vigorously developed under the plans of the american space shuttle (NASP), the Integrated High Performance Turbine Engine Technology (IHPTET), and the like, as well as similar plans in europe and japan. At present, foreign research focuses mainly on continuous fiber reinforced titanium-based composite materials, while domestic focus focuses on particle reinforced titanium-based composite materials, and because the domestic research time of titanium alloy and titanium-based composite materials is short, a large amount of titanium-based composite materials with excellent tissue properties are prepared by imitating and autonomously researching the existing foreign materials with better properties. The use of TiC and TiB reinforced titanium matrix composites is produced by Dynamet Technology, USA, for various production applications. The method comprises the steps of obtaining a TiB reinforced titanium-based composite material with uniform components and compact structure by a powder metallurgy method by the Toyota Japan company, forging and extruding a cast ingot to finally form an air inlet valve and an air outlet valve on an automobile engine, and applying the TiB reinforced titanium-based composite material to a Toyota Altezza automobile.
However, the quality of titanium diboride powder determines the performance of the product, and the current method for preparing titanium diboride generally has the defect of coarse particle size of the synthesized powder, so the preparation technology for obtaining high-end superfine titanium diboride powder is an opportunity and a challenge.
Therefore, the preparation method of the titanium diboride ultrafine powder is expected.
Disclosure of Invention
Aiming at the defects of the prior art, the invention mainly aims to provide a method for preparing solid-liquid combined high-end titanium diboride superfine powder, which utilizes a titanium source (titanium dioxide) and a boron source which are cheap and a dangerous reducing agent and adopts a scheme with short flow and low cost to prepare the high-end titanium diboride superfine powder which has high yield, short production period, no environmental pollution and certain industrial popularization. The invention forms a controllable synthesis process technology for preparing the titanium diboride high-end superfine powder in a solid-liquid combined mode and short flow, and a key technology for obtaining the superfine powder with uniform chemical composition.
In order to solve the technical problems, the invention adopts the following technical scheme:
according to an aspect of the present invention, the present invention provides a method for preparing titanium diboride ultrafine powder, comprising the steps of:
1) putting the composite molten salt into a vacuum drying oven for drying to remove moisture in the composite molten salt, so as to obtain a first substance;
2) mixing titanium dioxide and boron powder according to a ratio to obtain a second substance;
3) mixing the first substance and the second substance, then manually grinding the mixture to uniformly mix the first substance and the second substance, and putting the mixture into a corundum crucible;
4) putting the corundum crucible into a tubular furnace for calcination, heating and keeping the temperature for a period of time under the protection of argon atmosphere, and then cooling to obtain a third substance;
5) taking out the third substance cooled to room temperature, dissolving the third substance in deionized water, and removing residual molten salt and byproducts to obtain a fourth substance;
6) and filtering the fourth substance, repeatedly cleaning the fourth substance by using deionized water and absolute ethyl alcohol, and finally drying a product obtained by filtering to obtain the titanium diboride superfine powder.
In one embodiment of the present invention, the preparation method further comprises:
7) and carrying out SEM test and XRD test on the obtained titanium diboride superfine powder.
In one embodiment of the invention, in step 1), the composite molten salt is a NaCl-KCl composite molten salt mixed at a molar ratio of 1:1 or NaCl-CaCl mixed at a molar ratio of 1:1 2 And (3) compounding the molten salt.
In one embodiment of the invention, the drying temperature in the step 1) is 250-350 ℃, and the drying time is 20-32 h.
In one embodiment of the invention, titanium dioxide and boron powder are mixed in step 2) in a molar ratio of 3: 10.
In one embodiment of the invention, the first substance and the second substance are mixed in step 3) in a mass fraction ratio of 8:1 to 12: 1; the time for manual grinding is 15-30 min.
In one embodiment of the invention, the corundum crucible in the step 4) is heated to 850-1000 ℃ along with the tubular furnace during calcination in the tubular furnace, and the temperature is kept for 2-6 h.
In one embodiment of the invention, the third substance in step 5) is dissolved in deionized water at 85-100 ℃ for 30-90 min.
In one embodiment of the invention, in step 6), the deionized water used for repeated cleaning is hot deionized water with the temperature of 60-90 ℃, the number of times of repeated cleaning is 3-5, and the drying temperature is 80-100 ℃.
In one embodiment of the invention, the particle size of the obtained titanium diboride superfine powder is 50-300 nm.
By adopting the technical scheme, compared with the prior art, the invention has the following advantages:
(1) the solid-liquid combination mode is adopted: the method has the advantages that the low-melting-point salt is used as a reaction medium, a liquid phase appears in the synthesis process, and reactants have certain solubility in the liquid phase, so that the diffusion rate of ions is greatly increased, the reactants are mixed in the liquid phase at an atomic scale, and the reaction is converted from a solid-solid reaction into a solid-liquid reaction;
(2) the production process is simple: compared with the conventional solid phase method, the method has the advantages of simple process, low synthesis temperature, short heat preservation time, uniform chemical components of the synthesized powder, good crystal morphology, high phase purity and the like;
(3) the environment is friendly, and no high-risk substances are generated and remained in the production process and the postpartum: a high-risk reducing agent is not used in the reaction, the produced salt is easy to separate and can be reused, and the purpose of environmental protection and sustainability is achieved;
(4) the product has relatively low raw material price and good product performance: according to the invention, titanium dioxide is used as a titanium source, the prepared product is lower in price and more environment-friendly compared with other products using organic titanium sources or titanium powder, and the product prepared by the invention has the advantages of good particle appearance, good separation degree, controllable particle size of 50-300nm and high phase purity.
Drawings
FIG. 1 shows a schematic diagram of a preparation method of titanium diboride ultrafine powder provided by the invention.
Detailed Description
It should be understood that the embodiments of the invention shown in the exemplary embodiments are illustrative only. Although only a few embodiments of the present invention have been described in detail in this disclosure, those skilled in the art will readily appreciate that many modifications are possible without materially departing from the teachings of the present subject matter. Accordingly, all such modifications are intended to be included within the scope of this invention. Other substitutions, modifications, changes and omissions may be made in the design, operating conditions and parameters and the like of the following exemplary embodiments without departing from the spirit of the present invention.
As shown in figure 1, the preparation method of the titanium diboride superfine powder comprises the following steps:
s101: putting the composite molten salt into a vacuum drying oven for drying to remove moisture in the composite molten salt, so as to obtain a first substance;
s102: mixing titanium dioxide and boron powder according to a ratio to obtain a second substance;
s103: mixing the first substance and the second substance, then manually grinding the mixture to uniformly mix the first substance and the second substance, and putting the mixture into a corundum crucible;
s104: putting the corundum crucible into a tubular furnace for calcination, heating and keeping the temperature for a period of time under the protection of argon atmosphere, and then cooling to obtain a third substance;
s105: taking out the third substance cooled to room temperature, dissolving the third substance in deionized water, and removing residual molten salt and byproducts to obtain a fourth substance;
s106: and filtering the fourth substance, repeatedly cleaning the fourth substance by using deionized water and absolute ethyl alcohol, and finally drying a product obtained by filtering to obtain the titanium diboride superfine powder.
Through the technical scheme of the invention, the application can realize the following technical effects:
(1) the solid-liquid combination mode is adopted: the method has the advantages that the low-melting-point salt is used as a reaction medium, a liquid phase appears in the synthesis process, and reactants have certain solubility in the liquid phase, so that the diffusion rate of ions is greatly increased, the reactants are mixed in the liquid phase at an atomic scale, and the reaction is converted from a solid-solid reaction into a solid-liquid reaction;
(2) the production process is simple: compared with the conventional solid phase method, the method has the advantages of simple process, low synthesis temperature, short heat preservation time, uniform chemical components of the synthesized powder, good crystal morphology, high phase purity and the like;
(3) the environment is friendly, and no high-risk substances are generated and remained in the production process and the postpartum: high-risk reducing agents are not used in the reaction, the produced salt is easy to separate and can be reused, and the purpose of environmental protection and sustainability is achieved;
(4) the product has relatively low raw material price and good product performance: according to the invention, titanium dioxide is used as a titanium source, the prepared product is lower in price and more environment-friendly compared with other products using organic titanium sources or titanium powder, and the prepared particles are good in appearance, good in separation degree, controllable in particle size and high in phase purity.
In the above technical solution, the preparation method further comprises:
and carrying out SEM test and XRD test on the obtained titanium diboride superfine powder. Through SEM test, the particle size of the generated titanium diboride superfine powder can be observed to be 50-300nm, the agglomeration degree is small, and XRD test results show that the product phase purity is high and no other byproduct diffraction peaks exist.
In the above technical solution, in step S101, the composite molten salt is NaCl-KCl composite molten salt mixed according to a molar ratio of 1:1 or NaCl-CaCl mixed according to a molar ratio of 1:1 2 And (3) compounding the molten salt.
In the above technical solution, the drying temperature in step S101 is 250-; the drying time is 20-32h, preferably 24 h.
In the above technical solution, in step S102, titanium dioxide and boron powder are mixed in a molar ratio of 3: 10.
In the above technical solution, in step S103, the first substance and the second substance are mixed according to a mass fraction ratio of 8:1-12:1, preferably, the mass fraction ratio of the first substance to the second substance is 10: 1; the time for manual grinding is 15-30min, preferably 30 min.
In the above technical solution, in the step S104, the temperature of the corundum crucible is raised to 850-.
In the above technical solution, in step S105, the third substance is dissolved in deionized water at 85-100 ℃ for 30-90min, preferably 90 ℃ for 60 min.
In the above technical solution, in step S106, the deionized water used for repeated cleaning is hot deionized water with a temperature of 60-90 ℃, preferably 80 ℃, and the number of times of repeated cleaning is 3-5, preferably 5; the drying temperature is 80-100 deg.C, preferably 80 deg.C.
In the technical scheme, the particle size of the obtained titanium diboride superfine powder is 50-300 nm.
The above-described technical means of the present invention will be described in detail by way of specific examples.
The specific preparation method for preparing the titanium diboride superfine powder comprises the following steps:
1. selection of raw materials and systems
Titanium diboride (TiB) 2 ) The material has very wide application prospect due to the special physical and chemical characteristics. The invention considers that the solid-liquid combined molten salt method is adopted to prepare the titanium diboride high-end superfine powder, the variety of the molten salt is more, and the common molten salt for preparing the titanium diboride high-end superfine powder comprises NaCl, KCl and CaCl 2 And mixed salt systems thereof, and the like. NaCl-KCl and NaCl-CaCl 2 The phase diagram of the composite molten salt system shows that the NaCl-KCl composite molten salt and the NaCl-CaCl 2 The molar ratio of the composite molten salt with the eutectic point is l:1, and the composite molten salt used in the experiment is proportioned according to the molar ratio corresponding to the eutectic point (1: 1).
2. Selection of raw materials for preparing titanium diboride
The required boron and titanium sources are considered for preparing titanium diboride, a common titanium source being titanium dioxide (TiO) 2 ) And titanium powder (Ti), the boron source is diboron trioxide (B) 2 O 3 ) And boron powder (B), the reducing agents that can be considered for use are metallic magnesium powder (Mg) and metallic aluminum powder (Al), and for safety reasons the experimental protocol without reducing agent is adopted in the present invention. Based on abundant titanium dioxide resources, easy to obtain and low in price, the cheap titanium source selected by the invention is titanium dioxide (TiO) 2 ) The boron source is boron powder (B), and the reaction equation is as follows:
3TiO 2 +10B＝3TiB 2 +B 2 O 3 。
3. preparation of high-end superfine titanium diboride powder
According to the experimentEquation of reaction, TiO 2 The molar ratio of the powder to the powder B is 3:10, and the NaCl-KCl composite molten salt and the NaCl-CaCl are 2 The molar ratio of the composite molten salt with the lowest eutectic point is l:1, and the composite molten salt used in the invention is proportioned according to the molar ratio of 1:1 corresponding to the eutectic point. Before the experiment, NaCl-KCl or NaCl-CaCl is needed 2 Mixing according to the molar ratio of 1:1, drying the mixture in a vacuum drying box at the temperature of 250- 2 Mixing the/B (3:10) and the composite molten salt in a total mass fraction ratio of 1:8-1:12, manually grinding for 15-30min to uniformly mix, and placing into a corundum crucible. And then, putting the corundum crucible into a tubular furnace for calcination, heating to a certain temperature (850-. Cooling to room temperature, dissolving the obtained substance in deionized water at 85-100 deg.C for 30-90min, and removing residual salt and byproduct B 2 O 3 Then filtering the product, washing the product for 3 to 5 times by using hot deionized water and absolute ethyl alcohol at the temperature of between 60 and 90 ℃, and finally drying the filtered product at the temperature of between 80 and 100 ℃ to obtain the titanium diboride high-end superfine powder with the controllable particle size of between 50 and 300 nm.
The above-described preparation process of the present invention is illustrated in detail by the following detailed examples.
Example 1
The preparation method of the titanium diboride superfine powder comprises the following steps:
the method comprises the following steps: before the experiment, NaCl-KCl molten salt is mixed according to the molar ratio of 1:1 and is placed into a vacuum drying oven to be dried for 24 hours at 250 ℃ to remove moisture in the salt, and a substance A is obtained.
Step two: titanium dioxide and boron powder (TiO) were used for the experiments 2 /B) in a molar ratio of 3:10 to give substance B.
Step three: mixing the substance A and the substance B, wherein the total mass fraction ratio of the substance A to the substance B is 10:1, then grinding for 20min manually to mix evenly, and putting into a corundum crucible.
Step four: and (3) putting the corundum crucible into a tubular furnace for calcination, heating the corundum crucible to 950 ℃ along with the furnace under the protection of argon atmosphere, preserving the heat for 3 hours, and then cooling to obtain a substance C.
Step five: cooling to room temperature, taking out substance C, dissolving in 90 deg.C deionized water for 60min, and removing residual salt and by-product B 2 O 3 And obtaining a product D.
Step six: and filtering the product D, repeatedly washing the product D for 5 times by using hot deionized water and absolute ethyl alcohol at the temperature of 80 ℃, and finally drying the filtered product at the temperature of 80 ℃ to obtain the required product.
Step seven: the resulting product was subjected to SEM test and XRD test.
In the above example 1, the particle size of the generated particles can be observed to be about 100nm under the SEM test, the degree of agglomeration is small, and the XRD test result shows that the product phase purity is high, and there are no diffraction peaks of other by-products.
Example 2
The preparation method of the titanium diboride superfine powder comprises the following steps:
the method comprises the following steps: before the experiment, NaCl-CaCl is added 2 The molten salts are mixed according to the molar ratio of 1:1 and put into a vacuum drying oven to be dried for 22 hours at 300 ℃ to remove the moisture in the salts, and the substance A is obtained.
Step two: titanium dioxide and boron powder (TiO) were used for the experiments 2 /B) in a molar ratio of 3:10 to obtain substance B.
Step three: mixing the substance A and the substance B, wherein the total mass fraction ratio of the substance A to the substance B is 10:1, then manually grinding for 25min to mix well and placing into a corundum crucible.
Step four: and (3) putting the corundum crucible into a tubular furnace for calcination, heating the corundum crucible to 900 ℃ along with the furnace under the protection of argon atmosphere, preserving the heat for 5 hours, and then cooling to obtain a substance C.
Step five: cooling to room temperature, taking out substance C, dissolving in 100 deg.C deionized water for 60min, and removing residual salt and by-product B 2 O 3 And obtaining a product D.
Step six: and filtering the product D, repeatedly washing the product D for 5 times by using hot deionized water and absolute ethyl alcohol at the temperature of 80 ℃, and finally drying the filtered product at the temperature of 90 ℃ to obtain the required product.
Step seven: the resulting product was subjected to SEM test and XRD test.
In the above example 2, the particle size of the generated particles can be observed to be about 80nm under the SEM test, the degree of agglomeration is small, and the XRD test result shows that the product phase purity is high, and there are no diffraction peaks of other by-products.
Example 3
The preparation method of the titanium diboride superfine powder comprises the following steps:
the method comprises the following steps: before the experiment, NaCl-KCl molten salt is mixed according to the molar ratio of 1:1 and is placed into a vacuum drying oven to be dried for 20 hours at 300 ℃ to remove water in the salt, and a substance A is obtained.
Step two: titanium dioxide and boron powder (TiO) were used for the experiments 2 /B) in a molar ratio of 3:10 to obtain substance B.
Step three: mixing the substance A and the substance B, wherein the total mass fraction ratio of the substance A to the substance B is 10:1, then manually grinding for 30min to mix evenly, and putting into a corundum crucible.
Step four: and (3) putting the corundum crucible into a tubular furnace for calcination, heating the corundum crucible to 1000 ℃ along with the furnace under the protection of argon atmosphere, preserving the heat for 2 hours, and then cooling to obtain a substance C.
Step five: cooling to room temperature, taking out substance C, dissolving in deionized water at 85 deg.C for 60min, and removing residual salt and byproduct B 2 O 3 And obtaining a product D.
Step six: and filtering the product D, repeatedly washing the product D for 5 times by using hot deionized water and absolute ethyl alcohol at 90 ℃, and finally drying the filtered product at 95 ℃ to obtain the required product.
Step seven: the resulting product was subjected to SEM test and XRD test.
In the above example 3, the particle size of the generated particles can be observed to be about 120nm under the SEM test, the degree of agglomeration is small, and the XRD test result shows that the product phase purity is high, and there are no diffraction peaks of other by-products.
Example 4
The preparation method of the titanium diboride superfine powder comprises the following steps:
the method comprises the following steps: before the experiment, NaCl-KCl molten salt is mixed according to the molar ratio of 1:1 and is placed into a vacuum drying oven to be dried for 30 hours at 350 ℃ to remove water in the salt, and a substance A is obtained.
Step two: titanium dioxide and boron powder (TiO) were used for the experiments 2 /B) in a molar ratio of 3:10 to obtain substance B.
Step three: mixing the substance A and the substance B, wherein the total mass fraction ratio of the substance A to the substance B is 12:1, then grinding by hand for 15min to mix evenly, and putting into a corundum crucible.
Step four: and (3) putting the corundum crucible into a tubular furnace for calcination, heating the corundum crucible to 850 ℃ along with the furnace under the protection of argon atmosphere, preserving the heat for 6 hours, and then cooling to obtain a substance C.
Step five: cooling to room temperature, taking out substance C, dissolving in deionized water at 100 deg.C for 30min, and removing residual salt and byproduct B 2 O 3 And obtaining a product D.
Step six: and filtering the product D, repeatedly washing the product D for 4 times by using hot deionized water and absolute ethyl alcohol at the temperature of 75 ℃, and finally drying the filtered product at the temperature of 100 ℃ to obtain the product.
Step seven: the resulting product was subjected to SEM test and XRD test.
In the above example 4, the particle size of the generated particles can be observed to be about 50nm under the SEM test, the degree of agglomeration is small, and the XRD test result shows that the product phase purity is high, and there are no diffraction peaks of other by-products.
Example 5
The preparation method of the titanium diboride superfine powder comprises the following steps:
the method comprises the following steps: before the experiment, NaCl-CaCl is added 2 The molten salts are mixed according to the molar ratio of 1:1 and put into a vacuum drying oven to be dried for 32 hours at 300 ℃ to remove the moisture in the salts, and the substance A is obtained.
Step two: titanium dioxide and boron powder (TiO) were used for the experiments 2 /B) in a molar ratio of 3:10 to obtain substance B.
Step three: mixing the substance A and the substance B, wherein the total mass fraction ratio of the substance A to the substance B is 8:1, then grinding by hand for 25min to mix well, and placing into a corundum crucible.
Step four: and (3) putting the corundum crucible into a tubular furnace for calcination, heating the corundum crucible to 1000 ℃ along with the furnace under the protection of argon atmosphere, preserving the heat for 2 hours, and then cooling to obtain a substance C.
Step five: cooling to room temperature, taking out substance C, dissolving in deionized water at 85 deg.C for 90min, and removing residual salt and by-product B 2 O 3 And obtaining a product D.
Step six: and filtering the product D, repeatedly cleaning the product D for 3 times by using hot deionized water and absolute ethyl alcohol at 85 ℃, and finally drying the filtered product at 80 ℃ to obtain the product.
Step seven: the resulting product was subjected to SEM test and XRD test.
In the above example 5, the particle size of the generated particles can be observed to be about 300nm under the SEM test, the degree of agglomeration is small, and the XRD test result shows that the product phase purity is high, and there are no diffraction peaks of other by-products.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention; the invention is intended to cover by the appended claims, modifications and equivalents, which may fall within the true spirit and scope of the invention.
Claims (10)
1. A preparation method of titanium diboride superfine powder is characterized by comprising the following steps:
1) putting the composite molten salt into a vacuum drying oven for drying to remove moisture in the composite molten salt, so as to obtain a first substance;
2) mixing titanium dioxide and boron powder according to a ratio to obtain a second substance;
3) mixing the first substance and the second substance, then manually grinding the mixture to uniformly mix the first substance and the second substance, and putting the mixture into a corundum crucible;
4) putting the corundum crucible into a tubular furnace for calcination, heating and keeping the temperature for a period of time under the protection of argon atmosphere, and then cooling to obtain a third substance;
5) taking out the third substance cooled to room temperature, dissolving the third substance in deionized water, and removing residual molten salt and byproducts to obtain a fourth substance;
6) and filtering the fourth substance, repeatedly cleaning the fourth substance by using deionized water and absolute ethyl alcohol, and finally drying a product obtained by filtering to obtain the titanium diboride superfine powder.
2. The method for preparing the titanium diboride ultrafine powder according to claim 1, wherein the method further comprises:
7) and carrying out SEM test and XRD test on the obtained titanium diboride superfine powder.
3. The method for preparing titanium diboride ultrafine powder according to claim 1, wherein in the step 1), the composite molten salt is NaCl-KCl composite molten salt mixed according to a molar ratio of 1:1 or NaCl-CaCl composite molten salt mixed according to a molar ratio of 1:1 2 And (3) compounding the molten salt.
4. The method for preparing the titanium diboride ultrafine powder according to claim 3, wherein the drying temperature in the step 1) is 250-350 ℃, and the drying time is 20-32 h.
5. The method for preparing titanium diboride micropowder according to claim 1, wherein in step 2) titanium dioxide and boron powder are mixed in a molar ratio of 3: 10.
6. The method for preparing the titanium diboride ultrafine powder according to claim 1, wherein in the step 3), the first substance and the second substance are mixed according to the mass fraction ratio of 8:1-12: 1; the time for manual grinding is 15-30 min.
7. The method for preparing the titanium diboride ultrafine powder according to claim 1, wherein the temperature of the corundum crucible in the step 4) is raised to 850-.
8. The method for preparing titanium diboride ultrafine powder according to claim 1, wherein in the step 5), the third substance is dissolved in deionized water at 85-100 ℃ for 30-90 min.
9. The method for preparing titanium diboride micropowder of claim 1, wherein in the step 6), the deionized water used for repeated cleaning is hot deionized water at 60-90 ℃, the number of times of repeated cleaning is 3-5, and the drying temperature is 80-100 ℃.
10. The method for preparing titanium diboride micropowder according to claim 2, wherein the particle size of the obtained titanium diboride micropowder is 50-300 nm.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116444272A (en) * | 2023-03-13 | 2023-07-18 | 成都先进金属材料产业技术研究院股份有限公司 | Preparation method of rotating disc, rotating disc and application of rotating disc |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5948558A (en) * | 1997-03-27 | 1999-09-07 | National Patent Development Corporation | High energy density boride batteries |
| US20040197482A1 (en) * | 2001-10-15 | 2004-10-07 | Airy-Pierre Lamaze | Coating precursor and method for coating a substrate with a refractory layer |
| CN103950946A (en) * | 2014-05-22 | 2014-07-30 | 安徽工业大学 | Preparation method of nano niobium boride powder |
| CN104944432A (en) * | 2015-06-30 | 2015-09-30 | 莱芜亚赛陶瓷技术有限公司 | Superfine 10B-rich titanium diboride powder and preparation method thereof |
| CN106882815A (en) * | 2017-05-02 | 2017-06-23 | 东北大学 | A kind of wolfram diboride preparation method |
| CN108584972A (en) * | 2018-04-20 | 2018-09-28 | 华南理工大学 | A kind of TiB2Raw powder's production technology |
| CN109251036A (en) * | 2018-10-11 | 2019-01-22 | 武汉科技大学 | A kind of TiB2The preparation method of ceramic powder |
| CN109251037A (en) * | 2018-10-11 | 2019-01-22 | 武汉科技大学 | A kind of titanium boride ceramics raw powder's production technology based on ferrosilicon-titanium alloy |
-
2022
- 2022-06-14 CN CN202210668142.XA patent/CN115072732A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5948558A (en) * | 1997-03-27 | 1999-09-07 | National Patent Development Corporation | High energy density boride batteries |
| US20040197482A1 (en) * | 2001-10-15 | 2004-10-07 | Airy-Pierre Lamaze | Coating precursor and method for coating a substrate with a refractory layer |
| CN103950946A (en) * | 2014-05-22 | 2014-07-30 | 安徽工业大学 | Preparation method of nano niobium boride powder |
| CN104944432A (en) * | 2015-06-30 | 2015-09-30 | 莱芜亚赛陶瓷技术有限公司 | Superfine 10B-rich titanium diboride powder and preparation method thereof |
| CN106882815A (en) * | 2017-05-02 | 2017-06-23 | 东北大学 | A kind of wolfram diboride preparation method |
| CN108584972A (en) * | 2018-04-20 | 2018-09-28 | 华南理工大学 | A kind of TiB2Raw powder's production technology |
| CN109251036A (en) * | 2018-10-11 | 2019-01-22 | 武汉科技大学 | A kind of TiB2The preparation method of ceramic powder |
| CN109251037A (en) * | 2018-10-11 | 2019-01-22 | 武汉科技大学 | A kind of titanium boride ceramics raw powder's production technology based on ferrosilicon-titanium alloy |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116444272A (en) * | 2023-03-13 | 2023-07-18 | 成都先进金属材料产业技术研究院股份有限公司 | Preparation method of rotating disc, rotating disc and application of rotating disc |
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