CN114671435A - Preparation method of nano TiC for wet friction material - Google Patents
Preparation method of nano TiC for wet friction material Download PDFInfo
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- 239000002783 friction material Substances 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 66
- 238000000498 ball milling Methods 0.000 claims abstract description 49
- 238000000354 decomposition reaction Methods 0.000 claims abstract description 38
- 238000000034 method Methods 0.000 claims abstract description 34
- 230000032683 aging Effects 0.000 claims abstract description 14
- 229910052718 tin Inorganic materials 0.000 claims abstract description 12
- 229910052751 metal Inorganic materials 0.000 claims abstract description 11
- 239000002184 metal Substances 0.000 claims abstract description 11
- 229910052793 cadmium Inorganic materials 0.000 claims abstract description 5
- 229910052733 gallium Inorganic materials 0.000 claims abstract description 5
- 229910052738 indium Inorganic materials 0.000 claims abstract description 5
- 229910052745 lead Inorganic materials 0.000 claims abstract description 5
- 229910052716 thallium Inorganic materials 0.000 claims abstract description 5
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 5
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 3
- 238000001035 drying Methods 0.000 claims description 15
- 239000002253 acid Substances 0.000 claims description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 239000007791 liquid phase Substances 0.000 claims description 9
- 238000003760 magnetic stirring Methods 0.000 claims description 9
- 239000007790 solid phase Substances 0.000 claims description 9
- 238000003828 vacuum filtration Methods 0.000 claims description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- 239000012071 phase Substances 0.000 claims description 8
- 238000000746 purification Methods 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 7
- 238000007605 air drying Methods 0.000 claims description 6
- 239000012670 alkaline solution Substances 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- 239000000243 solution Substances 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 2
- 239000003570 air Substances 0.000 claims description 2
- 238000001085 differential centrifugation Methods 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 239000000919 ceramic Substances 0.000 abstract description 4
- 238000004134 energy conservation Methods 0.000 abstract description 2
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- 229910052719 titanium Inorganic materials 0.000 abstract description 2
- 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 68
- 239000010936 titanium Substances 0.000 description 22
- 239000000047 product Substances 0.000 description 19
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- 229910001220 stainless steel Inorganic materials 0.000 description 15
- 239000000463 material Substances 0.000 description 11
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 7
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- 125000004429 atom Chemical group 0.000 description 4
- 239000007772 electrode material Substances 0.000 description 4
- 238000005229 chemical vapour deposition Methods 0.000 description 3
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- 229910009600 Ti2CdC Inorganic materials 0.000 description 1
- 229910009930 Ti2GaC Inorganic materials 0.000 description 1
- 229910009927 Ti2InC Inorganic materials 0.000 description 1
- 229910009966 Ti2PbC Inorganic materials 0.000 description 1
- 229910010013 Ti2SnC Inorganic materials 0.000 description 1
- 229910010014 Ti2TlC Inorganic materials 0.000 description 1
- 229910009818 Ti3AlC2 Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical group [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 229910007426 ZnC2 Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
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- 229910052799 carbon Inorganic materials 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
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- 238000011031 large-scale manufacturing process Methods 0.000 description 1
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
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- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/921—Titanium carbide
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- 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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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01P2004/00—Particle morphology
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- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The invention relates to a preparation method of nano TiC for a wet friction material, which comprises the following steps: s1, taking Ti n+ 1AC n Ball milling the powder to Ti n+1AC n In (1),n=1 or 2, the A site is Sn, In, Ga, Zn, Cd, Pb, Tl or Al; s2, carrying out aging treatment on the powder obtained in the step S1 to enable the powder to reach an equilibrium state, and obtaining a decomposition product metal phase and TiC; s3, and purifying TiC in the decomposition product in the step S2 to obtain nano TiC powder. The method of the invention utilizes a layered carbide ceramic MAX phase (Ti) containing Ti and C n+1AC n ) The nano TiC is prepared by mechanochemical decomposition. The preparation method has the advantages of simple process, high purity, controllable size, fine granularity, high efficiency, energy conservation, environmental protection and the like.
Description
Technical Field
The invention belongs to the technical field of friction materials, and particularly relates to a preparation method of nano TiC for a wet friction material.
Background
Titanium carbide (TiC) is a transition metal carbide, belongs to a cubic system, carbon atoms are positioned in octahedral gaps formed by titanium atoms, the space group is Fm3m, and the lattice constant is 0.4327 nm. TiC with the stoichiometric ratio has the characteristics of high chemical stability, high hardness (32GPa), high strength, excellent wear resistance, corrosion resistance, electric conduction and heat conduction performance and the like, and is widely applied to reinforced phase materials, coating materials, friction materials, aerospace and the like. With the rapid development of industry, the demand of people on energy is further expanded, and the research on novel energy materials and technology is receiving wide attention. The high chemical stability, oxidation resistance and excellent conductivity of TiC make the TiC become a potential energy storage electrode material. The structure of the electrode material has great influence on the performance of the energy storage device, and how to reasonably design the structure of the TiC electrode material has important significance on the application of the TiC electrode material in the field of energy storage. The excellent wear resistance, corrosion resistance, electrical and thermal conductivity of TiC make it one of the components of a potential wet friction material. The structure of the wet friction material has great influence on the friction performance and the heat resistance and durability, and how to reasonably design the TiC material structure has important significance on the application of the TiC material structure in the field of wet friction materials. Meanwhile, high-quality TiC needs to meet the standards of ultra-fine particle size and high purity, and the problem of how to obtain high-quality ultra-fine particle size TiC needs to be solved urgently because TiC is difficult to refine by a mechanical method due to high hardness.
The TiC preparation method comprises the following steps: carbothermal reduction of TiO2A sol-gel method, a chemical vapor deposition method, a direct carbonization method (a reaction ball milling method, a high-temperature self-propagating synthesis method). At present, the main method for industrially producing TiC is to reduce TiO by carbothermal2The method, however, requires a higher reaction temperature and a longer reaction time, resulting in high energy consumptionThe reaction of the materials is incomplete, the prepared TiC has general purity, and the shape and the size are uncontrollable. The raw materials and intermediate products used in the chemical vapor deposition method are harmful to human bodies, and the yield is limited, so that the chemical vapor deposition method is not beneficial to large-scale production. The direct carbonization method comprises reaction ball milling and high-temperature self-propagating synthesis, the reaction ball milling method has high requirements on atmosphere, long required reaction time and small yield, and the high-temperature self-propagating synthesis method has high requirements on the purity and granularity of raw materials and poor controllability on appearance and size, and is difficult to meet production requirements.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides the preparation method of the nano TiC for the wet friction material, which has the advantages of simple process, high purity, controllable size, fine granularity, high efficiency, energy conservation and environmental protection.
According to the technical scheme provided by the invention, the preparation method of the nano TiC for the wet friction material comprises the following steps:
s1, taking Tin+1ACnBall milling the powder to Tin+1ACnWherein, n is 1 or 2, A is Sn, In, Ga, Zn, Cd, Pb, Tl or Al;
s2, carrying out aging treatment on the powder obtained in the step S1 to enable the powder to reach an equilibrium state, and obtaining a decomposition product metal phase and TiC;
s3, and purifying TiC in the decomposition product in the step S2 to obtain nano TiC powder.
Preferably, the Ti isn+1ACnWhen the A site In (A) is Sn, In, Ga, Zn, Cd, Pb or Tl, for example, Ti2SnC、Ti3SnC2；Ti2InC、Ti3InC2；Ti2GaC、Ti3GaC3；Ti2ZnC、Ti3ZnC2；Ti2CdC；Ti2PbC；Ti2TlC; the aging treatment in the step S2 is carried out in the environment of air, argon, nitrogen or vacuum, the aging temperature is 25-1000 ℃, and the aging time is 0.5-96 h.
Preferably, the Ti isn+1ACnWhen the A site in (A) is Al, e.g. Ti2AlC、Ti3AlC2(ii) a In the step S2, the aging treatment environment is argon or vacuum environment, the aging temperature is 25-1000 ℃, and the aging time is 0.5-96 h.
Preferably, the ball milling process in step S1 includes vibration ball milling, planetary ball milling, plasma ball milling or bearing ball milling.
Preferably, the ball milling treatment in the step S1 is planetary ball milling, the ball milling rotation speed is 500-.
Preferably, the purification method in step S3 includes acid washing, alkali washing or differential centrifugation.
Preferably, when the purification method in step S3 is acid washing, the acid includes hydrochloric acid, nitric acid or sulfuric acid, the acid concentration is 0.1-9mol/L, the acid washing temperature is 10-40 deg.C, the time is 0.5-48h, and magnetic stirring with rotation speed of 1-800r/min is carried out while acid washing, so that Ti is addedn+1ACnThe A-site metal in the TiC powder completely reacts with acid, then the liquid phase is removed by vacuum filtration, and the obtained TiC solid phase is placed into a blast drying oven to be dried, wherein the drying temperature is 30-80 ℃, and the drying time is 0.5-48h, so that TiC powder is obtained.
Preferably, when the purification method in step S3 is alkaline cleaning purification, the alkaline solution includes sodium hydroxide solution or potassium hydroxide solution, the concentration of the alkaline solution is 0.1-9mol/L, the alkaline cleaning temperature is 10-40 ℃, the time is 0.5-48h, and magnetic stirring with the rotation speed of 1-800r/min is performed while alkaline cleaning, so that Ti is obtainedn+1ACnThe A-site metal in the TiC powder completely reacts with the alkaline solution, then the liquid phase is removed by vacuum filtration, and the obtained TiC solid phase is placed into a forced air drying oven to be dried, wherein the drying temperature is 30-80 ℃, and the drying time is 0.5-48h, so that TiC powder is obtained.
Using a layered carbide ceramic MAX phase containing Ti and C (Ti)n+1ACn) The TiC, MAX phase is a general name of a layer carbide or nitride ceramic with a hexagonal crystal structure, and the space group is P63Per mm, from M6X octahedra and A atomic layers are alternately arranged, M6X is a radical of MClosely packed octahedra and X atom therein, M and X atom are combined through strong covalent bond, M atom is combined through metal bond, M atom6The X octahedron layer is combined with the A atom layer through interlayer weak ionic bonds. Due to the unique structure, the parent Tin+1ACnThe a layer easily comes out of the structure during ball milling. At the same time, the parent Tin+1ACnBecause the hardness of the alloy is lower than that of TiC, the grain diameter of the alloy can be continuously thinned in the ball milling process. Therefore, made of Tin+1ACnThe TiC generated by complete mechanochemical decomposition has fine grain diameter, and the preparation of nano TiC can be realized.
Compared with the prior art, the invention has the following advantages:
1. the invention provides a method for preparing nano TiC for a wet friction material, which utilizes layered carbide ceramic Tin+ 1ACnThe mechanochemical decomposition phenomenon can effectively control Ti by adjusting the ball milling mode and parametersn+1ACnThe mechanochemical decomposition degree realizes the preparation of nano TiC particles, and the size is controllable and the process is simple.
2. The invention provides a preparation method of nano TiC for a wet friction material, and Tin+1ACnAfter complete mechanochemical decomposition, the TiC in the system is purified, and the high-purity nano TiC can be obtained.
Drawings
FIG. 1 is an SEM picture of a nanoscale TiC powder prepared in example 1;
FIG. 2 is an XRD pattern of the nano-scale TiC powder prepared in example 1;
FIG. 3 is an SEM picture of a nano-scale TiC powder prepared in example 2;
FIG. 4 is an SEM picture of the nano-scale TiC powder prepared in example 3;
FIG. 5 is an SEM picture of the nano-scale TiC powder prepared in example 4.
Detailed Description
The technical solutions of the present invention are further described below with reference to the drawings and the embodiments, but the scope of the present invention is not limited thereto.
Example 1
This example utilizes Ti3SnC2Preparing nano TiC powder by mechanochemical decomposition:
s1, collecting 3g Ti3SnC2Adding the powder and 30g of stainless steel grinding balls (the ball material ratio is 10:1) into a stainless steel ball milling tank, and placing the stainless steel grinding balls in a planetary ball mill for ball milling, wherein the ball milling rotation speed is 645r/min, and the ball milling time is 12 hours, so as to obtain ball-milled sample powder;
s2, taking out the ball-milled sample powder, placing the ball-milled sample powder in an air environment, and storing the sample at 50 ℃ for 24 hours to ensure that the sample is completely subjected to mechanochemical decomposition to obtain a decomposition product TiC powder and Sn crystal whiskers;
s3, adding the decomposition product into 200ml of 1mol/L diluted hydrochloric acid, and completely reacting Sn in the decomposition product with the diluted hydrochloric acid by means of magnetic stirring at the rotation speed of 500r/min at the temperature of 40 ℃ for 5 hours;
s4, removing Sn in the decomposition product, removing a liquid phase by vacuum filtration, and drying the obtained TiC solid phase in a forced air drying oven at the drying temperature of 50 ℃ for 6 h; obtaining high-purity nano TiC powder.
The nano-scale TiC powder obtained in example 1 has a particle size of 20-100nm and a purity of 99.9%.
Example 2
This example utilizes Ti2And (3) carrying out mechanochemical decomposition on the SnC to prepare nano TiC powder:
s1, 2g of Ti2Adding SnC powder and 30g of stainless steel grinding balls (the ball-material ratio is 15:1) into a stainless steel ball milling tank, and placing the stainless steel ball milling tank in a planetary ball mill for ball milling, wherein the ball milling speed is 500r/min, and the ball milling time is 6 hours, so as to obtain ball-milled sample powder;
s2, taking out the ball-milled sample powder, placing the ball-milled sample powder in an air environment, and preserving the ball-milled sample powder for 3 hours at 150 ℃ to ensure that the sample is completely subjected to mechanochemical decomposition to obtain decomposition products TiC powder and Sn crystal whiskers;
s3, adding the decomposition product into 200ml of 1mol/L diluted hydrochloric acid, and completely reacting Sn in the decomposition product with the diluted hydrochloric acid by means of magnetic stirring at the rotation speed of 500r/min at the temperature of 40 ℃ for 5 hours;
s4, removing Sn in the decomposition product, removing a liquid phase by vacuum filtration, and drying the obtained TiC solid phase in a forced air drying oven at the drying temperature of 50 ℃ for 6 hours; obtaining high-purity nano TiC powder.
The nano-scale TiC powder obtained in example 2 has a particle size of 50-800nm and a purity of 99.9%.
Example 3
This example utilizes Ti2And (3) performing mechanochemical decomposition on the InC to prepare nano TiC powder:
s1, collecting 1g Ti2Adding InC powder and 30g of stainless steel grinding balls (the ball-material ratio is 30:1) into a stainless steel ball milling tank, and placing the stainless steel ball milling tank in a planetary ball mill for ball milling, wherein the ball milling rotation speed is 645r/min, and the ball milling time is 6 hours, so as to obtain ball-milled sample powder;
s2, taking out the ball-milled sample powder, placing the ball-milled sample powder In an air environment, and preserving the ball-milled sample powder for 2 hours at 100 ℃ to ensure that the sample is completely subjected to mechanochemical decomposition to obtain decomposition products TiC powder and In whiskers;
s3, adding the decomposition product into 100ml of dilute nitric acid with the concentration of 2mol/L, and completely reacting In with the dilute nitric acid by means of magnetic stirring at the rotation speed of 500r/min at the temperature of 50 ℃ for 5 hours;
s4, removing In the decomposition product, removing a liquid phase by vacuum filtration, and drying the obtained TiC solid phase In a forced air drying oven at the drying temperature of 50 ℃ for 6 h; obtaining high-purity nano TiC powder.
The nano-scale TiC powder obtained in example 3 has a particle size of 200-600nm and a purity of 99.9%.
Example 4
This example utilizes Ti2And (3) performing mechanochemical decomposition on the GaC to prepare nano TiC powder:
s1, collecting 1g Ti2Adding the GaC powder and 10g of stainless steel grinding balls (the ball-material ratio is 10:1) into a stainless steel ball milling tank, and placing the stainless steel ball milling tank in a planetary ball mill for ball milling, wherein the ball milling rotation speed is 800r/min, and the ball milling time is 8 hours, so as to obtain ball-milled sample powder;
s2, taking out the ball-milled sample powder, and storing in an air environment for 48h to ensure that the sample is completely subjected to mechanochemical decomposition to obtain decomposition products TiC powder and Ga whiskers;
s3, adding the decomposition product into 100ml of dilute hydrochloric acid with the concentration of 2mol/L, and completely reacting Ga and the dilute hydrochloric acid by magnetic stirring at the rotation speed of 500r/min at the temperature of 40 ℃ for 5 hours;
s4, removing Ga in the decomposition product, removing a liquid phase by vacuum filtration, and drying the obtained TiC solid phase in a forced air drying oven at the drying temperature of 50 ℃ for 6 hours; obtaining high-purity nano TiC powder.
The nano-scale TiC powder obtained in example 4 has a particle size of 300-500nm and a purity of 99.9%.
Example 5
This example utilizes Ti2And (3) performing mechanochemical decomposition on AlC to prepare nano TiC powder:
s1, collecting 1g Ti2Adding AlC powder and 10g of stainless steel grinding balls (the ball-to-material ratio is 10:1) into a stainless steel ball milling tank, and placing the stainless steel ball milling tank in a planetary ball mill for vacuum ball milling, wherein the ball milling rotation speed is 800r/min, and the ball milling time is 12 hours, so as to obtain ball-milled sample powder;
s2, taking out the ball-milled sample powder in a vacuum environment, placing the sample powder in the vacuum environment, preserving the sample powder for 72 hours at 1000 ℃ to ensure that the sample is completely subjected to mechanochemical decomposition to obtain a decomposition product TiC powder and a metal phase;
s3, adding the decomposition product into 100ml of 4mol/L NaOH solution, and completely reacting the metal phase with alkali liquor by magnetic stirring at the rotation speed of 500r/min and the temperature of 40 ℃ for 12 h;
s4, removing a metal phase in the decomposition product, removing a liquid phase by vacuum filtration, and drying the obtained TiC solid phase in a vacuum oven at the drying temperature of 40 ℃ for 6 h; obtaining high-purity nano TiC powder.
As can be seen from examples 1-5 in conjunction with FIGS. 1-5: the method can realize the preparation of high-purity nanoscale TiC particles, and has the advantages of controllable size and simple process.
Claims (8)
1. A preparation method of nano TiC for a wet friction material is characterized by comprising the following steps:
s1, taking Ti n+1AC n Ball milling the powder to Ti n+1AC n In (1),n=1 or 2, the A site is Sn, In, Ga, Zn, Cd, Pb, Tl or Al;
s2, carrying out aging treatment on the powder obtained in the step S1 to enable the powder to reach an equilibrium state, and obtaining a decomposition product metal phase and TiC;
s3, and S2 is used for purifying TiC in the decomposition product to obtain nano TiC powder.
2. The method of claim 1, wherein the nano TiC comprises: the Ti n+1AC n When the A site is Sn, In, Ga, Zn, Cd, Pb or Tl, the aging treatment environment In the step S2 is air, argon, nitrogen or vacuum environment, the aging temperature is 25-1000 ℃, and the aging time is 0.5-96 h.
3. The method of claim 1, wherein the nano TiC comprises: the Ti n+1AC n When the A site is Al, the aging treatment in the step S2 is performed in an argon or vacuum environment at an aging temperature of 25-1000 ℃ for 0.5-96 h.
4. The method of claim 1, wherein the nano TiC is prepared by the following steps: the ball milling treatment in the step S1 includes vibration ball milling, planetary ball milling, plasma ball milling or bearing ball milling.
5. The method of claim 4, wherein the nano TiC for the wet friction material comprises: the ball milling treatment in the step S1 is planetary ball milling, the ball milling rotating speed is 500-1000 r/min, the time is 2-96 h, and the mass ratio of the grinding balls to the raw materials is 5: 1-100: 1.
6. The method of claim 1, wherein the nano TiC is prepared by the following steps: the purification method in the step S3 comprises acid washing, alkali washing or differential centrifugation.
7. The method of claim 6, wherein the nano TiC is prepared by the following steps: when the purification method in the step S3 is acid washing, the acid comprises hydrochloric acid, nitric acid or sulfuric acid, the concentration of the acid is 0.1-9mol/L, the acid washing temperature is 10-40 ℃, the time is 0.5-48h, and magnetic stirring with the rotating speed of 1-800r/min is carried out while acid washing is carried out, so that Ti is obtained n+1AC n The A-site metal in the TiC powder completely reacts with acid, then the liquid phase is removed by vacuum filtration, and the obtained TiC solid phase is placed into a blast drying oven to be dried, wherein the drying temperature is 30-80 ℃, and the drying time is 0.5-48h, so that TiC powder is obtained.
8. The method of claim 6, wherein the nano TiC is prepared by the following steps: when the purification method in the step S3 is alkaline cleaning purification, the alkaline solution comprises sodium hydroxide solution or potassium hydroxide solution, the concentration of the alkaline solution is 0.1-9mol/L, the alkaline cleaning temperature is 10-40 ℃, the time is 0.5-48h, and magnetic stirring with the rotation speed of 1-800r/min is carried out while alkaline cleaning is carried out, so that Ti is purified by using the method, and the method can be used for purifying Ti by using the method n+1AC n The A-site metal in the TiC powder completely reacts with the alkaline solution, then the liquid phase is removed by vacuum filtration, and the obtained TiC solid phase is placed into a forced air drying oven to be dried, wherein the drying temperature is 30-80 ℃, and the drying time is 0.5-48h, so that TiC powder is obtained.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JPWO2016103312A1 (en) * | 2014-12-22 | 2017-08-03 | 株式会社島津製作所 | Analytical data processing method and apparatus |
| CN111646799A (en) * | 2020-05-10 | 2020-09-11 | 华北理工大学 | Combustion method for preparing Tin+1ACnMethod of producing a material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPWO2016103312A1 (en) * | 2014-12-22 | 2017-08-03 | 株式会社島津製作所 | Analytical data processing method and apparatus |
| CN111646799A (en) * | 2020-05-10 | 2020-09-11 | 华北理工大学 | Combustion method for preparing Tin+1ACnMethod of producing a material |
Non-Patent Citations (1)
| Title |
|---|
| QIANQIAN ZHANG ET AL: ""Rapid and massive growth of tin whisker on mechanochemically decomposed Ti2SnC"", 《MATERIALS TODAYCOMMUNICATIONS》, vol. 31, pages 1 - 5 * |
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