CN112441586A - Preparation method of non-stoichiometric titanium carbide TiCx powder - Google Patents
Preparation method of non-stoichiometric titanium carbide TiCx powder Download PDFInfo
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- CN112441586A CN112441586A CN202011345332.5A CN202011345332A CN112441586A CN 112441586 A CN112441586 A CN 112441586A CN 202011345332 A CN202011345332 A CN 202011345332A CN 112441586 A CN112441586 A CN 112441586A
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- 239000000843 powder Substances 0.000 title claims abstract description 35
- 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 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 238000000498 ball milling Methods 0.000 claims abstract description 40
- 239000000463 material Substances 0.000 claims abstract description 30
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 22
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000001816 cooling Methods 0.000 claims abstract description 13
- 238000000227 grinding Methods 0.000 claims abstract description 10
- 238000000713 high-energy ball milling Methods 0.000 claims abstract description 7
- 230000001681 protective effect Effects 0.000 claims abstract description 7
- 238000011049 filling Methods 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 21
- 239000002245 particle Substances 0.000 claims description 12
- 239000007789 gas Substances 0.000 claims description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000007789 sealing Methods 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 4
- 238000005551 mechanical alloying Methods 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 238000009736 wetting Methods 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 230000003014 reinforcing effect Effects 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910001338 liquidmetal Inorganic materials 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000011156 metal matrix composite Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 239000011208 reinforced composite material Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000010671 solid-state reaction Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000000844 transformation Methods 0.000 description 1
- 238000005406 washing Methods 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/77—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by unit-cell parameters, atom positions or structure diagrams
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crushing And Grinding (AREA)
- Powder Metallurgy (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention relates to a preparation method of non-stoichiometric titanium carbide TiCx powder, which comprises the following steps: titanium powder and carbon powder are mixed according to a non-stoichiometric ratio and put into a ball milling tank of a high-energy ball mill, and grinding balls are arranged in the ball milling tank; sealing the ball milling tank, vacuumizing, and then filling inert protective gas; starting a high-energy ball mill for high-energy ball milling; and after the ball milling is finished, cooling the ball milling tank, and then taking materials by a powder sieve to obtain the non-stoichiometric titanium carbide TiCx powder.
Description
Technical Field
The invention relates to a preparation method of titanium carbide TiCx powder with a non-stoichiometric ratio, belonging to the technical field of mechanical alloying.
Background
To the best of the applicant's knowledge, titanium carbide (TiC) has very high hardness, high melting point and modulus, and relatively low density, is widely used as a reinforcing phase of metal matrix composite materials or a reinforcing phase of composite coatings on metal surfaces to improve mechanical properties and wear resistance, and has been widely used in the fields of cutting tool materials, wear-resistant refractory materials, aviation, metallurgical minerals and the like.
The existing TiC powder synthesis method mainly uses titanium dioxide and CN101863663B as described in Chinese patents CN101462722B, CN101734659B, CN101792140B and CN101863663BCarbon (graphite or carbon black) is used as a raw material, and then the titanium carbide powder is prepared by carbothermic reduction (including sol-gel and carbothermic reduction methods), but very high reaction temperature (1700-2100 ℃) and long reaction time (10-24 h) are needed, so that the problems of complex raw materials, particle agglomeration, unreacted raw materials in products, further acid washing for obtaining high-purity powder and the like are caused. In addition, as a reinforcing phase of the metal material, TiC has poor wettability and weak binding force with metal, so that the physical and mechanical properties of the composite material are greatly influenced, and the development of the TiC particle reinforced composite material is restricted. How to improve the wettability and the interface bonding property of the titanium carbide material and a metal matrix through material design and optimization is also an urgent problem to be solved. Recent studies have shown that nonstoichiometric ratios of titanium carbide to metal have good wettability. Such as TiCx (x) of Cu energy to non-stoichiometric ratio<0.7) wetting occurred. And the wetting angle gradually decreases as the value of x decreases[1]. When x is 0.5, its wetting angle with Cu is close to 0 °. The good wettability can also reduce or avoid the occurrence of particle agglomeration, thereby being beneficial to obtaining a uniform material structure.
In the process of preparing materials, because crystal grains are refined, the area of a reaction interface is greatly increased, unreacted fresh interface contact is dynamically kept, and in addition, the temperature is increased in the process of crystal grain collision, some structural parameters are changed, the diffusion distance is reduced, the defect density is increased, so that the diffusion among crystals is promoted, the driving force of solid-state reaction is increased, the solid-solid reaction, the solid-liquid reaction and the solid-gas reaction at low temperature are induced, and the high-quality powder material is prepared at low temperature even at room temperature. However, no preparation process related to the method for preparing the non-stoichiometric TiCx titanium carbide powder is available.
Disclosure of Invention
The main purposes of the invention are: the method for preparing the titanium carbide TiCx powder with the non-stoichiometric ratio overcomes the problems in the prior art, is simple in process, and the particles of the obtained titanium carbide TiCx powder with the non-stoichiometric ratio are small.
The technical scheme for solving the technical problems of the invention is as follows:
a preparation method of non-stoichiometric titanium carbide TiCx powder adopts a high-energy ball mill, and is characterized by comprising the following steps:
firstly, titanium powder and carbon powder are mixed according to a non-stoichiometric ratio and put into a ball milling tank of a high-energy ball mill, and grinding balls are arranged in the ball milling tank; the non-stoichiometric ratio is that the molar ratio of titanium powder to carbon powder is 1: x, and x < 1;
secondly, after the ball milling tank is sealed, vacuumizing and then filling inert protective gas;
step three, starting a high-energy ball mill to perform high-energy ball milling;
and fourthly, after the ball milling is finished, cooling the ball milling tank, and then taking materials by a powder sieve to obtain the titanium carbide TiCx powder with the non-stoichiometric ratio.
The preparation method adopts a mechanical alloying technology, has simple process, small synthesized powder particles, short working procedure and low cost, and is suitable for large-scale industrial production.
The technical scheme of the invention is further perfected as follows:
preferably, in the first step, the value range of x is 0.5 ≦ x < 1.
More preferably, the value range of x is more than or equal to 0.5 and less than or equal to 0.7.
Preferably, in the first step, the titanium powder has a particle size of 10-200 microns and a purity of > 98.5%; the particle size of the carbon powder is 100-300 microns, and the purity is more than 99%.
By adopting the preferable scheme, the specific details of the first step can be further optimized, and the titanium carbide TiCx powder with non-stoichiometric ratio can be prepared better.
Preferably, in the second step, after evacuation, the pressure in the ball mill jar<1 Pa; after the inert protective gas is filled, the pressure in the ball milling tank is 103～105Pa。
More preferably, the inert shielding gas is argon with a purity > 99.99%.
By adopting the preferable scheme, the specific details of the second step can be further optimized, and the titanium carbide TiCx powder with non-stoichiometric ratio can be better prepared.
Preferably, in the third step, the conditions of the high-energy ball milling are as follows: the ball material mass ratio is (10-80): 1, ball milling rotation speed is 100-; the ball material mass ratio refers to the ratio of the total mass of the grinding balls to the total mass of the titanium powder and the carbon powder.
More preferably, the ball milling time is 6-10 h; or the ball milling time is 8-10 h.
By adopting the preferable scheme, the specific details of the mechanical alloying technology in the third step can be further optimized, and the titanium carbide TiCx powder with non-stoichiometric ratio can be prepared better.
Preferably, in the fourth step, the cooling treatment is closed air cooling treatment or water cooling treatment.
Preferably, the high-energy ball mill is a planetary high-energy ball mill; the material of the ball milling tank and the material of the grinding balls are stainless steel materials; the carbon powder is graphite powder.
By adopting the preferred scheme, various specific details can be further optimized.
Compared with the prior art, the invention adopts the mechanical alloying technology, has simple process, small synthesized powder particles, short working procedure and low cost, and is suitable for large-scale industrial production.
Drawings
FIG. 1 is a diagram showing the results of XRD phase analysis of example 1 of the present invention.
FIG. 2 is a diagram showing the results of XRD phase analysis of example 2 of the present invention.
Detailed Description
The invention relates to a preparation method of titanium carbide TiCx powder with non-stoichiometric ratio, which adopts a high-energy ball mill and comprises the following steps:
firstly, titanium powder and carbon powder are mixed according to a non-stoichiometric ratio and put into a ball milling tank of a high-energy ball mill, and grinding balls are arranged in the ball milling tank; the non-stoichiometric ratio is that the molar ratio of titanium powder to carbon powder is 1: x, and x < 1.
Wherein, the value range of x is more than or equal to 0.5 and less than 1, and preferably, x is more than or equal to 0.5 and less than or equal to 0.7. The particle size of the titanium powder is 10-200 microns, and the purity is more than 98.5%; the particle size of the carbon powder was 100-300 microns and the purity was > 99%.
And step two, after the ball milling tank is sealed, vacuumizing and then filling inert protective gas.
Wherein, after the vacuum pumping, the pressure in the ball milling tank<1 Pa; after the inert protective gas is filled, the pressure in the ball milling tank is 103～105Pa. Inert shielding gas is pure>99.99% argon.
And step three, starting a high-energy ball mill to perform high-energy ball milling.
Wherein, the conditions of the high-energy ball milling are as follows: the ball material mass ratio is (10-80): 1, the ball milling rotation speed is 100-; the ball material mass ratio refers to the ratio of the total mass of the grinding balls to the total mass of the titanium powder and the carbon powder.
And fourthly, after the ball milling is finished, cooling the ball milling tank, and then taking materials by a powder sieve to obtain the titanium carbide TiCx powder with the non-stoichiometric ratio. Wherein, the cooling treatment adopts closed air cooling treatment or water cooling treatment.
In addition, the high-energy ball mill is a planetary high-energy ball mill; the material of the ball milling tank and the material of the grinding balls are stainless steel materials; the carbon powder is graphite powder. Note: the high energy ball Mill is a commercially available product such as the variable rate ratio Planetary high energy ball Mill "pulveresette 4" Vario-Planetary Mill "by round park scientific instruments (shanghai).
The invention is described in further detail below with reference to embodiments and with reference to the drawings. The invention is not limited to the examples given.
Example 1
This example is TiC0.7Synthesis of powder (i.e., x is 0.7).
The embodiment adopts the technical scheme, and specific parameters are briefly summarized as follows:
weighing 21.4g of titanium powder and 3.6g of graphite powder; in the mechanical ball milling process, the mass ratio of ball materials is 40:1, the rotating speed is 400rpm, and the ball milling time is 1-8 h.
Taking different timeXRD phase analysis is carried out on the materials at the intermediate points, and the result is shown in figure 1, which shows that after 6 hours of ball milling, the diffraction peaks of Ti and C disappear completely, and only the diffraction peak of TiC is left, and the lattice parameter of the TiC
Indicating that the phase formed is TiC0.7. That is, this example successfully produced TiC0.7And (3) powder.
Example 2
This example is TiC0.5Synthesis of powder (i.e., x is 0.5).
The embodiment adopts the technical scheme, and specific parameters are briefly summarized as follows:
weighing 22.21g of titanium powder and 2.79g of graphite powder; in the mechanical ball milling process, the ball-material ratio is 20:1, the rotating speed is 400rpm, and the ball milling time is 1-8 h.
XRD phase analysis is carried out on materials at different time points, and the result is shown in figure 2, which shows that after 8 hours of ball milling, diffraction peaks of Ti and C disappear completely, only a peak of TiC is left, and lattice parameters of the TiC are shown
Indicating that the phase formed is TiC0.5. That is, this example successfully produced TiC0.5And (3) powder.
In addition to the above embodiments, the present invention may have other embodiments. All technical solutions formed by adopting equivalent substitutions or equivalent transformations fall within the protection scope of the claims of the present invention.
Reference documents:
[1]P.Xiao，B.Derby.Wetting of titanium nitride and titanium carbide by liquid metals[J].Acta Materialia，1996,44:307-314。
Claims (10)
1. a preparation method of non-stoichiometric titanium carbide TiCx powder adopts a high-energy ball mill, and is characterized by comprising the following steps:
firstly, titanium powder and carbon powder are mixed according to a non-stoichiometric ratio and put into a ball milling tank of a high-energy ball mill, and grinding balls are arranged in the ball milling tank; the non-stoichiometric ratio is that the molar ratio of titanium powder to carbon powder is 1: x, and x < 1;
secondly, after the ball milling tank is sealed, vacuumizing and then filling inert protective gas;
step three, starting a high-energy ball mill to perform high-energy ball milling;
and fourthly, after the ball milling is finished, cooling the ball milling tank, and then taking materials by a powder sieve to obtain the titanium carbide TiCx powder with the non-stoichiometric ratio.
2. The method of claim 1, wherein x is selected from the range of 0.5. ltoreq. x <1 in the first step.
3. The method of claim 2, wherein x is selected from the range of 0.5 and 0.7.
4. The method of claim 1, wherein the titanium carbide TiCx powder has a particle size of 10 to 200 μm and a purity of >98.5% in the first step; the particle size of the carbon powder is 100-300 microns, and the purity is more than 99%.
5. The method of claim 1, wherein in the second step, the pressure in the ball mill is increased after evacuation<1 Pa; after the inert protective gas is filled, the pressure in the ball milling tank is 103~105 Pa。
6. The method of claim 5, wherein the inert shielding gas is argon with a purity of > 99.99%.
7. The method for preparing the non-stoichiometric TiCx titanium carbide powder according to claim 1, wherein in the third step, the conditions of the high-energy ball milling are as follows: the ball material mass ratio is (10-80): 1, ball milling rotation speed is 100-; the ball material mass ratio refers to the ratio of the total mass of the grinding balls to the total mass of the titanium powder and the carbon powder.
8. The method for preparing the non-stoichiometric TiCx titanium carbide powder according to claim 7, wherein the ball milling time is 6-10 hours; or the ball milling time is 8-10 h.
9. The method of claim 1, wherein in the fourth step, the cooling treatment is performed by a closed air cooling treatment or a water cooling treatment.
10. The method for preparing a non-stoichiometric TiCx titanium carbide powder according to any of claims 1 to 9, wherein the high energy ball mill is a planetary high energy ball mill; the material of the ball milling tank and the material of the grinding balls are stainless steel materials; the carbon powder is graphite powder.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115367756A (en) * | 2022-06-20 | 2022-11-22 | 成都先进金属材料产业技术研究院股份有限公司 | Method for preparing titanium carbide powder by low-temperature molten salt ball milling |
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2020
- 2020-11-26 CN CN202011345332.5A patent/CN112441586A/en active Pending
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115367756A (en) * | 2022-06-20 | 2022-11-22 | 成都先进金属材料产业技术研究院股份有限公司 | Method for preparing titanium carbide powder by low-temperature molten salt ball milling |
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