CN102491328A - Titanium carbide powder and preparation method thereof - Google Patents
Titanium carbide powder and preparation method thereof Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 73
- 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 62
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 239000002245 particle Substances 0.000 claims abstract description 28
- 239000002994 raw material Substances 0.000 claims abstract description 28
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000000203 mixture Substances 0.000 claims abstract description 19
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 12
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000008367 deionised water Substances 0.000 claims abstract description 12
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000006229 carbon black Substances 0.000 claims abstract description 9
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 5
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical group [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims description 26
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 claims description 26
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 22
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 15
- 239000004411 aluminium Substances 0.000 claims description 11
- 229910052782 aluminium Inorganic materials 0.000 claims description 11
- 229910052786 argon Inorganic materials 0.000 claims description 11
- 239000007789 gas Substances 0.000 claims description 11
- 230000002000 scavenging effect Effects 0.000 claims description 11
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 4
- 238000000034 method Methods 0.000 abstract description 22
- 230000008569 process Effects 0.000 abstract description 11
- 238000006243 chemical reaction Methods 0.000 abstract description 10
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 238000002425 crystallisation Methods 0.000 abstract description 3
- 230000008025 crystallization Effects 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 239000012300 argon atmosphere Substances 0.000 abstract 1
- 238000004140 cleaning Methods 0.000 abstract 1
- 229910021641 deionized water Inorganic materials 0.000 abstract 1
- 239000012535 impurity Substances 0.000 abstract 1
- -1 lithium halide Chemical class 0.000 abstract 1
- 239000004408 titanium dioxide Substances 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract 1
- 239000000047 product Substances 0.000 description 19
- 238000001035 drying Methods 0.000 description 9
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 230000007812 deficiency Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 229940125368 controlled substance Drugs 0.000 description 1
- 239000000599 controlled substance Substances 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910052752 metalloid Inorganic materials 0.000 description 1
- 150000002738 metalloids Chemical class 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
本发明具体涉及一种碳化钛粉体及其制备方法。其技术方案是：先以10~25wt%的铝粉或镁粉、0.5~2wt%的土状石墨粉或炭黑、5~20wt%的二氧化钛和60~80wt%的锂的卤化物为原料，混合均匀；再将混合均匀的原料置于管式电炉内，在氩气气氛下以2~8℃/min的升温速率升至900~1100℃，保温1~5小时；然后将所得产物放入浓度为2~4mol/L的盐酸中浸泡3~6小时，过滤，用去离子水清洗至清洗液的pH值为7.0；最后在110℃条件下干燥10~24小时，即得碳化钛粉体。本发明具有反应温度低、工艺简单、合成过程可控和生产成本低等特点；所制备的碳化钛粉体结晶好，产物纯度高，无杂相，粉体粒度为100~400nm。The invention specifically relates to a titanium carbide powder and a preparation method thereof. The technical scheme is: firstly, 10-25wt% of aluminum powder or magnesium powder, 0.5-2wt% of earthy graphite powder or carbon black, 5-20wt% of titanium dioxide and 60-80wt% of lithium halide are used as raw materials, Mix evenly; then put the uniformly mixed raw materials in a tubular electric furnace, raise the temperature to 900~1100°C at a rate of 2~8°C/min in an argon atmosphere, and keep it warm for 1~5 hours; then put the obtained product into Soak in hydrochloric acid with a concentration of 2~4mol/L for 3~6 hours, filter, wash with deionized water until the pH of the cleaning solution is 7.0; finally dry at 110°C for 10~24 hours to obtain titanium carbide powder . The invention has the characteristics of low reaction temperature, simple process, controllable synthesis process and low production cost; the prepared titanium carbide powder has good crystallization, high product purity, no impurity phase, and the particle size of the powder is 100-400nm.
Description
Technical field
The invention belongs to the titanium carbide technical field.Be specifically related to a kind of titanium carbide powder and preparation method thereof.
Background technology
Titanium carbide is typical transition metal carbide.Titanium carbide have HS, high firmness, high temperature resistant, acid and alkali-resistance corrodes, wear-resistant, good electrical conductivity, thermal conductivity and to the excellent properties such as unreactiveness of iron and steel metalloid, is the material that the utmost point has using value.Especially it is fine, ultrafine powder equates the aspect as the enhancing of matrix material, has great exploitation value and application prospect.
The preparation method who carries out to the titanium carbide powder at present is a lot, like carbothermic method, chemical Vapor deposition process, self-propagating high-temperature synthesis method and sol-gel method etc.But all there is certain deficiency in these methods.
In a lot of methods of synthesizing titanium carbide, carbothermic method is a kind of traditional method, and synthesis mechanism is simple, is generally adopted at present.Under 1700 ~ 2100 ℃ of conditions, select for use carbon black reduction titanium oxide to make the titanium carbide powder in the industry.In the reduction reaction process, because grain growing and interparticle chemically bonded, the synthetic powder has the particle size distribution of broad, needs ball milling processing.In addition, the reaction times is longer, in the reaction owing to receive the influence of diffusion gradient to make synthetic powder purity lower.
Chemical Vapor deposition process can synthesize the titanium carbide powder of median size less than 100 nanometers, and can control TiC through the amount that changes reactant
xStoichiometric number can effectively be controlled the titanium carbide powder that synthesizes 1:1.This method weak point is that building-up process is complicated, and output is restricted, and gaseous feed TiCl
4With the HCl in the product intensive corrodibility is arranged, unfavorable to human body.
The reaction of self-propagating high-temperature synthesis method is exceedingly fast, and produces titanium carbide in case light the combustion wave of back generation through reactant titanium and carbon.The titanium carbide of separating out is not because of there being the time enough nodularization, and keeps the shape facility of carbon granule basically, so the porosity of product is bigger.These method needs are high-purity, the superfine titanium valve is made raw material, so the densification of product, size and porosity are to improve the emphasis of titanium carbide synthetic technology in the future.
Sol-gel method be with metallorganics through dissolving form solution, then become colloidal sol, produce gel at last and solidify, form final product through bakingout process again.Utilize this method synthesizing titanium carbide controlled substance composition preferably, but cost is higher relatively, operates also more complicated.
In a word, all there is certain deficiency in the technology of preparing to the titanium carbide powder at present: higher like cost of material, and complex technical process, wayward, yield poorly etc., greatly limited the industrialization production of titanium carbide powder.
Summary of the invention
The present invention is intended to overcome the deficiency that prior art exists; The preparation method of the titanium carbide powder that purpose provides that a kind of synthesis technique is simple, temperature of reaction is low, cost of material is cheap, building-up process is easy to control, productive rate height and industrialization prospect are big is high with even, the active height of particle size distribution and the purity of the titanium carbide powder of this method preparation.
Be to realize above-mentioned purpose, the technical scheme that the present invention adopts is: the halogenide with the lithium of the titanium oxide of the amorphous graphite powder of the aluminium powder of 10 ~ 25wt% or magnesium powder, 0.5 ~ 2wt% or carbon black, 5 ~ 20wt% and 60 ~ 80wt% is raw material earlier, mixes; The raw material that mixes is placed in the electric tube furnace, the temperature rise rate with 2 ~ 8 ℃/min under argon gas atmosphere rises to 900 ~ 1100 ℃ again, is incubated 1 ~ 5 hour; Then products therefrom being put into concentration is that the hydrochloric acid of 2 ~ 4mol/L soaked 3 ~ 6 hours, filters, and using the pH value of washed with de-ionized water to scavenging solution is 7.0; Under 110 ℃ of conditions dry 10 ~ 24 hours at last, promptly get the titanium carbide powder.Said titanium oxide is analytical pure, its purity >=99.5wt%.
The particle diameter of said amorphous graphite powder is less than 74 μ m.
Said sooty particle diameter is 2 ~ 3nm, and specific surface area is greater than 70m
2∕ g.
The halogenide of said lithium is lithium chloride or for lithium fluoride or be the mixture of lithium chloride and lithium fluoride; Wherein, lithium chloride is an analytical pure, and purity >=99wt%, lithium fluoride are analytical pure, purity >=99wt%.
The particle diameter of said aluminium powder is less than 74 μ m, purity >=99wt%.
The particle diameter of said magnesium powder is less than 125 μ m, purity >=99wt%.
Because adopt technique scheme, the present invention compared with prior art has following outstanding feature and is:
1, the mixing of realization response thing atomic scale in melting salt can effectively be controlled reaction process, reduces temperature of reaction and shorten the reaction times;
2, raw material sources are extensive, cheap, have very big industrialization prospect of production;
3, each component proportion speed of synthetic product, composition are even;
4, the product uniform particles is scattered in the melting salt, makes particles dispersed property fine, has reduced the generation of powder reuniting phenomenon;
Characteristics such as therefore, it is low that the present invention has temperature of reaction, and building-up process is simple, controlled, and production cost is low; Prepared titanium carbide powder advantages of good crystallization, high, the no dephasign of product purity, powder granularity is 100 ~ 400nm.
Embodiment
Below in conjunction with embodiment the present invention being done further description, is not the restriction to its protection domain.
For avoiding repetition, main chemical compositions and the granularity unification thereof that this embodiment is raw materials used earlier is described below, and repeat no more among each embodiment: titanium oxide is analytical pure, its purity>=99.5wt%.; The particle diameter of amorphous graphite powder is less than 74 μ m; The sooty particle diameter is 2 ~ 3nm, and specific surface area is greater than 70m
2∕ g; Lithium chloride is an analytical pure, purity>=99wt%; Lithium fluoride is an analytical pure, purity>=99wt%; The particle diameter of aluminium powder is less than 74 μ m, purity>=99wt%; The particle diameter of magnesium powder is less than 125 μ m, purity>=99wt%.
Embodiment 1
A kind of titanium carbide powder and preparation method thereof.Be raw material with the titanium oxide of 15 ~ 20wt%, the amorphous graphite powder of 1 ~ 2wt%, the lithium chloride of 60 ~ 69wt%, the aluminium powder of 15 ~ 22wt% earlier, mix; The raw material that mixes is placed in the electric tube furnace, the temperature rise rate with 2 ~ 5 ℃/min under argon gas atmosphere rises to 1000 ~ 1100 ℃ again, is incubated 1 ~ 3 hour; Then products therefrom being put into concentration is that the hydrochloric acid of 2 ~ 3mol/L soaked 3 ~ 5 hours, filters, and using washed with de-ionized water is 7.0 until the pH of scavenging solution value, and drying 10 ~ 16 hours under 110 ℃ of conditions promptly gets the titanium carbide powder at last.
The titanium carbide powder that present embodiment is prepared, purity is high, particle does not have reunion, and granularity is 260 ~ 400nm.
Embodiment 2
A kind of titanium carbide powder and preparation method thereof.Be raw material with the titanium oxide of 5 ~ 10wt%, the carbon black of 0.5 ~ 1.5wt%, the lithium fluoride of 70 ~ 80wt%, the magnesium powder of 10 ~ 20wt% earlier, mix; The raw material that mixes is placed in the electric tube furnace, the temperature rise rate with 3 ~ 6 ℃/min under argon gas atmosphere rises to 900 ~ 1050 ℃ again, is incubated 2 ~ 4 hours; Then products therefrom being put into concentration is that the hydrochloric acid of 3 ~ 4mol/L soaked 3 ~ 4 hours, filters, and using washed with de-ionized water is 7.0 until the pH of scavenging solution value, and drying 15 ~ 20 hours under 110 ℃ of conditions promptly gets the titanium carbide powder at last.
The titanium carbide powder that present embodiment is prepared, purity is high, particle does not have reunion, and granularity is 200 ~ 340nm.
Embodiment 3
A kind of titanium carbide powder and preparation method thereof.Be raw material with the titanium oxide of 10 ~ 15wt%, the amorphous graphite powder of 0.5 ~ 1wt%, the lithium chloride of 62 ~ 70wt% and the mixture of lithium fluoride, the aluminium powder of 18 ~ 25wt% earlier, mix; The raw material that mixes is placed in the electric tube furnace, the temperature rise rate with 5 ~ 8 ℃/min under argon gas atmosphere rises to 950 ~ 1100 ℃ again, is incubated 3 ~ 5 hours; Then products therefrom being put into concentration is that the hydrochloric acid of 2.5 ~ 3.5mol/L soaked 5 ~ 6 hours, filters, and using washed with de-ionized water is 7.0 until the pH of scavenging solution value, and drying 18 ~ 24 hours under 110 ℃ of conditions promptly gets the titanium carbide powder at last.
The titanium carbide powder that present embodiment is prepared, purity is high, particle does not have reunion, and granularity is 100 ~ 220nm.
Embodiment 4
A kind of titanium carbide powder and preparation method thereof.Be raw material with the titanium oxide of 5 ~ 9wt%, the carbon black of 1 ~ 2wt%, the lithium chloride of 68 ~ 75wt%, the aluminium powder of 14 ~ 21wt% earlier, mix; The raw material that mixes is placed in the electric tube furnace, the temperature rise rate with 3.5 ~ 5.5 ℃/min under argon gas atmosphere rises to 1050 ~ 1100 ℃ again, is incubated 3 ~ 4 hours; Then products therefrom being put into concentration is that the hydrochloric acid of 2 ~ 3.5mol/L soaked 3 ~ 4 hours, filters, and using washed with de-ionized water is 7.0 until the pH of scavenging solution value, and drying 18 ~ 24 hours under 110 ℃ of conditions promptly gets the titanium carbide powder at last.
The titanium carbide powder that present embodiment is prepared, purity is high, particle does not have reunion, and granularity is 120 ~ 220nm.
Embodiment 5
A kind of titanium carbide powder and preparation method thereof.Be raw material with the titanium oxide of 8 ~ 14wt%, the amorphous graphite powder of 0.7 ~ 1.8wt%, the lithium chloride of 74 ~ 80wt%, the aluminium powder of 10 ~ 16wt% earlier, mix; The raw material that mixes is placed in the electric tube furnace, the temperature rise rate with 4 ~ 6 ℃/min under argon gas atmosphere rises to 1000 ~ 1100 ℃ again, is incubated 1 ~ 3 hour; Then products therefrom being put into concentration is that the hydrochloric acid of 2.5 ~ 3.5mol/L soaked 4 ~ 5 hours, filters, and using washed with de-ionized water is 7.0 until the pH of scavenging solution value, and drying 20 ~ 24 hours under 110 ℃ of conditions promptly gets the titanium carbide powder at last.
The titanium carbide powder that present embodiment is prepared, purity is high, particle does not have reunion, and granularity is 200 ~ 300nm.
Embodiment 6
A kind of titanium carbide powder and preparation method thereof.Be raw material with the titanium oxide of 7 ~ 15wt%, the carbon black of 0.8 ~ 1.2wt%, the lithium fluoride of 60 ~ 68wt%, the magnesium powder of 17 ~ 25wt% earlier, mix; The raw material that mixes is placed in the electric tube furnace, the temperature rise rate with 6 ~ 8 ℃/min under argon gas atmosphere rises to 950 ~ 1050 ℃ again, is incubated 4 ~ 5 hours; Then products therefrom being put into concentration is that the hydrochloric acid of 3 ~ 4mol/L soaked 5 ~ 6 hours, filters, and using washed with de-ionized water is 7.0 until the pH of scavenging solution value, and drying 10 ~ 16 hours under 110 ℃ of conditions promptly gets the titanium carbide powder at last.
The titanium carbide powder that present embodiment is prepared, purity is high, particle does not have reunion, and granularity is 300 ~ 400nm.
Embodiment 7
A kind of titanium carbide powder and preparation method thereof.Be raw material with the titanium oxide of 12 ~ 18wt%, the carbon black of 1 ~ 1.5wt%, the lithium fluoride of 65 ~ 75wt%, the magnesium powder of 15 ~ 22wt% earlier, mix; The raw material that mixes is placed in the electric tube furnace, the temperature rise rate with 2 ~ 5 ℃/min under argon gas atmosphere rises to 900 ~ 1000 ℃ again, is incubated 1 ~ 3 hour; Then products therefrom being put into concentration is that the hydrochloric acid of 2 ~ 3mol/L soaked 3 ~ 4 hours, filters, and using washed with de-ionized water is 7.0 until the pH of scavenging solution value, and drying 18 ~ 24 hours under 110 ℃ of conditions promptly gets the titanium carbide powder at last.
The titanium carbide powder that present embodiment is prepared, purity is high, particle does not have reunion, and granularity is 200 ~ 300nm.
Embodiment 8
A kind of titanium carbide powder and preparation method thereof.Be raw material with the titanium oxide of 5 ~ 12wt%, the amorphous graphite powder of 0.5 ~ 1.3wt%, the lithium chloride of 70 ~ 80wt% and the mixture of lithium fluoride, the aluminium powder of 10 ~ 18wt% earlier, mix; The raw material that mixes is placed in the electric tube furnace, the temperature rise rate with 5 ~ 8 ℃/min under argon gas atmosphere rises to 1000 ~ 1100 ℃ again, is incubated 4 ~ 5 hours; Then products therefrom being put into concentration is that the hydrochloric acid of 3 ~ 4mol/L soaked 5 ~ 6 hours, filters, and using washed with de-ionized water is 7.0 until the pH of scavenging solution value, and drying 20 ~ 24 hours under 110 ℃ of conditions promptly gets the titanium carbide powder at last.
The titanium carbide powder that present embodiment is prepared, purity is high, particle does not have reunion, and granularity is 300 ~ 400nm.
Embodiment 9
A kind of titanium carbide powder and preparation method thereof.Be raw material with the titanium oxide of 8 ~ 16wt%, the carbon black of 0.7 ~ 1.2wt%, the lithium chloride of 60 ~ 69wt% and the mixture of lithium fluoride, the aluminium powder of 17 ~ 26wt% earlier, mix; The raw material that mixes is placed in the electric tube furnace, the temperature rise rate with 2 ~ 4 ℃/min under argon gas atmosphere rises to 900 ~ 1000 ℃ again, is incubated 1 ~ 3 hour; Then products therefrom being put into concentration is that the hydrochloric acid of 2 ~ 3mol/L soaked 3 ~ 5 hours, filters, and using washed with de-ionized water is 7.0 until the pH of scavenging solution value, and drying 10 ~ 15 hours under 110 ℃ of conditions promptly gets the titanium carbide powder at last.
The titanium carbide powder that present embodiment is prepared, purity is high, particle does not have reunion, and granularity is 100 ~ 180nm.
This embodiment compared with prior art has following outstanding feature:
1, the mixing of realization response thing atomic scale in melting salt can effectively be controlled reaction process, reduces temperature of reaction and shorten the reaction times;
2, raw material sources are extensive, cheap, have very big industrialization prospect of production;
3, each component proportion speed of synthetic product, composition are even;
4, the product uniform particles is scattered in the melting salt, makes particles dispersed property fine, has reduced the generation of powder reuniting phenomenon;
Characteristics such as therefore, it is low that this embodiment has temperature of reaction, and building-up process is simple, controlled, and production cost is low; Prepared titanium carbide powder advantages of good crystallization, high, the no dephasign of product purity, powder granularity is 100 ~ 400nm.
Claims (8)
1. the preparation method of a titanium carbide powder is characterized in that earlier the halogenide with the lithium of the titanium oxide of the amorphous graphite powder of the aluminium powder of 10 ~ 25wt% or magnesium powder, 0.5 ~ 2wt% or carbon black, 5 ~ 20wt% and 60 ~ 80wt% is raw material, mixes; The raw material that mixes is placed in the electric tube furnace, the temperature rise rate with 2 ~ 8 ℃/min under argon gas atmosphere rises to 900 ~ 1100 ℃ again, is incubated 1 ~ 5 hour; Then products therefrom being put into concentration is that the hydrochloric acid of 2 ~ 4mol/L soaked 3 ~ 6 hours, filters, and using the pH value of washed with de-ionized water to scavenging solution is 7.0; Under 110 ℃ of conditions dry 10 ~ 24 hours at last, promptly get the titanium carbide powder.
2. according to the preparation method of the said titanium carbide powder of claim 1, it is characterized in that said titanium oxide is analytical pure, its purity >=99.5wt%.
3. according to the preparation method of the said titanium carbide powder of claim 1, the particle diameter that it is characterized in that said amorphous graphite powder is less than 74 μ m.
4. according to the preparation method of the said titanium carbide powder of claim 1, it is characterized in that said sooty particle diameter is 2 ~ 3nm, specific surface area is greater than 70m
2∕ g.
5. according to the preparation method of the said titanium carbide powder of claim 1, the halogenide that it is characterized in that said lithium is lithium chloride or for lithium fluoride or be the mixture of lithium chloride and lithium fluoride; Wherein, lithium chloride is an analytical pure, and purity >=99wt%, lithium fluoride are analytical pure, purity >=99wt%.
6. according to the preparation method of the said titanium carbide powder of claim 1, the particle diameter that it is characterized in that said aluminium powder is less than 74 μ m, purity >=99wt%.
7. according to the preparation method of the said titanium carbide powder of claim 1, the particle diameter that it is characterized in that said magnesium powder is less than 125 μ m, purity >=99wt%.
8. according to the prepared titanium carbide powder of preparation method of each said titanium carbide powder in the claim 1 ~ 7.
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Cited By (14)
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| CN103286321A (en) * | 2013-06-25 | 2013-09-11 | 武汉科技大学 | Metal tungsten ultrafine powder and preparation method thereof |
| CN103449435A (en) * | 2013-08-27 | 2013-12-18 | 哈尔滨工业大学 | Method for producing micro-nanoscale carbide ceramics by carbon coating |
| CN103936007A (en) * | 2014-05-05 | 2014-07-23 | 湖南大学 | Method for preparing titanium carbide nano-powder material |
| CN104310398A (en) * | 2014-10-11 | 2015-01-28 | 云南民族大学 | Method for producing titanium carbide powder by using circulating fluidized bed reactor |
| CN105314635A (en) * | 2015-12-07 | 2016-02-10 | 武汉科技大学 | High-purity titanium carbide powder and preparation method thereof |
| CN105439146A (en) * | 2015-07-29 | 2016-03-30 | 洛阳新巨能高热技术有限公司 | Preparation method for nano titanium carbide particles |
| CN105502398A (en) * | 2016-03-01 | 2016-04-20 | 郑州大学 | Method for synthesizing tantalum carbide superfine powder through molten salt assisted magnesiothermic reduction |
| CN105732042A (en) * | 2016-03-01 | 2016-07-06 | 郑州大学 | Method for preparing ultrafine tantalum carbide powder by using fused salt under assistance of low temperature |
| CN105732043A (en) * | 2016-03-01 | 2016-07-06 | 郑州大学 | Method for preparing hafnium carbide ceramic powder body by using fused salt under assistance of carbon thermal reduction |
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| CN108975339A (en) * | 2018-08-29 | 2018-12-11 | 龙岩学院 | A kind of transition metal carbide powder and transition metal carbide-nitridation composite powder preparation process |
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| CN115676834A (en) * | 2022-10-02 | 2023-02-03 | 郑州大学 | A method for preparing boron carbide powder assisted by microwave molten salt |
| CN116119668A (en) * | 2023-03-16 | 2023-05-16 | 辽宁大学 | A low-cost Ti3C2MXene material prepared based on molten salt method and its preparation method |
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