CN102491328A - Titanium carbide powder and preparation method thereof - Google Patents
Titanium carbide powder and preparation method thereof Download PDFInfo
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- CN102491328A CN102491328A CN2011104046852A CN201110404685A CN102491328A CN 102491328 A CN102491328 A CN 102491328A CN 2011104046852 A CN2011104046852 A CN 2011104046852A CN 201110404685 A CN201110404685 A CN 201110404685A CN 102491328 A CN102491328 A CN 102491328A
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Abstract
The invention specifically relates to titanium carbide powder and a preparation method thereof. According to a technical scheme, the preparation method comprises the following steps of: uniformly mixing 10-25 percent by weight of aluminum powder or magnesium powder, 0.5-2 percent of amorphous graphite powder or carbon black, 5-20 percent by weight of titanium dioxide and 60-80 percent by weight of a halide of lithium serving as raw materials; putting the uniformly-mixed raw materials into a tubular electric furnace, raising the temperature to 900-1,100 DEG C at the temperature raising rate of 2-8 DEG C per minute under the atmosphere of argon, and preserving heat for 1-5 hours; putting an obtained product into hydrochloric acid of which the concentration is 2-4 mol/L for soaking for 3-6 hours, filtering, and cleaning with deionized water till the pH value of a cleaning solution is 7.0; and drying at the temperature of 110 DEG C for 10-24 hours to obtain titanium carbide powder. The method has the characteristics of low reaction temperature, simple process, controllable synthesis process, low production cost, and the like; and the prepared titanium carbide powder has the characteristics of high crystallization, high product purity, freeness from an impure phase and powder particle size of 100-400 nanometers.
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 (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| 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 |
| CN105777128A (en) * | 2016-03-01 | 2016-07-20 | 郑州大学 | Method for synthesizing hafnium carbide ceramic powder at low temperature through assisting of molten salts and magnesiothermic reduction |
| 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 |
| CN109231208A (en) * | 2018-11-30 | 2019-01-18 | 长江师范学院 | A kind of preparation method of transition metal carbide |
| CN115676834A (en) * | 2022-10-02 | 2023-02-03 | 郑州大学 | Method for preparing boron carbide powder with assistance of microwave molten salt |
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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 |
| CN103286321B (en) * | 2013-06-25 | 2015-01-28 | 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 |
| 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 |
| CN105314635A (en) * | 2015-12-07 | 2016-02-10 | 武汉科技大学 | High-purity titanium carbide powder and preparation method thereof |
| 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 |
| 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 |
| 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 |
| CN105777128A (en) * | 2016-03-01 | 2016-07-20 | 郑州大学 | Method for synthesizing hafnium carbide ceramic powder at low temperature through assisting of molten salts and magnesiothermic reduction |
| 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 |
| CN108975339B (en) * | 2018-08-29 | 2021-12-28 | 龙岩学院 | Preparation process of transition metal carbide powder and transition metal carbide-nitride composite powder |
| CN109231208A (en) * | 2018-11-30 | 2019-01-18 | 长江师范学院 | A kind of preparation method of transition metal carbide |
| CN115676834A (en) * | 2022-10-02 | 2023-02-03 | 郑州大学 | Method for preparing boron carbide powder with assistance of microwave molten salt |
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Application publication date: 20120613 |