CN103265031A - Method for low-temperature preparation of ZrC-WC or ZrC-TaC mixed powder through carbothermic method - Google Patents
Method for low-temperature preparation of ZrC-WC or ZrC-TaC mixed powder through carbothermic method Download PDFInfo
- Publication number
- CN103265031A CN103265031A CN2013101833785A CN201310183378A CN103265031A CN 103265031 A CN103265031 A CN 103265031A CN 2013101833785 A CN2013101833785 A CN 2013101833785A CN 201310183378 A CN201310183378 A CN 201310183378A CN 103265031 A CN103265031 A CN 103265031A
- Authority
- CN
- China
- Prior art keywords
- zrc
- carbon source
- tac
- obtains
- powder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Abstract
The invention relates to a method for low-temperature preparation of ZrC-WC or ZrC-TaC mixed powder through a carbothermic method, belonging to the technical field of structural ceramics. According to the method, sucrose, phenolic resin, epoxy resin or asphalt is used as a carbon source; and mixed oxide is used as a metal source, wherein the mixed oxide is a mixture of zirconium oxide and tungsten oxide or a mixture of zirconium oxide and tantalum pentoxide. According to the invention, the sucrose, phenolic resin, epoxy resin or asphalt and the mixed oxide are used as the raw materials, so that the raw material cost is low; the sucrose, phenolic resin, epoxy resin or asphalt and the oxide are evenly mixed through a wet method, so that the aggregation possibility is low; and the synthesis process is performed under a high-purity argon gas environment or in vacuum, so that ZrC-WC (ZrC-TaC) powder can be synthesized through reduction reaction at a low temperature.
Description
Technical field
The present invention relates to the method that a kind of carbothermic method low temperature prepares ZrC-WC or ZrC-TaC mixed powder, belong to the structural ceramics technical field.
Background technology
Ultrahigh-temperature pottery (Ultra-high Temperature Ceramics, UHTCs) refer to 1800 ° more than the C and in the reaction atmosphere (such as Sauerstoffatom) have carbide and the boride material of the transition metal of anti-oxidant, the anti-ablative and heat-shock resistance of excellent high-temperature, mainly comprise TaC, HfC, ZrC, HfB
2, ZrB
2Deng, its excellent high-temperature behavior makes them can adapt to the superelevation sonic flight, atmospheric layer reenters, strides extreme environments such as aerial flight and rocket propulsion system, can be used for various key positions or parts such as aircraft nose cone, the leading edge of a wing, numbers of hot-side engine.Refractory carbide TaC, HfC, ZrC are the material systems of 3500 ° of above high temperature of C of unique ability except carbon.Wherein, the high specific strength of ZrC, high ratio modulus and low preparation cost make one of its hyperthermal material that becomes tool application potential.
Yet hard-to-sinter and weak oxide are the subject matter that limits its application.Because ZrC is covalent bonds, its diffusivity is low, needs High Temperature High Pressure ability densified sintering product.At ZrC material hard-to-sinter, the problem of low-temperature sintering difficulty especially, preparation high pure and ultra-fine ZrC powder is crucial, can obviously improve its coking property.On the other hand, ZrC easy oxidation in high-temperature oxidation environment generates loose zirconia layer, and being difficult to effectively, obstruction oxygen spreads to material internal.In order to improve its oxidation-resistance, the researchist adds in the compound that contains Zr and contains high-valence cationic (as W
5+, Ta
5+And Nb
5+Deng) compound, as WC, TaC and NbC etc.This class material is in oxidising process, and generation has by the protective layer of dynamic oxidation, can hinder oxygen and spread to material internal, has effectively improved its oxidation-resistance.And, adding high price cation compounds such as WC in the material, its high-temperature bending strength can improve about 1 times, so the ZrC-WC complex phase ceramic can improve its oxidation-resistance can improve its high-temperature bending strength again, has improved the range of application of ZrC material to a great extent.Therefore, active demand has been proposed synthesizing high pure superfine ZrC-WC composite granule.
At present, the preparation method of synthetic ZrC powder mainly contains: direct synthesis technique, carbothermic method, sol-gel method, mechanical alloying method, self-propagating combustion synthesis method etc.Wherein, the technology that can realize suitability for industrialized production is carbothermic method, and the method for synthetic ZrC powder is to adopt carbon black reduction-oxidation zirconium method, and its chemical equation is as follows:
ZrO
2+3C=ZrC+2CO(g) (1)
Similar, the method carbon black of synthetic WC and TaC powder is reduced corresponding oxide compound, and chemical equation is as follows:
2WO
3+7C=W
2C+6CO(g) (2)
WO
3+4C=WC+3CO(g) (3)
Ta
2O
5+6C=Ta
2C+5CO(g) (4)
Ta
2O
5+7C=2TaC+5CO(g) (5)
According to calculation of thermodynamics (as Fig. 1 and Fig. 2) as can be known, the high-purity argon gas condition is the prerequisite of low temperature synthesizing high pure superfine powder.Adopt sucrose to make carbon source, can solve the solid uneven problem of mixing, realize the method that liquid-solid wet mixing is closed, make the oxidate powder surface evenly apply one deck sucrose (forming one deck C film after the cracking), be conducive to the reaction of carbothermic reduction, synthetic powder has the high and little characteristics of particle diameter of purity.
Summary of the invention
The objective of the invention is to prepare for a kind of carbothermic method low temperature the method for ZrC-WC or ZrC-TaC mixed powder, this method technology is simple, temperature is low, weak point consuming time, can obtain high pure and ultra-fine ZrC-WC (TaC) powder.
The objective of the invention is to be achieved through the following technical solutions.
A kind of carbothermic method low temperature of the present invention prepares the method for ZrC-WC or ZrC-TaC mixed powder, this method with sucrose, resol, Resins, epoxy or pitch as carbon source, with mixed oxide as source metal, mixed oxide is the mixture of zirconium white and Tungsten oxide 99.999 or the mixture of zirconium white and tantalum pentoxide, the mol ratio of zirconium white and Tungsten oxide 99.999 is 1:10～1:5, the mol ratio of zirconium white and tantalum pentoxide is 1:10～1:5, the molar weight of carbon is 3～20:1 with the ratio of the integral molar quantity of mixed oxide in the carbon source, steps of the method are:
1) mixed oxide is put into ball grinder, add solvent orange 2 A, the quality of the solvent orange 2 A that adds is 1%～5% of mixed oxide total mass, add the zirconia ball grinding media then, ball milling mixing 10-48h, oxide compound behind the mixing is moved in the vessel that solvent orange 2 A is housed, and ultra-sonic dispersion obtains mixing solutions;
2) carbon source is dissolved among the solvent B, obtains carbon source solution, then the carbon source solution that obtains is poured in the mixing solutions that obtains in the step 1); Heat then, stir, the reactant that obtains mixing;
3) with step 2) reactant that obtains packs in the plumbago crucible; plumbago crucible is put into flow argon shield or vacuum heat treatment furnace to be heated; cool to room temperature then with the furnace, obtain ZrC-WC (or ZrC-TaC) powder through grinding again, the particle diameter of the powder that obtains is 50～200nm.
The total concn of the mixing solutions that obtains above-mentioned steps 1) is 1～5mol/L, and the ultra-sonic dispersion time is 0.5～2h; Zirconic purity 〉=99.9wt.%, particle diameter are 50～120nm; Purity 〉=the 99.9wt.% of Tungsten oxide 99.999, particle diameter are 50～120nm; Purity 〉=the 99.9wt.% of tantalum pentoxide, particle diameter are 50～120nm.
Above-mentioned steps 2) concentration of carbon source solution is 3～15mol/L in, and when carbon source was sucrose, solvent B was water, and when carbon source was resol, Resins, epoxy or pitch, solvent B was ethanol, normal hexane or hexanaphthene; Carbon source is analytical pure; 100～250 ℃ of Heating temperatures, heat-up time 0.5～2h; Alr mode is magnetic agitation;
Above-mentioned steps 3) in the heat treatment furnace heating schedule be heated to 1200～1600 ° of C insulation 0.5～2h for the temperature rise rate with 10 ° of C/min.
Among the present invention, mechanical milling process adopts mixed oxide powder and sucrose (or resol, Resins, epoxy, pitch etc.) solution to carry out wet mixing, mixes, and has solved two kinds of solid phase powders and has mixed unevenly, and purity is the problem of high easy reunion not; Adopt high-purity argon gas or vacuum in the preparation process, reduction reaction can take place at a lower temperature prepare ultra-fine ZrC-WC (ZrC-TaC) powder.
Beneficial effect
Adopting sucrose, resol, Resins, epoxy or pitch and mixed oxide among the present invention is raw material, raw materials cost is low, and sucrose, resol, Resins, epoxy or pitch and oxide compound be mixed into wet mixing, mix, be difficult for reuniting, building-up process is carried out under the high-purity argon gas environment or in the vacuum, and synthetic ZrC-WC (ZrC-TaC) powder of reduction reaction can take place at a lower temperature, and namely this method technology is simple, temperature is low, weak point consuming time.The present invention adopts organism evenly to be coated on around the mixed oxide particle, reaches mixed uniformly purpose, prepares high-purity ZrC-WC (ZrC-TaC) mixed powder.
Description of drawings
Fig. 1 depresses the relation of Gibbs free energy and temperature for standard atmosphere;
Fig. 2 is Gibbs free energy under the high-purity Ar and the relation of temperature;
Fig. 3 is the ZrC-WC powder of preparation and the X ray diffracting spectrum of ZrC-TaC powder; Wherein, the unit of ordinate zou intensity is cps, and X-coordinate diffraction angular unit is °;
Fig. 4 is the stereoscan photograph of the ZrC-WC powder of embodiment preparation;
Fig. 5 is the stereoscan photograph of the ZrC-TaC powder of embodiment preparation.
Embodiment
The present invention will be further described below in conjunction with embodiment.
Embodiment 1
With sucrose as carbon source, with zirconium white and Tungsten oxide 99.999 as the refractory metal source;
1) takes by weighing 246.4g ZrO
2Powder, 23.2gWO
3Powder, its purity are 99.9wt.%, and particle diameter is 80nm, puts into ball grinder together, add the 100ml dehydrated alcohol, and zirconia ball ball milling mixing 24h moves to the oxide compound behind the mixing in the vessel that the 100ml dehydrated alcohol is housed ultra-sonic dispersion 0.5h;
2) take by weighing 365.1g sucrose and join in the 100ml water, stir it is mixed, join then in the solution that step 1) obtains, heating is magnetic agitation simultaneously, and Heating temperature is 120 ℃, and be 2h heat-up time, the reactant that obtains mixing;
3) with step 2) reactant that obtains packs in the plumbago crucible, the heat treatment furnace of then plumbago crucible being put into the high-purity argon gas protection heats, heating schedule is warming up to 1600 ℃ of insulation 1h for the temperature rise rate with 10 ℃/min, cool to room temperature then with the furnace, obtain the mixed powder material through grinding again; The X-ray diffractogram of the powder body material that obtains as shown in Figure 3, its stereoscan photograph as shown in Figure 4, sweep voltage is 15kv.As shown in Figure 3, the powder body material that obtains is the ZrC-5mol%WC mixed powder; As shown in Figure 4, the median size of ZrC-5mol%WC powder is 100nm.
Embodiment 2
With sucrose as carbon source, with zirconium white and Tungsten oxide 99.999 as the refractory metal source;
1) takes by weighing 246.4g ZrO
2Powder, 46.4gWO
3Powder, its purity are 99.9wt.%, and particle diameter is 70nm, puts into ball grinder together, add the 100ml dehydrated alcohol, and zirconia ball ball milling mixing 24h moves to the oxide compound behind the mixing in the vessel that the 100ml dehydrated alcohol is housed ultra-sonic dispersion 1h;
2) take by weighing 388g sucrose and join in the 100ml water, stir it is mixed, join then in the solution that step 1) obtains, heating is magnetic agitation simultaneously, and Heating temperature is 140 ℃, and be 2h heat-up time, the reactant that obtains mixing;
3) with step 2) reactant that obtains packs in the plumbago crucible, the heat treatment furnace of then plumbago crucible being put into the high-purity argon gas protection heats, heating schedule is warming up to 1600 ℃ of insulation 1h for the temperature rise rate with 10 ℃/min, cool to room temperature then with the furnace, obtain the mixed powder material through grinding again; The X-ray diffractogram of the powder body material that obtains as shown in Figure 3, as shown in Figure 3, the powder body material that obtains is the ZrC-10mol%WC mixed powder.
Embodiment 3
With sucrose as carbon source, with zirconium white and tantalum pentoxide as the refractory metal source;
1) takes by weighing 246.4g ZrO
2Powder, 44.2gTa
2O
5Powder, its purity are 99.9wt.%, and particle diameter is 60nm, puts into ball grinder together, add the 120ml dehydrated alcohol, and zirconia ball ball milling mixing 12h moves to the oxide compound behind the mixing in the vessel that the 100ml dehydrated alcohol is housed ultra-sonic dispersion 2h;
2) take by weighing 382.2g sucrose and join in the 110ml water, stir it is mixed, join then in the solution that step 1) obtains, heating is magnetic agitation simultaneously, and Heating temperature is 160 ℃, and be 1h heat-up time, the reactant that obtains mixing;
3) with step 2) reactant that obtains packs in the plumbago crucible, the heat treatment furnace of then plumbago crucible being put into the high-purity argon gas protection heats, heating schedule is warming up to 1500 ℃ of insulation 2h for the temperature rise rate with 10 ℃/min, cool to room temperature then with the furnace, obtain the mixed powder material through grinding again; The X-ray diffractogram of the powder body material that obtains as shown in Figure 3, its stereoscan photograph as shown in Figure 5, sweep voltage is 15kv.As shown in Figure 3, the powder body material that obtains is the ZrC-10mol%TaC mixed powder; As shown in Figure 5, the median size of ZrC-10mol%TaC powder is 100nm.
Embodiment 4
With sucrose as carbon source, with zirconium white and tantalum pentoxide as the refractory metal source;
1) takes by weighing 246.4g ZrO
2Powder, 88.4gTa
2O
5Powder, its purity are 99.9wt.%, and particle diameter is 90nm, puts into ball grinder together, add the 120ml dehydrated alcohol, and zirconia ball ball milling mixing 24h moves to the oxide compound behind the mixing in the vessel that the 150ml dehydrated alcohol is housed ultra-sonic dispersion 1.5h;
2) take by weighing 422.2g sucrose and join in the 120ml water, stir it is mixed, join then in the solution that step 1) obtains, heating is magnetic agitation simultaneously, and Heating temperature is 130 ℃, and be 2h heat-up time, the reactant that obtains mixing;
3) with step 2) reactant that obtains packs in the plumbago crucible, the heat treatment furnace of then plumbago crucible being put into the high-purity argon gas protection heats, heating schedule is warming up to 1600 ℃ of insulation 1h for the temperature rise rate with 10 ℃/min, cool to room temperature then with the furnace, obtain the mixed powder material through grinding again; The X-ray diffractogram of the powder body material that obtains as shown in Figure 3, as shown in Figure 3, the powder body material that obtains is the ZrC-20mol%TaC mixed powder.
Embodiment 5
With resol as carbon source, with zirconium white and Tungsten oxide 99.999 as the refractory metal source;
1) takes by weighing 246.4g ZrO
2Powder, 23.2gWO
3Powder, its purity are 99.9wt.%, and particle diameter is 60nm, puts into ball grinder together, add the 110ml dehydrated alcohol, and zirconia ball ball milling mixing 24h moves to the oxide compound behind the mixing in the vessel that the 110ml dehydrated alcohol is housed ultra-sonic dispersion 1h;
2) take by weighing 342g resol and join in the 150ml dehydrated alcohol, stir it is mixed, join then in the solution that step 1) obtains, heating is magnetic agitation simultaneously, and Heating temperature is 150 ℃, and be 1.5h heat-up time, the reactant that obtains mixing;
3) with step 2) reactant that obtains packs in the plumbago crucible; the heat treatment furnace of then plumbago crucible being put into the high-purity argon gas protection heats; heating schedule is warming up to 1400 ℃ of insulation 2h for the temperature rise rate with 10 ℃/min; cool to room temperature then with the furnace, obtain the ZrC-5mol%WC mixed powder through grinding again.
Embodiment 6
With resol as carbon source, with zirconium white and tantalum pentoxide as the refractory metal source;
1) takes by weighing 246.4g ZrO
2Powder, 88.4gTa
2O
5Powder, its purity are 99.9wt.%, and particle diameter is 80nm, puts into ball grinder together, add the 130ml dehydrated alcohol, and zirconia ball ball milling mixing 48h moves to the oxide compound behind the mixing in the vessel that the 150ml dehydrated alcohol is housed ultra-sonic dispersion 1.5h;
2) take by weighing 395.4g resol and join in the 130ml normal hexane, stir it is mixed, join then in the solution that step 1) obtains, heating is magnetic agitation simultaneously, and Heating temperature is 120 ℃, and be 2.5h heat-up time, the reactant that obtains mixing;
3) with step 2) reactant that obtains packs in the plumbago crucible; the heat treatment furnace of then plumbago crucible being put into the high-purity argon gas protection heats; heating schedule is warming up to 1300 ℃ of insulation 2h for the temperature rise rate with 10 ℃/min; cool to room temperature then with the furnace, obtain the ZrC-20mol%TaC mixed powder through grinding again.
Embodiment 7
With Resins, epoxy as carbon source, with zirconium white and Tungsten oxide 99.999 as the refractory metal source;
1) takes by weighing 246.4g ZrO
2Powder, 46.4gWO
3Powder, its purity are 99.9wt.%, and particle diameter is 90nm, puts into ball grinder together, add the 130ml dehydrated alcohol, and zirconia ball ball milling mixing 24h moves to the oxide compound behind the mixing in the vessel that the 150ml dehydrated alcohol is housed ultra-sonic dispersion 1h;
2) take by weighing 396.9g Resins, epoxy and join in the 130ml hexanaphthene, stir it is mixed, join then in the solution that step 1) obtains, heating is magnetic agitation simultaneously, and Heating temperature is 140 ℃, and be 2h heat-up time, the reactant that obtains mixing;
3) with step 2) reactant that obtains packs in the plumbago crucible; the heat treatment furnace of then plumbago crucible being put into the high-purity argon gas protection heats; heating schedule is warming up to 1700 ℃ of insulation 1h for the temperature rise rate with 10 ℃/min; cool to room temperature then with the furnace, obtain the ZrC-10mol%WC mixed powder through grinding again.
Embodiment 8
With pitch as carbon source, with zirconium white and tantalum pentoxide as the refractory metal source;
1) takes by weighing 246.4g ZrO
2Powder, 44.2gTa
2O
5Powder, its purity are 99.9wt.%, and particle diameter is 70nm, puts into ball grinder together, add the 140ml dehydrated alcohol, and zirconia ball ball milling mixing 12h moves to the oxide compound behind the mixing in the vessel that the 100ml dehydrated alcohol is housed ultra-sonic dispersion 2h;
2) take by weighing 380g pitch and join in the 210ml dehydrated alcohol, stir it is mixed, join then in the solution that step 1) obtains, heating is magnetic agitation simultaneously, and Heating temperature is 150 ℃, and be 0.5h heat-up time, the reactant that obtains mixing;
3) with step 2) reactant that obtains packs in the plumbago crucible; the heat treatment furnace of then plumbago crucible being put into the high-purity argon gas protection heats; heating schedule is warming up to 1400 ℃ of insulation 2h for the temperature rise rate with 10 ℃/min; cool to room temperature then with the furnace, obtain the ZrC-10mol%TaC mixed powder through grinding again.
Claims (8)
1. a carbothermic method low temperature prepares the method for ZrC-WC or ZrC-TaC mixed powder, it is characterized in that steps of the method are:
1) mixed oxide is put into ball grinder, add solvent orange 2 A, the quality of adding solvent orange 2 A is 1%～5% of mixed oxide total mass; Add the zirconia ball grinding media then, ball milling mixing 10-48h moves to the oxide compound behind the mixing in the vessel that solvent orange 2 A is housed, and ultra-sonic dispersion obtains mixing solutions;
2) carbon source is dissolved among the solvent B, obtains carbon source solution, then the carbon source solution that obtains is poured in the mixing solutions that obtains in the step 1); Heat then, stir, the reactant that obtains mixing;
3) with step 2) reactant that obtains packs in the plumbago crucible, plumbago crucible is put into flow argon shield or vacuum heat treatment furnace to be heated, cool to room temperature then with the furnace, obtain ZrC-WC (or ZrC-TaC) powder through grinding again, the particle diameter of the powder that obtains is 50～200nm;
Described carbon source is sucrose, resol, Resins, epoxy or pitch, and described mixed oxide is the mixture of zirconium white and Tungsten oxide 99.999 or the mixture of zirconium white and tantalum pentoxide;
Described solvent orange 2 A is water or dehydrated alcohol.
2. a kind of carbothermic method low temperature according to claim 1 prepares the method for ZrC-WC or ZrC-TaC mixed powder, it is characterized in that: the mol ratio of zirconium white and Tungsten oxide 99.999 is 1:10～1:5, and the molar weight of carbon is 3～20:1 with the ratio of the integral molar quantity of mixed oxide in the carbon source.
3. a kind of carbothermic method low temperature according to claim 1 prepares the method for ZrC-WC or ZrC-TaC mixed powder, it is characterized in that: the mol ratio of zirconium white and tantalum pentoxide is 1:10～1:5, and the molar weight of carbon is 3～20:1 with the ratio of the integral molar quantity of mixed oxide in the carbon source.
4. a kind of carbothermic method low temperature according to claim 1 prepares the method for ZrC-WC or ZrC-TaC mixed powder, it is characterized in that: the total concn of the mixing solutions that obtains in the step 1) is 1～5mol/L, and the ultra-sonic dispersion time is 0.5～2h; Zirconic purity 〉=99.9wt.%, particle diameter are 50～120nm; Purity 〉=the 99.9wt.% of Tungsten oxide 99.999, particle diameter are 50～120nm; Purity 〉=the 99.9wt.% of tantalum pentoxide, particle diameter are 50～120nm.
5. a kind of carbothermic method low temperature according to claim 1 prepares the method for ZrC-WC or ZrC-TaC mixed powder, it is characterized in that: step 2) in the concentration of carbon source solution be 3～15mol/L, carbon source is sucrose, solvent B is water.
6. a kind of carbothermic method low temperature according to claim 1 prepares the method for ZrC-WC or ZrC-TaC mixed powder, it is characterized in that: step 2) in the concentration of carbon source solution be 3～15mol/L, carbon source is resol, Resins, epoxy or pitch, and solvent B is ethanol, normal hexane or hexanaphthene.
7. a kind of carbothermic method low temperature according to claim 1 prepares the method for ZrC-WC or ZrC-TaC mixed powder, it is characterized in that: step 2) in carbon source be analytical pure; Heating temperature is 100～250 ℃, and be 0.5～2h heat-up time; Alr mode is magnetic agitation.
8. a kind of carbothermic method low temperature according to claim 1 prepares the method for ZrC-WC or ZrC-TaC mixed powder, it is characterized in that: in the step 3) in the heat treatment furnace heating schedule for be heated to 1200～1600 ° of C insulation 0.5～2h with the temperature rise rate of 10 ° of C/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310183378.5A CN103265031B (en) | 2013-05-17 | 2013-05-17 | A kind of method of carbothermic method low-temperature growth ZrC-WC or ZrC-TaC mixed powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310183378.5A CN103265031B (en) | 2013-05-17 | 2013-05-17 | A kind of method of carbothermic method low-temperature growth ZrC-WC or ZrC-TaC mixed powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103265031A true CN103265031A (en) | 2013-08-28 |
| CN103265031B CN103265031B (en) | 2015-10-21 |
Family
ID=49008711
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310183378.5A Active CN103265031B (en) | 2013-05-17 | 2013-05-17 | A kind of method of carbothermic method low-temperature growth ZrC-WC or ZrC-TaC mixed powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103265031B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104961465A (en) * | 2015-06-30 | 2015-10-07 | 中国人民解放军国防科学技术大学 | Ta-Hf-C ternary ceramic 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 |
| CN116443878A (en) * | 2023-04-12 | 2023-07-18 | 北京理工大学 | Method for synthesizing zirconium carbide aerogel by using inorganic zirconium salt and phenolic resin |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5942204A (en) * | 1997-03-31 | 1999-08-24 | Omg Americas, Inc. | Method to produce a transition metal carbide from a partially reduced transition metal compound |
| US6007598A (en) * | 1996-06-04 | 1999-12-28 | Omg Americas, Inc. | Metallic-carbide-group VIII metal powder and preparation methods thereof |
| US20060051281A1 (en) * | 2004-09-09 | 2006-03-09 | Bhabendra Pradhan | Metal carbides and process for producing same |
| CN1751990A (en) * | 2005-11-03 | 2006-03-29 | 武汉科技大学 | Preparation method of transition metal carbide material |
| CN101723367A (en) * | 2009-12-23 | 2010-06-09 | 北京科技大学 | Method for preparing powder of nanometer tantalum carbide |
| CN101830463A (en) * | 2010-05-31 | 2010-09-15 | 河南工业大学 | Method for preparing nano chromium carbide powder |
| CN102225764A (en) * | 2011-05-25 | 2011-10-26 | 山东理工大学 | Preparation method of tantalum carbide powder |
| CN102249231A (en) * | 2010-05-20 | 2011-11-23 | 燕山大学 | Process and method for preparing transitional metal carbide nanopowder at room temperature |
| CN102765720A (en) * | 2012-07-12 | 2012-11-07 | 上海大学 | Method for preparing nanocrystalline zirconium carbide powder |
| CN102910628A (en) * | 2011-08-05 | 2013-02-06 | 中国科学院上海硅酸盐研究所 | Synthetic method for high-melting-point transition metal carbide ultrafine powder |
-
2013
- 2013-05-17 CN CN201310183378.5A patent/CN103265031B/en active Active
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6007598A (en) * | 1996-06-04 | 1999-12-28 | Omg Americas, Inc. | Metallic-carbide-group VIII metal powder and preparation methods thereof |
| US5942204A (en) * | 1997-03-31 | 1999-08-24 | Omg Americas, Inc. | Method to produce a transition metal carbide from a partially reduced transition metal compound |
| US20060051281A1 (en) * | 2004-09-09 | 2006-03-09 | Bhabendra Pradhan | Metal carbides and process for producing same |
| CN1751990A (en) * | 2005-11-03 | 2006-03-29 | 武汉科技大学 | Preparation method of transition metal carbide material |
| CN101723367A (en) * | 2009-12-23 | 2010-06-09 | 北京科技大学 | Method for preparing powder of nanometer tantalum carbide |
| CN102249231A (en) * | 2010-05-20 | 2011-11-23 | 燕山大学 | Process and method for preparing transitional metal carbide nanopowder at room temperature |
| CN101830463A (en) * | 2010-05-31 | 2010-09-15 | 河南工业大学 | Method for preparing nano chromium carbide powder |
| CN102225764A (en) * | 2011-05-25 | 2011-10-26 | 山东理工大学 | Preparation method of tantalum carbide powder |
| CN102910628A (en) * | 2011-08-05 | 2013-02-06 | 中国科学院上海硅酸盐研究所 | Synthetic method for high-melting-point transition metal carbide ultrafine powder |
| CN102765720A (en) * | 2012-07-12 | 2012-11-07 | 上海大学 | Method for preparing nanocrystalline zirconium carbide powder |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104961465A (en) * | 2015-06-30 | 2015-10-07 | 中国人民解放军国防科学技术大学 | Ta-Hf-C ternary ceramic 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 |
| CN116443878A (en) * | 2023-04-12 | 2023-07-18 | 北京理工大学 | Method for synthesizing zirconium carbide aerogel by using inorganic zirconium salt and phenolic resin |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103265031B (en) | 2015-10-21 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103253670B (en) | Method for preparing TaC powder at low temperature by carbothermic method | |
| Cao et al. | Preparation and characterization of ultrafine ZrB2–SiC composite powders by a combined sol–gel and microwave boro/carbothermal reduction method | |
| CN103253669B (en) | Method for preparing HfC powder at low temperature by carbothermic method | |
| WO2017016079A1 (en) | Method for synthesizing high-purity ultrafine zrc-sic composite powder | |
| CN105218099B (en) | A kind of nonpolar zirconium carbide liquid phase ceramic forerunner and its preparation method and application | |
| El-Sheikh et al. | In situ synthesis of ZrC/SiC nanocomposite via carbothermic reduction of binary xerogel | |
| CN103754891A (en) | Method for preparing hafnium boride powder by using boron/carbothermic method | |
| Feng et al. | Nano-TaC powder synthesized using modified spark plasma sintering apparatus and its densification | |
| CN108794013B (en) | B4C ceramic block and rapid preparation method thereof | |
| CN108640663A (en) | A kind of graphene/carbon SiClx enhancing alumina matrix composite and preparation method thereof | |
| CN103265031B (en) | A kind of method of carbothermic method low-temperature growth ZrC-WC or ZrC-TaC mixed powder | |
| CN104016681B (en) | The method for preparing solid phase of a kind of boride and multiphase ceramic powder thereof | |
| CN106116586A (en) | A kind of molybdenum alloy MoSi2zrO2y2o3coating and its preparation method and application | |
| Hu et al. | Sintering mechanism and microstructure of TaC/SiC composites consolidated by plasma-activated sintering | |
| CN109369186A (en) | A kind of low temperature preparation method of titanium aluminum carbide | |
| He et al. | Self-healing performance of niobium suboxide-based solid solution for UHTC coating during oxyacetylene test | |
| CN106631009B (en) | A kind of composite powder and preparation method thereof for boronation zirconium based composite material | |
| CN102910628A (en) | Synthetic method for high-melting-point transition metal carbide ultrafine powder | |
| CN106800414B (en) | The method that reaction in-situ prepares the ultra-temperature ceramic-based composite material of nitrogen boron | |
| Yang et al. | Thermodynamics aided design of hBN-capsulated diboride powders from novel nitrate precursors for high entropy ceramics | |
| Tiwari et al. | Influence of SiC content to control morphology of in-situ synthesized ZrB2–SiC composite through single-step reduction process | |
| CN101186503A (en) | Zirconium boride-zirconium carbide composite diphase material and use thereof | |
| Liu et al. | A novel liquid hybrid precursor method via sol-gel for the preparation of ZrB2 films | |
| CN105483487A (en) | Zirconium-containing boron carbide and aluminum alloy composite and preparing method thereof | |
| Miao et al. | A novel in situ synthesis of SiBCN-Zr composites prepared by a sol–gel process and spark plasma sintering |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |