CN103265031B - A kind of method of carbothermic method low-temperature growth ZrC-WC or ZrC-TaC mixed powder - Google Patents
A kind of method of carbothermic method low-temperature growth ZrC-WC or ZrC-TaC mixed powder Download PDFInfo
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Abstract
The present invention relates to a kind of method of carbothermic method low-temperature growth ZrC-WC or ZrC-TaC mixed powder, belong to structural ceramics technical field.The method is using sucrose, resol, epoxy resin or pitch as carbon source, and using 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.Sucrose, resol, epoxy resin or pitch and mixed oxide is adopted to be raw material in the present invention, raw materials cost is low, and sucrose, resol, epoxy resin or pitch and oxide compound be mixed into wet mixing, mix, not easily reunite, building-up process is carried out under high-purity argon gas environment or in vacuum, and reduction reaction synthesis ZrC-WC (ZrC-TaC) powder can occur at a lower temperature.
Description
Technical field
The present invention relates to a kind of method of carbothermic method low-temperature growth ZrC-WC or ZrC-TaC mixed powder, belong to structural ceramics technical field.
Background technology
Superhigh temperature ceramics (Ultra-high Temperature Ceramics, UHTCs) refer to that (such as Sauerstoffatom) has carbide and the boride material of the transition metal of excellent high-temperature oxidation resistant, Burning corrosion resistance and heat-shock resistance in 1800 ° of more than C and reaction atmosphere, mainly comprises TaC, HfC, ZrC, HfB
2, ZrB
2high-temperature behavior Deng, its excellence makes that they can adapt to superelevation sonic flight, atmospheric layer reenters, the extreme environment such as Trans-atmospheric flight and rocket propulsion system, can be used for various key position or the 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 unique ability 3500 ° of more than C high temperature in addition to carbon.Wherein, the high specific strength of ZrC, high ratio modulus and low preparation cost become one of hyperthermal material of most application potential.
But hard-to-sinter and weak oxide are the subject matter limiting its application.Because ZrC is covalent bonds, its diffusivity is low, needs High Temperature High Pressure ability densified sintering product.For ZrC material hard-to-sinter, the especially problem of low-temperature sintering difficulty, it is crucial for preparing high pure and ultra-fine ZrC powder, can obviously improve its coking property.On the other hand, the ZrC zirconia layer that easily oxidation generation is loose in high-temperature oxidation environment, is difficult to effectively hinder oxygen to spread to material internal.In order to improve its oxidation-resistance, researchist adds containing high-valence cationic (as W to containing in the compound of Zr
5+, Ta
5+and Nb
5+deng) compound, as WC, TaC and NbC etc.This kind of material, in oxidising process, generates the protective layer with passive oxidation, oxygen can be hindered to spread to material internal, effectively improve its oxidation-resistance.And add the high price cation compounds such as WC in material, its high-temperature bending strength can improve about 1 times, so ZrC-WC complex phase ceramic can improve its oxidation-resistance can improve again its high-temperature bending strength, greatly enhances the range of application of ZrC material.Therefore, active demand is proposed to synthesizing high pure superfine ZrC-WC composite granule.
At present, synthesize ZrC raw powder's production technology to mainly contain: direct synthesis technique, carbothermic method, sol-gel method, mechanical alloying method, Self-propagating Sintering Synthetic method etc.Wherein, the technique that can realize suitability for industrialized production is carbothermic method, and the method for synthesis ZrC powder adopts 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 synthesis WC and TaC powder reduces 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)
Known according to calculation of thermodynamics (as Fig. 1 and Fig. 2), high-purity argon gas condition is the prerequisite of low temperature synthesizing high pure superfine powder.Sucrose is adopted to make carbon source, the problem that solid mixing is uneven can be solved, realize the method that liquid-solid wet mixing is closed, oxide powder surface uniform is made to apply one deck sucrose (forming one deck C film after cracking), be conducive to the reaction of carbothermic reduction, the powder of synthesis has the advantages that purity is high and particle diameter is little.
Summary of the invention
The object of the invention is a kind of method in order to carbothermic method low-temperature growth ZrC-WC or ZrC-TaC mixed powder, the method technique be simple, temperature is low, consuming time short, high pure and ultra-fine ZrC-WC (TaC) powder can be obtained.
The object of the invention is to be achieved through the following technical solutions.
The method of a kind of carbothermic method low-temperature growth ZrC-WC of the present invention or ZrC-TaC mixed powder, the method is using sucrose, resol, epoxy resin or pitch as carbon source, using 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, in carbon source, the molar weight of carbon is 3 ~ 20:1 with the ratio of the integral molar quantity of mixed oxide, 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 added is 1% ~ 5% of mixed oxide total mass, then zirconia ball grinding media is added, ball milling mixing 10-48h, being moved to by oxide compound after mixing is equipped with in the vessel of solvent orange 2 A, and ultrasonic disperse, obtains mixing solutions;
2) carbon source is dissolved in solvent B, obtains carbon source solution, then the carbon source solution obtained is poured in the mixing solutions obtained in step 1); Then heat, stir, obtain the reactant mixed;
3) by step 2) reactant that obtains loads in plumbago crucible; plumbago crucible is put into flowing argon shield or vacuum heat treatment furnace heat; then room temperature is cooled to the furnace; obtain ZrC-WC (or ZrC-TaC) powder through grinding again, the particle diameter of the powder obtained is 50 ~ 200nm.
Above-mentioned steps 1) in the total concn of mixing solutions that obtains be 1 ~ 5mol/L, the ultrasonic disperse time is 0.5 ~ 2h; Zirconic purity >=99.9wt.%, particle diameter is 50 ~ 120nm; Purity >=the 99.9wt.% of Tungsten oxide 99.999, particle diameter is 50 ~ 120nm; Purity >=the 99.9wt.% of tantalum pentoxide, particle diameter is 50 ~ 120nm.
Above-mentioned steps 2) in the concentration of carbon source solution be 3 ~ 15mol/L, when carbon source is sucrose, solvent B is water, and when carbon source is resol, epoxy resin or pitch, solvent B is ethanol, normal hexane or hexanaphthene; Carbon source is analytical pure; Heating temperature 100 ~ 250 DEG C, heat-up time 0.5 ~ 2h; Alr mode is magnetic agitation;
Above-mentioned steps 3) in heat treatment furnace heating schedule be heated to 1200 ~ 1600 ° of C with the temperature rise rate of 10 ° of C/min to be incubated 0.5 ~ 2h.
In the present invention, mechanical milling process adopts mixed oxide powder and sucrose (or resol, epoxy resin, pitch etc.) solution to carry out wet mixing, mixes, and solves two kinds of solid phase powder mixing uneven, the problem of the not high easy reunion of purity; Adopt high-purity argon gas or vacuum in preparation process, reduction reaction can occur at a lower temperature and prepare ultra-fine ZrC-WC (ZrC-TaC) powder.
Beneficial effect
Sucrose, resol, epoxy resin or pitch and mixed oxide is adopted to be raw material in the present invention, raw materials cost is low, and sucrose, resol, epoxy resin or pitch and oxide compound be mixed into wet mixing, mix, not easily reunite, building-up process is carried out under high-purity argon gas environment or in vacuum, and reduction reaction synthesis ZrC-WC (ZrC-TaC) powder can occur at a lower temperature, and namely the method technique is simple, temperature is low, consuming time short.The present invention adopts organism to be evenly coated on around mixed oxide particle, reaches mixed uniformly object, prepares high-purity ZrC-WC (ZrC-TaC) mixed powder.
Accompanying drawing explanation
Fig. 1 is the relation of standard atmosphere pressure Gibbs free energy and temperature;
Fig. 2 is the relation of Gibbs free energy under high-purity Ar and 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 ZrC-WC powder prepared by embodiment;
Fig. 5 is the stereoscan photograph of ZrC-TaC powder prepared by embodiment.
Embodiment
Below in conjunction with embodiment, the present invention will be further described.
Embodiment 1
Using sucrose as carbon source, using zirconium white and Tungsten oxide 99.999 as refractory metal source;
1) 246.4g ZrO is taken
2powder, 23.2gWO
3powder, its purity is 99.9wt.%, and particle diameter is 80nm, puts into ball grinder together, adds 100ml dehydrated alcohol, zirconia ball ball milling mixing 24h, moves in the vessel that 100ml dehydrated alcohol is housed, ultrasonic disperse 0.5h by the oxide compound after mixing;
2) taking 365.1g sucrose joins in 100ml water, stirs and makes it mix, and then join in the solution that step 1) obtains, heating is magnetic agitation simultaneously, and Heating temperature is 120 DEG C, and heat-up time is 2h, obtains the reactant mixed;
3) by step 2) reactant that obtains loads in plumbago crucible, then heat treatment furnace plumbago crucible being put into high-purity argon gas protection heats, heating schedule is for being warming up to 1600 DEG C of insulation 1h with the temperature rise rate of 10 DEG C/min, then cool to room temperature with the furnace, then obtain mixed powder material through grinding; As shown in Figure 3, as shown in Figure 4, sweep voltage is 15kv to its stereoscan photograph to the X-ray diffractogram of the powder body material obtained.As shown in Figure 3, the powder body material obtained is ZrC-5mol%WC mixed powder; As shown in Figure 4, the median size of ZrC-5mol%WC powder is 100nm.
Embodiment 2
Using sucrose as carbon source, using zirconium white and Tungsten oxide 99.999 as refractory metal source;
1) 246.4g ZrO is taken
2powder, 46.4gWO
3powder, its purity is 99.9wt.%, and particle diameter is 70nm, puts into ball grinder together, adds 100ml dehydrated alcohol, zirconia ball ball milling mixing 24h, moves in the vessel that 100ml dehydrated alcohol is housed, ultrasonic disperse 1h by the oxide compound after mixing;
2) taking 388g sucrose joins in 100ml water, stirs and makes it mix, and then join in the solution that step 1) obtains, heating is magnetic agitation simultaneously, and Heating temperature is 140 DEG C, and heat-up time is 2h, obtains the reactant mixed;
3) by step 2) reactant that obtains loads in plumbago crucible, then heat treatment furnace plumbago crucible being put into high-purity argon gas protection heats, heating schedule is for being warming up to 1600 DEG C of insulation 1h with the temperature rise rate of 10 DEG C/min, then cool to room temperature with the furnace, then obtain mixed powder material through grinding; As shown in Figure 3, as shown in Figure 3, the powder body material obtained is ZrC-10mol%WC mixed powder to the X-ray diffractogram of the powder body material obtained.
Embodiment 3
Using sucrose as carbon source, using zirconium white and tantalum pentoxide as refractory metal source;
1) 246.4g ZrO is taken
2powder, 44.2gTa
2o
5powder, its purity is 99.9wt.%, and particle diameter is 60nm, puts into ball grinder together, adds 120ml dehydrated alcohol, zirconia ball ball milling mixing 12h, moves in the vessel that 100ml dehydrated alcohol is housed, ultrasonic disperse 2h by the oxide compound after mixing;
2) taking 382.2g sucrose joins in 110ml water, stirs and makes it mix, and then join in the solution that step 1) obtains, heating is magnetic agitation simultaneously, and Heating temperature is 160 DEG C, and heat-up time is 1h, obtains the reactant mixed;
3) by step 2) reactant that obtains loads in plumbago crucible, then heat treatment furnace plumbago crucible being put into high-purity argon gas protection heats, heating schedule is for being warming up to 1500 DEG C of insulation 2h with the temperature rise rate of 10 DEG C/min, then cool to room temperature with the furnace, then obtain mixed powder material through grinding; As shown in Figure 3, as shown in Figure 5, sweep voltage is 15kv to its stereoscan photograph to the X-ray diffractogram of the powder body material obtained.As shown in Figure 3, the powder body material obtained is ZrC-10mol%TaC mixed powder; As shown in Figure 5, the median size of ZrC-10mol%TaC powder is 100nm.
Embodiment 4
Using sucrose as carbon source, using zirconium white and tantalum pentoxide as refractory metal source;
1) 246.4g ZrO is taken
2powder, 88.4gTa
2o
5powder, its purity is 99.9wt.%, and particle diameter is 90nm, puts into ball grinder together, adds 120ml dehydrated alcohol, zirconia ball ball milling mixing 24h, moves in the vessel that 150ml dehydrated alcohol is housed, ultrasonic disperse 1.5h by the oxide compound after mixing;
2) taking 422.2g sucrose joins in 120ml water, stirs and makes it mix, and then join in the solution that step 1) obtains, heating is magnetic agitation simultaneously, and Heating temperature is 130 DEG C, and heat-up time is 2h, obtains the reactant mixed;
3) by step 2) reactant that obtains loads in plumbago crucible, then heat treatment furnace plumbago crucible being put into high-purity argon gas protection heats, heating schedule is for being warming up to 1600 DEG C of insulation 1h with the temperature rise rate of 10 DEG C/min, then cool to room temperature with the furnace, then obtain mixed powder material through grinding; As shown in Figure 3, as shown in Figure 3, the powder body material obtained is ZrC-20mol%TaC mixed powder to the X-ray diffractogram of the powder body material obtained.
Embodiment 5
Using resol as carbon source, using zirconium white and Tungsten oxide 99.999 as refractory metal source;
1) 246.4g ZrO is taken
2powder, 23.2gWO
3powder, its purity is 99.9wt.%, and particle diameter is 60nm, puts into ball grinder together, adds 110ml dehydrated alcohol, zirconia ball ball milling mixing 24h, moves in the vessel that 110ml dehydrated alcohol is housed, ultrasonic disperse 1h by the oxide compound after mixing;
2) taking 342g resol joins in 150ml dehydrated alcohol, stirs and makes it mix, and then join in the solution that step 1) obtains, heating is magnetic agitation simultaneously, and Heating temperature is 150 DEG C, and heat-up time is 1.5h, obtains the reactant mixed;
3) by step 2) reactant that obtains loads in plumbago crucible; then heat treatment furnace plumbago crucible being put into high-purity argon gas protection heats; heating schedule is for being warming up to 1400 DEG C of insulation 2h with the temperature rise rate of 10 DEG C/min; then cool to room temperature with the furnace, then obtain ZrC-5mol%WC mixed powder through grinding.
Embodiment 6
Using resol as carbon source, using zirconium white and tantalum pentoxide as refractory metal source;
1) 246.4g ZrO is taken
2powder, 88.4gTa
2o
5powder, its purity is 99.9wt.%, and particle diameter is 80nm, puts into ball grinder together, adds 130ml dehydrated alcohol, zirconia ball ball milling mixing 48h, moves in the vessel that 150ml dehydrated alcohol is housed, ultrasonic disperse 1.5h by the oxide compound after mixing;
2) taking 395.4g resol joins in 130ml normal hexane, stirs and makes it mix, and then join in the solution that step 1) obtains, heating is magnetic agitation simultaneously, and Heating temperature is 120 DEG C, and heat-up time is 2.5h, obtains the reactant mixed;
3) by step 2) reactant that obtains loads in plumbago crucible; then heat treatment furnace plumbago crucible being put into high-purity argon gas protection heats; heating schedule is for being warming up to 1300 DEG C of insulation 2h with the temperature rise rate of 10 DEG C/min; then cool to room temperature with the furnace, then obtain ZrC-20mol%TaC mixed powder through grinding.
Embodiment 7
Using epoxy resin as carbon source, using zirconium white and Tungsten oxide 99.999 as refractory metal source;
1) 246.4g ZrO is taken
2powder, 46.4gWO
3powder, its purity is 99.9wt.%, and particle diameter is 90nm, puts into ball grinder together, adds 130ml dehydrated alcohol, zirconia ball ball milling mixing 24h, moves in the vessel that 150ml dehydrated alcohol is housed, ultrasonic disperse 1h by the oxide compound after mixing;
2) taking 396.9g epoxy resin joins in 130ml hexanaphthene, stirs and makes it mix, and then join in the solution that step 1) obtains, heating is magnetic agitation simultaneously, and Heating temperature is 140 DEG C, and heat-up time is 2h, obtains the reactant mixed;
3) by step 2) reactant that obtains loads in plumbago crucible; then heat treatment furnace plumbago crucible being put into high-purity argon gas protection heats; heating schedule is for being warming up to 1700 DEG C of insulation 1h with the temperature rise rate of 10 DEG C/min; then cool to room temperature with the furnace, then obtain ZrC-10mol%WC mixed powder through grinding.
Embodiment 8
Using pitch as carbon source, using zirconium white and tantalum pentoxide as refractory metal source;
1) 246.4g ZrO is taken
2powder, 44.2gTa
2o
5powder, its purity is 99.9wt.%, and particle diameter is 70nm, puts into ball grinder together, adds 140ml dehydrated alcohol, zirconia ball ball milling mixing 12h, moves in the vessel that 100ml dehydrated alcohol is housed, ultrasonic disperse 2h by the oxide compound after mixing;
2) taking 380g pitch joins in 210ml dehydrated alcohol, stirs and makes it mix, and then join in the solution that step 1) obtains, heating is magnetic agitation simultaneously, and Heating temperature is 150 DEG C, and heat-up time is 0.5h, obtains the reactant mixed;
3) by step 2) reactant that obtains loads in plumbago crucible; then heat treatment furnace plumbago crucible being put into high-purity argon gas protection heats; heating schedule is for being warming up to 1400 DEG C of insulation 2h with the temperature rise rate of 10 DEG C/min; then cool to room temperature with the furnace, then obtain ZrC-10mol%TaC mixed powder through grinding.
Claims (2)
1. a method for carbothermic method low-temperature growth ZrC-WC mixed powder, is characterized in that steps of the method are:
Using sucrose as carbon source, using zirconium white and tungstic oxide as refractory metal source;
1) 246.4g ZrO is taken
2powder, 23.2g WO
3powder, its purity is 99.9wt.%, and particle diameter is 80nm, puts into ball grinder together, adds 100ml dehydrated alcohol, zirconia ball ball milling mixing 24h, moves in the vessel that 100ml dehydrated alcohol is housed, ultrasonic disperse 0.5h by the oxide compound after mixing;
2) taking 365.1g sucrose joins in 100ml water, stirs and makes it mix, then join step 1) in the solution that obtains, heating is magnetic agitation simultaneously, and Heating temperature is 120 DEG C, and heat-up time is 2h, obtains the reactant mixed;
3) by step 2) reactant that obtains loads in plumbago crucible; then heat treatment furnace plumbago crucible being put into high-purity argon gas protection heats; heating schedule is for being warming up to 1600 DEG C of insulation 1h with the temperature rise rate of 10 DEG C/min; then cool to room temperature with the furnace, then obtain mixed powder material through grinding.
2. a method for carbothermic method low-temperature growth ZrC-TaC mixed powder, is characterized in that step is:
Using sucrose as carbon source, using zirconium white and tantalum pentoxide as refractory metal source;
1) 246.4g ZrO is taken
2powder, 44.2g Ta
2o
5powder, its purity is 99.9wt.%, and particle diameter is 60nm, puts into ball grinder together, adds 120ml dehydrated alcohol, zirconia ball ball milling mixing 12h, moves in the vessel that 100ml dehydrated alcohol is housed, ultrasonic disperse 2h by the oxide compound after mixing;
2) taking 382.2g sucrose joins in 110ml water, stirs and makes it mix, then join step 1) in the solution that obtains, heating is magnetic agitation simultaneously, and Heating temperature is 160 DEG C, and heat-up time is 1h, obtains the reactant mixed;
3) by step 2) reactant that obtains loads in plumbago crucible; then heat treatment furnace plumbago crucible being put into high-purity argon gas protection heats; heating schedule is for being warming up to 1500 DEG C of insulation 2h with the temperature rise rate of 10 DEG C/min; then cool to room temperature with the furnace, then obtain mixed powder material through grinding.
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| 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 |
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