CN103482626B - Zirconium carbide-silicon carbide composite powder and preparation method thereof - Google Patents
Zirconium carbide-silicon carbide composite powder and preparation method thereof Download PDFInfo
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Abstract
The invention relates to zirconium carbide-silicon carbide composite powder and a preparation method of the zirconium carbide-silicon carbide composite powder. According to the technical scheme, 80-91wt% of halide powder, 4-12wt% of zircon powder, 0.5-2.5wt% of powdered carbon and 2-10wt% of magnesium powder are mixed and placed in an electric furnace, and the temperature of the mixture is raised to 1000-1250 DEG C at the velocity of 2-8 DEG C/min in an argon atmosphere and then is kept for 2-6 hours; the product washed with distilled water is placed into 2.0-4.0mol/L hydrochloric acid to be soaked for 3-8 hours and then filtered, the filtered product is washed with distilled water till no precipitate is generated in the cleaning solution when being detected with silver nitrate, the product is dried for 11-24 hours at 45-55 DEG C, and the zirconium carbide-silicon carbide composite powder is obtained. The preparation method of the zirconium carbide-silicon carbide composite powder has the advantages of being low in reaction temperature, low in cost, simple in synthetic process, high in output and broad in industrial production prospects and the process is easy to control. The prepared zirconium diboride ultrafine powder is good in crystal, small in powder particle size, uniform in distribution, free of impurity phase, high in activity, small in particle aggregation and high in purity.
Description
Technical field
The invention belongs to refractory materials powder technology field.Be specifically related to a kind of Zirconium carbide-silicon carbide composite powder and preparation method thereof.
Background technology
ZrC and SiC has fusing point high (3530 DEG C), intensity is high, hardness is high, Young's modulus high (E=355GPa), heat conduction and conductivity excellence feature.Therefore, ZrC-SiC matrix material is the critical material preparing the high-technology fields such as high-performance carbide, aerospace, nuclear power, weaving, electronics, coating and metallurgical automation, is expected to be widely used in above-mentioned industry.
At present, the preparation method of Zirconium carbide powder has direct synthesis technique, mechanical alloying method, carbothermic method, sol-gel method, self-propagating high-temperature synthesis etc.; The preparation method of silicon carbide powder has carbothermic method, mechanical crushing method, sol-gel method, organic polymer thermal decomposition method, self-propagating high-temperature synthesis etc.
The preparation method of ZrC-SiC composite granule has liquid phase presoma conversion method.The method for presoma, with liquid hyperbranched polycarbosilanes for silicon source and carbon source, has prepared ZrC-SiC composite granule by Pintsch process reaction with the polymkeric substance of organic zirconium.Though this technique cycle is shorter, its shortcoming is with high costs and complex process.
Summary of the invention
The present invention is intended to the deficiency overcoming prior art existence, and object is to provide the preparation method of the Zirconium carbide-silicon carbide composite powder that a kind of temperature of reaction is low, cost is low, synthesis technique is simple, process is easy to control, productive rate is high and industrialization prospect of production is large.The Zirconium carbide-silicon carbide composite powder advantages of good crystallization prepared by the method, diameter of particle are evenly distributed, activity is high, without dephasign, particle agglomeration is little and purity is high.
For achieving the above object, technical scheme of the present invention is: first mixed by the magnesium powder of the zircon powder of the halogenide powder of 80 ~ 91wt%, 4 ~ 12wt%, the powdered carbon of 0.5 ~ 2.5wt% and 2 ~ 10wt%, obtained mixture; Mixture is placed in electric furnace, rises to 1000 ~ 1250 DEG C with the temperature rise rate of 2 ~ 8 DEG C/min under an argon atmosphere, be incubated 2 ~ 6 hours; Again by products therefrom distilled water wash, product after washing put into concentration be 2.0 ~ 4.0mol/L hydrochloric acid soak 3 ~ 8 hours, filter, product after filtering by washed with de-ionized water, cleaning detects with Silver Nitrate and produces without precipitation to scavenging solution, under 45 ~ 55 DEG C of conditions, drying 11 ~ 24 hours, obtains Zirconium carbide-silicon carbide composite powder.
ZrSiO in described zircon powder
4content>=99wt%, particle diameter≤38 μm.
C content >=99wt% in described carbon dust, particle diameter≤200 μm.
Mg content >=99wt% in described metal magnesium powder, particle diameter≤150 μm.
Described halogenide powder is the mixture of magnesium chloride or magnesium chloride and Sodium Fluoride; Magnesium chloride and Sodium Fluoride are technical pure or analytical pure, particle diameter all≤200 μm.
Purity >=99.8% of described Silver Nitrate.
Owing to adopting technique scheme, the present invention compared with prior art has following positively effect and outstanding feature:
1, the mixing of the present invention's realization response thing atomic scale in melting salt, reacted constituent mobility is in the liquid phase strengthened, and rate of diffusion significantly improves, and effectively can control reaction process, reduce temperature of reaction and Reaction time shorten, improve the service efficiency of reactant, and then improve productive rate;
2, the present invention more easily can control the shape and size of crystal grain by molten-salt growth method, and powder granularity is 3 ~ 10 μm.The each component proportion of synthetic product is accurate, advantages of good crystallization, uniform composition, segregation-free;
3, the present invention is in reaction process and cleaning process subsequently, does not need to use special instrument and supplies, and whole technological process is simple; Adopt pickling to combine the method for washing, be conducive to the removing of impurity, form high-purity reactant, without dephasign;
4, raw material sources of the present invention are extensive and cheap, and production cost is low, have very large industrialization prospect of production;
5, the even particulate dispersion of product prepared of the present invention is in melting salt, avoids and is interconnected, make seed activity high, very well dispersed, significantly reduces the generation of dissolving agglomeration after washing.
Therefore, the present invention has the advantages that temperature of reaction is low, cost is low, synthesis technique is simple, process is easy to control, productive rate is high and industrialization prospect of production is large; Prepared Zirconium boride ultrafine powder advantages of good crystallization, powder granularity is little and be evenly distributed, without dephasign, activity is high, particle agglomeration is little and purity is high.
Embodiment
With embodiment, the present invention will be further described below, the restriction not to its protection domain.
For avoiding repetition, first by as follows for the raw material Unify legislation involved by this embodiment, repeat no more in embodiment:
ZrSiO in described zircon powder
4content>=99wt%, particle diameter≤38 μm.
C content >=99wt% in described carbon dust, particle diameter≤200 μm.
Mg content >=99wt% in described metal magnesium powder, particle diameter≤150 μm.
Described magnesium chloride and Sodium Fluoride are technical pure or analytical pure, particle diameter all≤200 μm.
Purity >=99.8% of described Silver Nitrate.
Embodiment 1
A kind of Zirconium carbide-silicon carbide composite powder and preparation method thereof.The magnesium powder of the zircon powder of the magnesium chloride powder of 80 ~ 85wt%, 8 ~ 12wt%, the powdered carbon of 1.5 ~ 2.5wt% and 5 ~ 10wt% is mixed, obtained mixture; Mixture is placed in electric furnace, rises to 1100 ~ 1200 DEG C with the temperature rise rate of 2 ~ 4 DEG C/min under an argon atmosphere, be incubated 2 ~ 4 hours; Again by products therefrom distilled water wash, product after washing put into concentration be 2.0 ~ 2.5mol/L hydrochloric acid soak 3 ~ 5 hours, filter, product after filtering by washed with de-ionized water, cleaning detects with Silver Nitrate and produces without precipitation to scavenging solution, under 50 DEG C of conditions, drying 11 ~ 24 hours, obtains Zirconium carbide-silicon carbide composite powder.
Zirconium carbide-silicon carbide composite powder purity prepared by the present embodiment is high, particle soilless sticking, and granularity is 6 ~ 9 μm.
Embodiment 2
A kind of Zirconium carbide-silicon carbide composite powder and preparation method thereof.The magnesium powder of the zircon powder of the halogenide powder of 80 ~ 85wt%, 8 ~ 12wt%, the powdered carbon of 1.5 ~ 2.5wt% and 5 ~ 10wt% is mixed, obtained mixture; Mixture is placed in electric furnace, rises to 1000 ~ 1100 DEG C with the temperature rise rate of 2 ~ 4 DEG C/min under an argon atmosphere, be incubated 3 ~ 5 hours; Again by products therefrom distilled water wash, product after washing put into concentration be 3.0 ~ 3.5mol/L hydrochloric acid soak 4 ~ 6 hours, filter, product after filtering by washed with de-ionized water, cleaning detects with Silver Nitrate and produces without precipitation to scavenging solution, under 50 DEG C of conditions, drying 11 ~ 24 hours, obtains Zirconium carbide-silicon carbide composite powder.
In the present embodiment, halogenide is the mixture of 50 ~ 70wt% magnesium chloride and 30 ~ 50wt% Sodium Fluoride; Zirconium carbide-silicon carbide composite powder purity prepared by the present embodiment is high, particle soilless sticking, and granularity is 4 ~ 8 μm.
Embodiment 3
A kind of Zirconium carbide-silicon carbide composite powder and preparation method thereof.The magnesium powder of the zircon powder of the magnesium chloride powder of 83 ~ 88wt%, 6 ~ 10wt%, the powdered carbon of 1.2 ~ 2.0wt% and 2 ~ 5wt% is mixed, obtained mixture; Mixture is placed in electric furnace, rises to 1000 ~ 1150 DEG C with the temperature rise rate of 3 ~ 5 DEG C/min under an argon atmosphere, be incubated 3 ~ 5 hours; Again by products therefrom distilled water wash, product after washing put into concentration be 3.5 ~ 4.0mol/L hydrochloric acid soak 5 ~ 7 hours, filter, product after filtering by washed with de-ionized water, cleaning detects with Silver Nitrate and produces without precipitation to scavenging solution, under 50 DEG C of conditions, drying 11 ~ 24 hours, obtains Zirconium carbide-silicon carbide composite powder.
Zirconium carbide-silicon carbide composite powder purity prepared by the present embodiment is high, particle soilless sticking, and granularity is 3 ~ 6 μm.
Embodiment 4
A kind of Zirconium carbide-silicon carbide composite powder and preparation method thereof.The magnesium powder of the zircon powder of the halogenide powder of 83 ~ 88wt%, 6 ~ 10wt%, the powdered carbon of 1.2 ~ 2.0wt% and 2 ~ 5wt% is mixed, obtained mixture; Mixture is placed in electric furnace, rises to 1050 ~ 1250 DEG C with the temperature rise rate of 3 ~ 5 DEG C/min under an argon atmosphere, be incubated 5 ~ 6 hours; Again by products therefrom distilled water wash, product after washing put into concentration be 2.0 ~ 2.5mol/L hydrochloric acid soak 3 ~ 5 hours, filter, product after filtering by washed with de-ionized water, cleaning detects with Silver Nitrate and produces without precipitation to scavenging solution, under 50 DEG C of conditions, drying 11 ~ 24 hours, obtains Zirconium carbide-silicon carbide composite powder.
In the present embodiment, halogenide is the mixture of 60 ~ 85wt% magnesium chloride and 15 ~ 40wt% Sodium Fluoride; Zirconium carbide-silicon carbide composite powder purity prepared by the present embodiment is high, particle soilless sticking, and granularity is 3 ~ 7 μm.
Embodiment 5
A kind of Zirconium carbide-silicon carbide composite powder and preparation method thereof.The magnesium powder of the zircon powder of the magnesium chloride powder of 85 ~ 91wt%, 4 ~ 8wt%, the powdered carbon of 0.5 ~ 1.5wt% and 4 ~ 8wt% is mixed, obtained mixture; Mixture is placed in electric furnace, rises to 1000 ~ 1100 DEG C with the temperature rise rate of 5 ~ 8 DEG C/min under an argon atmosphere, be incubated 5 ~ 6 hours; Again by products therefrom distilled water wash, product after washing put into concentration be 2.0 ~ 2.5mol/L hydrochloric acid soak 6 ~ 8 hours, filter, product after filtering by washed with de-ionized water, cleaning detects with Silver Nitrate and produces without precipitation to scavenging solution, under 50 DEG C of conditions, drying 11 ~ 24 hours, obtains Zirconium carbide-silicon carbide composite powder.
Zirconium carbide-silicon carbide composite powder prepared by the present embodiment, purity is high, particle soilless sticking, and granularity is 5 ~ 9 μm.
Embodiment 6
A kind of Zirconium carbide-silicon carbide composite powder and preparation method thereof.The magnesium powder of the zircon powder of the halogenide powder of 85 ~ 91wt%, 4 ~ 8wt%, the powdered carbon of 0.5 ~ 1.5wt% and 4 ~ 8wt% is mixed, obtained mixture; Mixture is placed in electric furnace, rises to 1100 ~ 1250 DEG C with the temperature rise rate of 2 ~ 4 DEG C/min under an argon atmosphere, be incubated 2 ~ 4 hours; Again by products therefrom distilled water wash, product after washing put into concentration be 2.5 ~ 3.0mol/L hydrochloric acid soak 4 ~ 6 hours, filter, product after filtering by washed with de-ionized water, cleaning detects with Silver Nitrate and produces without precipitation to scavenging solution, under 50 DEG C of conditions, drying 11 ~ 24 hours, obtains Zirconium carbide-silicon carbide composite powder.
In the present embodiment, halogenide is the mixture of 50 ~ 60wt% magnesium chloride and 40 ~ 50wt% Sodium Fluoride; Zirconium boride powder prepared by the present embodiment, purity is high, particle soilless sticking, and granularity is 6 ~ 10 μm.
This embodiment compared with prior art has following positively effect and outstanding feature:
1, the mixing of this embodiment realization response thing atomic scale in melting salt, reacted constituent mobility is in the liquid phase strengthened, rate of diffusion significantly improves, effectively can control reaction process, reduce temperature of reaction and Reaction time shorten, improve the service efficiency of reactant, and then improve productive rate;
2, this embodiment more easily can control the shape and size of crystal grain by molten-salt growth method, and powder granularity is 3 ~ 10 μm.The each component proportion of synthetic product is accurate, advantages of good crystallization, uniform composition, segregation-free;
3, this embodiment is in reaction process and cleaning process subsequently, does not need to use special instrument and supplies, and whole technological process is simple; Adopt pickling to combine the method for washing, be conducive to the removing of impurity, form high-purity reactant, without dephasign;
4, the raw material sources of this embodiment are extensive and cheap, and production cost is low, have very large industrialization prospect of production;
5, the even particulate dispersion of product prepared of this embodiment is in melting salt, avoids and is interconnected, make seed activity high, very well dispersed, significantly reduces the generation of dissolving agglomeration after washing.
Therefore, this embodiment has the advantages that temperature of reaction is low, cost is low, synthesis technique is simple, process is easy to control, productive rate is high and industrialization prospect of production is large; Prepared Zirconium boride ultrafine powder advantages of good crystallization, powder granularity is little and be evenly distributed, without dephasign, activity is high, particle agglomeration is little and purity is high.
Claims (7)
1. a preparation method for Zirconium carbide-silicon carbide composite powder, is characterized in that first being mixed by the magnesium powder of the zircon powder of the halogenide powder of 80 ~ 91wt%, 4 ~ 12wt%, the powdered carbon of 0.5 ~ 2.5wt% and 2 ~ 10wt%, obtained mixture; Mixture is placed in electric furnace, rises to 1000 ~ 1250 DEG C with the temperature rise rate of 2 ~ 8 DEG C/min under an argon atmosphere, be incubated 2 ~ 6 hours; Again by products therefrom distilled water wash, product after washing put into concentration be 2.0 ~ 4.0mol/L hydrochloric acid soak 3 ~ 8 hours, filter, product after filtering by washed with de-ionized water, cleaning detects with Silver Nitrate and produces without precipitation to scavenging solution, under 45 ~ 55 DEG C of conditions, drying 11 ~ 24 hours, obtains Zirconium carbide-silicon carbide composite powder.
2., according to the preparation method of claim 1 Zirconium carbide-silicon carbide composite powder, it is characterized in that the ZrSiO in described zircon powder
4content>=99wt%, particle diameter≤38 μm.
3., according to the preparation method of claim 1 Zirconium carbide-silicon carbide composite powder, it is characterized in that the C content >=99wt% in described carbon dust, particle diameter≤200 μm.
4., according to the preparation method of claim 1 Zirconium carbide-silicon carbide composite powder, it is characterized in that the Mg content >=99wt% in described metal magnesium powder, particle diameter≤150 μm.
5., according to the preparation method of claim 1 Zirconium carbide-silicon carbide composite powder, it is characterized in that described halogenide powder is the mixture of magnesium chloride or magnesium chloride and Sodium Fluoride; Magnesium chloride and Sodium Fluoride are technical pure or analytical pure, particle diameter all≤200 μm.
6., according to the preparation method of claim 1 Zirconium carbide-silicon carbide composite powder, it is characterized in that purity >=99.8% of described Silver Nitrate.
7. a Zirconium carbide-silicon carbide composite powder, is characterized in that described Zirconium carbide-silicon carbide composite powder is the Zirconium carbide-silicon carbide composite powder prepared by the preparation method of Zirconium carbide-silicon carbide composite powder according to any one of claim 1 ~ 6.
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| CN105948762A (en) * | 2016-04-25 | 2016-09-21 | 武汉科技大学 | Composite powder of zirconium carbide cladding graphite and preparation method thereof |
| CN108585889B (en) * | 2018-04-28 | 2021-04-16 | 武汉科技大学 | Bar-shaped zirconium boride-sheet silicon carbide single crystal composite powder and preparation method thereof |
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| Mechanochemical synthesis of ZrB2–SiC–ZrC nanocomposite powder by metallothermic reduction of zircon;M. Jalaly et al.;《Journal of Alloys and Compounds》;20130731;第581卷;第782-787页 * |
| 熔盐介质中碳化物粉体的制备研究;丁娟;《中国优秀硕士学位论文全文数据库 工程科技I辑》;20111215(第12期);摘要，第56页 * |
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