CN101186503A - Zirconium boride-zirconium carbide composite diphase material and use thereof - Google Patents
Zirconium boride-zirconium carbide composite diphase material and use thereof Download PDFInfo
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- CN101186503A CN101186503A CNA2007101717011A CN200710171701A CN101186503A CN 101186503 A CN101186503 A CN 101186503A CN A2007101717011 A CNA2007101717011 A CN A2007101717011A CN 200710171701 A CN200710171701 A CN 200710171701A CN 101186503 A CN101186503 A CN 101186503A
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- zirconium
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- zirconium carbide
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Abstract
The invention relates to a zirconium diboride-zirconium carbide multiphase material, which pertains to the structural ceramics field. In the composite material of ZrB2-ZrC of the invention, the content of the ZrC is within 20 to 80wt%, and is continuously adjustable; granularity of the composite powder body is less than 200nm with good forming and sintering performance, can be used as starting material of conventional sintering and hot-press sintering, and is expected to be popularized in the field of electrode materials and refractory materials.
Description
Technical field
The present invention relates to a kind of Zirconium boride-zirconium carbide (ZrB
2-ZrC) composite diphase material and uses thereof belongs to the structural ceramic material field.
Background technology
ZrB
2All have high-melting-point with ZrC, high-modulus, high rigidity, high thermal conductivity and specific conductivity, no phase transformation and good thermal shock resistance become the potential candidate material that thermal structure is used.Compare ZrC, ZrB
2Low temperature resistance of oxidation in having is better compared ZrB
2, ZrC is having superiority aspect electricity and the anti-neutron radiation, if therefore can be in conjunction with the advantage of two aspect materials, the development of new composite diphase material be expected to be used for refractory materials, electrode materials and nuclear control material.
At present, industrial preparation ZrB
2Adopt solid phase method and vapor phase process with the ZrC powder, because its raw material adopts micron-sized powder, the diameter of particle of preparation is bigger more, and sintering activity is poor.And the super-refinement of powder can improve motivating force in the sintering process, improves microtexture, improve mechanical property, so the preparation of ultrathin composite powder is subjected to paying attention to widely.
Liquid phase method particularly sol-gel method forms unbodied metastable phase in preparation process, reaction contact area is big, is the common method that low temperature prepares superfine powder, is commonly used to prepare oxide powder, film and fiber and other glass and equates.But it is at present less to the liquid phase method preparation research of carbide, boride.(Preiss H et al.J Mater Sci., 1998,33 (19): 4697-4706) alkoxide sol-gel method of employing titanium and zirconium is prepared fiber and the film of TiC and ZrC to Preiss etc.(Sacks.et al.J.Mat.Sci., 2004,39 (9): 6057-6066) utilize the source of the alkoxide of zirconium and hafnium as Zr, polyalcohols is prepared the ZrC powder as the source of C to Sacks etc., and particle diameter is at 50～130nm.The liquid phase method research of boride powder seldom only has (Chen LY, Gu YL, et al.J alloy compd, 2004,368 (1-2): 353-356, Scripta Mater., 2004,50 (7): 959-961) utilize hydrothermal method, with ZrCl such as Chen and Gu at present
4, HfCl
4And NaBH
4Be reactant, prepare ZrB at 500～700 ℃
2And HfB
2Nano-powder, but output is little, only as laboratory study.
ZrB
2, the ZrC pottery has very strong covalent linkage characteristic, and industrialization synthetic powder sintering specific activity is relatively poor, normal pressure-sintered difficulty; Simple powder direct mixing method is adopted in the preparation of complex phase ceramic at present, and the phase homogeneity is poor; Though alkoxide sol-gel method is successfully prepared the ZrC powder, itself exists shortcoming.Alkoxide is relatively more expensive, and a small amount of toxicity is arranged, and there is certain cracking carbon amount in this under high temperature inert atmosphere, so C/Zr, and C/B/Zr is difficult for determining.
Summary of the invention
The objective of the invention is to adopt liquid phase method to prepare a kind of Zirconium boride-zirconium carbide composite diphase material.
Zirconium boride-zirconium carbide composite diphase material of the present invention, wherein ZrC content is accounting for the 20wt%～80wt% of gross weight, and adjustable continuously.
The present invention is achieved in that
At first zirconium oxychloride is dissolved in the mixing solutions that the second alcohol and water is made into, the concentration of zirconium oxychloride is about 0.2～1mol/L, and the volume ratio of second alcohol and water is 3: 1～5: 1.Amount by selected boron zirconium ratio joins boric acid in the mixing solutions, add polyoxyethylene glycol as dispersion agent, concentration is 0.5～2wt%, weak ammonia titration with 20～50vol% concentration, regulating pH is 3～5 o'clock formation zirconia sols, the phenol resin solution that adds 10～80vol% then, form binary colloidal sol, continue with 20～50vol% concentration ammonia water titration, until forming gel, then with gel drying, oven dry then, grind, sieve precursor powder, obtained composite granule in 0.5～3 hour in vacuum or inert atmosphere, heat-treating under 1300～1600 ℃ at last.
Zirconium boride-zirconium carbide composite diphase material provided by the invention, its advantage is conspicuous:
(1) diameter of particle is little, is evenly distributed, and specific surface area is big.
(2) preparation temperature is lower, and speed of response is fast.
(3) pass through to regulate H in the composite diphase material
3BO
3Amount, it is adjustable between 20wt%～80wt% just can to prepare ZrC content.
(4) by changing the content of ZrC, material is widely used in different Application Areass.As the starting raw material of electrode materials the time, the content of ZrC is controlled at about 50wt%, and during as the starting raw material of refractory materials, the content of ZrC is controlled at about 20wt%, and during as the starting raw material of electrode materials, ZrC content is controlled at about 80wt%.
Description of drawings
Fig. 1: liquid phase method prepares the schema of Zirconium boride-zirconium carbide composite diphase material
Fig. 2: 1500 ℃ of calcining 1h obtain the XRD figure (wherein the ZrC theoretical content is 50wt% in the composite granule) of composite granule.
Fig. 3: the SEM photo (as can be seen from the figure, powder has certain reunion, and median size is below 200nm) of the Zirconium boride-zirconium carbide composite diphase material of 1500 ℃ of calcining 1h preparation.
Embodiment
Embodiment 1:
It is 4: 1 mixing solutions that the 41.16g zirconium oxychloride is dissolved in 500ml ethanol and water volume ratio, stirs and makes its dissolving.Add 12.36g boric acid and mix, and add the 4.80g polyoxyethylene glycol, drip the weak ammonia of 25vol% then, regulate about pH to 3, form zirconia sol as dispersion agent.Add 23.28g resol (remaining carbon is about 50%, and concentration is 50vol%) and be made into mixed sols.Continue dropping ammonia, make its cohesion.Gel is transferred to ball grinder, is ball milling bulbec mill 24h with the zirconium white, and drying is 12 hours under 80 ℃, obtains the powder presoma.Calcining obtained the Zirconium boride-zirconium carbide composite granule in 1 hour under 1500 ℃, and the ZrC theoretical content is 20wt% in the composite granule, obviously finds out ZrB in the XRD figure
2Exist mutually with ZrC, do not have other intermediate phase.It is comparatively even that (see figure 2) finds out that from the SEM photo powder disperses, and median size is about 50～200nm.(see figure 3)
Embodiment 2:
It is 4: 1 mixing solutions that the 49.99g zirconium oxychloride is dissolved in 500ml ethanol and water volume ratio, stirs and makes its dissolving.Add 12.36g boric acid and mix, and add the 4.90g polyoxyethylene glycol, drip the weak ammonia of 25vol% then, regulate about pH to 3, form zirconia sol as dispersion agent.Add 26.55g resol (remaining carbon is about 50%, and concentration is 50vol%) and be made into mixed sols.Continue dropping ammonia, make its cohesion.Gel is transferred to ball grinder, is ball milling bulbec mill 24h with the zirconium white, and drying is 12 hours under 80 ℃, obtains the powder presoma.Calcining obtained the Zirconium boride-zirconium carbide composite granule in 1 hour under 1500 ℃, and the ZrC theoretical content is 50wt% in the composite granule.
Embodiment 3:
It is 4: 1 mixing solutions that the 58.81g zirconium oxychloride is dissolved in 500ml ethanol and water volume ratio, stirs and makes its dissolving.Add 12.36g boric acid and mix, and add the 5.40g polyoxyethylene glycol, drip the weak ammonia of 25vol% then, regulate about pH to 3, form zirconia sol as dispersion agent.Add 29.83g resol (remaining carbon is about 50%, and concentration is 50vol%) and be made into mixed sols.Continue dropping ammonia, make its cohesion.Gel is transferred to ball grinder, is ball milling bulbec mill 24h with the zirconium white, and drying is 12 hours under 80 ℃, obtains the powder presoma.Calcining obtained the Zirconium boride-zirconium carbide composite granule in 1 hour under 1500 ℃, and the ZrC theoretical content is 80wt% in the composite granule.
Claims (3)
1. a Zirconium boride-zirconium carbide composite diphase material comprises zirconium boride 99.5004323A8ure and zirconium carbide two phase materials.
2. by the described a kind of Zirconium boride-zirconium carbide composite diphase material of claim 1, it is characterized in that zirconium carbide content accounts for the 20wt%～80wt% of gross weight, and adjustable continuously.
3. press the starting raw material of claim 1 and 2 described a kind of Zirconium boride-zirconium carbide composite diphase material electrode materialss and refractory materials.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101717011A CN101186503A (en) | 2007-12-03 | 2007-12-03 | Zirconium boride-zirconium carbide composite diphase material and use thereof |
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|---|---|---|---|
| CNA2007101717011A CN101186503A (en) | 2007-12-03 | 2007-12-03 | Zirconium boride-zirconium carbide composite diphase material and use thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102219517A (en) * | 2010-04-14 | 2011-10-19 | 浙江晟翔电子科技有限公司 | Multiphase ceramic material with adjustable resistivity and preparation technology thereof |
| CN104087974A (en) * | 2014-07-25 | 2014-10-08 | 深圳市新星轻合金材料股份有限公司 | Box-type zirconium boride inert anode for aluminium electrolysis, preparation method and aluminium electrolysis system |
| CN105130446A (en) * | 2015-09-01 | 2015-12-09 | 广西南宁智翠科技咨询有限公司 | High-strength zirconium boride ceramic and preparing method thereof |
| CN105236989A (en) * | 2015-09-11 | 2016-01-13 | 杨洋 | High strength and high temperature zirconium boride ceramic and preparation method thereof |
| CN105837220A (en) * | 2015-01-15 | 2016-08-10 | 赵品麟 | Preparation method of zirconium diboride ceramic with in-situ introduction of boron/zirconium carbide binary additive |
| CN115612911A (en) * | 2022-12-19 | 2023-01-17 | 潍坊昌成耐磨材料有限公司 | Preparation method of wear-resistant metal framework ceramic |
-
2007
- 2007-12-03 CN CNA2007101717011A patent/CN101186503A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102219517A (en) * | 2010-04-14 | 2011-10-19 | 浙江晟翔电子科技有限公司 | Multiphase ceramic material with adjustable resistivity and preparation technology thereof |
| CN102219517B (en) * | 2010-04-14 | 2013-06-12 | 浙江晟翔电子科技有限公司 | Multiphase ceramic material with adjustable resistivity and preparation technology thereof |
| CN104087974A (en) * | 2014-07-25 | 2014-10-08 | 深圳市新星轻合金材料股份有限公司 | Box-type zirconium boride inert anode for aluminium electrolysis, preparation method and aluminium electrolysis system |
| CN104087974B (en) * | 2014-07-25 | 2015-10-28 | 深圳市新星轻合金材料股份有限公司 | A kind of box zirconium boride 99.5004323A8ure inert anode used for aluminium electrolysis, preparation method and electrolysis of aluminum system |
| CN105837220A (en) * | 2015-01-15 | 2016-08-10 | 赵品麟 | Preparation method of zirconium diboride ceramic with in-situ introduction of boron/zirconium carbide binary additive |
| CN105130446A (en) * | 2015-09-01 | 2015-12-09 | 广西南宁智翠科技咨询有限公司 | High-strength zirconium boride ceramic and preparing method thereof |
| CN105236989A (en) * | 2015-09-11 | 2016-01-13 | 杨洋 | High strength and high temperature zirconium boride ceramic and preparation method thereof |
| CN115612911A (en) * | 2022-12-19 | 2023-01-17 | 潍坊昌成耐磨材料有限公司 | Preparation method of wear-resistant metal framework ceramic |
| CN115612911B (en) * | 2022-12-19 | 2023-03-14 | 潍坊昌成耐磨材料有限公司 | Preparation method of wear-resistant metal framework ceramic |
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