CN102617148A - Novel boron carbide ceramic base composite material and preparation method thereof - Google Patents
Novel boron carbide ceramic base composite material and preparation method thereof Download PDFInfo
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- CN102617148A CN102617148A CN2012100986149A CN201210098614A CN102617148A CN 102617148 A CN102617148 A CN 102617148A CN 2012100986149 A CN2012100986149 A CN 2012100986149A CN 201210098614 A CN201210098614 A CN 201210098614A CN 102617148 A CN102617148 A CN 102617148A
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Abstract
The invention discloses a boron carbide ceramic base composite material. The preparation comprises the following steps of: adding B4C powder in an amount of 60-80 percent by volume; selecting ZrB2 particles and SiC particles as a reinforcement phase; selecting absolute ethanol or acetone as a solvent; wet-mixing the raw materials, reinforcement and the solvent and then drying; and performing hot pressing sintering under vacuum or under protection of inert atmosphere at the sintering temperature of 1,850-2,000 DEG C and under sintering pressure of 20-40 MPa for 20-60 minutes. Compared with single-component boron carbide ceramic, the sintering temperature of the high-hardness boron carbide ceramic base composite material can be reduced by 150-250 DEG C; the sintered material has higher hardness; meanwhile, the machining performance of the material is greatly improved to facilitate the machining of the complex shape of the boron carbide ceramic base composite material; and thus, the machining period and the cost of the ceramic material are effectively reduced, and a complex structural member can be prepared.
Description
Technical field
The present invention relates to a kind of novel boron carbide ceramics based composites and preparation method thereof.
Background technology
Norbide has good performances such as hardness height, light weight, wear-resistant, corrosion-resistant, high temperature resistant, intercept neutrons, is widely used in fields such as machinery, metallurgy, chemical industry, nuclear industry.Norbide is a kind of covalent linkage compound, has better chemical stability, makes that its sintering in the ceramic process of preparation is very difficult.The technology that adopt usually the home and abroad all is pressing methods under 2200 ℃ of left and right sides temperature, and manufacturing cost is high, can not be applied to the processing of special-shaped and specialty products, has limited its development.
With transition metal boride and the compound synthetic ceramic matric composite of carbide; Has excellent physicals; Comprise HMP, high thermal conductivity, high Young's modulus; And can at high temperature keep very high intensity, and also have good heat-shock resistance and moderate coefficient of thermal expansion simultaneously, become the most promising candidate material of some key positions under high temperature or the ultrahigh-temperature thermal environment condition.
At present all carrying out a large amount of work aspect the research of complicated shape boron carbide ceramics goods both at home and abroad,, reducing manufacturing cost, enlarging its Application Areas, adapting to the demand of every profession and trade development norbide in the hope of improving the sintering character and the processing characteristics of boron carbide ceramics.
Summary of the invention
Technical problem to be solved by this invention is: in order to solve the problem of existing boron carbide ceramics sintering temperature height, processing difficulties, manufacturing cost height, simple shape, a kind of novel boron carbide ceramics based composites that is applicable to low-temperature sintering technology and low-cost processing and preparation method thereof is provided.
Technical solution of the present invention is: a kind of novel boron carbide ceramics based composites is to be matrix with the norbide, and zirconium boride 99.5004323A8ure, silit form for the wild phase hot pressed sintering;
Preparing method's concrete steps are following:
(1) raw material: adopt B
4C powder, add-on are 60vol%～80vol%;
(2) strengthen body: select ZrB for use
2Particle and SiC particle are wild phase, and add-on is respectively 17vol%～34vol% and 3vol%～6vol%, and the volume ratio of the two satisfies 85%:15%;
(3) solvent: selecting absolute ethyl alcohol or acetone for use is solvent;
(4) batch mixing: with above-mentioned raw materials, strengthen body and solvent and carry out after the wet mixing dry again;
(5) sintering: under vacuum or inert atmosphere protection, 1850～2000 ℃ of sintering temperatures, sintering pressure 20～40MPa, hot pressed sintering under 20～60 minutes conditions of sintering time;
Said B
4C powder, ZrB
2Particle and SiC particle three's volume ratio sum satisfies very.
Technique effect of the present invention is: compare with the single component boron carbide ceramics; The sintering temperature of this high firmness boron carbide ceramics based composites can reduce by 150～250 ℃; Material behind the sintering has higher hardness, has greatly improved Drawing abillity simultaneously, is beneficial to the processing of boron carbide ceramics based composites complicated shape; Thereby effectively reduce the process-cycle and the cost of stupalith, and can carry out the preparation of complex structural member.
Description of drawings
Fig. 1 is the sintering process temperature-time curve.
Fig. 2 is the surface scan photo of boron carbide ceramics based composites.
Embodiment
It is matrix that the present invention adopts norbide, and zirconium boride 99.5004323A8ure and silit are wild phase, and at 1850～2000 ℃, 20～40MPa carries out hot pressed sintering under 20～60 minutes conditions.
Solution is following: is raw material with median size less than the boron carbide powder of 10 μ m, and adding median size is wild phase less than the zirconium boride 99.5004323A8ure powder of 5 μ m and median size less than the silicon carbide powder of 2 μ m.Wherein the add-on of boron carbide particles is the 60vol%～80vol% of TV; The add-on of zirconium boride 99.5004323A8ure powder is the 17vol%～34vol% of the two TV; The SiC particle is a wild phase, and add-on is 3vol%～6vol%, and the volume ratio of zirconium boride 99.5004323A8ure and silit satisfies 85%:15%.Adopt wet method high-energy ball milling batch mixing, after the drying, sintering in vacuum or inert atmosphere.1850～2000 ℃ of sintering temperatures, sintering pressure 20～40MPa, sintering time 20～60 minutes can obtain specific density and reach the novel boron carbide ceramics based composites more than 98%.
Concrete steps are following:
(1) raw material: adopt B
4C powder, median size are 0.5～10 μ m, and add-on is 60vol%～80vol%.
(2) strengthen body: select for use to strengthen body ZrB
2Particle, median size are 0.5～5 μ m, and add-on is 17vol%～34vol%, select for use to strengthen body SiC particle, and median size is 0.5～2 μ m, and add-on is 3vol%～6vol%, and the volume ratio of zirconium boride 99.5004323A8ure and silit satisfies 85%:15%.
(3) solvent: selecting absolute ethyl alcohol or acetone for use is solvent.
(4) batch mixing: above-mentioned raw materials, enhancing body and solvent are carried out wet mixing in required ratio, mix 6～8 hours after drying.
(5) sintering: under vacuum or inert atmosphere protection 1850～2000 ℃ of sintering temperatures, sintering pressure 20～40MPa, hot pressed sintering under 20～60 minutes conditions of sintering time.
Table 1 is the mechanical property of boron carbide ceramics and boron carbide ceramics based composites.Fig. 1 is the curve of sintering process temperature and load; Fig. 2 is the surface scan photo of boron carbide ceramics based composites, and is visible through contrasting, behind adding zirconium boride 99.5004323A8ure and the silit wild phase; Still kept high firmness, and the workability of boron carbide ceramics based composites can be improved significantly.
The mechanical property of table 1 boron carbide ceramics and boron carbide ceramics based composites
According to the factors such as proportioning, sintering process, microtexture and grain-size of boron carbide ceramics based composites, the density of boron carbide ceramics based composites of the present invention＞95.0%, the room temperature fracture toughness property is 3.7～4.2 MPam
1/2, three-point bending strength is 337.0～426.8 MPa, microhardness is 28.0～35.0GPa.
Compare with the single component boron carbide ceramics, although in the boron carbide ceramics based composites, gone into zirconium boride 99.5004323A8ure and silit as wild phase, the mechanical property of material changes little, and has kept high firmness.Simultaneously because the zirconium boride 99.5004323A8ure powder self has electroconductibility; The adding of zirconium boride 99.5004323A8ure powder has significantly improved the processing characteristics of boron carbide ceramics based composites; Its processing no longer relies on working methods such as traditional mechanical grinding, adopts accurate electrical spark or electric processing method can realize the processing of complicated shape, in addition; Energy consumption has been practiced thrift in the significantly reduction of sintering temperature, has reduced production cost.
Below through specific embodiment the present invention is further described, following instance only is used to explain the present invention, and is not used in the scope of the present invention that limits.
1. embodiment one: be the B of 5 μ m with mean particle size
4The C powder is a raw material, and adding the 17vol% mean particle size is the ZrB of 2 μ m
2Powder and 3 vol % mean particle sizes are that the SiC powder of 2 μ m is a wild phase.Carry out dried and screened behind the wet mixing ball milling, 1900 ℃ of hot pressed sinterings under vacuum or inert atmosphere protection, sintering pressure is 30MPa, soaking time 60 minutes.The specific density of prepared material is 96%.
2. embodiment two: adopting mean particle size is the B of 2 μ m
4The C powder is a raw material, and adding the 17vol% mean particle size is the ZrB of 1 μ m
2Powder and 3 vol % mean particle sizes are that the SiC powder of 1 μ m is wild phase, in 1950 ℃ of hot pressed sinterings, and soaking time 30 minutes, all the other conditions such as embodiment 1.The specific density of prepared material is 98.0%.
3. embodiment three: adopting mean particle size is the B of 0.5 μ m
4The C powder is a raw material, and adding the 25.5vol% mean particle size is the ZrB of 0.7 μ m
2Powder and 4.5 vol % mean particle sizes are that the SiC powder of 0.5 μ m is wild phase, in 1850 ℃ of hot pressed sinterings, and soaking time 30 minutes, all the other conditions such as embodiment 1.The specific density of prepared material is 98.5%.
4. embodiment four: according to the different proportionings of material, the composition proportion of boron carbide ceramics based composites is seen table 2.
The composition proportion of table 2 boron carbide ceramics based composites for example
Claims (9)
1. a boron carbide ceramics based composites is characterized in that, it is to be matrix with the norbide, and zirconium boride 99.5004323A8ure and silit form for the wild phase hot pressed sintering, and preparing method's concrete steps are following:
(1) raw material: adopt B
4C powder, add-on are 60vol%～80vol%;
(2) strengthen body: select ZrB for use
2Particle and SiC particle are wild phase, and add-on is respectively 17vol%～34vol% and 3vol%～6vol%, and the volume ratio of the two satisfies 85%:15%;
(3) solvent: selecting absolute ethyl alcohol or acetone for use is solvent;
(4) batch mixing: with above-mentioned raw materials, strengthen body and solvent and carry out after the wet mixing dry again;
(5) sintering: under vacuum or inert atmosphere protection 1850～2000 ℃ of sintering temperatures, sintering pressure 20～40MPa, hot pressed sintering under 20～60 minutes conditions of sintering time;
Said B
4C powder, ZrB
2Particle and SiC particle three's volume ratio sum satisfies very.
2. the preparation method of boron carbide ceramics based composites as claimed in claim 1 is characterized in that, preparing method's concrete steps are following:
(1) raw material: adopt B
4C powder, add-on are 60vol%～80vol%;
(2) strengthen body: select ZrB for use
2Particle and SiC particle are wild phase, and add-on is respectively 17vol%～34vol% and 3vol%～6vol%, and the volume ratio of the two satisfies 85%:15%;
(3) solvent: selecting absolute ethyl alcohol or acetone for use is solvent;
(4) batch mixing: with above-mentioned raw materials, strengthen body and solvent and carry out after the wet mixing dry again;
(5) sintering: under vacuum or inert atmosphere protection, 1850～2000 ℃ of sintering temperatures, sintering pressure 20～40MPa, hot pressed sintering under 20～60 minutes conditions of sintering time;
Said B
4C powder, ZrB
2Particle and SiC particle three's volume ratio sum satisfies 100%.
3. the preparation method of boron carbide ceramics based composites as claimed in claim 2 is characterized in that, said step 4 is for mixing 6～8 hours after drying.
4. the preparation method of boron carbide ceramics based composites as claimed in claim 2 is characterized in that, said B
4C powder median size is less than 10 μ m.
5. the preparation method of boron carbide ceramics based composites as claimed in claim 2 is characterized in that, said ZrB
2The particle median size is less than 5 μ m.
6. the preparation method of boron carbide ceramics based composites as claimed in claim 2 is characterized in that, said SiC particle median size is less than 2 μ m.
7. the preparation method of boron carbide ceramics based composites as claimed in claim 2 is characterized in that, said B
4C powder median size is 0.5～10 μ m.
8. the preparation method of boron carbide ceramics based composites as claimed in claim 2 is characterized in that, said ZrB
2The particle median size is 0.7～5 μ m.
9. the preparation method of boron carbide ceramics based composites as claimed in claim 2 is characterized in that, said SiC particle median size is 0.5～5 μ m.
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Cited By (4)
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|---|---|---|---|---|
| CN103011827A (en) * | 2012-12-20 | 2013-04-03 | 复旦大学 | Preparation method of zirconium diboride ceramic with in-situ-introduced boron as additive |
| CN109415268A (en) * | 2016-05-05 | 2019-03-01 | 圣戈本陶瓷及塑料股份有限公司 | Multiphase ceramic composite material |
| CN113121237A (en) * | 2021-04-16 | 2021-07-16 | 合肥工业大学 | Boron carbide-based composite ceramic and preparation process thereof |
| CN113582698A (en) * | 2021-08-20 | 2021-11-02 | 郑州大学 | Preparation method of ZrB2-SiC toughened B4C bulletproof piece |
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| US20070270302A1 (en) * | 2006-05-22 | 2007-11-22 | Zhang Shi C | Pressurelessly sintered zirconium diboride/silicon carbide composite bodies and a method for producing the same |
| CN101265108A (en) * | 2008-04-16 | 2008-09-17 | 哈尔滨工业大学 | Boride-silicon carbide-boron carbide ternary ceramic-base composite material and preparation method thereof |
| CN101838147A (en) * | 2010-05-21 | 2010-09-22 | 李艳 | Method for synthesizing ZrB2-SiC-based ultra-high temperature ceramic powder by vacuum auto-combustion method |
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| US20070270302A1 (en) * | 2006-05-22 | 2007-11-22 | Zhang Shi C | Pressurelessly sintered zirconium diboride/silicon carbide composite bodies and a method for producing the same |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103011827A (en) * | 2012-12-20 | 2013-04-03 | 复旦大学 | Preparation method of zirconium diboride ceramic with in-situ-introduced boron as additive |
| CN109415268A (en) * | 2016-05-05 | 2019-03-01 | 圣戈本陶瓷及塑料股份有限公司 | Multiphase ceramic composite material |
| US11498874B2 (en) | 2016-05-05 | 2022-11-15 | Saint-Gobain Ceramics & Plastics, Inc. | Multi-phasic ceramic composite |
| CN113121237A (en) * | 2021-04-16 | 2021-07-16 | 合肥工业大学 | Boron carbide-based composite ceramic and preparation process thereof |
| CN113582698A (en) * | 2021-08-20 | 2021-11-02 | 郑州大学 | Preparation method of ZrB2-SiC toughened B4C bulletproof piece |
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Application publication date: 20120801 |