CN103833403B - The preparation method of the toughness reinforcing boron carbide ceramics matrix material of a kind of silicon carbide whisker and product - Google Patents
The preparation method of the toughness reinforcing boron carbide ceramics matrix material of a kind of silicon carbide whisker and product Download PDFInfo
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- CN103833403B CN103833403B CN201410075504.XA CN201410075504A CN103833403B CN 103833403 B CN103833403 B CN 103833403B CN 201410075504 A CN201410075504 A CN 201410075504A CN 103833403 B CN103833403 B CN 103833403B
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Abstract
The present invention discloses preparation method and the product of the toughness reinforcing boron carbide ceramics matrix material of a kind of silicon carbide whisker, adopts low temperature reaction sintering to prepare B in conjunction with the method for isostatic cool pressing
4c base substrate, reduces sintering temperature, improves pressed compact relative density; On the other hand, by adopting crystal whisker toughened method, increasing crack growth resistance, improving B
4c Ceramic Fracture toughness.
Description
Technical field
The invention belongs to field of inorganic nonmetallic material, relate to the preparation technology of matrix material, especially a kind of preparation method of silicon carbide toughened boron carbide ceramics matrix material.
Background technology
B
4c is widely used because having a series of premium propertiess such as high rigidity, high-melting-point, low density, high-wearing feature, high-selenium corn neutron, but also there are two fatal weakness in it: one is sintering difficulty, because boron in boron carbide ceramics and carbon are with stronger covalent bonds (composition of covalent linkage is up to 93.9%); Two is the low (KIC<2.2MPam of fracture toughness property
1/2), two above defects make the application of boron carbide ceramics be greatly limited.
At present to B
4c pottery carry out toughness reinforcing maximum be SiCw.At B
4siCw is added, preparation SiCw/B in C pottery
4c composite.SiCw can occur in the breaking-down process of pottery that the unsticking of whisker is extracted, crack deflection, and this all consumes energy, enhances fracture toughness and the intensity of material.For B
4c Sintering Problem, general sintering method end gets up to mainly contain normal pressure-sintered, hot pressed sintering, high temperature isostatic pressing sintering etc.But the density of normal pressure-sintered material is lower, be difficult to reach necessary requirement; Hot pressed sintering, high temperature isostatic pressing sintering can obtain high-compactness and high performance stupalith, but sintering temperature is high, high and wayward to equipment requirements.
Current B
4there is sintering temperature high (2000 ~ 2300 DEG C), problem that cost is large in C ceramic product preparation technology, high temperature sintering can cause whisker to damage toward contact, and the product size adopting this technique to prepare is restricted, the simple goods of shape can only be done.
Instant invention overcomes above-mentioned defect.
Summary of the invention
The object of the invention is to overcome above-mentioned the deficiencies in the prior art, provide a kind of SiCw/B preparing high-compactness, high fracture toughness at a lower temperature
4c ceramic composite.
The present invention addresses the aforementioned drawbacks taked technical scheme: adopt low temperature reaction sintering to prepare B in conjunction with the method for isostatic cool pressing
4c base substrate, reduces sintering temperature, improves pressed compact relative density; On the other hand, by adopting crystal whisker toughened method, increasing crack growth resistance, improving B
4c Ceramic Fracture toughness.
Technical scheme of the present invention is realized by following processing step:
(1) following formula and method material with slurry is adopted:
The first: by mass percentage by the carbon black of 5%, 15%SiCw, 78% boron carbide particles join in ball grinder, add the paraffin of 1.5%, 0.5% Tetramethylammonium hydroxide again, using the dehydrated alcohol of powder quality 160% as ball-milling medium ball milling 24 hours, obtain slurry, or
The second: by mass percentage by the carbon black of 8%, 19%SiCw, 70% boron carbide particles join in ball grinder, then add paraffin, 1% Tetramethylammonium hydroxide of 2%, using powder quality 200% dehydrated alcohol as ball-milling medium ball milling 24 hours, obtain slurry;
(2) above-mentioned gained ball milling material to be poured in pallet and to be placed on 40 ~ 60 DEG C of dryings in baking oven, when oven dry is 2% ~ 3% to powder humidity, powder is taken out, 60 orders sieve, extracting screen underflow loads in mould, carry out pre-molding with 60 ~ 100MPa pressure on a hydraulic press, obtain the biscuit with certain density;
(3) biscuit that step (2) presses through in advance is carried out isostatic cool pressing process, concrete technology for be wrapped in rubber die sleeve by biscuit, and again suppresses 5 ~ 10 minutes with the pressure of 180 ~ 200MPa in cold isostatic press;
(4) green compact after step 3 isostatic cool pressing being suppressed are heat-treated, concrete technology is: be positioned over by biscuit in the hydrogen push boat type reduction furnace of flowing, be incubated at three temperature, the setting range of three temperature is respectively 350 ~ 400 DEG C, 450 ~ 600 DEG C, 650 ~ 800 DEG C, push away boat speed and be set to 15 ~ 20 points/boat, be incubated 25 ~ 35min respectively, after binder removal, obtain porous blank;
(5) porous blank step 4 obtained is placed in plumbago crucible, blank is placed powdery or buik silicon that theory needs silicon amount (theory needs silicon msi=base substrate porosity × blank apparent volume × ρ si) 2 times, 10
-2~ 10
-3at 1450 DEG C ~ 1600 DEG C temperature, be incubated 30 ~ 90min under the vacuum environment of Pa, the SiC of high-compactness, high fracture toughness after furnace cooling, can be obtained
w/ B
4c ceramic composite.
In above-mentioned steps (1), the granularity of norbide powder is 3.5 ~ 12.8 μm.
Length-to-diameter ratio >=20 of silicon carbide whisker in above-mentioned steps (1).
In above-mentioned steps (1), the amount of dehydrated alcohol is 1.5 ~ 2 times of powder quality.
The amount of the silicon placed on blank in above-mentioned steps (5) is powdery or buik silicon that theory needs silicon amount 2 times, and theory needs silicon silicon amount to be multiplied by silicon density again after base substrate porosity is multiplied by blank apparent volume.
Relative to prior art, the present invention has the following advantages:
1. preparation technology proposed by the invention obtains SiCw/B under lesser temps (1450 ~ 1600 DEG C)
4c composite, reduces sintering temperature, considerably reduces preparation cost.
2. the material density of gained of the present invention is up to 96% ~ 98%, and this result still reaches quite high fine and close effect in Whisker-Reinforced Ceramics.
3. the fracture toughness of materials prepared of the present invention is high, and SiCw is from B
4consume the energy of a part of extraneous load when extracting in C matrix, make B
4the fracture toughness property of C reaches 4.9 ~ 6.3MPam
1/2.The material fracture toughness that this method obtains on the basis of low temperature, low cost is not less than some high temperature hot pressing techniques.
Accompanying drawing explanation
Fig. 1,2 is respectively the microscopic appearance figure of boron carbide powder, silicon carbide whisker.
Fig. 3 is the metallographic structure photo of complex phase ceramic prepared by the present invention.
Fig. 4 is after the complex phase ceramic fracture prepared of the present invention, the shape appearance figure that the silicon carbide whisker unsticking observed at its section is extracted.
Embodiment
Embodiment 1
The toughness reinforcing B of a kind of SiCw
4the preparation method of C ceramic composite, it comprises the following steps:
(1) by mass percentage by the carbon black of 5%, 15%SiCw, 78% boron carbide particles, join in ball grinder, add the paraffin of 1.5%, 0.5% Tetramethylammonium hydroxide again, using the dehydrated alcohol of powder quality 160% as ball-milling medium ball milling 24 hours, obtain slurry.
(2) then ball milling material to be poured in pallet and to be placed on 60 DEG C of dryings in baking oven, taken out by powder when oven dry is about 3% to powder humidity, 60 orders sieve, and extracting screen underflow loads in mould, carry out pre-molding with 60MPa pressure on a hydraulic press, obtain the biscuit with certain density.
(3) the above-mentioned biscuit pressed through in advance is wrapped in rubber die sleeve, and the pressure with 180MPa in cold isostatic press is suppressed again.
(4) green compact after isostatic cool pressing being suppressed are positioned in the hydrogen push boat type reduction furnace of flowing, and at 380 DEG C, 550 DEG C, 700 DEG C three temperature, carry out insulation 30min respectively, binder removal obtains porous blank.
(5) by blank as plumbago crucible, blank is placed the silicon of 30g block, 10
-3in 1550 DEG C of insulation 30min under the vacuum environment of Pa, the SiCw/B of high-compactness, high fracture toughness after furnace cooling, can be obtained
4c stupalith.
Embodiment 2
The toughness reinforcing B of a kind of SiCw
4the preparation method of C ceramic composite, it comprises the following steps:
(1) by mass percentage by the carbon black of 8%, 19%SiCw, 70% boron carbide particles, join in ball grinder, then add paraffin, 1% Tetramethylammonium hydroxide of 2%, using powder quality 200% dehydrated alcohol as ball-milling medium ball milling 24 hours, obtain slurry.
(2) then ball milling material to be poured in pallet and to be placed on 50 DEG C of dryings in baking oven, taken out by powder when oven dry is about 2% to powder humidity, 60 orders sieve, and extracting screen underflow loads in mould, carry out pre-molding with 90MPa pressure on a hydraulic press, obtain the biscuit with certain density.
(3) the above-mentioned biscuit pressed through in advance is wrapped in rubber die sleeve, and the pressure with 200MPa in cold isostatic press is suppressed again.
(4) green compact after isostatic cool pressing being suppressed are positioned in the hydrogen push boat type reduction furnace of flowing, and at 400 DEG C, 600 DEG C, 800 DEG C three temperature, carry out insulation 35min respectively, binder removal obtains porous blank.
By blank as plumbago crucible, blank is placed 32g silica flour, 10
-3in 1480 DEG C of insulation 60min under the vacuum environment of Pa, the SiCw/B of high-compactness, high fracture toughness after furnace cooling, can be obtained
4c stupalith.
Claims (4)
1. the toughness reinforcing norbide (B of silicon carbide whisker (SiCw)
4c) preparation method of ceramic composite, comprises the steps:
Step one, adopts following formula and method material with slurry:
The first: by mass percentage by the carbon black of 5%, 15%SiCw, 78% boron carbide particles join in ball grinder, add the paraffin of 1.5%, 0.5% Tetramethylammonium hydroxide again, using the dehydrated alcohol of powder quality 160% as ball-milling medium ball milling 24 hours, obtain slurry, or
The second: by mass percentage by the carbon black of 8%, 19%SiCw, 70% boron carbide particles join in ball grinder, then add paraffin, 1% Tetramethylammonium hydroxide of 2%, using powder quality 200% dehydrated alcohol as ball-milling medium ball milling 24 hours, obtain slurry;
Step 2, above-mentioned steps one gained slurry to be poured in pallet and to be placed in baking oven dry at temperature is 40 ~ 60 DEG C, when oven dry is 2% ~ 3% to powder humidity, powder is taken out, 60 orders sieve, extracting screen underflow loads in mould, carry out pre-molding with 60 ~ 100MPa pressure on a hydraulic press, obtain the biscuit with certain density;
Step 3, biscuit above-mentioned steps two pressed through in advance carries out isostatic cool pressing process, is wrapped in rubber die sleeve by biscuit, and again suppresses 5 ~ 10 minutes with the pressure of 180 ~ 200MPa in cold isostatic press;
Step 4, green compact after isostatic cool pressing being suppressed are heat-treated, concrete technique is: be positioned over by biscuit in the hydrogen push boat type reduction furnace of flowing, be incubated at three temperature, the setting range of three temperature is respectively 350 ~ 400 DEG C, 450 ~ 600 DEG C, 650 ~ 800 DEG C, push away boat speed and be set to 15 ~ 20 points/boat, be incubated 25 ~ 35min respectively, after binder removal, obtain porous blank;
Step 5, is placed in plumbago crucible by gained porous blank in step 4, blank is placed appropriate powdery or buik silicon, 10
-2~ 10
-3at 1450 DEG C ~ 1600 DEG C temperature, be incubated 30 ~ 90min under the vacuum environment of Pa, the SiCw/B of high-compactness, high fracture toughness after furnace cooling, can be obtained
4c ceramic composite, is characterized in that, in step one, boron carbide powder material granularity is 3.5 ~ 12.8 μm, and length-to-diameter ratio>=20 of silicon carbide whisker in step one.
2. the toughness reinforcing norbide (B of silicon carbide whisker according to claim 1 (SiCw)
4c) preparation method of ceramic composite, is characterized in that:
In step one, the amount of dehydrated alcohol is 1.5 ~ 2 times of powder quality.
3. the toughness reinforcing norbide (B of silicon carbide whisker according to claim 1 (SiCw)
4c) preparation method of ceramic composite, is characterized in that:
The amount of the silicon placed on blank in step 5 is powdery or buik silicon that theory needs silicon amount 2 times, and theory needs silicon amount to be multiplied by silicon density again after base substrate porosity is multiplied by blank apparent volume.
4. according to the toughness reinforcing norbide (B of the preparation-obtained silicon carbide whisker of method described in claim 1 (SiCw)
4c) ceramic composite.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2016037316A1 (en) * | 2014-09-09 | 2016-03-17 | 南京工业大学 | Preparation method of sic porous ceramic material and porous ceramic material manufactured by using same |
| CN104591738A (en) * | 2015-02-04 | 2015-05-06 | 中国科学院上海硅酸盐研究所 | High-toughness boron carbide ceramic and preparation method thereof |
| CN104909789A (en) * | 2015-05-20 | 2015-09-16 | 铜陵宏正网络科技有限公司 | Alumina-fiber-enhanced boron carbide ceramic-based composite material and preparation method thereof |
| CN106478103A (en) * | 2015-09-01 | 2017-03-08 | 常熟佳合高级陶瓷材料有限公司 | A kind of preparation method of silicon carbide/carbon boron composite ceramic material |
| CN106673661A (en) * | 2016-12-26 | 2017-05-17 | 上海工程技术大学 | Thick-plate silicon carbide ceramic material and preparation method and application thereof |
| CN108911773A (en) * | 2018-06-20 | 2018-11-30 | 浙江立泰复合材料股份有限公司 | A kind of preparation method of silicon carbide fibre enhancing boron carbide ceramics material |
| CN109020587B (en) * | 2018-07-23 | 2021-06-01 | 吉林长玉特陶新材料技术股份有限公司 | Preparation method of boron nitride nanotube toughened titanium carbide neutron absorption ceramic |
| CN113345615B (en) * | 2021-05-31 | 2022-12-27 | 中国工程物理研究院材料研究所 | Paraffin/boron carbide neutron protection composite material and preparation method thereof |
| CN115403386A (en) * | 2022-08-24 | 2022-11-29 | 佛山国防科技工业技术成果产业化应用推广中心 | Whisker-reinforced boron carbide composite ceramic and preparation method thereof |
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| CN101164997A (en) * | 2006-10-16 | 2008-04-23 | 宁波大学 | Method for preparing silicon carbide ceramic plasticized by rod-like aluminum oxide particle and silicon carbide whisker combination |
| CN102219536A (en) * | 2011-04-27 | 2011-10-19 | 浙江大学 | B4C/SiC whisker/SiC multiphase ceramic matrix composite and preparation method thereof |
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