CN107417280A - A kind of normal pressure-sintered boron carbide ceramics preparation method - Google Patents
A kind of normal pressure-sintered boron carbide ceramics preparation method Download PDFInfo
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- CN107417280A CN107417280A CN201710609514.0A CN201710609514A CN107417280A CN 107417280 A CN107417280 A CN 107417280A CN 201710609514 A CN201710609514 A CN 201710609514A CN 107417280 A CN107417280 A CN 107417280A
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/563—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on boron carbide
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- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
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Abstract
The invention discloses a kind of normal pressure-sintered boron carbide ceramics preparation method, comprise the following steps：1st, raw material weighing；2nd, slurry is prepared；3rd, prepared by powder；4th, unsticking sinters.Wherein, B described in the step 14C diameter of particle is 0.1~1um, and the phenolic resin Residual carbon is 40~60wt%.A kind of normal pressure-sintered boron carbide ceramics preparation method of the present invention is completely using boron carbide as raw material, extra powder is not added, abrasive media is used as by the use of boron carbide ball, sieved after grinding through 100 mesh sieve, obtained powder is on purl machine so that 20 100Mpa are dry-pressing formed and/or 150 300MPa isostatic pressings, then it is sintered under normal pressure Ar gas atmospheric conditions, the density of prepared sintering boron carbide ceramic under constant pressure is 2.40 2.50gcm‑3, bending strength is 350 450MPa, and hardness is 33 35GPa.
Description
Technical field
The present invention relates to B4C ceramic fields, specially a kind of normal pressure-sintered boron carbide ceramics preparation method.
Background technology
B4C is the high hard material for being only second to diamond and cubic boron nitride, has low-density, high-modulus and excellent high temperature
Performance, fine and close B4C ceramics are then mainly used as mechanical part and Protective armor using its superior mechanical performance.Additionally, due to B element
With very high neutron absorption cross-section, B4C can be as nuclear reactor deceleration component or the radiation proof part of nuclear reactor.B4C
It is the very strong compound of covalent bond, and B4C plasticity is poor, and crystal boundary moving resistance is very big, surface tension very little during solid-state, these
Intrinsic characteristic determines B4C is a kind of ceramic material of extremely difficult sintering.In order to improve the sintered density of boron carbide ceramics and
Performance, generally use hot pressing sintering method and lqiuid phase sintering method.Hot pressing sintering method refers to load certain pressure in sintering process,
Promote boron carbide sintering densification.Hot pressing sintering method yields poorly, and cost is high, it is difficult to obtains the product of complicated shape simultaneously without regulation
Modelling produces.Lqiuid phase sintering method refers in B4Appropriate Y is added in C2O3、Al2O3、La2O3Deng low melting point rare earth mixture, formed
Eutectic point, in sintering process, Partial Liquid Phase is produced come acceleration of sintering using low melting point.The made carbonization of lqiuid phase sintering method
The performance of boron ceramics is relatively poor, and under the performance of material can be caused drastically because liquid phase occur and separating out when using at high temperature
Drop.Sintering boron carbide ceramic under constant pressure has that process costs are low, can preparation structure compared with complex product, be adapted to the protrusion of large-scale production
Advantage, also there is patent at present（CN102503429B）Using normal pressure-sintered preparation B4C ceramics, but the raw material ratio that this method needs
It is more complicated, it is necessary to add carbon dust, carborundum powder, be unfavorable for industrial production, while excessive carbon dust adds and is unfavorable for B4C ceramics are anti-
Oxidisability.
There is presently no a kind of consistency is high, raw material is simple, low manufacture cost, completely with B4C powders are raw material, with phenol
Urea formaldehyde reduces the quantity of additive, while help sintering as binding agent, and using the C of its cracking acquisition as sintering aid
The normal pressure-sintered B that agent is uniformly mixed4C ceramic preparations.
The content of the invention
The purpose of the present invention is that to solve the above problems and provides that a kind of consistency is high, raw material is simple, is fabricated to
This is low, completely with B4C powders are raw material, and using phenolic resin as binding agent, and the C obtained using its cracking helps as sintering
Agent, reduces the quantity of additive, while the normal pressure-sintered B for making sintering aid be uniformly mixed4C ceramic preparations.
The present invention is achieved through the following technical solutions：
A kind of normal pressure-sintered boron carbide ceramics preparation method, comprises the following steps：
1st, raw material weighing, by weight B4C：Phenolic resin=100:5~30 ratio has weighed B4C and phenolic resin；
2nd, slurry is prepared, using water or alcohol as solvent, by load weighted B in step 14C powders, phenolic resin are made into solid content and are
40~60wt% slurry, with B4C balls are well mixed as mill ball；
3rd, prepared by powder, and B is made by the slurry drying prepared in step 2, crushing, sieving, or through mist projection granulating4C powders,
The average grain diameter of mist projection granulating is controlled to be less than 100 μm；
4th, unsticking sinters, by obtained B in step 34C powders are after dry-pressing and/or isostatic pressing, through unsticking, then in Ar
Sintered under gas atmosphere, B is prepared4C microballoons.
Wherein, B described in the step 14C diameter of particle is 0.1~1um, the phenolic resin Residual carbon is 40~
60wt%。
Mill ball B described in the step 24C balls dosage is 1~5 times of raw material weight.
Incorporation time in the step 2 is 24h.
Drying temperature in the step 3 is 60~80 DEG C.
In the step 3 pulverize and sieve process select 100 mesh screen cloth.
The outlet temperature of mist projection granulating in the step 3 is 60~80 DEG C.
Dry-pressing pressure in the step 4 is 20 ~ 100Mpa.
Hydrostatic pressure in the step 4 is 150 ~ 300Mpa.
Sintering temperature in the step 4 is 2100 DEG C -2300 DEG C, and the sintered heat insulating time is 30min-90min.
A kind of normal pressure-sintered boron carbide ceramics preparation method of the present invention does not add volume completely using boron carbide as raw material
Outer powder, by the use of boron carbide ball as abrasive media, sieved after grinding through 100 mesh sieve, obtained powder is in purl machine
On so that 20-100Mpa is dry-pressing formed and/or 150-300MPa isostatic pressings, then burnt under normal pressure Ar gas atmospheric conditions
Knot, the density of prepared sintering boron carbide ceramic under constant pressure is 2.40-2.50gcm-3, bending strength 350-450MPa, hardness
For 33-35GPa.
Embodiment
The technical scheme in the present invention is clearly and completely described with reference to specific embodiment, it is clear that described
Embodiment be only part of the embodiment of the present invention, rather than whole embodiment.Based on the embodiment in the present invention, ability
The every other embodiment that domain those of ordinary skill is obtained under the premise of creative work is not made, belongs to guarantor of the present invention
The scope of shield.
Instantiation 1
Weigh B4C powder 100g, phenolic resin 5g, it is that powder is made into slurry of the solid content as 45wt% by solvent using water, with
B4C balls 150g is ball-milling medium, mixes 24h, is then then ground untill 70 DEG C of drying in insulating box, then by 100
After purpose sieve, obtained powder 16MPa pressure formings on vulcanizing press are then inferior quiet in 150MPa pressure
Press, sintered after unsticking under normal pressure Ar gas atmosphere, sintering temperature is 2100 DEG C, soaking time 90min, you can obtain B4C makes pottery
Porcelain, obtained B4C ceramic densities are 2.40gcm-3, bending strength 350MPa, hardness 33GPa.
Instantiation 2
Weigh B4C powder 100g, phenolic resin 10g, it is that powder is made into slurry of the solid content as 60wt% by solvent using alcohol,
With B4C balls 200g is ball-milling medium, mixes 24h, through mist projection granulating, outlet temperature is arranged to 65 DEG C, and obtained powder is in flat board
50Mpa pressure formings on vulcanizer, the then isostatic pressed under 200MPa pressure, sinter after unsticking, burn under normal pressure Ar gas atmosphere
Junction temperature is 2150 DEG C, soaking time 60min, you can obtain B4C ceramics, obtained B4C ceramic densities are 2.50gcm-3, resist
Curved intensity is 450MPa, hardness 35GPa.
Moreover, it will be appreciated that although the present specification is described in terms of embodiments, not each embodiment is only wrapped
Containing an independent technical scheme, this narrating mode of specification is only that those skilled in the art should for clarity
Using specification as an entirety, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
It is appreciated that other embodiment.
Claims (10)
1. a kind of normal pressure-sintered boron carbide ceramics preparation method, comprises the following steps：
First, raw material weighing, by weight B4C：Phenolic resin=100:5~30 ratio has weighed B4C and phenolic resin；
2nd, slurry is prepared, using water or alcohol as solvent, by load weighted B in step 14C powders, phenolic resin are made into solid content
For 40~60wt% slurry, with B4C balls are well mixed as mill ball；
3rd, prepared by powder, and B is made by the slurry drying prepared in step 2, crushing, sieving, or through mist projection granulating4C powder
Body, the average grain diameter of mist projection granulating is controlled to be less than 100 μm；
4th, unsticking sinters, by obtained B in step 34C powders are after dry-pressing and/or isostatic pressing, through unsticking, then in Ar
Sintered under gas atmosphere, B is prepared4C microballoons.
A kind of 2. normal pressure-sintered boron carbide ceramics preparation method according to claim 1, it is characterised in that the step
B described in one4C diameter of particle is 0.1~1um, and the phenolic resin Residual carbon is 40~60wt%.
A kind of 3. normal pressure-sintered boron carbide ceramics preparation method according to claim 1, it is characterised in that the step
Mill ball B described in two4C balls dosage is 1~5 times of raw material weight.
A kind of 4. normal pressure-sintered boron carbide ceramics preparation method according to claim 1, it is characterised in that the step
Incorporation time in two is 24h.
A kind of 5. normal pressure-sintered boron carbide ceramics preparation method according to claim 1, it is characterised in that the step
Drying temperature in three is 60~80 DEG C.
A kind of 6. normal pressure-sintered boron carbide ceramics preparation method according to claim 1, it is characterised in that the step
In three pulverize and sieve process select 100 mesh screen cloth.
A kind of 7. normal pressure-sintered boron carbide ceramics preparation method according to claim 1, it is characterised in that the step
The outlet temperature of mist projection granulating in three is 60~80 DEG C.
A kind of 8. normal pressure-sintered boron carbide ceramics preparation method according to claim 1, it is characterised in that the step
Dry-pressing pressure in four is 20 ~ 100Mpa.
A kind of 9. normal pressure-sintered boron carbide ceramics preparation method according to claim 1, it is characterised in that the step
Hydrostatic pressure in four is 150 ~ 300Mpa.
A kind of 10. normal pressure-sintered boron carbide ceramics preparation method according to claim 1, it is characterised in that the step
Sintering temperature in four is 2100 DEG C -2300 DEG C, and the sintered heat insulating time is 30min-90min.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108276003A (en) * | 2018-02-13 | 2018-07-13 | 苏州纳朴材料科技有限公司 | A method of preparing boron carbide complex phase ceramic using sapphire grinding dead meal |
| CN108298986A (en) * | 2018-03-01 | 2018-07-20 | 牡丹江金钢钻碳化硼有限公司 | Boron carbide cup inner bag production technology |
| CN108675793A (en) * | 2018-03-21 | 2018-10-19 | 北京清核材料科技有限公司 | A kind of double sintering method of boron carbide ceramics |
| CN108821773A (en) * | 2018-09-29 | 2018-11-16 | 吉林长玉特陶新材料技术股份有限公司 | A kind of method that the sintering of wet forming reaction in-situ prepares boron carbide ceramics |
| CN108911754A (en) * | 2018-09-29 | 2018-11-30 | 吉林长玉特陶新材料技术股份有限公司 | A kind of normal pressure-sintered method for preparing boron carbide ceramics of dry method |
| CN109279909A (en) * | 2018-10-29 | 2019-01-29 | 宁波伏尔肯科技股份有限公司 | A kind of preparation method of high strength carbonizing boron porous ceramics |
| CN109467436A (en) * | 2018-12-19 | 2019-03-15 | 中国兵器科学研究院宁波分院 | A kind of boron carbide ceramics ball and preparation method thereof |
| CN109608199A (en) * | 2018-10-09 | 2019-04-12 | 江苏新伊菲科技有限公司 | A kind of preparation method of the modified boron carbide composite ceramic of nitride |
| CN111319318A (en) * | 2020-01-07 | 2020-06-23 | 苏州第一元素纳米技术有限公司 | Bulletproof composite armor and preparation method thereof |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108276003A (en) * | 2018-02-13 | 2018-07-13 | 苏州纳朴材料科技有限公司 | A method of preparing boron carbide complex phase ceramic using sapphire grinding dead meal |
| CN108298986A (en) * | 2018-03-01 | 2018-07-20 | 牡丹江金钢钻碳化硼有限公司 | Boron carbide cup inner bag production technology |
| CN108675793A (en) * | 2018-03-21 | 2018-10-19 | 北京清核材料科技有限公司 | A kind of double sintering method of boron carbide ceramics |
| CN108821773A (en) * | 2018-09-29 | 2018-11-16 | 吉林长玉特陶新材料技术股份有限公司 | A kind of method that the sintering of wet forming reaction in-situ prepares boron carbide ceramics |
| CN108911754A (en) * | 2018-09-29 | 2018-11-30 | 吉林长玉特陶新材料技术股份有限公司 | A kind of normal pressure-sintered method for preparing boron carbide ceramics of dry method |
| CN109608199A (en) * | 2018-10-09 | 2019-04-12 | 江苏新伊菲科技有限公司 | A kind of preparation method of the modified boron carbide composite ceramic of nitride |
| CN109279909A (en) * | 2018-10-29 | 2019-01-29 | 宁波伏尔肯科技股份有限公司 | A kind of preparation method of high strength carbonizing boron porous ceramics |
| CN109279909B (en) * | 2018-10-29 | 2021-07-02 | 宁波伏尔肯科技股份有限公司 | Preparation method of high-strength boron carbide porous ceramic |
| CN109467436A (en) * | 2018-12-19 | 2019-03-15 | 中国兵器科学研究院宁波分院 | A kind of boron carbide ceramics ball and preparation method thereof |
| CN109467436B (en) * | 2018-12-19 | 2022-03-11 | 中国兵器科学研究院宁波分院 | Boron carbide ceramic ball and preparation method thereof |
| CN111319318A (en) * | 2020-01-07 | 2020-06-23 | 苏州第一元素纳米技术有限公司 | Bulletproof composite armor and preparation method thereof |
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Application publication date: 20171201 |