CN105130438A - Method for preparing boron carbide ceramic composite material based on reaction sintering - Google Patents
Method for preparing boron carbide ceramic composite material based on reaction sintering Download PDFInfo
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- CN105130438A CN105130438A CN201510519685.5A CN201510519685A CN105130438A CN 105130438 A CN105130438 A CN 105130438A CN 201510519685 A CN201510519685 A CN 201510519685A CN 105130438 A CN105130438 A CN 105130438A
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Abstract
The invention relates to a method for preparing boron carbide ceramic composite material based on reaction sintering. The method comprises the following steps: depositing a layer of metallic titanium on the surface of boron carbide powder, mixing the boron carbide powder with carbon black powder, phenolic resin powder and industrial alcohol, carrying out ball milling, drying, granulating to obtain a precursor mixed powder, placing the precursor mixed powder in a die to produce a precursor pressed compact, disposing powdery or blocky silicon on the precursor pressed compact, placing the obtained compact in a vacuum furnace, carrying out silicon infiltration reaction sintering, cooling in a furnace, and removing superfluous silicon on the surface to obtain the boron carbide ceramic composite material. Compared with the prior art, the method has the advantages of simple process steps, effective solving of the problem of high temperature and high pressure sintering needed by routine technologies, low production energy consumption and preparation cost, and very good application prospect.
Description
Technical field
The invention belongs to bulletproof ceramic technical field, relate to a kind of method preparing boron carbide ceramics matrix material, especially relate to a kind of method preparing boron carbide ceramics matrix material based on reaction sintering.
Background technology
At present, boron carbide ceramics is the material that physical protection material Midst density is minimum, hardness is the highest of practical application, and shellproof good combination property, can keep the battlefield maneuverability of equipment personnel largely.Norbide itself has a series of premium propertiess such as high rigidity, high-melting-point, low density, high-wearing feature, high-selenium corn neutron and is widely used, 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, and such as, boron carbide ceramics is extremely difficult to sinter, and usually need to adopt hot pressing and excessive temperature to sinter.
Based on silicon carbide reactor sintering theory, adopt reaction sintering technology to prepare boron carbide ceramics, significantly can reduce sintering temperature, thus reduce production energy consumption and preparation cost.But in reaction sintering process, norbide silicon liquid that is easy and melting reacts, and forms Si-B-C ternary compound and other carbide a series of, compromises the integrity of norbide phase.These carbide fragility are large, hardness is low, thus make reaction sintering boron carbide composite material penalty.
In order to suppress the reaction of norbide and silicon, usual employing carries out the treatment measures such as pickling and Surface coating carbon to boron carbide powder, but these treatment measures then can bring new environmental issue, and easily in sintering process, produce residual carbon, cause final material property significantly to reduce.
Authorization Notice No. is the preparation method that the Chinese invention patent of CN102464490B discloses a kind of boron-carbide-based ceramic composite material, comprises the following steps: (1) is by B
4c powder mixes with binding agent, or by B
4c mixed powder mixes with binding agent, then sieves, and chooses the particle of granularity between 24-60 order as mold pressing material; (2) by mold pressing material die forming, after drying, B is obtained
4c-C biscuit; (3) by B
4c-C biscuit, as skeleton, adopts Si as infiltration agent, carries out infiltration in vacuum.Adopt technique disclosed in this patented technology, Si while reacting with the C in biscuit, also can with B
4c reacts, and result makes the B in biscuit
4the integrity of the crystalline structure of C is damaged, and the mechanical property of pottery is worsened, and the stability of mechanical property is also adversely affected.In order to keep B
4the integrity of C crystalline structure, improves B
4the excellent properties of C pottery, patent of the present invention gives a solution, namely at B
4c powder surface coating layer of metal titanium layer, in order to suppress Si and B
4the reaction of C, also improves Si and B
4the wettability of C, accelerates the speed of response of C in Si and biscuit.The B that reaction generates
4c complex phase ceramic maintains B
4the integrity of C crystalline structure, the SiC that original position is formed and TiC and B
4c combines closely, thus improves the mechanical property of complex phase ceramic.
Summary of the invention
Object of the present invention is exactly provide a kind of processing step simple to overcome defect that above-mentioned prior art exists, silicon and norbide effectively can be suppressed to react, protect the method preparing boron carbide ceramics matrix material based on reaction sintering of norbide phase integrity.
Object of the present invention can be achieved through the following technical solutions:
Prepare a method for boron carbide ceramics matrix material based on reaction sintering, the method specifically comprises the following steps:
(1) be 15-20:0.5-5 by the mass ratio of boron carbide powder and titanium valve, boron carbide powder and titanium valve be placed in mixer, be uniformly mixed, obtained mixed powder;
(2) mixed powder is placed in crystal vessel, and puts into vacuum oven, control vacuum tightness>=2 × 10
-3pa, and at 900-1000 DEG C constant temperature process 1-2h, furnace cooling, comes out of the stove, and is sieved by powder, after the powder of removing particle diameter < 3 μm, namely obtains the compound carbonizing boron powder of coating surface layer of metal titanium;
(3) after by weight the resol of the compound carbonizing boron powder of 85-95 part, the carbon black of 5-12 part and 0-3 part being mixed, be placed in ball grinder, add ethanol and ball milling ball again, ball milling 12-24h, obtain mixed slurry, again mixed slurry is dried, cross 100 mesh sieves, be i.e. obtained presoma mixed powder;
(4) presoma mixed powder is placed in mould compression moulding, pressing pressure controls as 80-100MPa, i.e. obtained presoma pressed compact;
(5) presoma pressed compact is placed in plumbago crucible, and on presoma pressed compact, places the silicon of powder or block, in 1 × 10
-2-1 × 10
-3under the vacuum environment of Pa, control temperature is 1500-1580 DEG C, Isothermal sinter 1-2h, i.e. obtained sintered blank;
(6) after sintered blank furnace cooling, the silicon of sintered blank excess surface is removed, i.e. obtained described boron carbide ceramics matrix material.
Boron carbide powder described in step (1) to be mass percent be 80-90%, size range are at the boron carbide powder of 40-100 μm.
The titanium valve of to be mass percent be 10-20%, the granularity < 3 μm of the titanium valve described in step (1).
The thickness of the compound carbonizing boron powder coating surface titanium layer described in step (2) is 0.05-2 μm.
Ball mill ball quality described in step (3) is 1:1 with the ratio of the total mass of compound carbonizing boron powder, carbon black and resol.
The agate ball of described ball milling ball to be diameter be 5mm.
The solids content of the resol described in step (3) is 65-74%.
The quality of the powder described in step (5) or the silicon of block and the mass ratio of presoma pressed compact are (1-3): 10.
In preparation process of the present invention; first at boron carbide ceramics powder surface metal refining titanium; in sintering process subsequently; carbon in metal titanium and biscuit reacts; and define fine and close titanium carbide on norbide surface; it can not only suppress the reaction of silicon and norbide, the integrity of protection norbide phase, and can also improve the overall performance of boron carbide ceramics matrix material.
In the present invention, the optimum thickness of layer of titanium metal is 0.05-2 μm.The thickness of titanium is too low, can not play a protective role to norbide; The thickness of titanium coating is excessive, then the content of reaction product titanium carbide is excessive, and therefore the content of free titanium in pottery and free silica can improve, and can reduce the mechanical property of pottery like this.
Compared with prior art, the present invention has following characteristics:
1) due at boron carbide ceramics surface deposition metal titanium, after reaction sintering, surface metal titanium layer defines fine and close titanium carbide, the reaction of silicon and norbide can not only be suppressed, the integrity of protection norbide phase, and improve the overall performance of boron carbide ceramics matrix material, the flexural strength of the reaction sintering norbide obtained through reaction sintering reaches 350MPa, Young's modulus is greater than 380GPa, and Vickers' hardness is greater than 22GPa;
2) present invention, avoiding the necessary problem of carrying out sintering under high-temperature and high-pressure conditions of common process, greatly reduce difficulty and the process costs of preparation, and complex-shaped and that volume is larger goods can be prepared;
3) processing step is simple, and significantly reduce sintering temperature, effectively reduce production energy consumption and preparation cost, in reaction sintering process, norbide keeps complete mutually, improves the hardness of matrix material.
Embodiment
Below in conjunction with specific embodiment, exemplary illustration and help understand the present invention further.But embodiment detail is only in order to the present invention is described, do not represent the present invention conceive under whole technical schemes, therefore should not be construed as the restriction to technical scheme of the present invention.Some unsubstantialities not departing from the present invention's design are changed, such as, simply change with the technical characteristic with same or similar technique effect or replace, all belonging to rights protection scope of the present invention.
Embodiment 1:
Prepare a method for boron carbide ceramics matrix material based on reaction sintering, comprise the following steps:
Step one, by the boron carbide powder 170g of size range at 40 ~ 100 μm, the titanium valve 30g being less than 3 μm with granularity, puts into mixer and stirs 1h, obtains the powder mixed;
Step 2, puts into crystal vessel by mixed powder, puts into vacuum oven, keeps vacuum tightness to be not less than 2 × 10
-3pa, at 1000 DEG C after isothermal holding 1h; By the powder of coming out of the stove after furnace cooling, cross 320 order reciprocating sieves, remove undersize powder, obtain the compound carbonizing boron powder of coating surface layer of metal titanium;
Step 3, adds compound carbonizing boron powder 88g, carbon black powder 10g, Phenolic resin powder 2g in ball mill, then pours the agate ball 100g of industrial spirit 100ml and diameter 5mm into, then ball milling mixing 12h together, removes agate ball, obtains mixed slurry.After mixed slurry after ball milling is dried through 120 DEG C, cross 100 mesh sieves, extracting screen underflow is as presoma mixed powder.Presoma mixed powder 80g puts into mould, obtains presoma pressed compact at 100MPa Forming under Pressure;
Step 4, presoma pressed compact is positioned in plumbago crucible, presoma pressed compact is placed the Pure Silicon Metal cake of 20g, 6.8 × 10
-3under the vacuum environment of Pa, at 1500 DEG C, be incubated 2h, obtain sintered blank;
Step 5, after sintered blank furnace cooling, removes the unnecessary silicon on sintered blank surface, obtains reaction sintering boron carbide composite material.
Embodiment 2:
Prepare a method for boron carbide ceramics matrix material based on reaction sintering, comprise the following steps:
Step one, by the boron carbide powder 160g of size range at 40 ~ 100 μm, the titanium valve 40g being less than 3 μm with granularity, puts into mixer and stirs 2h, obtains the powder mixed;
Step 2, puts into crystal vessel by mixed powder, puts into vacuum oven, keeps vacuum tightness to be not less than 2 × 10
-3pa, at 900 DEG C after isothermal holding 2h; By the powder of coming out of the stove after furnace cooling, cross 320 order reciprocating sieves, remove undersize powder, obtain the compound carbonizing boron powder of coating surface layer of metal titanium;
Step 3, adds compound carbonizing boron powder 85g, carbon black powder 12g, Phenolic resin powder 3g in ball mill, then pours the agate ball 100g of industrial spirit 150ml and diameter 5mm into, then ball milling mixing 24h together, removes agate ball, obtains mixed slurry.After mixed slurry after ball milling is dried through 120 DEG C, cross 100 mesh sieves, extracting screen underflow is as presoma mixed powder.Get presoma mixed powder 80g and put into mould, obtain presoma pressed compact at 100MPa Forming under Pressure;
Step 4, presoma pressed compact is positioned in plumbago crucible, presoma pressed compact is placed the Pure Silicon Metal cake of 23g, 5 × 10
-3under the vacuum environment of Pa, at 1550 DEG C, be incubated 2h, obtain sintered blank;
Step 5, after sintered blank furnace cooling, removes the unnecessary silicon on sintered blank surface, obtains reaction sintering boron carbide composite material.
Embodiment 3:
Prepare a method for boron carbide ceramics matrix material based on reaction sintering, the method specifically comprises the following steps:
(1) be 15:0.5 by the mass ratio of boron carbide powder and titanium valve, boron carbide powder and titanium valve be placed in mixer, be uniformly mixed, obtained mixed powder;
(2) mixed powder is placed in crystal vessel, and puts into vacuum oven, control vacuum tightness>=2 × 10
-3pa, and at 1000 DEG C constant temperature process 2h, furnace cooling, comes out of the stove, and is sieved by powder, after the powder of removing particle diameter < 3 μm, namely obtains the compound carbonizing boron powder of coating surface layer of metal titanium;
(3) after by weight the resol of the compound carbonizing boron powder of 85 parts, the carbon black of 5 parts and 2 parts being mixed, be placed in ball grinder, add ethanol and ball milling ball again, ball milling 12h, obtain mixed slurry, again mixed slurry is dried, cross 100 mesh sieves, be i.e. obtained presoma mixed powder;
(4) presoma mixed powder is placed in mould compression moulding, pressing pressure controls as 80MPa, i.e. obtained presoma pressed compact;
(5) presoma pressed compact is placed in plumbago crucible, and on presoma pressed compact, places the silicon of powder or block, in 1 × 10
-2under the vacuum environment of Pa, control temperature is 1580 DEG C, Isothermal sinter 1h, i.e. obtained sintered blank;
(6) after sintered blank furnace cooling, the silicon of sintered blank excess surface is removed, i.e. obtained described boron carbide ceramics matrix material.
The boron carbide powder that wherein, in step (1), boron carbide powder is mass percent is 80%, granularity is 100 μm; To be mass percent be titanium valve 20%, the titanium valve of granularity < 3 μm.
In step (2), the thickness of compound carbonizing boron powder coating surface titanium layer is 0.05 μm.
In step (3), ball mill ball quality is 1:1 with the ratio of the total mass of compound carbonizing boron powder, carbon black and resol, the agate ball of ball milling ball to be diameter be 5mm; The solids content of resol is 65%.
In step (5), the quality of the silicon of powder or block and the mass ratio of presoma pressed compact are 1:10.
Embodiment 4:
Prepare a method for boron carbide ceramics matrix material based on reaction sintering, the method specifically comprises the following steps:
(1) be 20:5 by the mass ratio of boron carbide powder and titanium valve, boron carbide powder and titanium valve be placed in mixer, be uniformly mixed, obtained mixed powder;
(2) mixed powder is placed in crystal vessel, and puts into vacuum oven, control vacuum tightness>=2 × 10
-3pa, and at 1000 DEG C constant temperature process 2h, furnace cooling, comes out of the stove, and is sieved by powder, after the powder of removing particle diameter < 3 μm, namely obtains the compound carbonizing boron powder of coating surface layer of metal titanium;
(3) after by weight the resol of the compound carbonizing boron powder of 95 parts, the carbon black of 12 parts and 3 parts being mixed, be placed in ball grinder, add ethanol and ball milling ball again, ball milling 24h, obtain mixed slurry, again mixed slurry is dried, cross 100 mesh sieves, be i.e. obtained presoma mixed powder;
(4) presoma mixed powder is placed in mould compression moulding, pressing pressure controls as 100MPa, i.e. obtained presoma pressed compact;
(5) presoma pressed compact is placed in plumbago crucible, and on presoma pressed compact, places the silicon of powder or block, in 1 × 10
-3under the vacuum environment of Pa, control temperature is 1500 DEG C, Isothermal sinter 2h, i.e. obtained sintered blank;
(6) after sintered blank furnace cooling, the silicon of sintered blank excess surface is removed, i.e. obtained described boron carbide ceramics matrix material.
The boron carbide powder that wherein, in step (1), boron carbide powder is mass percent is 90%, granularity is 40 μm; To be mass percent be titanium valve 10%, the titanium valve of granularity < 3 μm.
In step (2), the thickness of compound carbonizing boron powder coating surface titanium layer is 2 μm.
In step (3), ball mill ball quality is 1:1 with the ratio of the total mass of compound carbonizing boron powder, carbon black and resol, the agate ball of ball milling ball to be diameter be 5mm; The solids content of resol is 74%.
In step (5), the quality of the silicon of powder or block and the mass ratio of presoma pressed compact are 3:10.
Embodiment 5:
Prepare a method for boron carbide ceramics matrix material based on reaction sintering, the method specifically comprises the following steps:
(1) be 18:3 by the mass ratio of boron carbide powder and titanium valve, boron carbide powder and titanium valve be placed in mixer, be uniformly mixed, obtained mixed powder;
(2) mixed powder is placed in crystal vessel, and puts into vacuum oven, control vacuum tightness>=2 × 10
-3pa, and at 900 DEG C constant temperature process 1h, furnace cooling, comes out of the stove, and is sieved by powder, after the powder of removing particle diameter < 3 μm, namely obtains the compound carbonizing boron powder of coating surface layer of metal titanium;
(3) after by weight the resol of the compound carbonizing boron powder of 92 parts, the carbon black of 6 parts and 1 part being mixed, be placed in ball grinder, add ethanol and ball milling ball again, ball milling 16h, obtain mixed slurry, again mixed slurry is dried, cross 100 mesh sieves, be i.e. obtained presoma mixed powder;
(4) presoma mixed powder is placed in mould compression moulding, pressing pressure controls as 90MPa, i.e. obtained presoma pressed compact;
(5) presoma pressed compact is placed in plumbago crucible, and on presoma pressed compact, places the silicon of powder or block, in 1 × 10
-3under the vacuum environment of Pa, control temperature is 1550 DEG C, Isothermal sinter 1h, i.e. obtained sintered blank;
(6) after sintered blank furnace cooling, the silicon of sintered blank excess surface is removed, i.e. obtained described boron carbide ceramics matrix material.
The boron carbide powder that wherein, in step (1), boron carbide powder is mass percent is 85%, granularity is 60 μm; To be mass percent be titanium valve 15%, the titanium valve of granularity < 3 μm.
In step (2), the thickness of compound carbonizing boron powder coating surface titanium layer is 1 μm.
In step (3), ball mill ball quality is 1:1 with the ratio of the total mass of compound carbonizing boron powder, carbon black and resol, the agate ball of ball milling ball to be diameter be 5mm; The solids content of resol is 68%.
In step (5), the quality of the silicon of powder or block and the mass ratio of presoma pressed compact are 2:10.
Embodiment 6:
Prepare a method for boron carbide ceramics matrix material based on reaction sintering, the method specifically comprises the following steps:
(1) be 16:5 by the mass ratio of boron carbide powder and titanium valve, boron carbide powder and titanium valve be placed in mixer, be uniformly mixed, obtained mixed powder;
(2) mixed powder is placed in crystal vessel, and puts into vacuum oven, control vacuum tightness>=2 × 10
-3pa, and at 980 DEG C constant temperature process 1.5h, furnace cooling, comes out of the stove, and is sieved by powder, after the powder of removing particle diameter < 3 μm, namely obtains the compound carbonizing boron powder of coating surface layer of metal titanium;
(3), after by weight the compound carbonizing boron powder of 87 parts, the carbon black of 9 parts being mixed, be placed in ball grinder, then add ethanol and ball milling ball, ball milling 20h, obtains mixed slurry, then is dried by mixed slurry, cross 100 mesh sieves, i.e. obtained presoma mixed powder;
(4) presoma mixed powder is placed in mould compression moulding, pressing pressure controls as 100MPa, i.e. obtained presoma pressed compact;
(5) presoma pressed compact is placed in plumbago crucible, and on presoma pressed compact, places the silicon of powder or block, in 1 × 10
-2under the vacuum environment of Pa, control temperature is 1570 DEG C, Isothermal sinter 1.5h, i.e. obtained sintered blank;
(6) after sintered blank furnace cooling, the silicon of sintered blank excess surface is removed, i.e. obtained described boron carbide ceramics matrix material.
The boron carbide powder that wherein, in step (1), boron carbide powder is mass percent is 82%, granularity is 80 μm; To be mass percent be titanium valve 18%, the titanium valve of granularity < 3 μm.
In step (2), the thickness of compound carbonizing boron powder coating surface titanium layer is 1.2 μm.
In step (3), ball mill ball quality is 1:1 with the ratio of the total mass of compound carbonizing boron powder, carbon black and resol, the agate ball of ball milling ball to be diameter be 5mm; The solids content of resol is 72%.
In step (5), the quality of the silicon of powder or block and the mass ratio of presoma pressed compact are 3:10.
Claims (8)
1. prepare a method for boron carbide ceramics matrix material based on reaction sintering, it is characterized in that, the method specifically comprises the following steps:
(1) be 15-20:0.5-5 by the mass ratio of boron carbide powder and titanium valve, boron carbide powder and titanium valve be placed in mixer, be uniformly mixed, obtained mixed powder;
(2) mixed powder is placed in crystal vessel, and puts into vacuum oven, control vacuum tightness>=2 × 10
-3pa, and at 900-1000 DEG C constant temperature process 1-2h, furnace cooling, comes out of the stove, and is sieved by powder, after the powder of removing particle diameter < 3 μm, namely obtains the compound carbonizing boron powder of coating surface layer of metal titanium;
(3) after by weight the resol of the compound carbonizing boron powder of 85-95 part, the carbon black of 5-12 part and 0-3 part being mixed, be placed in ball grinder, add ethanol and ball milling ball again, ball milling 12-24h, obtain mixed slurry, again mixed slurry is dried, cross 100 mesh sieves, be i.e. obtained presoma mixed powder;
(4) presoma mixed powder is placed in mould compression moulding, pressing pressure controls as 80-100MPa, i.e. obtained presoma pressed compact;
(5) presoma pressed compact is placed in plumbago crucible, and on presoma pressed compact, places the silicon of powder or block, in 1 × 10
-2-1 × 10
-3under the vacuum environment of Pa, control temperature is 1500-1580 DEG C, Isothermal sinter 1-2h, i.e. obtained sintered blank;
(6) after sintered blank furnace cooling, the silicon of sintered blank excess surface is removed, i.e. obtained described boron carbide ceramics matrix material.
2. a kind of method preparing boron carbide ceramics matrix material based on reaction sintering according to claim 1, it is characterized in that, to be mass percent the be 80-90% of the boron carbide powder described in step (1), size range are at the boron carbide powder of 40-100 μm.
3. a kind of method preparing boron carbide ceramics matrix material based on reaction sintering according to claim 1, is characterized in that, the titanium valve of to be mass percent be 10-20%, the granularity < 3 μm of the titanium valve described in step (1).
4. a kind of method preparing boron carbide ceramics matrix material based on reaction sintering according to claim 1, is characterized in that, the thickness of the compound carbonizing boron powder coating surface titanium layer described in step (2) is 0.05-2 μm.
5. a kind of method preparing boron carbide ceramics matrix material based on reaction sintering according to claim 1, it is characterized in that, the ball mill ball quality described in step (3) is 1:1 with the ratio of the total mass of compound carbonizing boron powder, carbon black and resol.
6. a kind of method preparing boron carbide ceramics matrix material based on reaction sintering according to claim 5, is characterized in that, the agate ball of described ball milling ball to be diameter be 5mm.
7. a kind of method preparing boron carbide ceramics matrix material based on reaction sintering according to claim 1, is characterized in that, the solids content of the resol described in step (3) is 65-74%.
8. a kind of method preparing boron carbide ceramics matrix material based on reaction sintering according to claim 1, is characterized in that, the quality of the powder described in step (5) or the silicon of block and the mass ratio of presoma pressed compact are 1-3:10.
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| CN105777130A (en) * | 2016-03-17 | 2016-07-20 | 东北大学 | Gel casing preparation method of reaction-sintered boron carbide ceramic composite material |
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| CN109354504B (en) * | 2018-11-27 | 2021-09-14 | 合肥工业大学 | Boron carbide-based composite ceramic sintering aid and sintering process |
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| CN114656277A (en) * | 2022-03-17 | 2022-06-24 | 南通三责精密陶瓷有限公司 | Method for manufacturing environment-friendly pressureless sintering boron carbide ceramic material |
| CN114656277B (en) * | 2022-03-17 | 2022-12-27 | 南通三责精密陶瓷有限公司 | Method for manufacturing environment-friendly pressureless sintering boron carbide ceramic material |
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Effective date of registration: 20230403 Address after: 313219 No.7, Zhenxing Road, LEIDIAN Town, Deqing County, Huzhou City, Zhejiang Province Patentee after: ZHEJIANG LIGHT-TOUGH COMPOSITE MATERIALS CO.,LTD. Address before: 201620 No. 333, Longteng Road, Shanghai, Songjiang District Patentee before: SHANGHAI University OF ENGINEERING SCIENCE |