CN107973608A - A kind of toughening sintering aid of sintering boron carbide ceramic under constant pressure and preparation method thereof - Google Patents

A kind of toughening sintering aid of sintering boron carbide ceramic under constant pressure and preparation method thereof Download PDF

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Publication number
CN107973608A
CN107973608A CN201711170235.5A CN201711170235A CN107973608A CN 107973608 A CN107973608 A CN 107973608A CN 201711170235 A CN201711170235 A CN 201711170235A CN 107973608 A CN107973608 A CN 107973608A
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powder
parts
sintering
preparation
sintering aid
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史秀梅
曹剑武
杨亚璋
李志鹏
张立君
陈刚
倪杨
郑阳升
任丽宏
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China Weapon Science Academy Ningbo Branch
Chinese Academy of Ordnance Science Ningbo Branch
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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
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/64—Burning or sintering processes
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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
    • C—CHEMISTRY; METALLURGY
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    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3232—Titanium oxides or titanates, e.g. rutile or anatase
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/38—Non-oxide ceramic constituents or additives
    • C04B2235/3817—Carbides
    • C04B2235/3821—Boron carbides
    • C—CHEMISTRY; METALLURGY
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/40—Metallic constituents or additives not added as binding phase
    • C04B2235/402—Aluminium
    • C—CHEMISTRY; METALLURGY
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    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
    • C04B2235/422—Carbon
    • C04B2235/424—Carbon black
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/52—Constituents or additives characterised by their shapes
    • C04B2235/5208—Fibers
    • C04B2235/5216—Inorganic
    • C04B2235/524—Non-oxidic, e.g. borides, carbides, silicides or nitrides
    • C04B2235/5244—Silicon carbide

Abstract

A kind of toughening sintering aid of sintering boron carbide ceramic under constant pressure, by the Al powder of 2.5 parts of molfraction, 19~20 parts of TiO2Powder, 47.5~50 parts of carbon black, 9~10 parts of SiC whiskers and 2~3 parts of B4Made of C powder, first by Al powder, TiO2Powder, carbon black, B4C powder, SiC whiskers weigh in proportion, add a small amount of dispersant and are put into ball mill mixing container, add deionized water and carry out ball milling slurrying, gained slurry solids content is 35~55%；Gained slurry is dried, and sieves after broken, grinding, powder is made, by powder in steel die pressed compact, be then sintered, cool to room temperature after sintering with the furnace, obtain sintered body, sintered body is ground into powder, that is, obtain the sintering aid containing boron titanium aluminium carbon silicon.The present invention is using boron titanium aluminium carbon silicon as B4The principal crystalline phase of the sintering aid of C ceramics, cost is low, using effect is good, effectively solves B4The problem of sintering temperature is high during C ceramic systems are standby, finished product fracture toughness is low.

Description

A kind of toughening sintering aid of sintering boron carbide ceramic under constant pressure and preparation method thereof
Technical field
The present invention relates to a kind of toughening sintering aid of sintering boron carbide ceramic under constant pressure and preparation method thereof.
Background technology
Boron carbide (B4C) it is a kind of advanced structural ceramic material that hardness is only below diamond and cubic boron nitride, with it High rigidity, low-density, good chemical stability and higher neutron absorption capability, nuclear industry, chemical industry, aerospace and Protection field, which is gathered around, to have wide practical use.The technique that tradition prepares boron carbide is that (median is little using pure boron carbide powder In 0.5 μm) carry out normal pressure-sintered, it is necessary to which more than 2300 DEG C of temperature, could realize that (relative sintered density is more than densification sintering 92%), and prepare ceramic intensity and fracture toughness ratio it is relatively low, therefore the large-scale production for boron carbide ceramics and Using all there are considerable influence.
Through looking into, the Chinese patent of existing Patent No. CN200910071576.6《A kind of cooling of sintering boron carbide increases Tough sintering aid and preparation method》, the toughening sintering aid be by molfraction be 8.1-8.2 parts Al powder, 5.8-6 parts Made of carbon black and 1-1.2 parts of B4C, during preparation, first, boron carbide powder, carbon black, aluminium powder and absolute ethyl alcohol are mixed, then ball Mill, drying；Next, the powder of drying is made preform in graphite jig, preform is then put into Vacuum Heat More mechanism sintering reactions are carried out in pressure stove, the furnace cooling of sample after reaction to be sintered to room temperature, has so just obtained porous Block materials, then, by this porous material grind into powder, that is, obtain the required sintering aid containing boron aluminium carbon.The increasing Tough sintering aid is using boron aluminium carbon as principal crystalline phase, plays the role of reducing sintering temperature, but cost is higher, in preparation process The time of ball milling is also longer, therefore need further to improve.
The content of the invention
First technical problem to be solved by this invention is to provide the normal pressure-sintered carbon that a kind of cost is low, using effect is good Change the toughening sintering aid of boron ceramics, can effectively reduce the sintering temperature of boron carbide, the enhancing intensity of boron carbide product and tough Property.
Second technical problem to be solved by this invention is to provide the normal pressure-sintered carbon that a kind of technique is simple and convenient to operate Change the preparation method of the toughening sintering aid of boron ceramics, the toughening sintering aid cost of preparation is low, using effect is good, can be effective Reduce the sintering temperature of boron carbide, strengthen the intensity and toughness of boron carbide product.
Technical solution is used by the present invention solves above-mentioned first technical problem：A kind of sintering boron carbide ceramic under constant pressure Toughening sintering aid, it is characterised in that：The toughening sintering aid is using boron titanium aluminium carbon silicon as principal crystalline phase, is by molar part Al powder, 19~20 part of TiO of the number for 2.5 parts2Powder, 47.5~50 parts of carbon black, 9~10 parts of SiC whiskers and 2~3 parts B4C powder is mixed.
Technical solution is used by the present invention solves above-mentioned second technical problem：A kind of sintering boron carbide ceramic under constant pressure The preparation method of toughening sintering aid, it is characterised in that comprise the following steps：
1) by Al powder of the molfraction for 2.5 parts, 19~20 parts of TiO2Powder, 47.5~50 parts of carbon black, 9~10 parts SiC whiskers and 2~3 parts of B4C powder mixes, and adds the dispersant that mass fraction is no more than 2%, is put into polyurethane ball-milling pot In, deionized water is added, the addition of deionized water is 1~2.5 times of mixed-powder volume, and slurry is made in ball milling 6~10 when small Material, gained slurry solids content are 35~55%, are crushed after slurry drying, grinding, cross 40 mesh or 60 mesh sieves, complete powder system It is standby；
2) powder of above-mentioned preparation is put into steel die of the diameter no more than 40mm, pressure is the condition of 1~5MPa Lower pressed compact；
3) preform is placed in graphite jig, enters and vacuumize process is carried out in high-temperature vacuum sintering furnace, then heat up Sintering；
4) sin-tering mechanism is：The programming rate of room temperature~600 DEG C is 10 DEG C/min, and 600 DEG C of whens keep the temperature 15min, then with The heating rate of 15 DEG C/min is warming up to 1200 DEG C, keeps the temperature 10~15min, is then continued with the heating rate of 5~10 DEG C/min 1600 DEG C are warming up to, after keeping the temperature 60~120min, furnace cooling obtains the sintered body of sintering aid；
5) sintered body is ground into powder, that is, obtains the sintering aid containing boron titanium aluminium carbon silicon.
Preferably, the Al powder purities described in the step 1) are more than 99%, median is not more than 3 μm.
Preferably, the TiO in the step 1)2Powder purity is more than 99.9%, and median is not more than 100nm.
Preferably, the carbon black in the step 1) is water colo(u)r carbon black, and median is not more than 200nm.
Further preferably, 45~55 μm of the length of the SiC whiskers in the step 1), 100~600nm of diameter.
Further preferably, the B in the step 1)4The purity of C powder is more than 98%, and median is not more than 1.0 μm.
Further preferably, the dispersant in the step 1) is ammonium polyacrylate, tetramethylammonium hydroxide, phenolic resin or poly- second One or more in enol butyral.
Finally, the sin-tering mechanism in the step 4) is：The programming rate of room temperature~600 DEG C is 10 DEG C/min, at 600 DEG C 15min is kept the temperature, is then warming up to 1200 DEG C with the heating rate of 15 DEG C/min, 15min is kept the temperature, then with the heating of 5 DEG C/min Speed is continuously heating to 1600 DEG C, and after keeping the temperature 60~120min, furnace cooling obtains the sintered body of sintering aid.
Compared with prior art, the advantage of the invention is that：
1st, sintering aid material of the invention is using boron titanium aluminium carbon silicon as principal crystalline phase, it has high-melting-point, high intensity, with B4C Similar thermal coefficient of expansion and excellent antioxygenic property, when sintering temperature is more than 1900 DEG C, boron titanium aluminium carbon silicon is with liquid shape Formula is distributed in B4Around C particles, B can be promoted4C particle flows, accelerate stomata discharge, while preferably purify B4C crystal boundaries, Abnormal grain growth and roughening are prevented to a certain extent, not only contribute to the densification sintering of boron carbide ceramics, and can be with Effectively improve B4The intensity and toughness of C ceramic materials；
2nd, present invention employs sintering aid of the interstitial compound that principal crystalline phase is boron titanium aluminium carbon silicon as boron carbide, have The characteristics of cost is low, using effect is good, with carrying out normal pressure-sintered knot using pure boron carbide powder (median is not more than 0.5 μm) Fruit is compared, and sintering temperature can be made to decline about 100~200 DEG C, the B of preparation4C ceramic post sinterings density is more than 2.4g/cm3, it is broken tough Property is more than 3.2MPam1/2, the problem of boron carbide ceramics product sintering temperature high, poor mechanical property can be efficiently solved.
Embodiment
The present invention is described in further detail with reference to embodiments.
Embodiment 1
Sintering aid material presses Al powder, 20 parts of the TiO of 2.5 parts of molfraction in present embodiment2Powder, 50 parts of charcoal Black, 9 parts of SiC whiskers and 2 parts of B4C powder mixes, and adds the dispersant of mass fraction 1%, dispersant is ammonium polyacrylate, is put into In polyurethane ball-milling pot, the deionized water of about 1.5 times of mixed-powder volume is added, then slurry, slurry drying is made in when ball milling 8 is small Crush, grind afterwards, cross 60 mesh sieves, powder is made；Powder is put into steel die of the diameter no more than 40mm, pressure 3MPa Under conditions of preform is made；Place the blanks in graphite jig, enter and vacuumize process is carried out in high-temperature vacuum sintering furnace, so Heating sintering afterwards；Sin-tering mechanism is：The programming rate of room temperature~600 DEG C is 10 DEG C/min, and 600 DEG C of whens keep the temperature 15min, then with The heating rate of 15 DEG C/min is warming up to 1200 DEG C, keeps the temperature 15min, is then continuously heating to the heating rate of 5 DEG C/min 1600 DEG C, after keeping the temperature 120min, furnace cooling obtains the sintered body of sintering aid, and sintered body is ground into powder, that is, is contained There is the sintering aid of boron titanium aluminium carbon silicon.
Embodiment 2
Present embodiment presses the Al powder of 2.5 parts of molfraction, 19 from sintering aid material unlike embodiment 1 The TiO of part2Powder, 47.5 parts of carbon black, 10 parts of SiC whiskers and 3 parts of B4C powder mixes, and adds the dispersant of mass fraction 0.5%, Dispersant is phenolic resin, is put into polyurethane ball-milling pot, and the deionized water of about 1 times of addition mixed-powder volume, then ball milling 6 are small When slurry is made, other are identical with embodiment 1.
Embodiment 3
Present embodiment presses the Al powder of 2.5 parts of molfraction, 20 from sintering aid material unlike embodiment 1 The TiO of part2Powder, 50 parts of carbon black, 10 parts of SiC whiskers, 2 parts of B4C powder mixes, and adds the dispersant of mass fraction 1.5%, point Powder is ammonium polyacrylate, tetramethylammonium hydroxide mixture, is put into polyurethane ball-milling pot, adds mixed-powder volume about Slurry is made in 2.5 times of deionized water, then when ball milling 10 is small, other are identical with embodiment 1.
B prepared by sintering aid using the present invention4C ceramic post sinterings density is more than 2.4g/cm3, fracture toughness is more than 3.2MPa·m1/2, substantially increase B4The intensity and toughness of C ceramic materials, while sintering temperature can decline about 100~200 DEG C, reduce cost.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art For member, without departing from the technical principles of the invention, some improvements and modifications can also be made, these improvements and modifications Also it should be regarded as protection scope of the present invention.

Claims (9)

  1. A kind of 1. toughening sintering aid of sintering boron carbide ceramic under constant pressure, it is characterised in that：The toughening sintering aid be with Boron titanium aluminium carbon silicon is principal crystalline phase, is by Al powder of the molfraction for 2.5 parts, 19~20 parts of TiO2Powder, 47.5~50 parts of charcoal Black, 9~10 parts of SiC whiskers and 2~3 parts of B4C powder is mixed.
  2. 2. a kind of preparation method of the toughening sintering aid of sintering boron carbide ceramic under constant pressure, it is characterised in that including following step Suddenly：
    1) by Al powder of the molfraction for 2.5 parts, 19~20 parts of TiO2Powder, 47.5~50 parts of carbon black, 9~10 parts of SiC are brilliant Palpus and 2~3 parts of B4C powder mixes, and adds the dispersant that mass fraction is no more than 2%, is put into polyurethane ball-milling pot, adds Deionized water, the addition of deionized water are 1~2.5 times of mixed-powder volume, and slurry, gained is made in ball milling 6~10 when small Slurry solids content is 35~55%, is crushed after slurry drying, grinding, crosses 40 mesh or 60 mesh sieves, completes powder and prepares；
    2) powder of above-mentioned preparation is put into steel die of the diameter no more than 40mm, pressure is pressed under conditions of being 1~5MPa Base；
    3) preform is placed in graphite jig, enters and vacuumize process is carried out in high-temperature vacuum sintering furnace, then heating sintering；
    4) sin-tering mechanism is：The programming rate of room temperature~600 DEG C is 8~12 DEG C/min, and 600 DEG C of whens keep the temperature 10~20min, then 1150~1250 DEG C are warming up to the heating rate of 13~17 DEG C/min, 10~15min is kept the temperature, then with 5~10 DEG C/min's Heating rate is continuously heating to 1550~1650 DEG C, and after keeping the temperature 60~120min, furnace cooling obtains the sintered body of sintering aid；
    5) sintered body is ground into powder, that is, obtains the sintering aid containing boron titanium aluminium carbon silicon.
  3. 3. preparation method according to claim 2, it is characterised in that：Al powder purities described in the step 1) are more than 99%, median is not more than 3 μm.
  4. 4. preparation method according to claim 2, it is characterised in that：TiO in the step 1)2Powder purity is more than 99.9%, median is not more than 100nm.
  5. 5. preparation method according to claim 2, it is characterised in that：Carbon black in the step 1) is water colo(u)r carbon Black, median is not more than 200nm.
  6. 6. preparation method according to claim 2, it is characterised in that：The length of SiC whiskers in the step 1) is 45 ~55 μm, 100~600nm of diameter.
  7. 7. preparation method according to claim 2, it is characterised in that：B in the step 1)4The purity of C powder is more than 98%, median is not more than 1.0 μm.
  8. 8. preparation method according to claim 2, it is characterised in that：Dispersant in the step 1) is polyacrylic acid One or more in ammonium, tetramethylammonium hydroxide, phenolic resin or polyvinyl butyral resin.
  9. 9. preparation method according to claim 2, it is characterised in that：Sin-tering mechanism in the step 4) is：Room temperature~ 600 DEG C of programming rate is 10 DEG C/min, and 600 DEG C of whens keep the temperature 15min, are then warming up to 1200 with the heating rate of 15 DEG C/min DEG C, 15min is kept the temperature, is then continuously heating to 1600 DEG C with the heating rate of 5 DEG C/min, after keeping the temperature 60~120min, with furnace cooling But the sintered body of sintering aid is obtained.
CN201711170235.5A 2017-11-22 2017-11-22 A kind of toughening sintering aid of sintering boron carbide ceramic under constant pressure and preparation method thereof Pending CN107973608A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108911753A (en) * 2018-08-26 2018-11-30 扬州北方三山工业陶瓷有限公司 A kind of high tenacity pressureless sintering boron carbide ceramics preparation method
CN109467446A (en) * 2018-10-17 2019-03-15 中国兵器科学研究院宁波分院 A kind of toughening sintering aid and preparation method thereof of hot pressed sintering boron carbide ceramics
CN111410543A (en) * 2020-04-24 2020-07-14 朔州西廊煤炭科技有限公司 Method for preparing functional ceramic engineering material combustion-supporting catalyst by utilizing coal solid waste or bauxite solid waste

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Publication number Priority date Publication date Assignee Title
CN86103862A (en) * 1985-05-06 1987-01-21 加州大学评议会 Aluminium-boron-carbide sintering metal and reactive metal-boron-carbide sintering metal
CN101503301A (en) * 2009-03-19 2009-08-12 哈尔滨工程大学 Cooling toughening sintering aid for sintering boron carbide and preparation
CN102219518A (en) * 2011-03-31 2011-10-19 浙江立泰复合材料有限公司 Boron carbide-silicon carbide complex ceramic and preparation method thereof
CN102757224A (en) * 2012-07-31 2012-10-31 中国科学院上海硅酸盐研究所 Method for preparing dense boron carbide matrix ceramic material by sintering
CN103613389A (en) * 2013-11-29 2014-03-05 宁波伏尔肯机械密封件制造有限公司 Sintering preparation method of boron carbide ceramic

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN86103862A (en) * 1985-05-06 1987-01-21 加州大学评议会 Aluminium-boron-carbide sintering metal and reactive metal-boron-carbide sintering metal
CN101503301A (en) * 2009-03-19 2009-08-12 哈尔滨工程大学 Cooling toughening sintering aid for sintering boron carbide and preparation
CN102219518A (en) * 2011-03-31 2011-10-19 浙江立泰复合材料有限公司 Boron carbide-silicon carbide complex ceramic and preparation method thereof
CN102757224A (en) * 2012-07-31 2012-10-31 中国科学院上海硅酸盐研究所 Method for preparing dense boron carbide matrix ceramic material by sintering
CN103613389A (en) * 2013-11-29 2014-03-05 宁波伏尔肯机械密封件制造有限公司 Sintering preparation method of boron carbide ceramic

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108911753A (en) * 2018-08-26 2018-11-30 扬州北方三山工业陶瓷有限公司 A kind of high tenacity pressureless sintering boron carbide ceramics preparation method
CN109467446A (en) * 2018-10-17 2019-03-15 中国兵器科学研究院宁波分院 A kind of toughening sintering aid and preparation method thereof of hot pressed sintering boron carbide ceramics
CN111410543A (en) * 2020-04-24 2020-07-14 朔州西廊煤炭科技有限公司 Method for preparing functional ceramic engineering material combustion-supporting catalyst by utilizing coal solid waste or bauxite solid waste

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