CN110282977A - A kind of B4C/TiB2The preparation method of layered composite ceramic material - Google Patents

A kind of B4C/TiB2The preparation method of layered composite ceramic material Download PDF

Info

Publication number
CN110282977A
CN110282977A CN201910520314.7A CN201910520314A CN110282977A CN 110282977 A CN110282977 A CN 110282977A CN 201910520314 A CN201910520314 A CN 201910520314A CN 110282977 A CN110282977 A CN 110282977A
Authority
CN
China
Prior art keywords
tib
powder
ceramic material
composite ceramic
mixed
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201910520314.7A
Other languages
Chinese (zh)
Other versions
CN110282977B (en
Inventor
张翠萍
茹红强
尤田
张金东
夏乾
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Northeastern University China
Original Assignee
Northeastern University China
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Northeastern University China filed Critical Northeastern University China
Priority to CN201910520314.7A priority Critical patent/CN110282977B/en
Publication of CN110282977A publication Critical patent/CN110282977A/en
Application granted granted Critical
Publication of CN110282977B publication Critical patent/CN110282977B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • 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
    • 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
    • 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
    • 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
    • C04B35/565—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 silicon carbide
    • C04B35/573—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 silicon carbide obtained by reaction sintering or recrystallisation
    • 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
    • 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
    • C04B35/58—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 borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
    • C04B35/5805—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 borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on borides
    • C04B35/58064—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 borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on borides based on refractory borides
    • C04B35/58071—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 borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on borides based on refractory borides based on titanium borides
    • 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
    • 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
    • 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
    • C04B2235/30—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
    • C04B2235/428—Silicon
    • 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
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/48—Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
    • 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
    • C04B2235/54—Particle size related information
    • C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
    • C04B2235/5436—Particle size related information expressed by the size of the particles or aggregates thereof micrometer sized, i.e. from 1 to 100 micron
    • 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
    • C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/612—Machining
    • 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
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6562—Heating rate
    • 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
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6567—Treatment time
    • 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
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/74—Physical characteristics
    • C04B2235/77—Density
    • 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
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Ceramic Products (AREA)

Abstract

The invention belongs to field of material technology, provide a kind of B4C/TiB2The preparation method of layered composite ceramic material sequentially includes the following steps: (1) for B4C powder, TiB2Powder or B4C/TiB2Mixed powder is uniformly mixed with carbon source in proportion, is ground and is granulated after abundant drying, then is sieved, and particle of the selection granularity between 24~60 mesh, which is used as, is molded material；(2) according to target molding material filling mold is successively pressed and molded by layer structure, and B is obtained after being carbonized4C/TiB2/ C stratiform biscuit；(3) by B4C/TiB2/ C stratiform biscuit carries out infiltration in vacuum using Si as infiltrant as skeleton, and B is made4C/TiB2Layered composite ceramic material.Method and step of the invention is simple, temperature requirement is low, and the B that consistency is high, comprehensive mechanical property is excellent can be obtained under conditions of lower preparation cost4C/TiB2Layered composite ceramic material, sample change in size < 0.1%, belongs to net-shape-sinter during the preparation process；And method of the invention is able to produce the product of various shape complexity.

Description

A kind of B4C/TiB2The preparation method of layered composite ceramic material
Technical field
The invention belongs to field of material technology, in particular to a kind of B4C/TiB2The preparation method of layered composite ceramic material.
Background technique
Boron carbide (B4C) ceramics have many advantages, such as low-density, exceptional hardness, high-melting-point, resistant to chemical etching, titanium boride (TiB2) Ceramics have high rigidity, high elastic modulus, high-wearing feature, thermally conductive and good conductivity, good chemical stability, by B4C and TiB2In conjunction with manufactured layered composite ceramic material by imitating the shell structure that shell etc. is biological in the Nature, energy dissipation is utilized Toughening mechanisms, substantially improve the fracture toughness of single-layer ceramic material, while ensure that B4C ceramics and TiB2Ceramics high rigidity and High intensity can preferably be suitable for the industries such as military project, machinery and space flight and aviation.
Current layered composite ceramic material is all based on hot-pressing sintering method preparation, such as reaction in-situ hot pressed sintering The Ti of preparation2AlC/Al2O3And Ti3AlC2/Al2O3Layered composite ceramic, the preparation of metal powder painting combination hot pressing sintering method SiC/W layered composite ceramic, in addition there are the B using the preparation of tape casting combination hot pressing sintering method4C/TiB2、B4C/BN stratiform Composite ceramics and hot pressing sintering method combine the TiB of subsequent aluminising preparation2/B4C-A1/B4C、B4C-B4C/Al two-layer compound ceramics Material.Currently, B4C/TiB2Layered composite ceramic material is prepared using tape casting combination hot pressing sintering method, firstly, for being based on The B of hot-pressing sintering method manufacture4C/TiB2Laminate ceramic, although excellent comprehensive mechanical property and higher may be implemented Consistency, but its sintering temperature is generally at 1800 DEG C or more, and hot-press sintering equipment is expensive, production technology is complicated, production Low efficiency, higher cost are difficult to produce the component of oversized shape complexity；Secondly, forefathers use tape casting method, also into One step increases the complexity of material preparation cost and technique, and problem above makes B4C/TiB2The popularization of layered composite ceramic material Using being limited by very large.Therefore, guaranteeing B4C/TiB2Layered composite ceramic material consistency with higher, and tie up While holding its high rigidity and preferable fracture toughness, how to simplify preparation process and reduce preparation cost, become B4C/TiB2Stratiform It is solved the problems, such as required for composite ceramic material development.
Summary of the invention
For existing B4C/TiB2Layered composite ceramic material preparation method there are the problem of, the present invention provides a kind of B4C/ TiB2The preparation method of layered composite ceramic material, with B4C、TiB2, Si and phenolic resin be raw material, it is unidirectional by layer-by-layer filler It after compression molding, then carries out without pressure vacuum siliconising, in the case where the low sintering process of sintering temperature is undeformed, being made has High-compactness and the preferable B of comprehensive mechanical property4C/TiB2Layered composite ceramic material.
Method of the invention sequentially includes the following steps:
A kind of B4C/TiB2The preparation method of layered composite ceramic material, comprises the following steps that
(1) by B4C powder, TiB2Powder or B4C/TiB2Mixed powder is uniformly mixed with carbon source in proportion, and mixed proportion is Carbon content accounts for the 9~18% of mixed powder total weight, and the mixed material of different target structure sheaf is made, by different target structure sheaf Mixed material be sieved respectively, choose particle molding material as each object construction layer of the granularity between 24~60 mesh；
(2) by the molding material of each object construction layer, according to target layered composite ceramic material structure is layered filler, is molded into Shape, then be carbonized at 700-800 DEG C, obtain B4C/TiB2/ C stratiform biscuit；
(3) by B4C/TiB2/ C stratiform biscuit carries out infiltration in vacuum, infiltration process using Si as infiltrant as skeleton It is first to be warming up to 1350 DEG C, is then warming up to 1500~1600 DEG C with the speed of 0.8~1.2 DEG C/min and keeps the temperature 30~60min, It is that liquid is coated on biscuit surface that this process silico briquette, which melts, is penetrated into inside biscuit under capillary force action from biscuit surface, with Biscuit material reacts and densifies, and completes sintering process, obtains B4C/TiB2Layered composite ceramic material.
When using B in step (1)4C powder and carbon source prepare method when mixed material are as follows: by carbon source, B4C powder and nothing Water-ethanol uniformly mixes, and mixed proportion is by the C element and B in carbon source4The weight ratio of C powder is 9:91, then drying removal nothing B is made in water-ethanol4C/C mixed material；
When using TiB2Powder and carbon source prepare method when mixed material are as follows: by carbon source, TiB2Powder and dehydrated alcohol are equal Even mixing, mixed proportion is by the C element and TiB in carbon source2The weight ratio of powder is 3:17, then drying removal dehydrated alcohol, TiB is made2/ C mixed material；
When using B4C/TiB2Mixed powder and carbon source prepare method when mixed material are as follows: by carbon source, B4C powder, TiB2 Powder and dehydrated alcohol uniformly mix, and mixed proportion is by the C element and B in carbon source4C powder adds TiB2The total weight ratio of powder is 1:6~9, then drying removal dehydrated alcohol, is made B4C/TiB2/ C mixed material.
Step (2) described die forming method are as follows: according to target layered composite ceramic material structure is layered filler, at last Before layer filler, the equal first preliminary consolidation at 50~100MPa after each layer filler, after carrying out the last layer filler, 200~ It is pressed and molded under 300MPa, keeps each thickness degree identical.
B described in step (1)4C powder granularity D50It is 3.5~45 μm, TiB2Powder granularity D50It is 2.9~104 μm.
Above-mentioned carbon source selects alcohol-soluble phenolic resin.
Above-mentioned drying removal dehydrated alcohol refers to 48~240h of drying under the conditions of 50~60 DEG C.
Vacuum degree≤100Pa when infiltration in vacuum is carried out in the above method.
Above-mentioned B4C/TiB2The phase composition of layered composite ceramic material is B12(C,Si,B)3、B13C2、TiB2, SiC and Si.
Above-mentioned B4C/TiB2The Vickers hardness of layered composite ceramic material in 20~25GPa, bending strength 135~ 213MPa, fracture toughness is in 3.2~3.8MPam1/2, for apparent porosity 0.3~0.4%, bulk density is 2.8~3.0g/ cm3, relative density is 98.63~99.72%.
The principle of the present invention is penetrated into and is contained under the action of capillary force using the liquid-state silicon impregnant with reactivity The porous laminated biscuit of carbon, and reacted with wherein carbon and generate silicon carbide, impregnant fills original stomata in stratiform biscuit, and makes Good combination is realized in each bed boundary, completes densification process.Method and step of the invention is simple, temperature requirement is low, in lower system The B that consistency is high, comprehensive mechanical property is excellent can be obtained under conditions of standby cost4C/TiB2Layered composite ceramic material is being made Sample change in size < 0.1% during standby belongs to net-shape-sinter；And method of the invention is able to produce various shape complexity Product, be easy in B4C/TiB2Layered composite ceramic material manufacturing field promotes and applies.
Detailed description of the invention
Fig. 1 is the B prepared in the embodiment of the present invention4C/TiB2Layered composite ceramic material X-ray diffractogram, (1) is in figure The product of embodiment 3, (2) are the product of embodiment 4, and (3) are the product of embodiment 5；
Fig. 2 is the B in the embodiment of the present invention4C/TiB2The B of layered composite ceramic material4C layers of stereoscan photograph figure and The EDS constituent analysis figure in each region, (a) is B in figure4C/TiB2The B of layered composite ceramic material4C layers of stereoscan photograph figure, It (b) is B4C/TiB2The B of layered composite ceramic material4C/TiB2Layer stereoscan photograph figure (c) is B4C/TiB2Lamellar composite pottery The TiB of ceramic material2Layer stereoscan photograph figure, (d) the EDS constituent analysis figure for being region I are (e) the EDS ingredient of region II point Analysis figure, (f) the EDS constituent analysis figure for being region Ш are (g) the EDS constituent analysis figure in region IV；
Fig. 3 is the B of the embodiment of the present invention 34C/TiB2Layered composite ceramic scanning of materials electromicroscopic photograph figure, (a) is in figure B4C/TiB2The stereoscan photograph figure of two layers of interface of layered composite ceramic material (b) is B4C layers of stereoscan photograph figure, It (c) is TiB2The stereoscan photograph figure of layer；
Fig. 4 is the B of the embodiment of the present invention 44C/TiB2Layered composite ceramic scanning of materials electromicroscopic photograph figure, (a) is in figure B4C/TiB2Stereoscan photograph figure at three bed boundary of layered composite ceramic material (b) is B4C layers of stereoscan photograph figure, It (c) is B4C/TiB2The stereoscan photograph figure of layer (d) is TiB2The stereoscan photograph figure of layer.
Fig. 5 is the B of the embodiment of the present invention 54C/TiB2Layered composite ceramic scanning of materials electromicroscopic photograph figure, (a) is in figure B4C/TiB2Stereoscan photograph figure at four bed boundary of layered composite ceramic material (b) is B4C layers of stereoscan photograph figure, (c) and (d) is B4C/TiB2The stereoscan photograph figure of layer (e) is TiB2The stereoscan photograph figure of layer.
Specific embodiment
The B used in the embodiment of the present invention4C powder weight purity > 98%, granularity D50It is 3.5~45 μm；The TiB of use2 Powder weight purity > 98%, granularity D50It is 2.9~104 μm.
The phenolic resin used in the embodiment of the present invention is technical grade product.
Carbon source, B in the embodiment of the present invention4C powder, TiB2The mixing of powder and dehydrated alcohol is by the way of mechanical mixture.
The equipment that compression moulding uses in the embodiment of the present invention is WE-10A type universal hydraulic testing machine.
The equipment that infiltration uses in the embodiment of the present invention is graphite vacuum heating furnace.
The test method of Vickers hardness is Vickers identation hardness method in the embodiment of the present invention, hard using 450SVD Vickers Degree meter.
The test method of bending strength is three-point bending resistance intensity method in the embodiment of the present invention, using electronic universal stretching-machine.
The test method of fracture toughness is SENB method in the embodiment of the present invention, using electronic universal stretching-machine.
The test method of split shed of the embodiment of the present invention porosity and bulk density uses Archimedes's drainage.
The method of drying removal dehydrated alcohol refers to 48~240h of drying under the conditions of 50~60 DEG C in the embodiment of the present invention.
Embodiment 1
It is 14%3.5 μm by ratio, 43%10 μm, 14%20 μm, 29%45 μm of B4C powder and carbon source and dehydrated alcohol It is uniformly mixed, mixed proportion is that carbon content accounts for B4The 9.9% of C powder total weight, by ratio be 70%104 μm, 15%25 μm, 15%104 μm of TiB2Powder is uniformly mixed with carbon source and dehydrated alcohol, and mixed proportion is that carbon content accounts for TiB2Powder total weight 17.6%, grinding granulation will be carried out after the sufficiently dry removal dehydrated alcohol of two kinds of mixtures, then be sieved, chooses granularity 24 The part of~60 mesh is as molding material, first by appropriate B4C/C mixed material is put into mold, under the pressure of 50MPa just Step compacting, then by appropriate TiB2/ C mixed material is put into mold, is pressed and molded, is made after molding two layers under the pressure of 200MPa The thickness of mixed material is identical, and 3h carbonization is then kept the temperature under 700 DEG C of vacuum conditions, obtains B4C/C-TiB2/ C bilayer biscuit；
Carbon source is the alcohol-soluble phenolic resin that C content is 42wt.%；
By B4C/C-TiB2/ C bilayer biscuit is as skeleton, using Si as infiltrant, carries out infiltration in vacuum, and when infiltration is true Reciprocal of duty cycle≤100Pa, infiltration process are first to be warming up to 1350 DEG C with the speed of 5 DEG C/min, then be warming up to the speed of 0.8 DEG C/min 1500 DEG C, 30min is kept the temperature, obtains B4C/TiB2Two-layer compound ceramic material；
B4C/TiB2The phase composition of two-layer compound ceramic material is B12(C,Si,B)3、B13C2、TiB2, SiC and Si；
B4C/TiB2The Vickers hardness of two-layer compound ceramic material, B4C layers are 24.1GPa, TiB2Layer is 20.3GPa, bending resistance Intensity 156.7MPa, fracture toughness 3.40MPam1/2, apparent porosity 0.40%, bulk density 2.92g/cm3, relative density 99.72%.
In conjunction with XRD and EDS composition analysis result, in the B of different layer structures design4C/TiB2Laminar composite scanning In electromicroscopic photograph, black region I is B in Fig. 24C phase, gray area II are TiB2Particle, dark gray areas III are SiC phase, shallowly Gray area IV is using Si as the mixed phase of the Si of main phase and SiC.As seen from the figure, material structure even compact, pore-free and its Its defect exists, meanwhile, layer structure interface is tightly combined, it ensure that B4C/TiB2Layered composite ceramic material is excellent Mechanical property.
Embodiment 2
It is 14%3.5 μm by ratio, 43%10 μm, 14%20 μm, 29%45 μm of B4C powder and carbon source and dehydrated alcohol It is uniformly mixed, mixed proportion is that carbon content accounts for B4The 9.9% of C powder total weight；By ratio be 70%104 μm, 15%25 μm, 15%104 μm of TiB2Powder is uniformly mixed with carbon source and dehydrated alcohol, and mixed proportion is that carbon content accounts for TiB2Powder total weight 17.6%；The B for being 3.5 μm by partial size4C powder and 5 μm of TiB2Powder is uniformly mixed with carbon source and dehydrated alcohol, mixed proportion B is accounted for for carbon content4C powder and TiB2The 13.6% of powder total weight, wherein B4C powder and TiB2The weight ratio of powder is 1:1. Grinding granulation will be carried out after the sufficiently dry removal dehydrated alcohol of three kinds of mixtures, then be sieved, chooses granularity in 24~60 mesh Part as molding material, first by appropriate B4C/C mixed material is put into mold, the preliminary consolidation under the pressure of 50MPa, Again by appropriate B4C/TiB2/ C mixed material is put into mold, is compacted under the pressure of 75MPa, finally by appropriate TiB2/ C mixing Material is put into mold, is pressed and molded under the pressure of 250MPa, is made the thickness of three layers of mixed material identical after molding, is then existed 3h carbonization is kept the temperature under 750 DEG C of vacuum conditions, obtains B4C/C-B4C/TiB2/C-TiB2Tri- laminin base of/C；
Carbon source is the alcohol-soluble phenolic resin that C content is 48wt.%；
By B4C/C-B4C/TiB2/C-TiB2It is molten to carry out vacuum using Si as infiltrant as skeleton for tri- laminin base of/C It seeps, vacuum degree≤100Pa when infiltration, infiltration process is first to be warming up to 1350 DEG C with the speed of 5 DEG C/min, then with 1 DEG C/min's Speed is warming up to 1550 DEG C, keeps the temperature 45min, obtains B4C/TiB2Three layers of composite ceramic material；
B4C/TiB2The phase composition of three layers of composite ceramic material is B12(C,Si,B)3、B13C2、TiB2, SiC and Si；
B4C/TiB2The Vickers hardness of three layers of composite ceramic material, B4C layers are 24.1GPa, TiB2Layer is 20.3GPa, intermediate Layer is 21.9GPa, bending strength 182.5MPa, fracture toughness 3.31MPam1/2, apparent porosity is 0.34%, bulk density For 2.91g/cm3, relative density 99.38%.
Embodiment 3
The B for being 3.5 μm by partial size4C powder is uniformly mixed with carbon source and dehydrated alcohol, and mixed proportion is that carbon content accounts for B4C powder The 9.9% of last total weight, the TiB for being 5 μm by partial size2Powder is uniformly mixed with carbon source and dehydrated alcohol, and mixed proportion contains for carbon Amount accounts for TiB2The 17.6% of powder total weight will carry out grinding granulation after the sufficiently dry removal dehydrated alcohol of two kinds of mixtures, then It is sieved, chooses granularity in the part of 24~60 mesh as molding material, first by appropriate B4C/C mixed material is put into mold In, the preliminary consolidation under the pressure of 50MPa, then by appropriate TiB2/ C mixed material is put into mold, under the pressure of 200MPa Compression molding, makes the thickness of two layers of mixed material identical after molding, 3h carbonization is then kept the temperature under 700 DEG C of vacuum conditions, is obtained B4C/C-TiB2/ C bilayer biscuit；
Carbon source is the alcohol-soluble phenolic resin that C content is 42wt.%；
By B4C/C-TiB2/ C bilayer biscuit is as skeleton, using Si as infiltrant, carries out infiltration in vacuum, and when infiltration is true Reciprocal of duty cycle≤100Pa, infiltration process are first to be warming up to 1350 DEG C with the speed of 5 DEG C/min, then be warming up to the speed of 0.8 DEG C/min 1500 DEG C, 30min is kept the temperature, obtains B4C/TiB2Two-layer compound ceramic material；
B4C/TiB2The phase composition of two-layer compound ceramic material is B12(C,Si,B)3、B13C2、TiB2, SiC and Si；
B4C/TiB2The Vickers hardness of two-layer compound ceramic material, B4C layers are 22.1GPa, TiB2Layer is 20.1GPa, bending resistance Intensity 142.2MPa, fracture toughness 3.30MPam1/2, apparent porosity 0.43%, bulk density 2.89g/cm3, relative density 99.52%.
Embodiment 4
The B for being 3.5 μm by partial size4C powder is uniformly mixed with carbon source and dehydrated alcohol, and mixed proportion is that carbon content accounts for B4C powder The 9.9% of last total weight；The TiB for being 5 μm by partial size2Powder is uniformly mixed with carbon source and dehydrated alcohol, and mixed proportion contains for carbon Amount accounts for TiB2The 17.6% of powder total weight；The B for being 3.5 μm by partial size4C powder and 5 μm of TiB2Powder and carbon source and anhydrous second Alcohol is uniformly mixed, and mixed proportion is that carbon content accounts for B4C powder and TiB2The 13.6% of powder total weight, wherein B4C powder and TiB2 The weight ratio of powder is 1:1.Grinding granulation will be carried out after the sufficiently dry removal dehydrated alcohol of three kinds of mixtures, then is sieved, Granularity is chosen in the part of 24~60 mesh as molding material, first by appropriate B4C/C mixed material is put into mold, Preliminary consolidation under the pressure of 50MPa, then by appropriate B4C/TiB2/ C mixed material is put into mold, is pushed in the pressure of 75MPa It is real, finally by appropriate TiB2/ C mixed material is put into mold, is pressed and molded under the pressure of 250MPa, makes three layers to mix after molding The thickness for closing material is identical, and 3h carbonization is then kept the temperature under 750 DEG C of vacuum conditions, obtains B4C/C-B4C/TiB2/C-TiB2/ C tri- Laminin base；
Carbon source is the alcohol-soluble phenolic resin that C content is 48wt.%；
By B4C/C-B4C/TiB2/C-TiB2It is molten to carry out vacuum using Si as infiltrant as skeleton for tri- laminin base of/C It seeps, vacuum degree≤100Pa when infiltration, infiltration process is first to be warming up to 1350 DEG C with the speed of 5 DEG C/min, then with 1 DEG C/min's Speed is warming up to 1550 DEG C, keeps the temperature 45min, obtains B4C/TiB2Three layers of composite ceramic material；
B4C/TiB2The phase composition of three layers of composite ceramic material is B12(C,Si,B)3、B13C2、TiB2, SiC and Si；
B4C/TiB2The Vickers hardness of three layers of composite ceramic material, B4C layers are 23.2GPa, TiB2Layer is 20.7GPa, intermediate Layer is 22.1GPa, bending strength 162.5MPa, fracture toughness 3.27MPam1/2, apparent porosity is 0.35%, bulk density For 2.90g/cm3, relative density 99.31%.
Embodiment 5
It is 3.5 μm of B by partial size4C powder is uniformly mixed with carbon source and dehydrated alcohol, and mixed proportion is that carbon content accounts for B4C powder The 9.9% of total weight；It is 5 μm of TiB by partial size2Powder is uniformly mixed with carbon source and dehydrated alcohol, and mixed proportion accounts for for carbon content TiB2The 17.6% of powder total weight；It is 3.5 μm of B by partial size4C powder and partial size are 5 μm of TiB2Powder and carbon source and dehydrated alcohol It is uniformly mixed, mixed proportion is that carbon content accounts for B4C powder and TiB2The 12.4% of powder total weight, wherein B4C powder and TiB2Powder The weight ratio at end is 2:1, is 3.5 μm of B by partial size4C powder and partial size are 5 μm of TiB2Powder mixes with carbon source and dehydrated alcohol Even, mixed proportion is that carbon content accounts for B4C powder and TiB2The 14.9% of powder total weight, wherein B4C powder and TiB2The weight of powder Amount is than being 1:2.Grinding granulation will be carried out after the sufficiently dry removal dehydrated alcohol of four kinds of mixtures, then be sieved, chooses granularity In the part of 24~60 mesh as molding material, first by appropriate B4C/C mixed material is put into mold, in the pressure of 50MPa Lower preliminary consolidation, then by appropriate B4C powder and TiB2The weight ratio of powder is the B of 2:14C/TiB2/ C mixed material is put into mold, It is compacted under the pressure of 75MPa, then by appropriate B4C powder and TiB2The weight ratio of powder is the B of 1:24C/TiB2/ C mixed material It is put into mold, is equally compacted under the pressure of 100MPa, finally by appropriate TiB2/ C mixed material is put into mold, It is finally pressed and molded under the pressure of 300MPa, makes the thickness of four layers of mixed material identical after molding, then in 800 DEG C of vacuum conditions Lower heat preservation 3h carbonization, obtains B4C/C-B4C/TiB2/C-B4C/TiB2/C-TiB2Tetra- laminin base of/C；
Carbon source is the alcohol-soluble phenolic resin that C content is 52wt.%；
By B4C/C-B4C/TiB2/C-B4C/TiB2/C-TiB2Tetra- laminin base of/C is as skeleton, using Si as infiltrant, Carry out infiltration in vacuum, vacuum degree≤100Pa when infiltration, infiltration process be first be warming up to 1350 DEG C with the speed of 5 DEG C/min, then with The speed of 1.2 DEG C/min is warming up to 1600 DEG C, keeps the temperature 60min, obtains B4C/TiB2Four layers of composite ceramic material；
B4C/TiB2The phase composition of four layers of composite ceramic material is B12(C,Si,B)3、B13C2、TiB2, SiC and Si；
B4C/TiB2The Vickers hardness of four layers of composite ceramic material, B4C layers are 24.1GPa, TiB2Layer is 20.3GPa, intermediate Layer is respectively 21.5GPa and 23.2GPa, bending strength 212.6MPa, fracture toughness 3.71MPam1/2, apparent porosity exists 0.37%, bulk density 2.81g/cm3, relative density 98.63%.

Claims (9)

1. a kind of B4C/TiB2The preparation method of layered composite ceramic material, which is characterized in that comprise the following steps that
(1) by B4C powder, TiB2Powder or B4C/TiB2Mixed powder is uniformly mixed with carbon source in proportion, and mixed proportion contains for carbon Amount accounts for the 9~18% of mixed powder total weight, and the mixed material of different target structure sheaf is made, by the mixed of different target structure sheaf It closes material to be sieved respectively, chooses particle molding material as each object construction layer of the granularity between 24~60 mesh；
(2) by the molding material of each object construction layer according to target layered composite ceramic material structure be layered filler, die forming, then It is carbonized at 700-800 DEG C, obtains B4C/TiB2/ C stratiform biscuit；
(3) by B4C/TiB2/ C stratiform biscuit carries out infiltration in vacuum using Si as infiltrant as skeleton, and infiltration process is first 1350 DEG C are warming up to, be then warming up to 1500~1600 DEG C with the speed of 0.8~1.2 DEG C/min and keeps the temperature 30~60min, is obtained B4C/TiB2Layered composite ceramic material.
2. a kind of B according to claim 14C/TiB2The preparation method of layered composite ceramic material, which is characterized in that step Suddenly when using B in (1)4C powder and carbon source prepare method when mixed material are as follows: by carbon source, B4C powder and dehydrated alcohol are uniform Mixing, mixed proportion is by the C element and B in carbon source4The weight ratio of C powder is 9:91, and then drying removal dehydrated alcohol, is made B4C/C mixed material；
When using TiB2Powder and carbon source prepare method when mixed material are as follows: by carbon source, TiB2Powder and dehydrated alcohol uniformly mix It closes, mixed proportion is by the C element and TiB in carbon source2The weight ratio of powder is 3:17, and then drying removal dehydrated alcohol, is made TiB2/ C mixed material；
When using B4C/TiB2Mixed powder and carbon source prepare method when mixed material are as follows: by carbon source, B4C powder, TiB2Powder It is uniformly mixed with dehydrated alcohol, mixed proportion is by the C element and B in carbon source4C powder adds TiB2The total weight ratio of powder be 1:6~ 9, then drying removal dehydrated alcohol, is made B4C/TiB2/ C mixed material.
3. a kind of B according to claim 1 or 24C/TiB2The preparation method of layered composite ceramic material, which is characterized in that Step (2) described die forming method are as follows: according to target layered composite ceramic material structure be layered filler, the last layer filler it Before, the first preliminary consolidation at 50~100MPa after each layer filler, after carrying out the last layer filler, in 200~300MPa lower die It is molded, keep each thickness degree identical.
4. a kind of B according to claim 1 or 24C/TiB2The preparation method of layered composite ceramic material, which is characterized in that B described in step (1)4C powder granularity D50It is 3.5~45 μm, TiB2Powder granularity D50It is 2.9~104 μm.
5. a kind of B according to claim 1 or 24C/TiB2The preparation method of layered composite ceramic material, which is characterized in that The carbon source of the step (1) selects alcohol-soluble phenolic resin.
6. a kind of B according to claim 1 or 24C/TiB2The preparation method of layered composite ceramic material, which is characterized in that Step (3) carries out vacuum degree≤100Pa when infiltration in vacuum.
7. a kind of B according to claim 24C/TiB2The preparation method of layered composite ceramic material, which is characterized in that institute The drying removal dehydrated alcohol stated refers to 48~240h of drying under the conditions of 50~60 DEG C.
8. B made from any preparation method of claim 1-54C/TiB2Layered composite ceramic material, which is characterized in that The B4C/TiB2The Vickers hardness of layered composite ceramic material is in 20~25GPa, and bending strength is in 135~213MPa, fracture Toughness is in 3.2~3.8MPam1/2, for apparent porosity 0.3~0.4%, bulk density is 2.8~3.0g/cm3, relatively close Degree is 98.63~99.72%.
9. B according to claim 84C/TiB2Layered composite ceramic material, which is characterized in that the B4C/TiB2Lamellar composite The phase composition of ceramic material is B12(C,Si,B)3、B13C2、TiB2, SiC and Si.
CN201910520314.7A 2019-06-17 2019-06-17 B4C/TiB2Preparation method of layered composite ceramic material Active CN110282977B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201910520314.7A CN110282977B (en) 2019-06-17 2019-06-17 B4C/TiB2Preparation method of layered composite ceramic material

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201910520314.7A CN110282977B (en) 2019-06-17 2019-06-17 B4C/TiB2Preparation method of layered composite ceramic material

Publications (2)

Publication Number Publication Date
CN110282977A true CN110282977A (en) 2019-09-27
CN110282977B CN110282977B (en) 2021-01-08

Family

ID=68005031

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201910520314.7A Active CN110282977B (en) 2019-06-17 2019-06-17 B4C/TiB2Preparation method of layered composite ceramic material

Country Status (1)

Country Link
CN (1) CN110282977B (en)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111484331A (en) * 2020-04-02 2020-08-04 武汉理工大学 Fine-grain boron-rich boron carbide-based composite ceramic material and preparation method thereof
CN111499385A (en) * 2020-03-19 2020-08-07 武汉理工大学 Boron carbide-graphene micro-laminated composite material and preparation method thereof
CN111777427A (en) * 2020-06-24 2020-10-16 清华大学 Preparation method of nacre-like layered high-strength super-tough ceramic
CN113173790A (en) * 2021-06-02 2021-07-27 哈尔滨工业大学 B4C-TiB2BN layered ceramic material and preparation method thereof
CN113582700A (en) * 2021-06-29 2021-11-02 东北大学 Preparation method of low-cost titanium boride ceramic composite material

Citations (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3808012A (en) * 1971-04-19 1974-04-30 Carborundum Co Dense composite ceramic bodies
CN102886942A (en) * 2011-07-19 2013-01-23 东北大学 Layered composite boron carbide ceramic material and its preparation method
WO2014110478A1 (en) * 2013-01-14 2014-07-17 Coi Ceramics, Inc. Methods of forming ceramic matrix composite structures, apparatuses for forming ceramic matrix composite structures, and ceramic matrix composite structures
CN105084902A (en) * 2015-07-31 2015-11-25 东北大学 Method for preparing titanium-diboride-based ceramic composite material
EP3061603A1 (en) * 2015-02-27 2016-08-31 General Electric Company Cmc laminate structure fabricated using chemical vapor infiltration (cvi)
CN106278281A (en) * 2016-08-16 2017-01-04 东北大学 A kind of boronation titanio composite cathode material and preparation method thereof
CN107117981A (en) * 2017-05-19 2017-09-01 北京理工大学 A kind of stratiform Ti/B4C composite and preparation method thereof
CN107500769A (en) * 2017-08-22 2017-12-22 巩义市泛锐熠辉复合材料有限公司 A kind of C/TiB2The surface treatment method of composite
CN108439990A (en) * 2018-05-11 2018-08-24 东北大学 A kind of titanium diboride based composite ceramic material and preparation method thereof
CN108610052A (en) * 2018-05-17 2018-10-02 广东工业大学 A kind of titanium diboride base complex phase ceramic and its preparation method and application
CN109081697A (en) * 2018-08-28 2018-12-25 东北大学 It is a kind of to prepare B4The method of C/SiC composite ceramic
CN109824363A (en) * 2017-11-23 2019-05-31 陈瑞凯 Toughness pottery material

Patent Citations (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3808012A (en) * 1971-04-19 1974-04-30 Carborundum Co Dense composite ceramic bodies
CN102886942A (en) * 2011-07-19 2013-01-23 东北大学 Layered composite boron carbide ceramic material and its preparation method
WO2014110478A1 (en) * 2013-01-14 2014-07-17 Coi Ceramics, Inc. Methods of forming ceramic matrix composite structures, apparatuses for forming ceramic matrix composite structures, and ceramic matrix composite structures
EP3061603A1 (en) * 2015-02-27 2016-08-31 General Electric Company Cmc laminate structure fabricated using chemical vapor infiltration (cvi)
CN105084902A (en) * 2015-07-31 2015-11-25 东北大学 Method for preparing titanium-diboride-based ceramic composite material
CN106278281A (en) * 2016-08-16 2017-01-04 东北大学 A kind of boronation titanio composite cathode material and preparation method thereof
CN107117981A (en) * 2017-05-19 2017-09-01 北京理工大学 A kind of stratiform Ti/B4C composite and preparation method thereof
CN107500769A (en) * 2017-08-22 2017-12-22 巩义市泛锐熠辉复合材料有限公司 A kind of C/TiB2The surface treatment method of composite
CN109824363A (en) * 2017-11-23 2019-05-31 陈瑞凯 Toughness pottery material
CN108439990A (en) * 2018-05-11 2018-08-24 东北大学 A kind of titanium diboride based composite ceramic material and preparation method thereof
CN108610052A (en) * 2018-05-17 2018-10-02 广东工业大学 A kind of titanium diboride base complex phase ceramic and its preparation method and application
CN109081697A (en) * 2018-08-28 2018-12-25 东北大学 It is a kind of to prepare B4The method of C/SiC composite ceramic

Non-Patent Citations (5)

* Cited by examiner, † Cited by third party
Title
MENGYONG SUN等: ""Structural design of laminated B4C/TiC composite fabricated by"", 《JOURNAL OF ALLOYS AND COMPOUNDS》 *
XINYAN YUE等: ""Synthesis of B4C/Al-B4C/TiB2 Composite with a Two-Layer Structure"", 《ADVANCED MATERIALS RESEARCH》 *
ZAKI ISMAIL ZAKI: ""Combustion synthesis of mullite–titanium boride composite"", 《CERAMICS INTERNATIONAL》 *
刘维良等: ""B4C/TiB2层状复合陶瓷的制备与性能研究"", 《中国陶瓷》 *
张翠萍等: ""纳米 SiC 颗粒增强反应结合碳化硼陶瓷复合材料的研究"", 《稀有金属材料与工程》 *

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111499385A (en) * 2020-03-19 2020-08-07 武汉理工大学 Boron carbide-graphene micro-laminated composite material and preparation method thereof
CN111499385B (en) * 2020-03-19 2021-03-16 武汉理工大学 Boron carbide-graphene micro-laminated composite material and preparation method thereof
CN111484331A (en) * 2020-04-02 2020-08-04 武汉理工大学 Fine-grain boron-rich boron carbide-based composite ceramic material and preparation method thereof
CN111777427A (en) * 2020-06-24 2020-10-16 清华大学 Preparation method of nacre-like layered high-strength super-tough ceramic
CN113173790A (en) * 2021-06-02 2021-07-27 哈尔滨工业大学 B4C-TiB2BN layered ceramic material and preparation method thereof
CN113582700A (en) * 2021-06-29 2021-11-02 东北大学 Preparation method of low-cost titanium boride ceramic composite material

Also Published As

Publication number Publication date
CN110282977B (en) 2021-01-08

Similar Documents

Publication Publication Date Title
CN110282977A (en) A kind of B4C/TiB2The preparation method of layered composite ceramic material
CN102464490B (en) Method for preparing boron-carbide-based ceramic composite material
Meyers et al. Direct laser sintering of reaction bonded silicon carbide with low residual silicon content
JP3096716B1 (en) Method for producing fiber-reinforced silicon carbide composite
Perevislov et al. High density boron carbide ceramics
CN105084902A (en) Method for preparing titanium-diboride-based ceramic composite material
CN102219536B (en) B4C/SiC whisker/SiC multiphase ceramic matrix composite and preparation method thereof
CN1600742A (en) Compact foamy thyrite in high intensity and preparation method
JP2006290670A (en) Fiber reinforced silicon carbide composite material, and method of manufacturing the same
CN110317073A (en) A kind of preparation method of multistage fiber coordination plasticizing oxidation-resistant ceramic based composites
CN109851362B (en) SiC prepared by 3D formingfMethod for preparing/SiC ceramic composite material
CN110304923B (en) Preparation method of boron carbide-based ceramic composite material based on particle grading
CN103771859B (en) Silicon carbide/tungsten boride composite material and preparation method thereof
CN112592194A (en) C/HfC-ZrC-SiC superhigh temperature ceramic matrix composite and preparation method thereof
CN100418923C (en) Compact Ti2AlC-TiB2 composite material and preparation method therefor
CN114736022B (en) High-density, high-strength and ultrahigh-hardness boron carbide/high-entropy diboride complex phase ceramic and preparation method thereof
CN113233899A (en) B4B4C-SiC-Si composite material generated by siliconizing reaction of C/graphite preform and preparation method thereof
CN113582700B (en) Preparation method of low-cost titanium boride ceramic composite material
CN108101543A (en) A kind of silicon carbide-based carbon ceramic friction material and its molding preparation method
CN117658641A (en) Method for preparing high-density SiC ceramic based on selective laser 3D printing and two-step sintering
CN108439990A (en) A kind of titanium diboride based composite ceramic material and preparation method thereof
JP2019189500A (en) Method for producing diamond/silicon carbide composite with improved hardness and such composite
JP5168451B2 (en) Method for producing porous molded body and method for producing porous filled molded body
CN109665847A (en) A kind of complete fine and close boron carbide ceramic composite and preparation method
JPS63288974A (en) Production of fiber reinforced ceramics

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant