CN107117981A - A kind of stratiform Ti/B4C composite and preparation method thereof - Google Patents

A kind of stratiform Ti/B4C composite and preparation method thereof Download PDF

Info

Publication number
CN107117981A
CN107117981A CN201710357463.7A CN201710357463A CN107117981A CN 107117981 A CN107117981 A CN 107117981A CN 201710357463 A CN201710357463 A CN 201710357463A CN 107117981 A CN107117981 A CN 107117981A
Authority
CN
China
Prior art keywords
composite
stratiform
layers
sintering
thin slices
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
CN201710357463.7A
Other languages
Chinese (zh)
Other versions
CN107117981B (en
Inventor
李云凯
吴超
程兴旺
张朝晖
陈义文
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.)
Beijing Institute of Technology BIT
Original Assignee
Beijing Institute of Technology BIT
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 Beijing Institute of Technology BIT filed Critical Beijing Institute of Technology BIT
Priority to CN201710357463.7A priority Critical patent/CN107117981B/en
Publication of CN107117981A publication Critical patent/CN107117981A/en
Application granted granted Critical
Publication of CN107117981B publication Critical patent/CN107117981B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/71Ceramic products containing macroscopic reinforcing agents
    • C04B35/74Ceramic products containing macroscopic reinforcing agents containing shaped metallic materials
    • C04B35/76Fibres, filaments, whiskers, platelets, or the like
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515Shaped 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
    • C04B35/56Shaped 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
    • C04B35/563Shaped 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
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/40Metallic constituents or additives not added as binding phase
    • C04B2235/404Refractory metals
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/54Particle size related information
    • C04B2235/5418Particle size related information expressed by the size of the particles or aggregates thereof
    • C04B2235/5436Particle size related information expressed by the size of the particles or aggregates thereof micrometer sized, i.e. from 1 to 100 micron
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/74Physical characteristics
    • C04B2235/77Density
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96Properties 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)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Ceramic Products (AREA)
  • Powder Metallurgy (AREA)

Abstract

The present invention relates to a kind of stratiform Ti/B4C composite and preparation method thereof, belongs to metal enhancing ceramic composite technical field.The composite is by Ti layers and B4C layers are alternately formed by stacking successively, due to Ti and B4C has different thermal coefficient of expansions and modulus of elasticity, so that crack deflection occurs when crackle extends in the composite and energy to failure is gradually used up, is beneficial to improve fracture of composite materials toughness;In addition, by adding a small amount of Al, boundary strength can be improved, so as to improve the mechanical property for meeting material;Furthermore, utilize Ti layers and B4The mode of C interlayers particle-surface contact reduces Ti layers and B4Interfacial reaction degree between C layers.The method of the invention technique is simple, it is easy to operate, with good prospects for commercial application;And the stratiform Ti/B prepared4C composite microstructure is good, the porosity is relatively low and good mechanical property.

Description

A kind of stratiform Ti/B4C composite and preparation method thereof
Technical field
The present invention relates to a kind of stratiform Ti/B4C composite and preparation method thereof, belongs to metal enhancing ceramic composite Technical field.
Background technology
B4C ceramics have low-density (2.52g/cm3), high rigidity (27.5GPa~49.5GPa), high-wearing feature, extensive chemical The features such as stability and excellent neutron-absorbing, it is widely studied in recent years and is gradually applied to Protective armor, engineering knot The field such as component and nuclear industry.But, due to B4Covalent linkage content reaches 93.94% in C, causes it compared to other ceramic materials Material possesses higher sintering temperature and worse fracture toughness, so as to seriously limit boron carbide ceramics in engineering field and army The extensive use in work field.
Proposing first for ceramic layered based composites is in nineteen ninety《Nature》Magazine (Clegg W J, Kendall K,Alford N M,et al.A simple way to make tough ceramics[J].Nature, 1990, 347(4):455-457.), it is method using graphite linings as ductile layers toughness reinforcing SiC ceramic.Then with research by Step is carried out, and occurs in that many laminated ceramic composites, wherein most of is ceramic to ceramic laminar composite, but due to it Each layer is fragile material so that toughening effect is not obvious.The proposition of metal-ceramic laminate composite is built upon intensity Ceramic layer and ductile metal layer mutually overlap, proposed on the basis of supplying each other, but be due between metal and ceramics Often with uncontrollable interfacial reaction in sintering process, and the stability of interlayer is influenceed, thus laminated metal-ceramic composite Still it is in conceptual phase.
Metal Ti is a kind of light weight and stable magnesium-yttrium-transition metal, is commonly applied under aviation field and harsh Service Environment. In recent years, metal Ti is used as enhancing and the toughness reinforcing phase of ceramic material, but because it has stronger reproducibility, thus pole Easily reacted with ceramics, so that substantial amounts of Ti compounds are generated, so as to influence the overall performance of composite.
The content of the invention
Easily reacted for Ti in the prior art with ceramic material, so as to influence Ti to strengthen ceramic composite performance Problem, an object of the present invention is to provide a kind of stratiform Ti/B4C composite, the composite is by Ti toughening layers and B4C Strength layer is alternately formed by stacking, Ti layers and B4C interlayers can cause crack deflection in fracture so that the composite possesses excellent Different fracture toughness.
The second object of the present invention is to provide a kind of stratiform Ti/B4The preparation method of C composite, this method utilizes Ti Layer and B4The mode of C interlayers particle-surface contact instead of the pattern that conventional uniform bulk material is integrally contacted so that Ti and B4C it Between interfacial reaction degree reduction, while the interface dispersal behavior of interlayer can cause Ti layers and B4C layers are tightly combined, so as to carry The mechanical property of high composite;Moreover, methods described technique is simple, it is easy to operate, with good prospects for commercial application.
The purpose of the present invention is achieved through the following technical solutions.
A kind of stratiform Ti/B4C composite, the composite is by Ti layers and B4C layers are alternately formed by stacking successively;Wherein, Every a Ti layers of thickness is 0.2mm~0.4mm, every B4C layers of thickness is the mm of 0.4mm~0.8.
Further, Al is also contained in the composite, Al can produce liquid as sintering aid in sintering process Phase, so as to promote the interface bond strength of ceramic layer and metal level;Al quality and Ti mass ratio are 4~8:100, and Al exists Mass fraction in the composite is no more than 3%.
A kind of stratiform Ti/B of the present invention4The preparation method of C composite, methods described step is as follows:
(1) stratiform Ti/B is prepared4C composite green compact
(a) when being not added with Al:Using polyvinyl alcohol as binding agent, respectively by titanium valve, B4The progress of C powders is dry-pressing formed, accordingly Ground obtains the B that the Ti thin slices and thickness that thickness is 0.2mm~0.4mm are 0.4mm~0.8mm4C thin slices, then by Ti thin slices with And B4C thin slices are alternately superimposed successively, obtain stratiform Ti/B4The green compact of C composite;
(b) when adding Al:Titanium valve, aluminium powder, absolute ethyl alcohol and polyethylene glycol are first subjected to wet ball grinding mixing, then by ball Slurry after mill is placed under vacuum condition and dried, and obtains Al/Ti mixed powders;Using polyvinyl alcohol as binding agent, respectively by Al/Ti Mixed powder, B4C powders carry out it is dry-pressing formed, be correspondingly made available thickness for 0.2mm~0.4mm and adulterate Al Ti thin slices and Thickness is 0.4mm~0.8mm B4C thin slices, then by Ti thin slices and B4C thin slices are alternately superimposed successively, obtain stratiform Ti/B4C is answered The green compact of condensation material;
(2) vacuum heating-press sintering
By stratiform Ti/B4The green compact of C composite, which are placed in vacuum sintering funace, carries out vacuum heating-press sintering, cooling, Obtain layered Ti/B4C composite;
Dry-pressing formed pressure is 10MPa~30MPa, and the dwell time is 5min~10min;
Vacuum in vacuum sintering funace is not less than 6.63 × 10-3Pa, 1700 DEG C~1800 DEG C of sintering temperature, sintering Pressure 20MPa~30MPa, sintering time 1h~2h.
Preferably 5 μm~10 μm of the average grain diameter of titanium valve, preferably 1 μm of the average grain diameter of aluminium powder~3 μm, B4C powders are averaged Preferably 3 μm~5 μm of particle diameter.
Beneficial effect:
(1) proposed in the present invention using metal Ti as toughening layer, with ceramic B4C makes Ti layers and B as strength layer4C layers Between successively alternately be superimposed and sinter and the Ti/B of layered4C composite, the Ti layers and high-strength B of high-ductility4C layers are arranged alternately, And Ti and B4C has different thermal coefficient of expansions and modulus of elasticity, so that when stratified material extends crackle occurs for crackle Deflect and gradually use up energy to failure, extend crack extending length, be beneficial to stratiform Ti/B4C composite fracture toughness is carried It is high;
(2) in preparation process of the present invention, Ti layers and B are utilized4The mode of C interlayers particle-surface contact instead of conventional uniform block The pattern that shape material is integrally contacted, so as to reduce Ti layers and B4Interfacial reaction degree between C layers;Further, since Ti and Al tools There is stronger reproducibility, this makes Ti/B4Elements diffusion phenomenon occurs at C interface layers, while generating such as TiB2, TiAlX and Al8B4C7Interfacial reaction products, this causes physical bond of the combination between metal and ceramics before sintering to be changed into metallurgical junction Close, its interface bond strength is improved, so as to improve the mechanical property of composite;
(3) the method for the invention technique is simple, it is easy to operate, with good prospects for commercial application;And prepare Stratiform Ti/B4C composite microstructure is good, the porosity is relatively low and good mechanical property.
Brief description of the drawings
Fig. 1 is embodiment laminate Ti/B4X-ray diffraction (XRD) collection of illustrative plates of C composite.
Fig. 2 is embodiment laminate Ti/B4Low power cross-sectional scanning electron microscope (SEM) figure of C composite.
Fig. 3 is the laminate Ti/B of embodiment 14The high power section SEM figures of C composite.
Fig. 4 is the laminate Ti/B of embodiment 14The Crack Extension photo of C composite.
Embodiment
With reference to embodiment, the present invention will be further described.
In following examples:
Titanium valve:Average grain diameter is 5 μm, Shanghai paddy field science and technology;
Aluminium powder:Average grain diameter is 1 μm, Shanghai paddy field science and technology;
B4C powders:Average grain diameter is 3 μm, Shanghai paddy field science and technology;
Polyvinyl alcohol:High polymerization degree PVAl7-92 (molecular weight 170,000), traditional Chinese medicines are controlled interest Tianjin Co., Ltd.
Relative density:Tested using drainage;
Mechanics Performance Testing:Bending strength is tested according to standard GB/T 4741-1999, GB/T GB/T 23806-2009 And fracture toughness;
XRD is characterized:The model D8-ADVANCE of the X-ray diffractometer used, producer:German Bu Luoke electronics;
SEM morphology characterizations:The model S-4800 of the SEM used, producer:Japanese Hitachi is public Department.
Embodiment 1
(1) 50g titanium valves, 3g aluminium powders, 400mL absolute ethyl alcohols and 0.5g polyethylene glycol (molecular weight 4000) are added to ball In grinding jar, according still further to 10:1 ratio of grinding media to material adds ZrO2Ball, then the ball milling 12h under 150r/min rotating speed, then by after ball milling Well mixed slurry, which is placed in 80 DEG C of vacuum drying chambers, dries 8h, obtains Al/Ti mixed powders;
(2) using polyvinyl alcohol as binding agent, respectively to Al/Ti mixed powders, B under 30MPa pressure4C powders are carried out It is dry-pressing formed, after pressurize 10min, be correspondingly made available thickness be 0.2mm and adulterate Al Ti thin slices and thickness be 0.4mm's B4C thin slices, then by Ti thin slices and B4C thin slices are alternately superimposed successively, obtain stratiform Ti/B4The green compact of C composite;
(3) by stratiform Ti/B4The green compact of C composite are placed in vacuum sintering funace, treat vacuum reach 6.63 × 10-3During Pa, 2h is sintered under 1800 DEG C of sintering temperature and 30MPa sintering pressure, furnace cooling obtains layered Ti/B4C composite;Wherein, prepared stratiform Ti/B4Contain the Al that mass fraction is 3% in C composite.
Composite prepared by the present embodiment is characterized:It is 98.2% to measure relative density, and bending strength is 622.3MPa, fracture toughness is 7.88MPam1/2.Understood according in Fig. 1, the principal phase in prepared composite is B4C、 Ti and TiB2, in addition with intermetallic compound TiAlXWith Al-B-C solid solution Al8B4C7, it can be seen that, in sintering process Ti layers and B4C layers there occurs interfacial reaction, generate TiB2, and the Al in Ti layers is also while and B4C there occurs that reaction is generated Al8B4C7, the presence of interfacial product can greatly improve Ti layers and B4The adhesion of C interlayers, improves bond strength.Fig. 2's and Fig. 3 In SEM figures, color is deeper for B4C layers, color is shallower for Ti layers, it follows that toughness in prepared composite Ti layers of metal and high-strength ceramic B4C layers of mutual overlaps form a kind of tough alternate layer structure, and interface is clearly combined Closely.It can determine whether with reference to the result of XRD and SEM figures:Ti layers and B4Physical bond of the combination of C interlayers before sintering is changed into smelting Gold is combined, and improves its interface bond strength.White dashed line in Fig. 4 is crackle in stratiform Ti/B4Propagated in C composite Path, it is seen that crack deflection occurs in primarily in Ti layers and B4At C bed boundarys, this is due to Ti and B4C has different thermal expansion systems Number and modulus of elasticity, so that crackle can occur crack deflection when being extended between stratified material and gradually use up energy to failure, prolong Crack extending length has been grown, and then has made stratiform Ti/B4C composite fracture toughness makes moderate progress.
Embodiment 2
(1) 50g titanium valves, 2g aluminium powders, 400mL absolute ethyl alcohols and 0.5g polyethylene glycol (molecular weight 4000) are added to ball In grinding jar, according still further to 10:1 ratio of grinding media to material adds ZrO2Ball, then the ball milling 12h under 150r/min rotating speed, then by after ball milling Well mixed slurry, which is placed in 80 DEG C of vacuum drying chambers, dries 8h, obtains Al/Ti mixed powders;
(2) using polyvinyl alcohol as binding agent, respectively to Al/Ti mixed powders, B under 10MPa pressure4C powders are carried out It is dry-pressing formed, after pressurize 5min, be correspondingly made available thickness be 0.4mm and adulterate Al Ti thin slices and thickness be 0.8mm's B4C thin slices, then by Ti thin slices and B4C thin slices are alternately superimposed successively, obtain stratiform Ti/B4The green compact of C composite;
(3) by stratiform Ti/B4The green compact of C composite are placed in vacuum sintering funace, treat vacuum reach 6.63 × 10-3During Pa, 2h is sintered under 1800 DEG C of sintering temperature and 30MPa sintering pressure, furnace cooling obtains layered Ti/B4C composite;Wherein, prepared stratiform Ti/B4Contain the Al that mass fraction is 2% in C composite.
Composite prepared by the present embodiment is characterized:It is 97.5% to measure relative density, and bending strength is 601.3MPa, fracture toughness is 7.22MPam1/2.It can be seen from XRD characterizes obtained collection of illustrative plates, in prepared composite Principal phase be B4C, Ti and TiB2, in addition with a small amount of intermetallic compound TiAlXWith Al-B-C solid solution Al8B4C7, these The presence of interfacial product greatly improves Ti layers and B4The adhesion of C interlayers, improves bond strength.Obtained according to morphology characterization SEM is schemed it is known that there is the deeper B of color in prepared composite4C layers and the shallower Ti layers of color, illustrate institute The composite of preparation is Ti layers of the metal of toughness and high-strength ceramic B4C layers alternate the layer structure to be formed successively.Root It may determine that according to XRD and SEM characterization results:Ti layers and B4Physical bond of the combination of C interlayers before sintering is changed into metallurgical junction Close, improve its interface bond strength.Crackle can equally occur when being extended in the composite prepared by the present embodiment Crack deflection and the phenomenon for gradually using up energy to failure, extend crack extending length, and then make stratiform Ti/B4C composite is broken Toughness is split to make moderate progress.
Embodiment 3
(1) 50g titanium valves, 3g aluminium powders, 400mL absolute ethyl alcohols and 0.5g polyethylene glycol (molecular weight 4000) are added to ball In grinding jar, according still further to 10:1 ratio of grinding media to material adds ZrO2Ball, then the ball milling 12h under 150r/min rotating speed, then by after ball milling Well mixed slurry, which is placed in 80 DEG C of vacuum drying chambers, dries 8h, obtains Al/Ti mixed powders;
(2) using polyvinyl alcohol as binding agent, respectively to Al/Ti mixed powders, B under 20MPa pressure4C powders are carried out It is dry-pressing formed, after pressurize 8min, be correspondingly made available thickness be 0.4mm and adulterate Al Ti thin slices and thickness be 0.8mm's B4C thin slices, then by Ti thin slices and B4C thin slices are alternately superimposed successively, obtain stratiform Ti/B4The green compact of C composite;
(3) by stratiform Ti/B4The green compact of C composite are placed in vacuum sintering funace, treat vacuum reach 6.63 × 10-3During Pa, 1h is sintered under 1700 DEG C of sintering temperature and 20MPa sintering pressure, furnace cooling obtains layered Ti/B4C composite;Wherein, prepared stratiform Ti/B4Contain the Al that mass fraction is 3% in C composite.
Composite prepared by the present embodiment is characterized:It is 96.4% to measure relative density, and bending strength is 589.7MPa, fracture toughness is 6.92MPam1/2.It can be seen from XRD characterizes obtained collection of illustrative plates, in prepared composite Principal phase be B4C, Ti and TiB2, in addition with a small amount of intermetallic compound TiAlXWith Al-B-C solid solution Al8B4C7, these The presence of interfacial product greatly improves Ti layers and B4The adhesion of C interlayers, improves bond strength.Obtained according to morphology characterization SEM is schemed it is known that there is the deeper B of color in prepared composite4C layers and the shallower Ti layers of color, illustrate institute The composite of preparation is Ti layers of the metal of toughness and high-strength ceramic B4C layers alternate the layer structure to be formed successively.Root It may determine that according to XRD and SEM characterization results:Ti layers and B4Physical bond of the combination of C interlayers before sintering is changed into metallurgical junction Close, improve its interface bond strength.Crackle can equally occur when being extended in the composite prepared by the present embodiment Crack deflection and the phenomenon for gradually using up energy to failure, extend crack extending length, and then make stratiform Ti/B4C composite is broken Toughness is split to make moderate progress.
Embodiment 4
(1) using polyvinyl alcohol as binding agent, respectively to titanium valve, B under 20MPa pressure4The progress of C powders is dry-pressing formed, After pressurize 5min, the B that Ti thin slices and thickness that thickness is 0.2mm are 0.4mm is correspondingly made available4C thin slices, then by Ti thin slices with And B4C thin slices are alternately superimposed successively, obtain stratiform Ti/B4The green compact of C composites;
(2) by stratiform Ti/B4The green compact of C composite are placed in vacuum sintering funace, treat vacuum reach 6.63 × 10-3During Pa, 1.5h is sintered under 1800 DEG C of sintering temperature and 30MPa sintering pressure, furnace cooling obtains layered Ti/B4C composite;
Composite prepared by the present embodiment is characterized:It is 97.1% to measure relative density, and bending strength is 608.2MPa, fracture toughness is 7.14MPam1/2.It can be seen from XRD characterizes obtained collection of illustrative plates, in prepared composite Principal phase is B4C, Ti and TiB2And a small amount of TiC.Composite wood it is known that prepared is schemed according to the SEM that morphology characterization is obtained There is the deeper B of color in material4C layers and the shallower Ti layers of color, illustrate the metal Ti that prepared composite is toughness Layer and high-strength ceramic B4C layers alternate the layer structure to be formed successively.It may determine that according to XRD and SEM characterization results:Ti Layer and B4Physical bond of the combination of C interlayers before sintering is changed into metallurgical binding, improves its interface bond strength.Crackle exists Equally can occur crack deflection when being extended in the composite prepared by the present embodiment and gradually use up the phenomenon of energy to failure, Crack extending length is extended, and then makes stratiform Ti/B4C composite fracture toughness makes moderate progress.
In summary, presently preferred embodiments of the present invention is these are only, is not intended to limit the scope of the present invention. Within the spirit and principles of the invention, any modification, equivalent substitution and improvements made etc., should be included in the present invention's Within protection domain.

Claims (6)

1. a kind of stratiform Ti/B4C composite, it is characterised in that:The composite is by Ti layers and B4C layers are alternately superimposed successively Form;Wherein, every a Ti layers of thickness is 0.2mm~0.4mm, every B4C layers of thickness is 0.4mm~0.8mm.
2. a kind of stratiform Ti/B according to claim 14The preparation method of C composite, it is characterised in that:It is described compound Al in material containing mass fraction no more than 3%, and Al quality and Ti mass ratio are 4~8:100.
3. a kind of stratiform Ti/B as claimed in claim 14The preparation method of C composite, it is characterised in that:Methods described is walked It is rapid as follows:
(1) using polyvinyl alcohol as binding agent, respectively by titanium valve, B4The progress of C powders is dry-pressing formed, is correspondingly made available thickness for 0.2mm ~0.4mm Ti thin slices and thickness is 0.4mm~0.8mm B4C thin slices;Again by Ti thin slices and B4C thin slices are alternately folded successively Plus, obtain stratiform Ti/B4The green compact of C composite;
(2) by stratiform Ti/B4The green compact of C composite, which are placed in vacuum sintering funace, carries out vacuum heating-press sintering, cooling, obtains To layered Ti/B4C composite;
In step (1), dry-pressing formed pressure is 10MPa~30MPa, and the dwell time is 5min~10min;
In step (2), the vacuum in vacuum sintering funace is not less than 6.63 × 10-3Pa, sintering temperature 1700 DEG C~1800 DEG C, sintering pressure 20MPa~30MPa, sintering time 1h~2h.
4. a kind of stratiform Ti/B as claimed in claim 24The preparation method of C composite, it is characterised in that:Methods described is walked It is rapid as follows:
(1) titanium valve, aluminium powder, absolute ethyl alcohol and polyethylene glycol are first subjected to wet ball grinding mixing, then the slurry after ball milling is put In being dried under vacuum condition, Al/Ti mixed powders are obtained;Using polyvinyl alcohol as binding agent, respectively by Al/Ti mixed powders, B4C Powder carry out it is dry-pressing formed, be correspondingly made available thickness be 0.2mm~0.4mm and adulterate Al Ti thin slices and thickness be 0.4mm ~0.8mm B4C thin slices;Again by Ti thin slices and B4C thin slices are alternately superimposed successively, obtain stratiform Ti/B4The life of C composite Base;
(2) by stratiform Ti/B4The green compact of C composite, which are placed in vacuum sintering funace, carries out vacuum heating-press sintering, cooling, obtains To layered Ti/B4C composite;
In step (1), dry-pressing formed pressure is 10MPa~30MPa, and the dwell time is 5min~10min;
In step (2), the vacuum in vacuum sintering funace is not less than 6.63 × 10-3Pa, sintering temperature 1700 DEG C~1800 DEG C, sintering pressure 20MPa~30MPa, sintering time 1h~2h.
5. a kind of stratiform Ti/B according to claim 34The preparation method of C composite, it is characterised in that:Titanium valve it is flat Equal particle diameter is 5 μm~10 μm, B4The average grain diameter of C powders is 3 μm~5 μm.
6. a kind of stratiform Ti/B according to claim 44The preparation method of C composite, it is characterised in that:Titanium valve it is flat Equal particle diameter is 5 μm~10 μm, the average grain diameter of aluminium powder for 1 μm~3 μm, B4The average grain diameter of C powders is 3 μm~5 μm.
CN201710357463.7A 2017-05-19 2017-05-19 Layered Ti/B4C composite material and preparation method thereof Expired - Fee Related CN107117981B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201710357463.7A CN107117981B (en) 2017-05-19 2017-05-19 Layered Ti/B4C composite material and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201710357463.7A CN107117981B (en) 2017-05-19 2017-05-19 Layered Ti/B4C composite material and preparation method thereof

Publications (2)

Publication Number Publication Date
CN107117981A true CN107117981A (en) 2017-09-01
CN107117981B CN107117981B (en) 2020-10-16

Family

ID=59727338

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201710357463.7A Expired - Fee Related CN107117981B (en) 2017-05-19 2017-05-19 Layered Ti/B4C composite material and preparation method thereof

Country Status (1)

Country Link
CN (1) CN107117981B (en)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108947536A (en) * 2018-07-05 2018-12-07 重庆文理学院 A kind of high-densit B-Ti-C system ceramics of strong ultrasonic wave added method preparation even tissue
CN110282977A (en) * 2019-06-17 2019-09-27 东北大学 A kind of B4C/TiB2The preparation method of layered composite ceramic material
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
CN112590327A (en) * 2020-12-23 2021-04-02 南京工程学院 Ti/B4Preparation method of C ceramic and aluminum pyramid structure layer combined layered armor and pyramid structure layer
CN113956062A (en) * 2021-10-25 2022-01-21 燕山大学 Ceramic substrate AlN/Ti layered composite material and preparation method and application thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105571400A (en) * 2015-12-18 2016-05-11 中国航空工业集团公司北京航空制造工程研究所 Titanium-based composite armor and manufacturing method thereof

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105571400A (en) * 2015-12-18 2016-05-11 中国航空工业集团公司北京航空制造工程研究所 Titanium-based composite armor and manufacturing method thereof

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108947536A (en) * 2018-07-05 2018-12-07 重庆文理学院 A kind of high-densit B-Ti-C system ceramics of strong ultrasonic wave added method preparation even tissue
CN110282977A (en) * 2019-06-17 2019-09-27 东北大学 A kind of B4C/TiB2The preparation method of layered composite ceramic material
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
CN112590327A (en) * 2020-12-23 2021-04-02 南京工程学院 Ti/B4Preparation method of C ceramic and aluminum pyramid structure layer combined layered armor and pyramid structure layer
CN113956062A (en) * 2021-10-25 2022-01-21 燕山大学 Ceramic substrate AlN/Ti layered composite material and preparation method and application thereof
CN113956062B (en) * 2021-10-25 2022-11-15 燕山大学 Ceramic substrate AlN/Ti layered composite material and preparation method and application thereof

Also Published As

Publication number Publication date
CN107117981B (en) 2020-10-16

Similar Documents

Publication Publication Date Title
CN107117981A (en) A kind of stratiform Ti/B4C composite and preparation method thereof
US20210323875A1 (en) Short-Fiber-Reinforced Oriented MAX-Phase Ceramic-Based Composite and Preparation Method Therefor
She et al. Effect of additive content on liquid-phase sintering on silicon carbide ceramics
CN101215164B (en) Method for preparing boron carbide composite material
CN107141004B (en) Boron carbide composite material and preparation method thereof
CN108558422A (en) The preparation method of the carbon fiber-reinforced ultra-temperature ceramic-based composite material of three-dimensional with high work to break
CN102964139B (en) Preparation method of whisker and particle synergistically toughened laminar ceramic matrix composite
CN102701773B (en) Authigenic silicon nitride crystal whisker toughening tungsten carbide composite material and preparation method thereof
CN106904984A (en) A kind of SiC short fiber composite materials and compound cladding tubes and preparation method thereof
WO2002098819A1 (en) Method for producing sic fiber-reinforced sic composite material
CN110423119A (en) A kind of preparation method of resistance to ablation C/SiC ceramic matric composite
JPH1135376A (en) Silicon-silicon carbide material with silicon concentration gradient and silicon carbide fiber reinforced silicon-silicon carbide composite material with silicon concentration gradient and their production
CN108640687A (en) A kind of boron carbide/carborundum composite-phase ceramic and preparation method thereof
CN113480320B (en) High-stress-cracking-resistance SiC f SiC ceramic matrix composite material and preparation method thereof
Hu et al. Mechanical and dielectric properties of SiCf/SiC composites fabricated by PIP combined with CIP process
CN105294084A (en) High-hardness and high-toughness alumina ceramic composite material and preparing method thereof
CN110818428A (en) Preparation method of eutectic reinforced toughened silicon nitride ceramic
CN108467272A (en) A kind of preparation method of boron carbide/silicon carbide stratiform composite ceramic material
CN103979974A (en) Preparation method of C/SiC-HfB2-HfC ultrahigh-temperature ceramic-based composite material
CN111716494A (en) Method for preparing layered complex phase ceramic by using reaction sintering method
Wang et al. Fabrication of carbon fiber reinforced ceramic matrix composites with improved oxidation resistance using boron as active filler
Tani et al. SiC matrix composites reinforced with internally synthesized TiB 2
CN106966749B (en) It is a kind of to use Ti3Si(Al)C2The method of modified thermostructural composite
CN115677351A (en) Multi-lamination boron carbide composite ceramic with strong bonding interface and preparation method thereof
CN111995418B (en) Preparation method of high-strength and high-toughness silicon carbide nanowire reinforced silicon carbide ceramic composite material

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
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20201016

Termination date: 20210519

CF01 Termination of patent right due to non-payment of annual fee