CN107056304A - A kind of TiB2Based composite ceramic material and preparation method thereof - Google Patents

A kind of TiB2Based composite ceramic material and preparation method thereof Download PDF

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CN107056304A
CN107056304A CN201710261290.9A CN201710261290A CN107056304A CN 107056304 A CN107056304 A CN 107056304A CN 201710261290 A CN201710261290 A CN 201710261290A CN 107056304 A CN107056304 A CN 107056304A
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tic
powder
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王玉金
张翰超
刘冠杞
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Harbin Institute of Technology
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    • 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
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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
    • C04B2235/3839—Refractory metal carbides
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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
    • C04B2235/3852—Nitrides, e.g. oxynitrides, carbonitrides, oxycarbonitrides, lithium nitride, magnesium nitride
    • C04B2235/3856—Carbonitrides, e.g. titanium carbonitride, zirconium carbonitride
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    • 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
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    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance

Abstract

The present invention discloses a kind of TiB2Based composite ceramic material and preparation method thereof, is related to ceramic composite and preparation method thereof, product is by TiB2Based composite ceramic material TiB2Mixed with Ti powders precentagewise is added in TiC, obtain mixed powder after being placed in the processing of ball mill spheroidal graphite, TiB is prepared after carrying out pressureless sintering2‑TiC1‑xCeramic composite.The invention solves the problems that the low-melting-point metal such as existing Ni, Co reduces ceramic crystalline grain abnormal growth in sintering temperature, the sintering process that can be brought, reduction mechanical property and the heat endurance and red hardness for reducing composite as Binder Phase.

Description

A kind of TiB2Based composite ceramic material and preparation method thereof
Technical field
The present invention relates to ceramic composite field, and in particular to a kind of TiB2Based composite ceramic material and its preparation side Method.
Background technology
TiB2Based composite ceramic material has high-melting-point, high rigidity, high specific strength, excellent thermal conductivity due to it, friction Coefficient is low, and thermal coefficient of expansion is small, and enjoys pass with preferable wearability, chemical stability and the features such as inoxidizability Note, the features such as still having preferable heat endurance and chemical stability especially at 1700 DEG C, makes it as Advanced Ceramic Tool Application provide may, therefore with as forth generation cutter material potentiality.
TiC, TiN and Ti (CN) have high-melting-point, high rigidity and preferable tribological property, and and TiB2Excellent thing Reason and chemical compatibility so that it is often and TiB2It is combined, to improve TiB2Mechanical property, and a certain degree of reduction TiB2Ceramic sintering difficulty.
However, due to TiB2-TiC、TiB2- TiN and TiB2The high-melting-point that-Ti (CN) ceramic composite has, it is high covalent Bond energy and low self-diffusion coefficient so that sintering temperature needs to burn higher than 2000 DEG C or using hot pressed sintering or plasma discharging The method of knot could be fine and close.And Ni is used, the low-melting-point metal such as Co reduces sintering temperature as Binder Phase, and two aspects can be brought to ask Topic, on the one hand due to Ni, the metal such as Co and TiB2The wetability of based composite ceramic material is poor, causes ceramics in sintering process brilliant Grain abnormal growth, reduces mechanical property；On the other hand, metal adhesive, which is met, reduces the heat endurance and red hardness of composite.
In view of drawbacks described above, creator of the present invention obtains the present invention finally by prolonged research and practice.
The content of the invention
To solve above-mentioned technological deficiency, the present invention provides a kind of TiB2Based composite ceramic material and preparation method thereof.
A kind of TiB2The preparation method of based composite ceramic material, comprises the following steps：
The first step, by 40%~60% TiC powder, 8%~35% Ti powders, and surplus are TiB2Powder, is pressed Ball mill spheroidal graphite is placed in after mass percent mixing, ball material mass ratio is (20~40):1, the spheroidal graphite time is 5~20h, then mistake 100~400 mesh sieves, obtain TiB2- TiC-Ti mixed powders；
Second step, by the pressureless sintering under vacuum or argon gas atmosphere of above-mentioned mixed powder, sintering temperature is 1500~1700 DEG C, 30~120min of soaking time obtains TiB2-TiC1-xCeramic composite.
Preferably, TiN powders replace the TiC powder, TiB is obtained2-TiN1-xCeramic composite.
Preferably, Ti (CN) powder replaces the TiC powder, TiB is obtained2-Ti(C1-x,N1-y) ceramic composite.
Preferably, TiH2Instead of the Ti powders, and before second step progress, first it is incubated at 600~800 DEG C 30min dehydrogenations.
Preferably, the crystallite dimension of the mixed powder is less than 100nm.
Preferably, raw material prepares TiB prepared by other alternative schemes of composite2, TiC, TiN and Ti (CN) powder.
Preferably, Ti and TiH2Additive is alternative using others Ti sources, for example, can be decomposed into adding for Ti at high temperature Plus agent.
Beneficial effects of the present invention:
Present invention process is simple, and Ti reduces sintering temperature and than Ni as low-melting-point metal as Binder Phase, Co into This is cheap, and operational sequence process of the present invention is simple, and the composite compactness being prepared by the method for the present invention is high, in sintering process Ceramic crystalline grain is small, and the mechanical property of composite obtained from is good and chemical stability is high.
Brief description of the drawings
In order to illustrate more clearly of the technical scheme in various embodiments of the present invention, required in being described below to embodiment The accompanying drawing used is briefly described.
Fig. 1 is TiB of the present invention2A represents TiB in the XRD spectrum of based composite ceramic material, figure2-40TiC0.68；B is represented TiB2-40TiC0.84；C represents TiB2-40TiC0.96。
Embodiment
Below in conjunction with accompanying drawing, the forgoing and additional technical features and advantages are described in more detail.
The diameter of particle of the compound material used in the embodiment of the present invention is no more than 20 μm.
Embodiment 1
60g TiB2(39.1g TiC and 1.3g Ti generate 40g's with the Ti of addition 1.3g in 39.1g TiC TiC0.96), mechanical ball mill after being well mixed, Ball-milling Time is 20h, and ball material mass ratio is 40:1, obtain TiB after crossing 200 mesh sieves2- TiC-Ti mixed powders, the crystallite dimension of powder is not more than 100nm.Powder is subjected to pressureless sintering, sintering temperature rises to 1600 DEG C, sintering atmosphere is argon gas, and TiB is prepared after insulation 60min2-40TiC0.96Ceramic composite.TiB2-40TiC0.96Ceramics The consistency of composite is 94.4%, and bending strength is 554~579MPa, and Vickers hardness is 18.1~19.5Gpa, is broken tough Property be 8.65~9.23MPam1/2。
Embodiment 2
50g TiB2(48.8g TiC and 1.6g Ti generate 50g's with the Ti of addition 1.6g in 48.8g TiC TiC0.96), mechanical ball mill after being well mixed, Ball-milling Time is 20h, and ball material mass ratio is 40:1, obtain TiB after crossing 200 mesh sieves2- TiC-Ti mixed powders, the crystallite dimension of powder is not more than 100nm.Powder is subjected to pressureless sintering, sintering temperature rises to 1600 DEG C, sintering atmosphere is argon gas, and TiB is prepared after insulation 60min2-50TiC0.96Ceramic composite.TiB2-50TiC0.96Ceramics The consistency of composite is 95.2%, and bending strength is 547~568MPa, and Vickers hardness is 17.8~18.5Gpa, is broken tough Property be 7.58~8.12MPam1/2。
Embodiment 3
40g TiB2Ti (57g TiC and 2.0g Ti generations 60g TiC with adding 2.0g in 57g TiC0.96), Mechanical ball mill after well mixed, Ball-milling Time is 20h, and ball material mass ratio is 40:1, obtain TiB after crossing 200 mesh sieves2-TiC-Ti Mixed powder, the crystallite dimension of powder is not more than 100nm.Powder is subjected to pressureless sintering, sintering temperature rises to 1600 DEG C, sintering Atmosphere is argon gas, and TiB is prepared after insulation 60min2-60TiC0.96Ceramic composite.TiB2-60TiC0.96Ceramic Composite material The consistency of material is 94.8%, and bending strength is 544~553MPa, and Vickers hardness is 17.3~18.0Gpa, and fracture toughness is 8.56~9.54MPam1/2。
Embodiment 4
60g TiB2(34.8g TiC and 5.4g Ti generate 40g's with the Ti of addition 5.4g in 34.8g TiC TiC0.84), mechanical ball mill after being well mixed, Ball-milling Time is 20h, and ball material mass ratio is 40:1, obtain TiB after crossing 200 mesh sieves2- TiC-Ti mixed powders, the crystallite dimension of powder is not more than 100nm.Powder is subjected to pressureless sintering, sintering temperature rises to 1600 DEG C, sintering atmosphere is argon gas, and TiB is prepared after insulation 60min2-40TiC0.84Ceramic composite.TiB2-40TiC0.84Ceramics The consistency of composite is 95.7%, and bending strength is 576~588MPa, and Vickers hardness is 19.6~20.1Gpa, is broken tough Property be 8.69~9.65MPam1/2。
Embodiment 5
60g TiB2(34.8g TiC and 5.4g Ti generate 40g's with the Ti of addition 5.4g in 34.8g TiC TiC0.84), mechanical ball mill after being well mixed, Ball-milling Time is 20h, and ball material mass ratio is 40:1, obtain TiB after crossing 200 mesh sieves2- TiC-Ti mixed powders, the crystallite dimension of powder is not more than 100nm.Powder is subjected to pressureless sintering, sintering temperature rises to 1500 DEG C, sintering atmosphere is argon gas, and TiB is prepared after insulation 60min2-40TiC0.84Ceramic composite.TiB2-40TiC0.84Ceramics The consistency of composite is 96.1%, and bending strength is 564~573MPa, and Vickers hardness is 19.2~21.9Gpa, is broken tough Property be 9.38~10.34MPam1/2。
Embodiment 6
50g TiB2(43.4g TiC and 6.6g Ti generate 50g's with the Ti of addition 6.6g in 43.4g TiC TiC0.84), mechanical ball mill after being well mixed, Ball-milling Time is 20h, and ball material mass ratio is 40:1, obtain TiB after crossing 200 mesh sieves2- TiC-Ti mixed powders, the crystallite dimension of powder is not more than 100nm.Powder is subjected to pressureless sintering, sintering temperature rises to 1600 DEG C, sintering atmosphere is argon gas, and TiB is prepared after insulation 60min2-50TiC0.84Ceramic composite.TiB2-50TiC0.84Ceramics The consistency of composite is 97.3%, and bending strength is 597~621MPa, and Vickers hardness is 20.5~22.5Gpa, is broken tough Property be 9.10~10.91MPam1/2。
Embodiment 7
50g TiB2(43.4g TiC and 6.6g Ti generate 60g's with the Ti of addition 6.6g in 43.4g TiC TiC0.84), mechanical ball mill after being well mixed, Ball-milling Time is 20h, and ball material mass ratio is 40:1, obtain TiB after crossing 200 mesh sieves2- TiC-Ti mixed powders, the crystallite dimension of powder is not more than 100nm.Powder is subjected to pressureless sintering, sintering temperature rises to 1700 DEG C, sintering atmosphere is argon gas, and TiB is prepared after insulation 60min2-50TiC0.84Ceramic composite.TiB2-50TiC0.84Ceramics The consistency of composite is 98.5%, and bending strength is 566~594MPa, and Vickers hardness is 19.4~20.7Gpa, is broken tough Property be 8.65~9.18MPam1/2。
Embodiment 8
40g TiB2(51.7g TiC and 8.0g Ti generate 50g's with the Ti of addition 8.0g in 51.7g TiC TiC0.84), mechanical ball mill after being well mixed, Ball-milling Time is 20h, and ball material mass ratio is 40:1, obtain TiB after crossing 200 mesh sieves2- TiC-Ti mixed powders, the crystallite dimension of powder is not more than 100nm.Powder is subjected to pressureless sintering, sintering temperature rises to 1600 DEG C, sintering atmosphere is argon gas, and TiB is prepared after insulation 60min2-60TiC0.84Ceramic composite.TiB2-60TiC0.84Ceramics The consistency of composite is 98.6%, and bending strength is 570~582MPa, and Vickers hardness is 17.0~18.3Gpa, is broken tough Property be 7.78~8.45MPam1/2。
Embodiment 9
60g TiB2(29.1g TiC and 10.9g Ti generate 40g's with the Ti of addition 10.9g in 29.1g TiC TiC0.68), mechanical ball mill after being well mixed, Ball-milling Time is 20h, and ball material mass ratio is 40:1, obtain TiB after crossing 200 mesh sieves2- TiC-Ti mixed powders, the crystallite dimension of powder is not more than 100nm.Powder is subjected to pressureless sintering, sintering temperature rises to 1600 DEG C, sintering atmosphere is argon gas, and TiB is prepared after insulation 60min2-40TiC0.68Ceramic composite.TiB2-40TiC0.68Ceramics The consistency of composite is 98.4%, and bending strength is 551~576MPa, and Vickers hardness is 17.6~18.4Gpa, is broken tough Property be 9.61~8.98MPam1/2。
Embodiment 10
50g TiB2(36.4g TiC and 18.7g Ti generate 50g's with the Ti of addition 13.7g in 36.4g TiC TiC0.68), mechanical ball mill after being well mixed, Ball-milling Time is 20h, and ball material mass ratio is 40:1, obtain TiB after crossing 200 mesh sieves2- TiC-Ti mixed powders, the crystallite dimension of powder is not more than 100nm.Powder is subjected to pressureless sintering, sintering temperature rises to 1600 DEG C, sintering atmosphere is argon gas, and TiB is prepared after insulation 60min2-50TiC0.68Ceramic composite.TiB2-50TiC0.68Ceramics The consistency of composite is 98.5%, and bending strength is 569~577MPa, and Vickers hardness is 18.86~19.2Gpa, fracture Toughness is 8.12~9.27MPam1/2。
Embodiment 11
40g TiB2(43.7g TiC and 16.4g Ti generate 60g's with the Ti of addition 16.4g in 43.7g TiC TiC0.68), mechanical ball mill after being well mixed, Ball-milling Time is 20h, and ball material mass ratio is 40:1, obtain TiB after crossing 200 mesh sieves2- TiC-Ti mixed powders, the crystallite dimension of powder is not more than 100nm.Powder is subjected to pressureless sintering, sintering temperature rises to 1600 DEG C, sintering atmosphere is argon gas, and TiB is prepared after insulation 60min2-60TiC0.68Ceramic composite.TiB2-60TiC0.68Ceramics The consistency of composite is 98.7%, and bending strength is 573~585MPa, and Vickers hardness is 19.0~20.2Gpa, is broken tough Property be 9.13~9.40MPam1/2。
TiH in the present invention2The hydrogen produced in certain embodiments, local reduction atmosphere is formd in powder surface, and is gone back Originality atmosphere is conducive to TiB2-TiC1-xThe elimination of powder surface oxide-film, promotes diffusion mass transfer, reduces sintering temperature. In the present invention, why fine and close, excellent performance material can be prepared with relatively low temperature sintering, on the one hand had benefited from non-chemical Measure the TiC of ratio1-xFormation, on the other hand have benefited from the generation of reducing atmosphere, and in terms of removing any of which, be difficult to Obtain the material described in the present invention.
TiB prepared by final sintering of the invention2-TiC1-xIn composite, TiC1-xContent be in TiB2-TiC1-xPhase In figure near eutectic composition point, and depart from the material of this scope, hardly result in the microstructure and performance of material in the present invention.
Present invention process is simple, and Ti is than Ni, and Co's is with low cost, the TiB prepared by above-described embodiment2Base Ceramic Composite Material, the present invention is effective to solve Ni, low-melting-point metal and the TiB such as Co2The wetability of based composite ceramic material is poor, causes The problem of ceramic crystalline grain abnormal growth in sintering process, reduction mechanical property；Metal adhesive is also solved to meet reduction composite wood The problem of heat endurance and red hardness of material.
Presently preferred embodiments of the present invention is the foregoing is only, is merely illustrative for the purpose of the present invention, and it is non-limiting 's.Those skilled in the art understands, many changes can be carried out to it in the spirit and scope that the claims in the present invention are limited, Modification, in addition it is equivalent, but fall within protection scope of the present invention.

Claims (6)

1. a kind of TiB2The preparation method of based composite ceramic material, it is characterised in that comprise the following steps：
The first step, by 40%~60% TiC powder, 8%~35% Ti powders, and surplus are TiB2Powder, by quality hundred Divide than being placed in ball mill spheroidal graphite after mixing, ball material mass ratio is (20~40):1, the spheroidal graphite time be 5~20h, then cross 100~ 400 mesh sieves, obtain TiB2- TiC-Ti mixed powders；
Second step, by the pressureless sintering under vacuum or argon gas atmosphere of above-mentioned mixed powder, sintering temperature is 1500~1700 DEG C, is protected Warm 30~120min of time, obtains TiB2-TiC1-xCeramic composite.
2. a kind of TiB as claimed in claim 12The preparation method of based composite ceramic material, it is characterised in that replaced with TiN powders The TiC powder is changed, TiB is obtained2-TiN1-xCeramic composite.
3. a kind of TiB as claimed in claim 12The preparation method of based composite ceramic material, it is characterised in that use Ti (CN) powder Body replaces the TiC powder, obtains TiB2-Ti(C1-x,N1-y) ceramic composite.
4. a kind of TiB as claimed in claim 12The preparation method of based composite ceramic material, it is characterised in that use TiH2Instead of The Ti powders, and before second step progress, 30min dehydrogenations are first incubated at 600~800 DEG C.
5. a kind of TiB as described in claim any one of 1-42The preparation method of based composite ceramic material, it is characterised in that institute The crystallite dimension for stating mixed powder is less than 100nm.
6. TiB as claimed in claim 52A kind of TiB prepared by the preparation method of based composite ceramic material2Base Ceramic Composite material Material.
CN201710261290.9A 2017-04-20 2017-04-20 A kind of TiB2Based composite ceramic material and preparation method thereof Pending CN107056304A (en)

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Cited By (4)

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Publication number Priority date Publication date Assignee Title
CN109355521A (en) * 2018-09-12 2019-02-19 张家港市山牧新材料技术开发有限公司 A kind of preparation method of titanium diboride Base Metal composite material
CN113416078A (en) * 2021-08-09 2021-09-21 燕山大学 Non-stoichiometric titanium boride and high-entropy boride ceramic prepared from same
CN114605156A (en) * 2022-03-15 2022-06-10 北京理工大学 TiB2Composite ceramic material for base armor
CN115557793A (en) * 2022-09-19 2023-01-03 广东工业大学 High-entropy ceramic with fine grains, high hardness and high toughness, and preparation method and application thereof

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