CN107043261A - A kind of Ti strengthens B4C/SiC complex phase ceramics - Google Patents

A kind of Ti strengthens B4C/SiC complex phase ceramics Download PDF

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CN107043261A
CN107043261A CN201710257082.1A CN201710257082A CN107043261A CN 107043261 A CN107043261 A CN 107043261A CN 201710257082 A CN201710257082 A CN 201710257082A CN 107043261 A CN107043261 A CN 107043261A
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complex phase
sic
powders
ceramic
sintering
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李云凯
吴超
程兴旺
张朝晖
陈义文
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Beijing Institute of Technology BIT
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Abstract

Strengthen B the present invention relates to a kind of Ti4C/SiC complex phase ceramics, belonging to metallic particles strengthens the technical field of ceramic composite.Ti of the present invention strengthens B4In C/SiC complex phase ceramics, Ti and B4Interfacial reaction generation TiB occurs for C2Phase, can play optimization thing phase composition, the effect of crystal grain thinning, so as to improve the mechanical property of complex phase ceramic;And Ti produces a large amount of liquid phases during vacuum heating-press sintering, promote the sintering and densification process of complex phase ceramic, and prepared complex phase ceramic dense micro-structure;In addition, there is the mixed fracture pattern that transgranular fracture and grain boundary fracture coexist in complex phase ceramic of the present invention, so as to improve the fracture toughness of complex phase ceramic.

Description

A kind of Ti strengthens B4C/SiC complex phase ceramics
Technical field
Strengthen B the present invention relates to a kind of Ti4C/SiC complex phase ceramics, belonging to metallic particles strengthens the skill of ceramic composite Art field.
Background technology
B4C ceramics are widely used in structural material because its density is low, hardness is high and the characteristic such as corrosion-resistant.Study and real Issue after examination and approval now, in B4Second phases such as oxide, activated carbon, boride, carbide and metal simple-substance are added in C can effectively improve B4C The sintering character and mechanical property of product, compared to pure boron carbide, can obtain at a relatively low sintering temperature has higher densification The diphase ceramic material of degree.
It has now been found that, as the B in ceramic matric composite4When C phases content is higher than SiC phases, in high-temperature oxidation environment Under, the surface of composite can form the B of densification2O3Glass phase, so as to completely cut off the inside propagation of oxygen element and heat, and then has There is excellent high temperature oxidation resistance.SiC is B4The conventional toughness reinforcing phase of C ceramic post sinterings, calculation of thermodynamics shows both this 2500 Still it is stabilising system more than DEG C.SiC can be introduced by presoma, for example Polycarbosilane (PSCS).The hot pressing at 1900 DEG C Standby B4C/SiC(PSCS)/A12O3Composite (Guo Quangui, Song Jinren, Liu Lang, Zhang Bijiang .B4C-SiC/C composites are aoxidized TG/DTA analysis [J] carbon techniques of process, 1999,100 (2):12-16), it can form a kind of multiple in composite intercrystalline Miscellaneous structure:B4C and A12O3Lamellar SiC and B at nano SiC, crystal particle crystal boundary inside particle4The intercrystalline SiC of C are sub- Grain boundary structure.This diphase ceramic material bending strength 375MPa, fracture toughness 5.08MPam1/2, microhardness 34.4GPa.
B4C ceramic matric composite hardness high tenacity is poor, and metal material generally has excellent toughness.Thus, in B4C Metal phase is added in the preparation of ceramics, although can be reduced the hardness of ceramic composite to a certain degree, but can effectively be changed It is apt to its toughness.The preparation of boron carbide/metallic composite is, it is necessary to solve two key issues, i.e. boron carbide and intermetallic profit Reaction between moist property and boron carbide and metal.Research work main at present concentrates on the metals such as Fe, Cu, Mg, Ti, Al On the composite of boron carbide, preparation temperature is usually 1000 DEG C, but because metal phase and ceramic phase wetability are poor, it is impossible to Unified stable structure is formed, so that the finished product with stability can not be obtained.
The content of the invention
For the deficiencies in the prior art, B is strengthened it is an object of the invention to provide a kind of Ti4C/SiC complex phases are made pottery There is the mixed fracture pattern that transgranular fracture and grain boundary fracture coexist in porcelain, the complex phase ceramic, improve its fracture toughness;And And, enhancing phase Ti and B4Interfacial reaction generation TiB occurs for C2Phase, can play and optimize thing phase composition, the effect of crystal grain thinning, from And improve the mechanical property of composite.
The mesh of the present invention is achieved through the following technical solutions:
A kind of Ti strengthens B4C/SiC complex phase ceramics, the complex phase ceramic is adopted to be prepared with the following method:
Step 1. prepares Ti, B4C and SiC complex phase powder
By Ti powders, SiC powder, B4C powders, polyethylene glycol (PEG) and absolute ethyl alcohol are according to 0.1~1:1.5:2.5: 0.1:20 mass ratio is mixed and moved into ball grinder, ball-milling medium is added, then in 150r/min~200r/min Rotating speed under ball milling 12h~48h, then the mixed slurry after ball milling is dried in vacuo, obtains complex phase powder;
Step 2. vacuum heating-press sintering
Complex phase powder obtained by step 1 is placed in vacuum sintering funace and carries out vacuum heating-press sintering, cools down, obtains institute State Ti enhancings B4C/SiC complex phase ceramics;
Wherein, the vacuum in vacuum sintering funace is not less than 6.63 × 10-3Pa, sintering temperature 1800 DEG C~1950 DEG C, sintering pressure 20MPa~30MPa, sintering time 1h~2h.
Preferably 3 μm~5 μm of the average grain diameter of Ti powders, preferably 1 μm of the average grain diameter of SiC powder~5 μm, B4C powders Preferably 3 μm~10 μm of average grain diameter.
The preferred ZrO of material of the ball-milling medium2
In step 1, Ti powders, SiC powder, B4The mass ratio of C powders, polyethylene glycol and absolute ethyl alcohol preferably 1:1.5: 2.5:0.1:20。
Beneficial effect:
Ti of the present invention strengthens B4In C/SiC complex phase ceramics, Ti and B4Interfacial reaction generation TiB occurs for C2Phase, can be with Play optimization thing phase composition, the effect of crystal grain thinning, so as to improve the mechanical property of complex phase ceramic;And Ti is in sintering process A large amount of liquid phases are produced, promote the sintering and densification process of complex phase ceramic, and prepared complex phase ceramic dense micro-structure. In addition, there is the mixed fracture pattern that transgranular fracture and grain boundary fracture coexist in complex phase ceramic of the present invention, so as to improve The fracture toughness of complex phase ceramic.
Brief description of the drawings
Fig. 1 strengthens B for the Ti prepared in embodiment 14X-ray diffraction (XRD) collection of illustrative plates of C/SiC complex phase ceramics.
Fig. 2 strengthens B for the Ti prepared in embodiment 14The cross-sectional scanning electron microscope of C/SiC complex phase ceramics (SEM) figure.
Fig. 3 strengthens B for the Ti prepared in embodiment 14The section high power SEM of C/SiC complex phase ceramics Figure.
Fig. 4 strengthens B for the Ti prepared in embodiment 14The Crack Extension SEM of C/SiC complex phase ceramics Figure.
Fig. 5 is to be not added with Ti B in comparative example 14The cross-sectional scanning electron microscope figure of C/SiC complex phase ceramics.
Embodiment
The present invention will be further described with reference to the accompanying drawings and detailed description.
In following examples:
Ti powders:Average grain diameter is 5 μm, Shanghai paddy field material Science and Technology Ltd.;
SiC powder:Average grain diameter is 1 μm, Shanghai paddy field material Science and Technology Ltd.;
B4C powders:Average grain diameter is 3 μm, Shanghai paddy field material Science and Technology Ltd..
Relative density:Tested using drainage;
Micro-hardness testing:Using the microhardness measurement of the HV-10B models of the silver-colored laboratory apparatus manufacturer production of Laizhou China Examination;
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 companies, And carry out energy disperse spectroscopy (EDS) sign.
Embodiment 1
Step 1. is by Ti powders, SiC powder, B4C powders, PEG4000 and absolute ethyl alcohol are according to 1:1.5:2.5:0.1: 20 mass ratio is mixed and moved into polytetrafluoroethylene (PTFE) ball grinder, according still further to 4:1 ratio of grinding media to material adds ball-milling medium ZrO2 Ball, then the ball milling 48h under 150r/min rotating speed, then the mixed slurry after ball milling is placed in drying in 80 DEG C of vacuum drying chambers 8h, obtains complex phase powder;
Complex phase powder obtained by step 1 is placed in vacuum sintering funace by step 2., treats that vacuum reaches 6.63 × 10- 3During Pa, 2h is sintered under 1950 DEG C of sintering temperature and 30MPa sintering pressure, furnace cooling obtains Ti enhancings B4C/SiC Complex phase ceramic.
Complex phase ceramic prepared by the present embodiment is characterized:It is 98.7% to measure relative density, and microhardness is 40.7GPa, bending strength is 576.7MPa, and fracture toughness is 5.41MPam1/2.From Fig. 1 it is known that the present embodiment is made The main thing phase composition of standby complex phase ceramic is TiB2、B4C, SiC and C, wherein TiB2It is Ti and B with C4Interfacial reaction occurs between C Obtained product.With the B for being not added with Ti prepared in comparative example4C/SiC complex phase ceramics are compared, the complex phase prepared by the present embodiment Ceramics have the lower porosity, more tiny crystal grain, more clearly grain contours, refer to Fig. 2 and Fig. 5.To what is marked in Fig. 3 Region carries out EDS analyses, and interfacial product TiB can be determined according to analysis result2Presence, refer to table 1.Fig. 4 has then annotated this The reason for complex phase ceramic tenacity excellent prepared by embodiment, i.e., there is transgranular fracture in the complex phase ceramic prepared by the present embodiment The pattern coexisted with grain boundary fracture so that complex phase ceramic has longer crack propagation path, improves its toughness.
Table 1
Embodiment 2
Step 1. is by Ti powders, SiC powder, B4C powders, PEG4000 and absolute ethyl alcohol are according to 0.5:1.5:2.5: 0.1:20 mass ratio is mixed and moved into polytetrafluoroethylene (PTFE) ball grinder, according still further to 4:1 ratio of grinding media to material adds ball-milling medium ZrO2Ball, then the ball milling 24h under 200r/min rotating speed, then the mixed slurry after ball milling is placed in 80 DEG C of vacuum drying chambers 8h is dried, complex phase powder is obtained;
Complex phase powder obtained by step 1 is placed in vacuum sintering funace by step 2., treats that vacuum reaches 6.63 × 10- 3During Pa, 2h is sintered under 1950 DEG C of sintering temperature and 30MPa sintering pressure, furnace cooling obtains Ti enhancings B4C/SiC Complex phase ceramic.
Complex phase ceramic prepared by the present embodiment is characterized:It is 97.9% to measure relative density, and microhardness is 38.1GPa, bending strength is 495.2MPa, and fracture toughness is 5.13MPam1/2.The SEM figures obtained according to morphology characterization can be with Learn, the compact structure of the complex phase ceramic prepared by the present embodiment, grain size distribution is uniform, grain contours are clear, Er Qiecun The mixed fracture pattern coexisted in transgranular fracture and grain boundary fracture.XRD signs are carried out to the complex phase ceramic prepared by the present embodiment, It can be seen from the spectrogram of gained, main thing phase component is B4C, SiC and more low intensive TiB2, TiB2It is Ti and B4Occur between C The product that interfacial reaction is obtained.
Embodiment 3
Step 1. is by Ti powders, SiC powder, B4C powders, PEG4000 and absolute ethyl alcohol are according to 1:1.5:2.5:0.1: 20 mass ratio is mixed and moved into polytetrafluoroethylene (PTFE) ball grinder, according still further to 4:The ratio of grinding media to material of 1 ratio of grinding media to material adds ball milling Medium ZrO2Ball, then the ball milling 48h under 150r/min rotating speed, then the mixed slurry after ball milling is placed in 80 DEG C of vacuum drying 8h is dried in case, complex phase powder is obtained;
Complex phase powder obtained by step 1 is placed in vacuum sintering funace by step 2., treats that vacuum reaches 6.63 × 10- 3During Pa, 1h is sintered under 1800 DEG C of sintering temperature and 20MPa sintering pressure, furnace cooling obtains Ti enhancings B4C/SiC Complex phase ceramic.
Complex phase ceramic prepared by the present embodiment is characterized:It is 97.4% to measure relative density, and microhardness is 37.5GPa, bending strength is 486.2MPa, and fracture toughness is 4.96MPam1/2.The SEM figures obtained according to morphology characterization can be with Learn, the structure of the complex phase ceramic prepared by the present embodiment is dense, grain size distribution is uniform, and average grain diameter is smaller, it is brilliant Grain is clear-cut, and there is the mixed fracture pattern that transgranular fracture and grain boundary fracture coexist.To answering prepared by the present embodiment Phase ceramics carry out XRD signs, it can be seen from the spectrogram of gained, and main thing phase component is B4C, SiC and obvious TiB2, TiB2It is Ti and B4The product that interfacial reaction is obtained occurs between C.
Embodiment 4
Step 1. is by Ti powders, SiC powder, B4C powders, PEG4000 and absolute ethyl alcohol are according to 0.1:1.5:2.5: 0.1:20 mass ratio is mixed and moved into polytetrafluoroethylene (PTFE) ball grinder, according still further to 4:The ratio of grinding media to material of 1 ratio of grinding media to material is added Ball-milling medium ZrO2Ball, then the ball milling 48h under 200r/min rotating speed, then the mixed slurry after ball milling is placed in 80 DEG C of vacuum 8h is dried in drying box, complex phase powder is obtained;
Complex phase powder obtained by step 1 is placed in vacuum sintering funace by step 2., treats that vacuum reaches 6.63 × 10- 3During Pa, 1h is sintered under 1800 DEG C of sintering temperature and 20MPa sintering pressure, furnace cooling obtains Ti enhancings B4C/SiC Complex phase ceramic.
Complex phase ceramic prepared by the present embodiment is characterized:It is 97.2% to measure relative density, and microhardness is 36.3GPa, bending strength is 456.6MPa, and fracture toughness is 4.76MPam1/2.The SEM figures obtained according to morphology characterization can be with Learn, the close structure of the complex phase ceramic prepared by the present embodiment simultaneously there are part Minute pores, and grain size distribution difference is larger, There is the ceramic particle of large-size, grain contours are clear, possess grain boundary fracture and with the mixed fracture mould of a small amount of transgranular fracture Formula.XRD signs are carried out to the complex phase ceramic prepared by the present embodiment, it can be seen from the spectrogram of gained, main thing phase component is B4C, SiC and unconspicuous TiB2, TiB2It is Ti and B4The product that interfacial reaction is obtained occurs between C.
Comparative example 1
Step 1. is by SiC powder, B4C powders, PEG4000 and absolute ethyl alcohol are according to 1.5:2.5:0.1:20 mass ratio Mixed and moved into polytetrafluoroethylene (PTFE) ball grinder, according still further to 4:1 ratio of grinding media to material adds ball-milling medium ZrO2Ball, Ran Hou Ball milling 48h under 150r/min rotating speed, then the mixed slurry after ball milling is placed in 80 DEG C of vacuum drying chambers dry 8h, answered Phase powder;
Complex phase powder obtained by step 1 is placed in vacuum sintering funace by step 2., treats that vacuum reaches 6.63 × 10- 3During Pa, 2h is sintered under 1950 DEG C of sintering temperature and 30MPa sintering pressure, furnace cooling obtains B4C/SiC complex phases are made pottery Porcelain.
Complex phase ceramic prepared by this comparative example is characterized:It is 94.1% to measure relative density, and microhardness is 44.5GPa, bending strength is 337.2MPa, and fracture toughness is 3.13MPam1/2.It can be seen from Fig. 5, prepared by this comparative example Complex phase ceramic in crystal grain it is larger, stomata is more, and fracture is generally the splitting fracture of whole crystal grain, and material property is poor, is not implemented and causes Densification is sintered.
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 (4)

1. a kind of Ti strengthens B4C/SiC complex phase ceramics, it is characterised in that:The complex phase ceramic is to adopt to prepare with the following method 's:
Step 1. is by Ti powders, SiC powder, B4C powders, polyethylene glycol and absolute ethyl alcohol are according to 0.1~1:1.5:2.5:0.1: 20 mass ratio is mixed and moved into ball grinder, adds ball-milling medium, then turning in 150r/min~200r/min The lower ball milling 12h~48h of speed, then the mixed slurry after ball milling is dried in vacuo, obtain complex phase powder;
Complex phase powder is placed in vacuum sintering funace and carries out vacuum heating-press sintering by step 2., cooling, obtains the Ti enhancings B4C/SiC complex phase ceramics;
Wherein, the vacuum in vacuum sintering funace is not less than 6.63 × 10-3Pa, 1800 DEG C~1950 DEG C of sintering temperature is burnt Knot pressure power 20MPa~30MPa, sintering time 1h~2h.
2. a kind of Ti enhancings B according to claim 14C/SiC complex phase ceramics, it is characterised in that:The average grain diameter of Ti powders For 3 μm~5 μm, the average grain diameter of SiC powder for 1 μm~5 μm, B4The average grain diameter of C powders is 3 μm~10 μm.
3. a kind of Ti enhancings B according to claim 14C/SiC complex phase ceramics, it is characterised in that:The material of the ball-milling medium Matter is ZrO2
4. a kind of Ti enhancings B according to claim 14C/SiC complex phase ceramics, it is characterised in that:Ti powders, SiC powder, B4The mass ratio of C powders, polyethylene glycol and absolute ethyl alcohol is 1:1.5:2.5:0.1:20.
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Cited By (8)

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CN108558428A (en) * 2018-05-21 2018-09-21 合肥工业大学 A kind of composite interlayer and its Joining Technology for spreading connection silicon carbide ceramics
CN108751997A (en) * 2018-07-26 2018-11-06 北京理工大学 A kind of B4C-TiB2- SiC composite ceramics block and its fast preparation method
CN108794013A (en) * 2018-07-26 2018-11-13 北京理工大学 A kind of B4C ceramic blocks and its fast preparation method
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CN108558428A (en) * 2018-05-21 2018-09-21 合肥工业大学 A kind of composite interlayer and its Joining Technology for spreading connection silicon carbide ceramics
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
CN108751997B (en) * 2018-07-26 2021-04-27 北京理工大学 B4C-TiB2-SiC composite ceramic block and rapid preparation method thereof
CN108794013A (en) * 2018-07-26 2018-11-13 北京理工大学 A kind of B4C ceramic blocks and its fast preparation method
CN108751997A (en) * 2018-07-26 2018-11-06 北京理工大学 A kind of B4C-TiB2- SiC composite ceramics block and its fast preparation method
CN108794013B (en) * 2018-07-26 2021-05-04 北京理工大学 B4C ceramic block and rapid preparation method thereof
CN110204337A (en) * 2019-06-04 2019-09-06 中南大学 A kind of preparation method and its boron carbide ceramics material of space flight gyroscope bearing boron carbide ceramics material
CN110204337B (en) * 2019-06-04 2021-04-30 中南大学 Preparation method of boron carbide ceramic material for aerospace gyroscope bearing and boron carbide ceramic material
CN110976886A (en) * 2019-12-20 2020-04-10 中南大学 Boride/alloy composite material and preparation method and application thereof
CN110976886B (en) * 2019-12-20 2022-03-04 中南大学 Boride/alloy composite material and preparation method and application thereof
CN113213941A (en) * 2021-05-24 2021-08-06 南京工程学院 BCN nano amorphous phase strengthening and toughening TiB2-B4Preparation method of C complex phase ceramic
CN113213941B (en) * 2021-05-24 2022-03-18 南京工程学院 BCN nano amorphous phase strengthening and toughening TiB2-B4Preparation method of C complex phase ceramic
CN114907126A (en) * 2022-04-29 2022-08-16 南京工程学院 Multi-dimensional nanocarbon structure TiB 2 -SiC-B 4 C-structure function integrated composite material and preparation method thereof
CN114907126B (en) * 2022-04-29 2022-12-02 南京工程学院 Multi-dimensional nano carbon structure TiB 2 -SiC-B 4 C-structure function integrated composite material and preparation method thereof

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