CN105967186A - Method for purifying SiC powder crystal structure and improving roundness of SiC powder crystal structure - Google Patents

Method for purifying SiC powder crystal structure and improving roundness of SiC powder crystal structure Download PDF

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CN105967186A
CN105967186A CN201610292864.4A CN201610292864A CN105967186A CN 105967186 A CN105967186 A CN 105967186A CN 201610292864 A CN201610292864 A CN 201610292864A CN 105967186 A CN105967186 A CN 105967186A
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sic powder
sic
crystal structure
carrying
deionized water
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CN105967186B (en
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汪冬梅
吴玉程
汤文明
郑治祥
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Hefei University of Technology
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Hefei University of Technology
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity

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Abstract

The invention relates to a method for purifying a SiC powder crystal structure and improving roundness of the SiC powder crystal structure. The method comprises a, putting SiC powder in a high temperature tank-type resistance furnace, heating the SiC powder to a temperature of 1300-1600 DEG C, carrying out calcining in air for 3-7h and carrying out furnace cooling to the room temperature, b, adding mixed acid into the product, stirring the mixture for 10-12h, carrying out standing for 12-24h, washing the mixture by deionized water until pH is 7.0 and then carrying out drying, c, putting the SiC powder in a high temperature sintering furnace, heating the SiC powder to a temperature of 1800-2200 DEG C, carrying out calcining in argon for 3-7h and carrying out furnace cooling to the room temperature, and d, adding the SiC powder in the mixed acid, carrying out stirring for 10-12h, carrying out standing for 12-24h, washing the SiC powder by deionized water until pH is 7.0 and carrying out drying. The method improves a SiC crystal crystallization degree, improves SiC particle isomer phenomenon and reduces crystal structure and geometric profile defect-caused influence on SiC/Al composite material performances.

Description

A kind of purification SiC powder crystal structure and the method improving its roundness
Technical field
A kind of method that the present invention relates to SiC powder Regularization pretreatment, specifically a kind of purification SiC is brilliant Body structure and the method for regular SiC particulate profile.
Background technology
High-volume fractional SiC/Al composite has high thermal conductivity and low thermal coefficient of expansion concurrently, at electronics and optics The aspects such as device have important application.And SiC/Al composite gauge good stability, specific strength and compare bullet Property modulus high, the prices of raw materials are less than the l/10 of encapsulating material tungsten-copper alloy, and the most not and 1/5, this does not makes weight Obtain it and have irreplaceable advantage in electronic package material field, at Aeronautics and Astronautics structural member, automobile component Etc. aspect also will have wide application space.SiC/Al composite is mainly by aluminium alloy phase and SiC ceramic phase Constituting, wherein the crystal structure of SiC and granule-morphology thereof affect preparation and the performance of SiC/Al composite. From structure, the most basic construction unit of SiC lattice is by SiC4 and the CSi4 tetrahedron group mutually interted Become, there is more than 250 kind of isomer, and the C/Si diatomic layer stacking order of each of the configurations body is each not Identical.The polytype structure mixed necessarily affects the excellent properties of SiC and is not fully exerted.From SiC Seeing in particle shape looks, owing to SiC hardness is high, self-sharpening is strong, profile is many in irregular cerioid.SiC shape is more When irregularly will make compression molding, forming pressure is bigger, and the abrasion of shaping dies is more serious, the life-span of mould The shortest.And, in prepared SiC/Al composite, on the one hand, SiC particulate shape more irregularly, Corner angle are the most sharp-pointed, easily cause stress to be concentrated, and reduce composite material strength.On the other hand, SiC particulate shape More irregularly, under same volume mark, its surface area is the biggest, and interface resistance is the biggest, and therefore its thermal conductivity is the lowest. Therefore, good high-volume fractional SiC/Al composite, the simplification of SiC crystal structure and SiC to be prepared The regularization of granule profile is particularly important.
Summary of the invention
It is contemplated that: a kind of purification SiC powder crystal structure and the method improving its roundness are provided, are used for Improve the degree of crystallinity of SiC crystal, improve the isomer phenomenon of SiC particulate, thus reduce crystal structure and geometry The defects such as profile are on follow-up prepared SiC/Al composite property impact.
In order to realize foregoing invention purpose, the present invention provides following technical scheme:
A kind of purification SiC powder crystal structure and the method improving its roundness, comprise the following steps:
A, SiC powder is placed in high temperature box type resistance furnace, is warming up to 1300～1600 DEG C and calcines in air After 3～7h, cool to room temperature with the furnace；
B, will by a step process SiC powder add mixed acid stirring 10～12h after, stand 12～24h, With deionized water clean to pH value be 7.0 post-dryings；
C, by through b step pickling dry after SiC powder be placed in high temperature sintering furnace, be warming up to 1800～ In argon, calcine 3～7h, cool to room temperature with the furnace for 2200 DEG C；
D, the SiC powder addition mixed acid that will process by step c stir 10～12h, stand 12～24h, Deionized water clean to pH value be in drying after 7.0；
Wherein, the mixed acid in step b, d is by deionized water, HF, HCl, HNO3Configuration forms.
Further, in step a, c, heating rate is 5～10 DEG C/min.
Further, the mixed acid in step b be by deionized water, concentration be 40%HF, concentration be 37.5% HCl, concentration are the HNO of 65%～68%3Being prepared from, its volume proportion is 100:(20～60): 30: 10。
Further, the mixed acid in step d be by deionized water, concentration be 40%HF, concentration be 37.5% HCl, concentration are the HNO of 65%～68%3Being prepared from, its volume proportion is 100:(10～40): 30: 10。
Further, the drying temperature in step b and d is 40～120 DEG C.
Compared with the prior art, beneficial effects of the present invention is embodied in:
1, the present invention uses high-temperature calcination and mixing pickling to process SiC powder.Purification and Regularization SiC particulate, in the preparation of follow-up SiC/Al composite, reduces compacting during beneficially SiC prefabricated component compression molding Power, alleviates the abrasion of mould.
2, the SiC/Al that the SiC frit use of regularization of the present invention is prepared at follow-up employing pressureless infiltration is combined In material, improve the wellability of SiC and Al, and regular SiC particulate is uniformly distributed and subtracts in the composite Little stress concentration, reduces interface resistance, beneficially composite material strength and the improvement of heat conductivility.
Accompanying drawing explanation
Fig. 1 is the XRD figure spectrum before and after SiC powder processes；
Fig. 2 is SiC powder stereoscan photograph SEM before treatment；
Fig. 3 is stereoscan photograph SEM after SiC powder processes.
Detailed description of the invention
Below by way of detailed description of the invention, the invention will be further described, and non-limiting examples is as follows.
Embodiment 1:
A kind of purification SiC powder crystal structure and the method improving its roundness, comprise the following steps:
A, powder is placed in chamber type electric resistance furnace, is warming up to air at 1600 DEG C with the heating rate of 5 DEG C/min Middle calcining 5h, cools to room temperature with the furnace；
B, by adding by deionized water, HF (40%), HCl (37.5%) by the SiC powder of a step process and HNO3The certain density mixed acid stirring 12h that (65%～68%) is prepared, stands 12h, and deionized water cleans extremely PH value is to dry in 60 DEG C of temperature after 7.0, mixed acid volume proportion: H2O:HF (40%): HCl (37.5%): HNO3(65%～68%)=100:30:30:10.
C, again by through b step pickling dry after SiC powder be placed in high temperature sintering furnace, with 5 DEG C/min's Heating rate calcines 3h at 1900 DEG C in argon, cool to room temperature with the furnace；
D, the SiC powder that processes by step c is added by deionized water, HF (40%), HCl (37.5%) and HNO3Stirring 10h in the certain density mixed acid that (65%～68%) is prepared, stand 12h, deionized water cleans It is to dry in 60 DEG C of temperature after 7.0 to pH value.Mixed acid volume proportion: H2O:HF (40%): HCl (37.5%): HNO3(65%～68%)=100:20:30:10.
Embodiment 2
A kind of purification SiC powder crystal structure and the method improving its roundness, comprise the following steps:
A, powder is placed in chamber type electric resistance furnace, is warming up to air at 1300 DEG C with the heating rate of 8 DEG C/min Middle calcining 7h, cools to room temperature with the furnace；
B, by adding by deionized water, HF (40%), HCl (37.5%) by the SiC powder of a step process and HNO3The certain density mixed acid stirring 10h that (65%～68%) is prepared, stands 15h, and deionized water cleans extremely PH value is to dry in 120 DEG C of temperature after 7.0, mixed acid proportioning: H2O:HF (40%): HCl (37.5%): HNO3(65%～68%)=100:40:30:10.
C, again by through b step pickling dry after SiC powder be placed in high temperature sintering furnace, with 8 DEG C/min's Heating rate calcines 7h at 1300 DEG C in argon, cool to room temperature with the furnace；
D, the SiC powder that processes by step c is added by deionized water, HF (40%), HCl (37.5%) and HNO3Stirring 10h in the certain density mixed acid that (65%～68%) is prepared, stand 15h, deionized water cleans It is to dry in 120 DEG C of temperature after 7.0 to pH value.Mixed acid proportioning: H2O:HF (40%): HCl (37.5%): HNO3(65%～68%)=100:10:30:10.
Embodiment 3
A kind of purification SiC powder crystal structure and the method improving its roundness, comprise the following steps:
A, powder is placed in chamber type electric resistance furnace, is warming up to air at 1500 DEG C with the heating rate of 10 DEG C/min Middle calcining 5h, cools to room temperature with the furnace；
B, by adding by deionized water, HF (40%), HCl (37.5%) by the SiC powder of a step process and HNO3The certain density mixed acid stirring 11h that (65%～68%) is prepared, stands 18h, and deionized water cleans extremely PH value is to dry in 80 DEG C of temperature after 7.0, mixed acid proportioning: H2O:HF (40%): HCl (37.5%): HNO3(65%～68%)=100:20:30:10.
C, again by through b step pickling dry after SiC powder be placed in high temperature sintering furnace, with 10 DEG C/min's Heating rate calcines 5h at 1500 DEG C in argon, cool to room temperature with the furnace；
D, the SiC powder that processes by step c is added by deionized water, HF (40%), HCl (37.5%) and HNO3Stirring 11h in the certain density mixed acid that (65%～68%) is prepared, stand 18h, deionized water cleans It is to dry in 80 DEG C of temperature after 7.0 to pH value.Mixed acid proportioning: H2O:HF (40%): HCl (37.5%): HNO3(65%～68%)=100:20:30:10.
Fig. 1 is the XRD figure spectrum before and after SiC powder processes；SiC powder X-ray diffraction peak value after process Being remarkably reinforced, SiC degree of crystallinity is improved.
Fig. 2,3 it is that SiC powder processes forward and backward stereoscan photograph SEM；SiC particulate particle diameter before processing Not of uniform size, corner angle are sharply clearly demarcated, mostly are irregular block or strip.After process, SiC particulate particle diameter is distributed relatively Uniformly, grain corner is passivated, and it is blunt that contour edge tends to circle, and corner angle acuteness disappears substantially, SiC particulate shape Tend to regular.
The present invention illustrates the detailed process flow of the present invention by above-described embodiment, but the invention is not limited in Above-mentioned detailed process flow, does not i.e. mean that the present invention has to rely on above-mentioned detailed process flow and could implement.Institute Belong to those skilled in the art it will be clearly understood that any improvement in the present invention, raw material each to product of the present invention Equivalence is replaced and the interpolation of auxiliary element, concrete way choice etc., all falls within protection scope of the present invention and public affairs Within the scope of opening.

Claims (5)

1. a purification SiC powder crystal structure and the method improving its roundness, it is characterised in that: include Following steps:
A, SiC powder is placed in high temperature box type resistance furnace, is warming up to 1300～1600 DEG C and calcines in air After 3～7h, cool to room temperature with the furnace；
B, will by a step process SiC powder add mixed acid stirring 10～12h after, stand 12～24h, With deionized water clean to pH value be 7.0 post-dryings；
C, by through b step pickling dry after SiC powder be placed in high temperature sintering furnace, be warming up to 1800～ In argon, calcine 3～7h, cool to room temperature with the furnace for 2200 DEG C；
D, the SiC powder addition mixed acid that will process by step c stir 10～12h, stand 12～24h, Deionized water cleaning is 7.0 post-dryings to pH value；
Wherein, the mixed acid in step b, d is by deionized water, HF, HCl, HNO3Configuration forms.
Purification SiC powder crystal structure the most according to claim 1 and the method improving its roundness, It is characterized in that: in step a, c, heating rate is 5～10 DEG C/min.
Purification SiC powder crystal structure the most according to claim 1 and the method improving its roundness, It is characterized in that: the mixed acid in step b be by deionized water, concentration be 40%HF, concentration be 37.5% HCl, concentration are the HNO of 65%～68%3Being prepared from, its volume proportion is 100:(20～60): 30: 10。
Purification SiC powder crystal structure the most according to claim 1 and the method improving its roundness, It is characterized in that: the mixed acid in step d be by deionized water, concentration be 40%HF, concentration be 37.5% HCl, concentration are the HNO of 65%～68%3Being prepared from, its volume proportion is 100:(10～40): 30: 10。
Purification SiC powder crystal structure the most according to claim 1 and the method improving its roundness, It is characterized in that: the drying temperature in step b and d is 40～120 DEG C.
CN201610292864.4A 2016-05-03 2016-05-03 A method of purifying SiC powders crystal structure and its roundness of improvement Active CN105967186B (en)

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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101659412A (en) * 2009-09-18 2010-03-03 江苏乐园新材料集团有限公司 Preparation method of single crystal silicon carbide special materials

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101659412A (en) * 2009-09-18 2010-03-03 江苏乐园新材料集团有限公司 Preparation method of single crystal silicon carbide special materials

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