CN104841944A - Gel method preparation process for SiC/Al composite powder - Google Patents

Gel method preparation process for SiC/Al composite powder Download PDF

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Publication number
CN104841944A
CN104841944A CN201410747019.2A CN201410747019A CN104841944A CN 104841944 A CN104841944 A CN 104841944A CN 201410747019 A CN201410747019 A CN 201410747019A CN 104841944 A CN104841944 A CN 104841944A
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sic
slurry
premixed liquid
gel
composite granule
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CN201410747019.2A
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杜晓明
刘凤国
张学萍
衣爱丽
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Shenyang Ligong University
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Shenyang Ligong University
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Abstract

The invention discloses a gel method preparation process for SiC/Al composite powder. The gel method preparation process for the SiC/Al composite powder includes the following steps that a premixed solution A and a premixed solution B with certain components are obtained through wet method mixing; 7.24 parts of SiC powder is added into the premixed solution A and stirred for 2-5 min through an ultrasonic blending machine, and a slurry A is obtained; 6.73 parts of Al powder is added into the premixed solution B and stirred for 10-20 min mechanically, and a slurry B is obtained; the slurry A is added into the slurry B multiple times and mixed for 20-30 min, then catalysts-initiators for catalyzing gel component gel-clot reaction are added, the slurry is promoted to be solidified to form a wet blank, and the process is less than 30 s; after the wet blank is dried and degreased, two-phase uniformly dispersed composite powder is obtained. Instability of mechanical properties caused by enhanced phase agglomeration in the composite materials is avoided, the enhanced phase proportion in the composite powder can be adjusted within the range of 5-38 percent, and the application range is enlarged.

Description

A kind of gel method preparation technology of SiC/Al composite granule
Technical field
The present invention relates to the preparation field of composite granule, be specifically related to a kind of gel method preparation technology of SiC/Al composite granule.
Background technology
SiC/Al composite is widely used in multiple field such as electronic package material, high-abrasive material with its excellent electric property, anti-wear performance and high-temperature stability.At present, what the preparation method of SiC/Al composite was comparatively ripe is high-energy ball milling method, pressure infiltration method etc., it is not high that the composite Problems existing of preparation is mainly the finished product rate that two-phase disperses not thoroughly to cause, and in use there is the problems such as serious, the unstable properties of short, Aging Damage in service life in certified products, the performance of drastic delimitations SiC/Al composite and the field of use.
Summary of the invention
For solving the problem, the invention provides a kind of gel method preparation technology of SiC/Al composite granule, the dispersing uniformity of two-phase in composite obtained by improving, avoid in composite because the reunite mechanical property brought of wild phase is unstable, and in composite powder, wild phase ratio is adjustable between 5%-38% (volume fraction), has expanded the range of application of this material.
For achieving the above object, the technical scheme that the present invention takes is:
A gel method preparation technology for SiCAl composite granule, comprises the steps:
S1, employing material by wet type mixing, the premixed liquid of preparation certain ingredients, obtains premixed liquid A and premixed liquid B;
S2, add in the premixed liquid A of step S1 gained by 7.24 parts of SiC powder, ultrasonic cooperative mechanical stirs 2-5min, obtains slurry A; 6.73 parts of A1 powder power are entered the premixed liquid B of step S1 gained, mechanical agitation 10-20min, obtains slurry B simultaneously;
S3, add in slurry B several times by above-mentioned slurry A, after mixing 20-30min, add the catalyst-initiator of catalysis colloid composition gel reaction, impel slurry curing to form wet base, this process is no more than 30s;
S4, to after the wet base drying of step S3 gained, ungrease treatment, obtain the finely dispersed composite granule of two-phase.
Wherein, in described step S1, the composition of premixed liquid A is: percentage by weight is the acrylamide of 2%, and all the other are deionized water (or absolute ethyl alcohol or acetone).
Wherein, in described step S1, the composition of premixed liquid B is: percentage by weight is the acrylamide of 2%, and all the other are deionized water (or absolute ethyl alcohol or acetone).
Wherein, in described step S3, dispersant, catalyst and initator are respectively polyvinylpyrrolidone (2.0wt.%), N-N ,-bismethacrylamide (0.225g/100ml slurry) and tetramethylethylenediamine (0.5ml/100ml slurry).
Wherein, in described step S4, the method for wet base drying is after drying at room temperature 48h, dry 24h at the temperature of 70 DEG C.
Wherein, in described step S4, the temperature of ungrease treatment is 100 DEG C-450 DEG C.
The present invention has following beneficial effect:
The problem that composite two-phase is not disperseed can be solved completely, the uniformity of two-phase dispersion in the raising material of the SiC/Al composite energy high degree produced, and then improve serviceability and the product design qualification rate of product formed thereby, in composite, wild phase ratio is adjustable between 5%-38% (volume fraction), and forming property is stablized, the profile qualification rate of product can reach more than 98%, and the scope of application is wide; Process operation is simple, does not need complexity, special process equipment; Except raw material reasonable loss, the utilization rate of solid phase powder can reach 100%, reduces production cost.
Accompanying drawing explanation
Fig. 1 is present invention process procedure chart;
The composition of premixed liquid and consumption when Fig. 2 is material by wet type mixing of the present invention, in figure, monomer is acrylamide (2.0wt.%), dispersant be polyvinylpyrrolidone (2.0wt.%), catalyst and initator is N-N '-bismethacrylamide (0.225g/100ml slurry) and tetramethylethylenediamine (0.5ml/100ml slurry).
Fig. 3 is the drying technology process in Fig. 1.
Fig. 4 is the equipment drawing adopted in Debinding Process of the present invention.
In figure, 1-resistive heater; 2-sample; 3-cushion block; 4-bell; 5-body of heater.
Fig. 5 is the electron scanning micrograph after composite granule degreasing:
A () SiC volume fraction is 17%.
B () SiC volume fraction is 25%.
Detailed description of the invention
In order to make objects and advantages of the present invention clearly understand, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
As shown in Figure 4, this equipment specifically implementing to adopt comprises body of heater 5 and is arranged on the bell 4 on body of heater 5, is provided with some resistive heaters 1, is also provided with cushion block 3 in described body of heater 5, for placing sample 2 in described body of heater 5.
As shown in Figure 1, Figure 3, embodiments provide a kind of gel method preparation technology of SiC/Al composite granule, comprise the steps:
S1, employing material by wet type mixing, the premixed liquid of preparation certain ingredients, obtains premixed liquid A and premixed liquid B;
S2, add in the premixed liquid A of step S1 gained by 7.24 parts of SiC powder, ultrasonic cooperative mechanical stirs 2-5min, obtains slurry A; 6.73 parts of Al powder are added the premixed liquid B of step S1 gained, mechanical agitation 10-20min, obtains slurry B simultaneously;
S3, add in slurry B several times by above-mentioned slurry A, after mixing 20-30min, add the catalyst-initiator of catalysis colloid composition gel reaction, impel slurry curing to form wet base, this process is no more than 30s;
S4, to after the wet base drying of step S3 gained, ungrease treatment, obtain the finely dispersed composite granule of two-phase.
In described step S1, the composition of premixed liquid A is: percentage by weight is the acrylamide of 2%, and all the other are deionized water.
In described step S1, the composition of premixed liquid B is: percentage by weight be 2% acrylamide, N-N '-bismethacrylamide (0.225g/100ml slurry), tetramethylethylenediamine (0.5ml/100ml slurry), percentage by weight be the polyvinylpyrrolidone of 2%, all the other are deionized water.
In described step S3, dispersant, catalyst and initator are respectively polyvinylpyrrolidone
(2.0wt.%), N-N '-bismethacrylamide (0.225g/100ml slurry) and tetramethylethylenediamine (0.5ml/100ml slurry).In described step S4, the method for wet base drying is after drying at room temperature 48h, dry 24h at the temperature of 70 DEG C.The temperature of ungrease treatment in described step S4 is 100 DEG C-450 DEG C.
Embodiment 1
According to slurry A and the slurry B of different premixed liquid composition, repeatedly added in slurry B on a small quantity by slurry A and mix 20-30min, now in slurry, solid phase tends towards stability uniform dispersion substantially; Add catalysis-initiator system in the slurry, impel colloid composition solidification in slurry, this process is no more than 30s; According to Fig. 3 technical process, room temperature/48h, 70 DEG C/24h drying is carried out to base substrate, base substrate after drying is carried out 100 DEG C of-450 DEG C of ungrease treatments in Fig. 4 equipment, namely obtains the composite granule of uniform composition.It is electron scanning micrograph after the composite granule degreasing of 17% and 25% that Fig. 5 (a) and (b) are respectively SiC volume fraction content.Out-of-shape in figure and to be with angular be SiC.Observe the distribution of SiC in composite powder, in known composite powder, SiC is dispersed in around Al particle uniformly, without obvious clustering phenomena, shows that in composite granule, the deployment conditions of two-phase is good.
This concrete enforcement can solve the problem that composite two-phase is not disperseed completely, the uniformity of two-phase dispersion in the raising material of the SiC/Al composite energy high degree produced, and then improve serviceability and the product design qualification rate of product formed thereby, in composite, wild phase ratio is adjustable between 5%-38% (volume fraction), and forming property is stablized, the profile qualification rate of product can reach more than 98%, and the scope of application is wide; Process operation is simple, does not need complexity, special process equipment; Except raw material reasonable loss, the utilization rate of solid phase powder can reach 100%, reduces production cost.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.

Claims (6)

1. a gel method preparation technology for SiC/Al composite granule, is characterized in that, comprise the steps:
S1, employing material by wet type mixing, the premixed liquid of preparation certain ingredients, obtains premixed liquid A and premixed liquid B;
S2, add in the premixed liquid A of step S1 gained by 7.24 parts of SiC powder, ultrasonic cooperative mechanical stirs 2-5min, obtains slurry A; 6.73 parts of Al powder are added the premixed liquid B of step S1 gained, mechanical agitation 10-20min, obtains slurry B simultaneously;
S3, add in slurry B several times by above-mentioned slurry A, after mixing 20-30min, add the catalyst-initiator of catalysis colloid composition gel reaction, impel slurry curing to form wet base, this process is no more than 30s;
S4, to after the wet base drying of step S3 gained, ungrease treatment, obtain the finely dispersed composite granule of two-phase.
2. the gel mixing procedure of SiC/Al composite granule according to claim 1, is characterized in that, in described step S1, the composition of premixed liquid A is: percentage by weight is the acrylamide of 2%, and all the other are deionized water.
3. the gel mixing procedure of SiC/Al composite granule according to claim 1, is characterized in that, in described step S1, the composition of premixed liquid B is: percentage by weight is the acrylamide of 2%, and all the other are deionized water.
4. the gel mixing procedure of SiC/Al composite granule according to claim 1, is characterized in that, in described step S3, dispersant, catalyst and initator are respectively polyvinylpyrrolidone, N-N '-bismethacrylamide and tetramethylethylenediamine.
5. the gel mixing procedure of SiC/Al composite granule according to claim 1, is characterized in that, in described step S4, the method for wet base drying is after drying at room temperature 48h, dry 24h at the temperature of 70 DEG C.
6. the gel mixing procedure of SiC/Al composite granule according to claim 1, is characterized in that, the temperature of ungrease treatment in described step S4 is 100 DEG C-450 DEG C.。
CN201410747019.2A 2014-12-01 2014-12-01 Gel method preparation process for SiC/Al composite powder Pending CN104841944A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108580922A (en) * 2018-04-13 2018-09-28 东北大学 A method of preparing high-performance aluminum base silicon carbide

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101016591A (en) * 2007-03-08 2007-08-15 北京科技大学 Method of preparing SiCp/Al composite material with complicated shape and high volume percent ratio
CN101892398A (en) * 2010-07-01 2010-11-24 西安理工大学 Method for preparing ceramic/aluminum alloy gradient composite material

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101016591A (en) * 2007-03-08 2007-08-15 北京科技大学 Method of preparing SiCp/Al composite material with complicated shape and high volume percent ratio
CN101892398A (en) * 2010-07-01 2010-11-24 西安理工大学 Method for preparing ceramic/aluminum alloy gradient composite material

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
衣爱丽等: "SiCp /Al 复合材料的凝胶法混料工艺研究", 《沈阳理工大学学报》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108580922A (en) * 2018-04-13 2018-09-28 东北大学 A method of preparing high-performance aluminum base silicon carbide

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