CN109848415B - Preparation method of 3D-shaped SiCp/Al complex structure - Google Patents

Preparation method of 3D-shaped SiCp/Al complex structure Download PDF

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CN109848415B
CN109848415B CN201910185391.1A CN201910185391A CN109848415B CN 109848415 B CN109848415 B CN 109848415B CN 201910185391 A CN201910185391 A CN 201910185391A CN 109848415 B CN109848415 B CN 109848415B
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sicp
complex structure
powder
silica sol
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CN109848415A (en
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成夙
靳来振
许腾腾
曾涛
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Harbin University of Science and Technology
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Abstract

A preparation method of a 3D forming SiCp/Al complex structure relates to a preparation method of a SiCp/Al complex structure (lattice structure), in particular to a method for preparing a SiCp/Al lattice structure by adopting a 3D forming technology. The invention aims to solve the problem that the traditional processing method can not manufacture the SiCp/Al complex structure. The preparation method comprises the following steps: firstly, preparing mixed powder; secondly, setting parameters; thirdly, preparing a prefabricated part; fourthly, thermal curing; fifthly, glue permeation; sixthly, degreasing; and seventhly, sintering to obtain the SiCp/Al complex structure. Has the advantages that: the SLS forming machine is used, the laser sintering technology is selected, 3D forming is carried out, a mold is not needed, digital forming of the SiCp/Al prefabricated part with the complex structure is achieved, secondary processing forming of the SiCp/Al composite material is avoided, and the problem that the SiCp/Al complex structure is difficult to form is solved. The method is mainly used for preparing the SiCp/Al complex structure.

Description

Preparation method of 3D-shaped SiCp/Al complex structure
Technical Field
The invention relates to a preparation method of a SiCp/Al complex structure (lattice structure), in particular to a method for preparing the SiCp/Al lattice structure by adopting a 3D forming technology.
Background
The silicon carbide particle reinforced aluminum matrix composite has the advantages of high strength, high rigidity, good electrical conductivity, excellent wear resistance, high temperature resistance and the like, and has been practically applied as a bearing structural member, an optical and precise instrument member, an electronic packaging and a thermal control element in the field of aerospace. However, the SiCp/Al material is difficult to machine and form due to the excellent wear resistance of the SiCp/Al material, and the part with a complex inner cavity structure cannot be manufactured by the traditional machining method. The method comprises the steps of forming a prefabricated part of silicon carbide and aluminum powder through Selective Laser Sintering (SLS), degreasing and sintering the prefabricated part to obtain the SiCp/Al composite material, and finally realizing near-net forming of the SiCp/Al complex structural part.
Document 1 "Xiong Hupping, Xiong Bowen, et Al. effects of composites on dimensional access and mechanical properties of SiC composites for a modulated by selective laser sintering. composites Part B,2013,44(1): 480-.
Document 2 "Astfalck Lachlan Connor, Kelly Gemma Kaye, et Al, on the Break down of SiC reducing the Selective Laser mean of Aluminum matrix Materials, 2017,19(8): 1600835" discloses a process for preparing SiCp/Al composite Materials by Selective Laser Melting, in which SiC reacts directly with Al during the shaping process to form a large amount of Al4C3The reaction product has a great influence on the interface combination and the material performance.
The traditional method for preparing the SiCp/Al complex structure has the characteristics of difficult molding and difficult processing, and parts with complex inner cavity structures cannot be manufactured by the traditional processing method.
Disclosure of Invention
The invention aims to solve the problem that the traditional processing method cannot manufacture a SiCp/Al complex structure, and provides a preparation method of a 3D forming SiCp/Al complex structure.
A preparation method of a 3D forming SiCp/Al complex structure comprises the following steps:
firstly, preparing mixed powder: mixing SiC powder and aluminum powder, adding a binder, and mixing for 24-48 h in a V-shaped mixer to obtain mixed powder; the mass ratio of the SiC powder to the aluminum powder is (50-70) to (30-50); the mass fraction of the binder in the mixed powder is 5-15%;
secondly, setting parameters: introducing the STL format file into an SLS forming machine, setting the scanning speed to be 1000-2000 mm/s, the thickness of each layer to be 0.05-0.2 mm, and the preheating temperature to be 40-70 ℃, and then processing the model into a sheet with a set thickness by using computer layered slicing software;
thirdly, preparing a prefabricated part: adding the mixed powder into a working cylinder of an SLS forming machine, spreading the powder by using a rolling shaft, standing for 25-35 min, heating the working cylinder to a preheating temperature according to the preheating temperature set in the second step of 40-70 ℃, starting processing according to the scanning speed set in the second step of 1000-2000 mm/s and the thickness of each layer of 0.05-0.2 mm, carrying out laser sintering, feeding and spreading the powder by using a powder feeding cylinder, sintering layer by layer, drying for 50-70 min at the temperature of 40-70 ℃, and taking out to obtain a SiCp/Al prefabricated part;
fourthly, thermal curing: carrying out heat curing on the SiCp/Al prefabricated member for 2-3 h at the temperature of 200-300 ℃ to obtain a heat-cured SiCp/Al prefabricated member;
fifthly, glue permeation: impregnating silica sol on the surface of the SiCp/Al prefabricated member after thermosetting to obtain a glue-impregnated SiCp/Al prefabricated member;
sixthly, degreasing: placing the infiltrated SiCp/Al prefabricated member in a vacuum sintering furnace, and degreasing at 500-700 ℃ for 1-2 h to obtain a degreased SiCp/Al prefabricated member;
seventhly, sintering: sintering the degreased SiCp/Al prefabricated member in a vacuum sintering furnace at the temperature of 700-1200 ℃, wherein the sintering time is 1-3 h, and cooling to room temperature along with the furnace to obtain the SiCp/Al complex structure.
The principle and the beneficial effects of the invention are as follows: the SiCp/Al complex structure prepared by the method is a SiCp/Al lattice structure, 3D forming is carried out by using an SLS forming machine and selecting a laser sintering technology without a mould, digital forming of the SiCp/Al prefabricated member with the complex structure is realized, secondary processing forming of the SiCp/Al composite material is avoided, and the problem that the SiCp/Al complex structure is difficult to form is solved; secondly, the invention impregnates the silica sol, so that a firm film can be formed on the surface of the prefabricated member in the degreasing process, and the structure of the prefabricated member is ensured to be kept unchanged in the degreasing process; the method of degreasing first and then sintering is adopted, aluminum powder is converted into a matrix of the composite material after sintering, a SiCp/Al lattice structure with higher precision and higher strength is obtained, generation of reaction products of SiC and Al interfaces is reduced, and the problems of influence of the reaction products on interface bonding, material performance and the like are solved; the preparation process is simple, the working hours are few, the process is stable and the reproducibility is good.
Drawings
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is a three-dimensional model of the SiCp/Al preform in the STL format file in step two of example 1;
FIG. 3 is a photograph of a complex SiCp/Al structure obtained in example 1.
Detailed Description
The first embodiment is as follows: the embodiment is a preparation method of a 3D forming SiCp/Al complex structure, which is specifically completed according to the following steps:
firstly, preparing mixed powder: mixing SiC powder and aluminum powder, adding a binder, and mixing for 24-48 h in a V-shaped mixer to obtain mixed powder; the mass ratio of the SiC powder to the aluminum powder is (50-70) to (30-50); the mass fraction of the binder in the mixed powder is 5-15%;
secondly, setting parameters: introducing the STL format file into an SLS forming machine, setting the scanning speed to be 1000-2000 mm/s, the thickness of each layer to be 0.05-0.2 mm, and the preheating temperature to be 40-70 ℃, and then processing the model into a sheet with a set thickness by using computer layered slicing software;
thirdly, preparing a prefabricated part: adding the mixed powder into a working cylinder of an SLS forming machine, spreading the powder by using a rolling shaft, standing for 25-35 min, heating the working cylinder to a preheating temperature according to the preheating temperature set in the second step of 40-70 ℃, starting processing according to the scanning speed set in the second step of 1000-2000 mm/s and the thickness of each layer of 0.05-0.2 mm, carrying out laser sintering, feeding and spreading the powder by using a powder feeding cylinder, sintering layer by layer, drying for 50-70 min at the temperature of 40-70 ℃, and taking out to obtain a SiCp/Al prefabricated part;
fourthly, thermal curing: carrying out heat curing on the SiCp/Al prefabricated member for 2-3 h at the temperature of 200-300 ℃ to obtain a heat-cured SiCp/Al prefabricated member;
fifthly, glue permeation: impregnating silica sol on the surface of the SiCp/Al prefabricated member after thermosetting, repeatedly dipping the silica sol by using a brush and brushing the silica sol on the surface of the prefabricated member until the silica sol is not impregnated any more, and obtaining a glue-impregnated SiCp/Al prefabricated member;
sixthly, degreasing: placing the infiltrated SiCp/Al prefabricated member in a vacuum sintering furnace, and degreasing at 500-700 ℃ for 1-2 h to obtain a degreased SiCp/Al prefabricated member;
seventhly, sintering: sintering the degreased SiCp/Al prefabricated member in a vacuum sintering furnace at the temperature of 700-1200 ℃, wherein the sintering time is 1-3 h, and cooling to room temperature along with the furnace to obtain the SiCp/Al complex structure.
FIG. 1 is a process flow diagram of the present invention.
The second embodiment is as follows: the present embodiment differs from the first embodiment in that: the grain size of the SiC powder in the step one is 280 meshes, and the grain size of the aluminum powder is 280 meshes. The rest is the same as the first embodiment.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: in the step one, the adhesive is epoxy resin. The others are the same as in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment and one of the first to third embodiments is as follows: in the first step, the mass ratio of the SiC powder to the aluminum powder is 1:1, and the mass fraction of the binder in the mixed powder is 5%. The others are the same as the first to third embodiments.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: in the second step, the preheating temperature was set to 57 ℃. The rest is the same as the first to fourth embodiments.
The sixth specific implementation mode: the difference between this embodiment and one of the first to fifth embodiments is as follows: and fifthly, the silica sol is alkaline silica sol, and the viscosity of the alkaline silica sol is less than 10MPa & s at normal temperature. The rest is the same as the first to fifth embodiments.
The seventh embodiment: the difference between this embodiment and one of the first to sixth embodiments is: the concrete process of impregnating the silica sol in the step five is as follows: repeatedly dipping the silica sol by a brush and brushing the silica sol on the surface of the SiCp/Al prefabricated member after the heat curing till the silica sol does not permeate any more. The rest is the same as the first to sixth embodiments.
The specific implementation mode is eight: the difference between this embodiment and one of the first to seventh embodiments is: and in the sixth step, degreasing is carried out at the temperature of 550 ℃, and the degreasing time is 1 h. The rest is the same as the first to seventh embodiments.
The specific implementation method nine: the difference between this embodiment and the first to eighth embodiments is: and seventhly, sintering the degreased SiCp/Al prefabricated member in a vacuum sintering furnace at the temperature of 1000 ℃ for 3 hours, and cooling to room temperature along with the furnace to obtain the SiCp/Al complex structure. The others are the same as the first to eighth embodiments.
The invention is not limited to the above embodiments, and one or a combination of several embodiments may also achieve the object of the invention.
The following tests were carried out to confirm the effects of the present invention
Example 1: a preparation method of a 3D forming SiCp/Al complex structure comprises the following steps:
firstly, preparing mixed powder: mixing SiC powder and aluminum powder, adding a binder, and mixing for 36 hours in a V-shaped mixer to obtain mixed powder; the mass ratio of the SiC powder to the aluminum powder is 50: 50; the mass fraction of the binder in the mixed powder is 5%;
secondly, setting parameters: introducing the STL format file into an SLS forming machine, setting the scanning speed to be 2000mm/s, the thickness of each layer to be 0.1mm, and the preheating temperature to be 57 ℃, and then processing the model into a sheet with the set thickness by using computer layered slicing software;
thirdly, preparing a prefabricated part: adding the mixed powder into a working cylinder of an SLS forming machine, spreading the powder by using a roller, standing for 30min, heating the working cylinder to a preheating temperature according to the preheating temperature set in the step two being 57 ℃, starting processing according to the scanning speed set in the step two being 2000mm/s and the thickness of each layer being 0.1mm, carrying out laser sintering, feeding and spreading the powder by a powder feeding cylinder, then sintering layer by layer, drying for 60min at the temperature of 57 ℃, and taking out to obtain a SiCp/Al prefabricated member;
fourthly, thermal curing: carrying out heat curing on the SiCp/Al prefabricated member for 3h at the temperature of 200 ℃ to obtain a heat-cured SiCp/Al prefabricated member;
fifthly, glue permeation: impregnating silica sol on the surface of the SiCp/Al prefabricated member after thermosetting, repeatedly dipping the silica sol by using a brush and brushing the silica sol on the surface of the prefabricated member until the silica sol is not impregnated any more, and obtaining a glue-impregnated SiCp/Al prefabricated member;
sixthly, degreasing: placing the infiltrated SiCp/Al prefabricated member in a vacuum sintering furnace, and degreasing at 550 ℃ for 1h to obtain a degreased SiCp/Al prefabricated member;
seventhly, sintering: and sintering the degreased SiCp/Al prefabricated member in a vacuum sintering furnace at the temperature of 1000 ℃ for 3h, and cooling to room temperature along with the furnace to obtain the SiCp/Al complex structure.
The grain size of the SiC powder in the step one is 280 meshes, and the grain size of the aluminum powder is 280 meshes.
In the step one, the adhesive is epoxy resin.
And fifthly, the silica sol is alkaline silica sol, and the viscosity of the alkaline silica sol is less than 10MPa & s at normal temperature.
The concrete process of impregnating the silica sol in the step five is as follows: repeatedly dipping the silica sol by a brush and brushing the silica sol on the surface of the SiCp/Al prefabricated member after the heat curing till the silica sol does not permeate any more.
FIG. 2 is a three-dimensional model of the SiCp/Al preform in the STL format file in step two of example 1; FIG. 3 is a photograph of a complex SiCp/Al structure obtained in example 1; it can be seen from FIGS. 2 and 3 that the complex SiCp/Al structure obtained in example 1 is a SiCp/Al lattice structure.
The shrinkage of the SiCp/Al composite material obtained in example 1 was measured to be 0.2%,
the compressive strength of the SiCp/Al lattice structure obtained in example 1 was measured and found to be 47 MPa.

Claims (8)

1. A preparation method of a 3D forming SiCp/Al complex structure is characterized by comprising the following steps:
firstly, preparing mixed powder: mixing SiC powder and aluminum powder, adding a binder, and mixing for 24-48 h in a V-shaped mixer to obtain mixed powder; the mass ratio of the SiC powder to the aluminum powder is (50-70) to (30-50); the mass fraction of the binder in the mixed powder is 5-15%;
the adhesive in the first step is epoxy resin;
secondly, setting parameters: introducing the STL format file into an SLS forming machine, setting the scanning speed to be 1000-2000 mm/s, the thickness of each layer to be 0.05-0.2 mm, and the preheating temperature to be 40-70 ℃, and then processing the model into a sheet with a set thickness by using computer layered slicing software;
thirdly, preparing a prefabricated part: adding the mixed powder into a working cylinder of an SLS forming machine, spreading the powder by using a rolling shaft, standing for 25-35 min, heating the working cylinder to a preheating temperature according to the preheating temperature set in the second step of 40-70 ℃, starting processing according to the scanning speed set in the second step of 1000-2000 mm/s and the thickness of each layer of 0.05-0.2 mm, carrying out laser sintering, feeding and spreading the powder by using a powder feeding cylinder, sintering layer by layer, drying for 50-70 min at the temperature of 40-70 ℃, and taking out to obtain a SiCp/Al prefabricated part;
fourthly, thermal curing: carrying out heat curing on the SiCp/Al prefabricated member for 2-3 h at the temperature of 200-300 ℃ to obtain a heat-cured SiCp/Al prefabricated member;
fifthly, glue permeation: impregnating silica sol on the surface of the SiCp/Al prefabricated member after thermosetting to obtain a glue-impregnated SiCp/Al prefabricated member;
sixthly, degreasing: placing the infiltrated SiCp/Al prefabricated member in a vacuum sintering furnace, and degreasing at 500-700 ℃ for 1-2 h to obtain a degreased SiCp/Al prefabricated member;
seventhly, sintering: sintering the degreased SiCp/Al prefabricated member in a vacuum sintering furnace at the temperature of 700-1200 ℃, wherein the sintering time is 1-3 h, and cooling to room temperature along with the furnace to obtain a SiCp/Al complex structure;
the SiCp/Al complex structure is a SiCp/Al lattice structure.
2. The method of claim 1, wherein the SiC powder of step one has a 280 mesh particle size and the aluminum powder of step one has a 280 mesh particle size.
3. The method for preparing a 3D formed SiCp/Al complex structure as claimed in claim 1, wherein the mass ratio of the SiC powder to the aluminum powder in the step one is 1:1, and the mass fraction of the binder in the mixed powder is 5%.
4. The method of claim 1, wherein the preheating temperature in step two is set to 57 ℃.
5. The method of claim 1, wherein the silica sol in step five is an alkaline silica sol, and the viscosity of the alkaline silica sol at normal temperature is less than 10 MPa-s.
6. The method for preparing a 3D formed SiCp/Al complex structure according to claim 1, wherein the specific process of impregnating silica sol in the step five is as follows: repeatedly dipping the silica sol by a brush and brushing the silica sol on the surface of the SiCp/Al prefabricated member after the heat curing till the silica sol does not permeate any more.
7. The method for preparing 3D formed SiCp/Al complex structure as claimed in claim 1, wherein in the sixth step, the degreasing is performed at 550 ℃ for 1 h.
8. The method for preparing a 3D formed SiCp/Al complex structure as claimed in claim 1, wherein in the seventh step, the degreased SiCp/Al preform is sintered in a vacuum sintering furnace at a temperature of 1000 ℃ for 3h, and is cooled to room temperature along with the furnace to obtain the SiCp/Al complex structure.
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JP6078885B2 (en) * 2013-04-02 2017-02-15 日本碍子株式会社 Composite refractory and method for producing composite refractory
CN106927846B (en) * 2017-04-13 2018-05-04 华中科技大学 A kind of preparation method of C/C-SiC composite material parts and products thereof
CN107117982A (en) * 2017-06-01 2017-09-01 北京化工大学 A kind of material model of space in-situ carburization Material reinforcement ceramics and preparation method thereof
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CN107602130A (en) * 2017-10-17 2018-01-19 哈尔滨理工大学 The method that porous SiC ceramics are prepared based on 3D forming techniques
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