CN112500699A - Composite heat conduction material and preparation method thereof - Google Patents
Composite heat conduction material and preparation method thereof Download PDFInfo
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- CN112500699A CN112500699A CN202011298231.7A CN202011298231A CN112500699A CN 112500699 A CN112500699 A CN 112500699A CN 202011298231 A CN202011298231 A CN 202011298231A CN 112500699 A CN112500699 A CN 112500699A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0066—Use of inorganic compounding ingredients
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C64/00—Additive manufacturing, i.e. manufacturing of three-dimensional [3D] objects by additive deposition, additive agglomeration or additive layering, e.g. by 3D printing, stereolithography or selective laser sintering
- B29C64/30—Auxiliary operations or equipment
- B29C64/307—Handling of material to be used in additive manufacturing
- B29C64/314—Preparation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y10/00—Processes of additive manufacturing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y40/00—Auxiliary operations or equipment, e.g. for material handling
- B33Y40/10—Pre-treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y40/00—Auxiliary operations or equipment, e.g. for material handling
- B33Y40/20—Post-treatment, e.g. curing, coating or polishing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
- B33Y70/10—Composites of different types of material, e.g. mixtures of ceramics and polymers or mixtures of metals and biomaterials
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/36—After-treatment
- C08J9/40—Impregnation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/36—After-treatment
- C08J9/40—Impregnation
- C08J9/405—Impregnation with polymerisable compounds
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2377/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
Abstract
The invention belongs to the field of heat conduction materials, and particularly relates to a composite heat conduction material and a preparation method thereof. Preparing a porous heat conduction structural member by SLS printing of mixed powder of glass beads and PA12, putting the heat conduction structural member into dispersion liquid containing enough small heat conduction powder, fixing enough heat conduction powder on the surfaces of the structural member and the glass beads by co-condensation of a silane coupling agent and tetraethyl orthosilicate to form a heat conduction layer, and finally preparing the composite heat conduction material. Through the mode that the porous structure is directly printed in the 3D printing, enough seed positions can be left in the heat conduction material, and then the heat conduction powder is fixed on the structural member in a co-condensation mode to fully fill the space before the heat conduction powder is prepared, so that the content of the heat conduction powder can be effectively reduced, the reduction of the electric conductivity of the heat conduction material is facilitated, and the cost can be saved to a certain extent.
Description
Technical Field
The invention belongs to the field of heat conduction materials, and particularly relates to a composite heat conduction material and a preparation method thereof.
Background
With the miniaturization of electronic components and the rapid development of microelectronic integrated circuits, the heat generated by electronic devices tends to rapidly accumulate and increase. The reliability of the electronic components is reduced by about 10% when the temperature of the electronic components rises by 2 ℃, so that the timely heat dissipation becomes an important factor influencing the service life of the electronic components. In order to ensure that electronic components can still normally work with high reliability at the temperature of the use environment, a novel heat conduction material needs to be developed to replace the traditional material.
The 3D printing technology is a new technology in the field of rapid prototyping, and is a technology for constructing an object by using a bonding material such as powdered plastic and the like in a layer-by-layer printing mode on the basis of a CAD digital model file. The basic principle is laminate manufacturing, a technique of adding material layer by layer to create a three-dimensional entity. At present, the 3D printing technology is mainly applied to the fields of product prototyping, mold manufacturing, artistic creation, jewelry making, and the like. In addition, the 3D printing technology is gradually applied to the fields of medicine, bioengineering, construction, clothing, aviation and the like, and a wide space is opened for innovation. However, the dimensional stability of the product prepared by the 3D printing process is not good with pure nylon powder material.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a composite heat conduction material and a preparation method thereof.
The invention provides a composite heat conduction material and a preparation method thereof, wherein a porous heat conduction structural member is prepared by SLS printing of mixed powder of glass beads and PA12, then the heat conduction structural member is placed into dispersion liquid containing heat conduction powder small enough, the heat conduction powder in enough quantity is fixed on the surfaces of the structural member and the glass beads through co-condensation of a silane coupling agent and tetraethyl orthosilicate to form a heat conduction layer, and finally the composite heat conduction material is prepared.
The composite heat conduction material provided by the invention has the advantages of simple and easy preparation of raw materials, convenience in manufacturing, low cost, outstanding heat conduction performance, excellent mechanical performance and good surface state.
Preferably, the composite heat conducting material is made of Al as the heat conducting powder2O3BN, SiC, Ag and Cu.
Preferably, the diameter of the heat conducting powder is 0.1-3 μm.
Preferably, the diameter of the glass bead is 15 μm to 100 μm.
Preferably, the mass ratio of the glass beads to the PA12 is 1: 5-1: 20.
Preferably, the catalyst is one of ammonia water, acetic acid and hydrochloric acid.
Preferably, in the composite thermal conductive material, the silane coupling agent is one of gamma-aminopropyltriethoxysilane, gamma- (2, 3-glycidoxy) propyltrimethoxysilane and gamma-methacryloxypropyltrimethoxysilane.
Preferably, in the composite heat conduction material, the ethanol water solution accounts for 85-95% of the total mass of the ethanol.
Preferably, the composite heat conduction material has a mass ratio of the heat conduction powder to tetraethyl orthosilicate to the silane coupling agent of 2: 1-5: 1.
Has the advantages that:
through the mode that the porous structure is directly printed in the 3D printing, enough seed positions can be left in the heat conduction material, and then the heat conduction powder is fixed on the structural member in a co-condensation mode to fully fill the space before the heat conduction powder is prepared, so that the content of the heat conduction powder can be effectively reduced, the reduction of the electric conductivity of the heat conduction material is facilitated, and the cost can be saved to a certain extent. The workpiece printed by the mixed powder has the advantages of being capable of customizing, printing a complex structure and the like, and a porous structure can be directly printed. The glass beads modify the material and then the hydrolytic polymerization reaction is carried out to ensure that the heat conducting powder is fully fixed on the porous structural member. The traditional method of printing the material containing the foaming agent can solve the problems of the traditional foaming mode, the control of the foaming time and the uniformity of the size of the formed holes. The heat conduction material prepared by the method has uniform and controllable hole size, simple preparation method and controllable time, and is beneficial to reducing the cost and large-scale industrial production.
Drawings
Fig. 1 is a schematic structural diagram of a porous heat-conducting structural member.
Fig. 2 is an enlarged view of fig. 1.
FIG. 3 is a schematic diagram of the operation of the present invention.
FIG. 4 is an infrared spectrum of example 1.
Detailed Description
The invention is further illustrated by the following specific examples, which are illustrative and intended to illustrate the problem and explain the invention, but not limiting.
Example 1
A composite heat conduction material and a preparation method thereof.
The component PA12 (diameter 0.1 μm) and glass microspheres (diameter 15 μm) were added to a blender and mixed for 60 min.
And filling the mixed powder into a 3D printer, setting an SLS printing process, and then 3D printing and forming to prepare the heat-conducting structural member. Wherein the temperature of the forming cylinder is 170 ℃, the temperature of the powder supply cylinder is 140 ℃, the temperature of the piston is 145 ℃, the temperature of the periphery of the cylinder body is 140 ℃, the laser power is 45W, the scanning distance is 0.3mm, and the scanning speed is 10160 mm/s.
Taking the 3D printed porous structural member out of an SLS machine, carrying out sand blasting and polishing, then soaking the porous structural member in an ethanol water solution of heat conduction powder, silicate ester, gamma-aminopropyl triethoxysilane and a catalyst for rotation, wherein the mass ratio of the heat conduction powder to the tetraethyl orthosilicate and the gamma-aminopropyl triethoxysilane is 2:1, the mass ratio of ethanol to the gamma-aminopropyl triethoxysilane is 95%, and the catalyst is ammonia water, and carrying out hydrolytic condensation reaction to prepare the composite heat conduction material.
Example 2
A composite heat conduction material and a preparation method thereof.
The component PA12 (diameter 0.2 μm) and glass microspheres (diameter 30 μm) were added to the mixer and mixed for 60 min.
And filling the mixed powder into a 3D printer, setting an SLS printing process, and then 3D printing and forming to prepare the heat-conducting structural member. Wherein the temperature of the forming cylinder is 170 ℃, the temperature of the powder supply cylinder is 140 ℃, the temperature of the piston is 145 ℃, the temperature of the periphery of the cylinder body is 140 ℃, the laser power is 45W, the scanning distance is 0.3mm, and the scanning speed is 10160 mm/s.
Taking the 3D printed porous structural member out of an SLS machine, carrying out sand blasting and polishing, then soaking the porous structural member in an ethanol water solution of heat conduction powder, silicate ester, gamma-aminopropyl triethoxysilane and a catalyst for rotation, wherein the mass ratio of the heat conduction powder to the tetraethyl orthosilicate and the gamma-aminopropyl triethoxysilane is 2:1, the mass ratio of ethanol to the gamma-aminopropyl triethoxysilane is 95%, and the catalyst is ammonia water, and carrying out hydrolytic condensation reaction to prepare the composite heat conduction material.
Example 3
A composite heat conduction material and a preparation method thereof.
The component PA12 (diameter 0.3 μm) and glass microspheres (diameter 50 μm) were added to a blender and mixed for 60 min.
And filling the mixed powder into a 3D printer, setting an SLS printing process, and then 3D printing and forming to prepare the heat-conducting structural member. Wherein the temperature of the forming cylinder is 170 ℃, the temperature of the powder supply cylinder is 140 ℃, the temperature of the piston is 145 ℃, the temperature of the periphery of the cylinder body is 140 ℃, the laser power is 45W, the scanning distance is 0.3mm, and the scanning speed is 10160 mm/s.
Taking the 3D printed porous structural member out of an SLS machine, carrying out sand blasting and polishing, then soaking the porous structural member in an ethanol water solution of heat conduction powder, silicate ester, gamma-aminopropyl triethoxysilane and a catalyst for rotation, wherein the mass ratio of the heat conduction powder to the tetraethyl orthosilicate and the gamma-aminopropyl triethoxysilane is 2:1, the mass ratio of ethanol to the gamma-aminopropyl triethoxysilane is 95%, and the catalyst is ammonia water, and carrying out hydrolytic condensation reaction to prepare the composite heat conduction material.
Example 4
A composite heat conduction material and a preparation method thereof.
The component PA12 (diameter 0.3 μm) and glass microspheres (diameter 70 μm) were added to the mixer and mixed for 60 min.
And filling the mixed powder into a 3D printer, setting an SLS printing process, and then 3D printing and forming to prepare the heat-conducting structural member. Wherein the temperature of the forming cylinder is 170 ℃, the temperature of the powder supply cylinder is 140 ℃, the temperature of the piston is 145 ℃, the temperature of the periphery of the cylinder body is 140 ℃, the laser power is 45W, the scanning distance is 0.3mm, and the scanning speed is 10160 mm/s.
Taking the 3D printed porous structural member out of an SLS machine, carrying out sand blasting and polishing, then soaking the porous structural member in an ethanol water solution of heat conduction powder, silicate ester, gamma-aminopropyl triethoxysilane and a catalyst for rotation, wherein the mass ratio of the heat conduction powder to the tetraethyl orthosilicate and the gamma-aminopropyl triethoxysilane is 2:1, the mass ratio of ethanol to the gamma-aminopropyl triethoxysilane is 95%, and the catalyst is ammonia water, and carrying out hydrolytic condensation reaction to prepare the composite heat conduction material.
Example 5
A composite heat conduction material and a preparation method thereof.
The component PA12 (diameter 0.3 μm) and glass microspheres (diameter 100 μm) were added to a blender and mixed for 60 min.
And filling the mixed powder into a 3D printer, setting an SLS printing process, and then 3D printing and forming to prepare the heat-conducting structural member. Wherein the temperature of the forming cylinder is 170 ℃, the temperature of the powder supply cylinder is 140 ℃, the temperature of the piston is 145 ℃, the temperature of the periphery of the cylinder body is 140 ℃, the laser power is 45W, the scanning distance is 0.3mm, and the scanning speed is 10160 mm/s.
Taking the 3D printed porous structural member out of an SLS machine, carrying out sand blasting and polishing, then soaking the porous structural member in an ethanol water solution of heat conduction powder, silicate ester, gamma-aminopropyl triethoxysilane and a catalyst for rotation, wherein the mass ratio of the heat conduction powder to the tetraethyl orthosilicate and the gamma-aminopropyl triethoxysilane is 2:1, the mass ratio of ethanol to the gamma-aminopropyl triethoxysilane is 95%, and the catalyst is ammonia water, and carrying out hydrolytic condensation reaction to prepare the composite heat conduction material.
Comparative example 1
According to the preparation method of example 1, only the porous heat-conductive structural member was replaced with a solid member of the same size, and the remaining steps were completely performed as in example 1 to prepare a heat-conductive member.
Comparative example 2
According to the preparation method of the embodiment 1, the porous heat-conducting structural member is prepared, and the subsequent operation steps are omitted.
In each example, the mass percentage of the glass beads is 40%, and the structure of the heat-conducting structural member is shown in fig. 1 and 2. The preparation operation of each example is schematically shown in FIG. 3. FIG. 4 is an infrared spectrum of 1065.29cm of the composite heat conductive material prepared in example 1-1Is located at 1700cm of Si-O bending vibration absorption peak-1Is carbonyl (C ═ O) stretching vibration peak, 1570cm-11260cm, which is a combination of N-H bending vibration and C-N stretching vibration-1Is C-N-H vibration peak, 800cm-1The infrared characteristic absorption peak of the alumina is shown. Indicating that the heat-conducting powder is fully fixed on the surfaces of the structural member and the glass beads. The results of the thermal conductivity and mechanical properties tests of each sample are shown in table 1.
TABLE 1
The foregoing is only a preferred embodiment of the present invention, and it should be noted that modifications can be made by those skilled in the art without departing from the principle of the present invention, and these modifications should also be construed as the protection scope of the present invention.
Claims (10)
1. A preparation method of a composite heat conduction material is characterized by comprising the following steps: the composite heat conduction material is prepared by printing mixed powder of glass beads and PA12 powder through an SLS process to prepare a porous structural member, putting the porous structural member subjected to sand blasting and polishing into an ethanol water solution of heat conduction powder, tetraethyl orthosilicate and a silane coupling agent, adding a catalyst while stirring, taking out after reaction, cleaning and drying.
2. The method for preparing composite heat conduction material according to claim 1, characterized in that: the heat-conducting powder is Al2O3BN, SiC, Ag and Cu.
3. The method for preparing composite heat conduction material according to claim 1, characterized in that: the diameter of the heat conduction powder is 0.1-3 mu m.
4. The method for preparing composite heat conduction material according to claim 1, characterized in that: the diameter of the glass beads is 15 to 100 mu m.
5. The method for preparing composite heat conduction material according to claim 1, characterized in that: the catalyst is one of ammonia water, acetic acid and hydrochloric acid.
6. The method for preparing composite heat conduction material according to claim 1, characterized in that: the mass ratio of the glass beads to the PA12 is 1: 5-1: 20.
7. The method for preparing composite heat conduction material according to claim 1, characterized in that: the silane coupling agent is one of gamma-aminopropyltriethoxysilane, gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane and gamma-methacryloxypropyltrimethoxysilane.
8. The method for preparing composite heat conduction material according to claim 1, characterized in that: the mass ratio of the ethanol in the ethanol water solution is 85-95%.
9. The method for preparing composite heat conduction material according to claim 1, characterized in that: the mass ratio of the heat conducting powder to the tetraethyl orthosilicate to the silane coupling agent is 2: 1-5: 1.
10. A composite heat conductive material, characterized by: the process according to any one of claims 1 to 9.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113462200A (en) * | 2021-07-01 | 2021-10-01 | 本时智能技术发展(上海)有限公司 | Amino polymerization-resistant modified heat-conducting particle and preparation method thereof |
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| CN104760296A (en) * | 2015-03-24 | 2015-07-08 | 浙江工业大学 | A selective laser sintering molding method for a heat-conducting functional material |
| CN107254163A (en) * | 2016-03-25 | 2017-10-17 | 中国科学院理化技术研究所 | A kind of nylon/SiO 2 composite microsphere, preparation method and application |
| CN107841128A (en) * | 2016-09-20 | 2018-03-27 | 黑龙江鑫达企业集团有限公司 | A kind of SLS 3D printings PA 12/GB composites |
| CN109825068A (en) * | 2019-01-18 | 2019-05-31 | 常州先风三维科技有限公司 | A kind of nylon composite powder and preparation method thereof for selective laser sintering |
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2020
- 2020-11-19 CN CN202011298231.7A patent/CN112500699A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101691227A (en) * | 2009-10-13 | 2010-04-07 | 厦门大学 | Method for preparing silica aerogel material |
| CN104760296A (en) * | 2015-03-24 | 2015-07-08 | 浙江工业大学 | A selective laser sintering molding method for a heat-conducting functional material |
| CN107254163A (en) * | 2016-03-25 | 2017-10-17 | 中国科学院理化技术研究所 | A kind of nylon/SiO 2 composite microsphere, preparation method and application |
| CN107841128A (en) * | 2016-09-20 | 2018-03-27 | 黑龙江鑫达企业集团有限公司 | A kind of SLS 3D printings PA 12/GB composites |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113462200A (en) * | 2021-07-01 | 2021-10-01 | 本时智能技术发展(上海)有限公司 | Amino polymerization-resistant modified heat-conducting particle and preparation method thereof |
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