[go: up one dir, main page]
More Web Proxy on the site http://driver.im/

CN114456738A - Heat conduction material and preparation method and application thereof - Google Patents

Heat conduction material and preparation method and application thereof Download PDF

Info

Publication number
CN114456738A
CN114456738A CN202210101397.8A CN202210101397A CN114456738A CN 114456738 A CN114456738 A CN 114456738A CN 202210101397 A CN202210101397 A CN 202210101397A CN 114456738 A CN114456738 A CN 114456738A
Authority
CN
China
Prior art keywords
modified carbon
heat conduction
preparation
silicon particles
conduction material
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN202210101397.8A
Other languages
Chinese (zh)
Other versions
CN114456738B (en
Inventor
俞国金
周佩先
赖金洪
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Hunan Chuangjin Technology Research Institute Co ltd
Original Assignee
Hunan Chuangjin Technology Research Institute Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Hunan Chuangjin Technology Research Institute Co ltd filed Critical Hunan Chuangjin Technology Research Institute Co ltd
Priority to CN202210101397.8A priority Critical patent/CN114456738B/en
Publication of CN114456738A publication Critical patent/CN114456738A/en
Application granted granted Critical
Publication of CN114456738B publication Critical patent/CN114456738B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/04Non-macromolecular additives inorganic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J163/00Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/002Physical properties
    • C08K2201/005Additives being defined by their particle size in general
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/002Physical properties
    • C08K2201/006Additives being defined by their surface area
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/011Nanostructured additives
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/04Carbon
    • C08K3/041Carbon nanotubes
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00Use of pretreated ingredients
    • C08K9/10Encapsulated ingredients

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Sealing Material Composition (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention discloses a heat conduction material and a preparation method and application thereof. A thermally conductive material, comprising: modified carbon nanotubes and silicon particles dispersed on the surface of the modified carbon nanotubes; the particle size of the silicon particles is 1-5 nm; the mass of the silicon particles accounts for 50-60% of the mass of the heat conducting material. According to the heat conduction material, the insulating silicon particles are wrapped on the conductive modified carbon nano tubes, so that the insulation of the modified carbon nano tubes is realized, and the high heat conduction material with the insulating property can be obtained. The invention also provides a preparation method and application of the heat conduction material.

Description

Heat conduction material and preparation method and application thereof
Technical Field
The invention belongs to the technical field of insulation encapsulation, and particularly relates to a heat conduction material, and a preparation method and application thereof.
Background
The pouring sealant is mainly used for bonding, sealing and protecting industrial elements. At present, pouring sealant is widely used in the electronic device manufacturing industry, is an indispensable insulating material in the electronic industry, can strengthen the integrity of electronic devices, improve the resistance to external impact and vibration, and can provide insulation between internal elements and circuits.
With the development of microelectronics and integrated circuits toward high speed, high density, miniaturization and light weight, the volumes of electronic components and logic circuits are compressed, and the heat generated by electronic devices per unit volume is rapidly increased, so that the heat conductivity affects the service life and reliability of the electronic components and electronic devices. This requires that the potting adhesive for electronic components have excellent heat conductivity and insulation properties.
In the related art, the method of adding heat-conducting filler is usually adopted to improve the heat conductivity of the traditional pouring sealant, and metal, metal oxide, ceramic and carbon-based materials are several commonly used heat-conducting fillers. Wherein the metal and the carbon-based material have no insulation; the heat-conducting property of the metal oxide and the ceramic is poor, the heat-conducting coefficient of the pouring sealant containing the metal oxide and the ceramic is usually about 1Wm/K, and the requirement of the pouring sealant with high heat-conducting property can not be met.
In conclusion, the existing heat-conducting filler is difficult to meet the requirements of high heat conductivity and high insulation at the same time, and cannot be used for preparing pouring sealant suitable for electronic components.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art described above. Therefore, the invention provides a heat conduction material, which wraps insulated silicon particles on a conductive modified carbon nano tube to realize insulation of the modified carbon nano tube, so that the high heat conduction material with insulation property can be obtained.
The invention also provides a preparation method of the heat conduction material.
The invention also provides application of the heat conduction material.
According to an aspect of the present invention, there is provided a heat conductive material comprising:
modified carbon nanotubes and silicon particles dispersed on the surface of the modified carbon nanotubes;
the particle size of the silicon particles is 1-5 nm;
the mass of the silicon particles accounts for 50-60% of the mass of the heat conduction material.
According to a preferred embodiment of the invention, at least the following advantages are achieved:
(1) at normal temperature (about 25 ℃), the thermal conductivity of the silicon simple substance is about 150W/m.K, and the unit area ballistic thermal conductivity of the carbon nano tube is as high as 5.88 multiplied by 109W/m2K, the radial thermal conductivity is usually more than or equal to 650W/m.K (the thermal conductivity of the carbon nano tube changes along with the change of the diameter, the length and the length-diameter ratio of the carbon nano tube); therefore, the silicon and the modified carbon nano tube are compounded together, and the high-heat-conduction material can be obtained.
(2) In the invention, the nano-sized silicon particles are arranged on the surface of the modified carbon nano-tube to form the insulating coating layer, which is equivalent to the insulating modification of the modified carbon nano-tube by the silicon particles, so that the heat conduction material provided by the invention has high heat conductivity and insulativity.
(3) The heat conduction material provided by the invention inherits the linear structure of the modified carbon nano tube, and compared with a point-shaped particle structure, the linear structure is easier to form a heat conduction path in the pouring sealant, so that the heat conduction purpose is achieved, therefore, the addition amount of the heat conduction material in the pouring sealant can be reduced to a certain extent, and the storage stability of the pouring sealant is further improved.
(4) The silicon particles can completely wrap the modified carbon nano tubes by adjusting the particle size of the silicon particles and the mass ratio of the silicon particles, so that the purpose of insulation modification is achieved; but also can effectively control the thickness of the shell layer formed by arranging the silicon particles and avoid influencing the heat conductivity of the heat conduction material.
In some embodiments of the present invention, the modified carbon nanotube has an outer diameter of 30 to 50 nm.
In some embodiments of the present invention, the modified carbon nanotube has a length of 1 to 2 μm.
In some embodiments of the present invention, the modified carbon nanotube comprises at least one of a carboxyl group and a hydroxyl group thereon.
In some embodiments of the present invention, the modified carbon nanotube has a carboxyl group content of 0.5 to 1% by mass.
The carboxyl group and the hydroxyl group help to improve the bonding strength between the modified carbon nanotube and the silicon particle.
In some embodiments of the present invention, the heat conductive material has a specific surface area of 95 to 130m2/g。
In some embodiments of the present invention, the heat conductive material has a specific surface area of 100 to 120m2/g。
According to another aspect of the invention, a preparation method of the heat conducting material is provided, which comprises mixing and ball milling silicon powder and the modified carbon nano tube.
The preparation method according to a preferred embodiment of the present invention has at least the following advantageous effects:
(1) silicon particles with the particle size of 1-5 nm are difficult to purchase and obtain, and are too active in property and difficult to store stably; the invention adopts simple ball milling to realize the preparation of the nano silicon particles by a top-down method (preparing nano materials from bulk substances, correspondingly forming nano particles from bottom to top by the polymerization of atomic substances); compared with the traditional vapor deposition (bottom-up) method and the like, the method provided by the invention is simpler and has lower equipment cost.
(2) The ball milling method is a physical-chemical method, not only can realize the regulation and control of the particle size, but also can form defects on the surface of the obtained silicon particles, promote the firm combination between the silicon particles and the modified carbon nano tubes, and form stable insulating coating.
In some embodiments of the invention, the silicon powder has a diameter of 500nm to 5 μm.
In some embodiments of the invention, the milling balls have a diameter of 0.1 to 4 mm.
In some embodiments of the present invention, the grinding balls comprise 1 part of grinding balls having a diameter of 0.1 to 1mm and 2 to 5 parts of grinding balls having a diameter of 2 to 4mm, by weight ratio.
In some embodiments of the invention, the ball-milling has a ball-to-feed ratio of 2 to 20: 1.
The ball-material ratio represents the ratio of the mass of the grinding balls to the sum of the mass of the silicon powder and the modified carbon nano tube.
In some embodiments of the present invention, the material of the grinding ball includes at least one of alumina and zirconia.
In some embodiments of the invention, the rotation speed of the ball mill is 300-1200 rpm.
In some embodiments of the invention, the ball milling time is 2 to 24 hours.
In some preferred embodiments of the invention, the method of preparation further comprises adding a grinding aid prior to said ball milling.
In some embodiments of the invention, the grinding aid comprises at least one of diethylene glycol, ethylene glycol, and glucose.
On one hand, the grinding aid can prevent silicon particles obtained by ball milling from adsorbing and agglomerating with each other, so that the ball milling efficiency is improved; on the other hand, the grinding aids are all reducing alcohol, and provide a reducing environment for the ball milling.
In some embodiments of the invention, the mass of the grinding aid is 0.5-3 wt% of the mass of the silicon powder.
In some embodiments of the invention, the preparation method further comprises calcining after the ball milling.
In some embodiments of the invention, the temperature of the calcination is 280 to 400 ℃.
In some embodiments of the invention, the calcination is for a period of 1 to 5 hours.
In some preferred embodiments of the present invention, the calcination time is 3 to 4 hours.
The calcining can further remove the moisture in the heat conduction material so as to prepare the pouring sealant with more excellent performance; the calcination can also further improve the bonding strength between the silicon particles and the modified carbon nanotubes, so that the silicon particles are prevented from falling off; and during the calcination, the grinding aid can be removed and volatilized, or a carbon-based connecting part between the modified carbon nano tube and the silicon particle is formed through pyrolysis, so that the adhesion strength between the carbon nano tube and the silicon particle is improved.
In some embodiments of the invention, the preparation process is carried out under a protective atmosphere.
In some embodiments of the invention, the protective atmosphere comprises at least one of nitrogen and an inert gas.
According to another aspect of the invention, the pouring sealant comprises a component A and a component B;
the raw materials for preparing the component A comprise the heat conduction material or the heat conduction material prepared by the preparation method.
The pouring sealant according to a preferred embodiment of the present invention has at least the following beneficial effects:
the linear heat conducting material can reduce the content of the heat conducting material in the pouring sealant and further improve the storage stability of the pouring sealant; meanwhile, the adopted heat conduction material has excellent heat conduction and insulation, so that the obtained pouring sealant also has excellent heat conduction and insulation.
In some embodiments of the present invention, the raw materials for preparing the a component further include an epoxy resin and an organic solvent.
In some embodiments of the invention, the epoxy resin comprises at least one of a bisphenol a epoxy resin, a bisphenol F epoxy resin, a novolac epoxy resin, and a cycloaliphatic epoxy resin.
In some embodiments of the invention, the organic solvent comprises at least one of castor oil triglycidyl ether and 1, 4-butyl glycidyl ether.
In some embodiments of the present invention, the preparation raw materials of the a component comprise, by weight:
70 parts of epoxy resin;
8-15 parts of heat conduction material;
1-20 parts of an organic solvent.
In some embodiments of the present invention, the raw materials for preparing the a component further comprise an auxiliary agent.
In some embodiments of the present invention, the addition amount of the additive is 1 to 10 parts by weight.
In some embodiments of the invention, the adjuvant comprises at least one of a dispersant, a toughener, and a defoamer.
In some embodiments of the present invention, the toughening agent comprises at least one of a polyester polyol and a silicone polymer.
In some embodiments of the invention, the dispersant comprises at least one of BYK163, dispersant NNO, and dispersant 5040.
In some embodiments of the invention, the antifoaming agent comprises at least one of BYKA530 and BYKA 535.
In some embodiments of the present invention, the raw materials for preparing the B component include a curing agent.
In some embodiments of the invention, the curing agent comprises at least one of an aliphatic amine, an aromatic amine, a polyamide, methyl tetrahydrophthalic anhydride, and methyl hexahydrophthalic anhydride.
In some embodiments of the invention, the raw material for preparing the B component further comprises an accelerator.
In some embodiments of the invention, the accelerator comprises at least one of dimethylbenzylamine and triethanolamine.
In some embodiments of the invention, in the component B, the mass ratio of the curing agent to the accelerator is 10-20: 1.
in some embodiments of the invention, the mass ratio of the A component to the B component is 1-20: 1.
In some embodiments of the present invention, the component a and the component B of the pouring sealant are packaged separately and mixed uniformly before use.
According to another aspect of the invention, the application of the pouring sealant in the preparation of electronic products is provided.
Detailed Description
The concept and technical effects of the present invention will be clearly and completely described below in conjunction with the embodiments to fully understand the objects, features and effects of the present invention. It is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments, and those skilled in the art can obtain other embodiments without inventive effort based on the embodiments of the present invention, and all embodiments are within the protection scope of the present invention.
If no special description is provided, the silicon powder and the modified carbon nano tube adopted in the invention are purchased from Annaiji chemistry; wherein:
the particle size of the silicon powder is 2-3 mu m, and the purity is more than or equal to 98.5 wt%;
the modified carbon nanotube has an inner diameter of 5 to 12nm, an outer diameter of 30 to 50nm, a length of 1 to 2 μm, a purity of more than 98 wt%, and contains 0.7 wt% of carboxyl.
Since none of the silicon powder-modified carbon nanotubes is of a single size, but is a mixture of materials of similar sizes, the above parameters regarding size are all range values.
Example 1
The embodiment prepares the heat conduction material, and the specific process is as follows:
s1, mixing 20g of modified carbon nano tube and 25g of silicon powder in a ball milling tank; the ball milling tank contains 90g of grinding beads of zirconium oxide, wherein the diameter of the grinding beads is 0.8mm, and the diameter of the grinding beads is 4mm, and the grinding beads are 360 g;
s2, adding 0.42g of ethylene glycol into the mixture obtained in the step S1;
s3, ball-milling the mixture obtained in the step S2 at the rotating speed of 800rpm for 5 hours, and screening out grinding beads;
s4, carrying out heat treatment on the mixture obtained in the step S3 at 300 ℃ for 3.5 h.
The preparation process of this example was carried out under nitrogen protection.
Example 2
The embodiment prepares a heat conducting material, and the specific process is different from that of embodiment 1:
and (4) directly drying the mixture obtained in the step (S3) at 60 ℃ in vacuum without performing the step (S4).
Example 3
The embodiment prepares a heat conducting material, and the specific process is different from that of embodiment 1:
only steps S1 and S3 were performed, i.e., no grinding aid ethylene glycol was added, and the calcination treatment of step S4 was not performed.
Example 4
The embodiment prepares the heat conduction material, and the specific process is as follows:
s1, mixing 20g of modified carbon nanotubes and 20g of silicon powder in a ball milling tank; the ball milling tank contains 80g of grinding beads of zirconium oxide, wherein the grinding beads are 0.8mm in diameter, and 320g of grinding beads are 4mm in diameter;
s2, adding 0.3g of ethylene glycol into the mixture obtained in the step S1;
s3, ball-milling the mixture obtained in the step S2 at the rotating speed of 800rpm for 5 hours, and screening out grinding beads;
s4, carrying out heat treatment on the mixture obtained in the step S3 at 300 ℃ for 3.5 h.
The preparation process of this example was carried out under nitrogen protection.
Example 5
In the embodiment, the pouring sealant is prepared from the heat conduction material obtained in the embodiment 1, and comprises the following specific components in parts by weight:
the component A comprises:
epoxy resin: 70 parts of bisphenol A epoxy resin, which is purchased from Jiaxing Baolilai resin chemical industry Co., Ltd;
heat conduction material: 12 parts, from example 1;
organic solvent: 8 parts of castor oil triglycidyl ether, which is purchased from Wuhanfeng Yaohui chemicals GmbH and has the purity of more than or equal to 99 wt%;
a toughening agent: 4 parts, specifically polyester polyol, the average relative molecular weight is about 2000, the hydroxyl value is about 360mgKOH/g, the acid value is less than or equal to 2mgKOH/g, and the viscosity is about 3800mPa & s;
and B component:
is a mixture of methylhexahydrophthalic anhydride (CAS: 25550-51-0) and dimethylbenzylamine (available from Wuhan Carnoz, Inc.) in a mass ratio of 20: 1.
The preparation method of the pouring sealant in the embodiment comprises the steps of respectively mixing the preparation raw materials of the component A and the component B, and mixing the component A and the component B according to the mass ratio of 2:1 before use.
Examples 6 to 8 respectively prepare a pouring sealant, and the differences from example 5 are as follows: the thermally conductive material of example 6 was from example 2, the thermally conductive material of example 7 was from example 3, and the thermally conductive material of example 8 was from example 4.
Comparative example 1
This comparative example prepared a thermally conductive material, which differs from example 1 in that:
(1) in step S1, the mass of the silicon powder is 16 g; 72g of grinding beads with a diameter of 0.8mm and 288g of grinding beads with a diameter of 4 mm;
(2) accordingly, the amount of ethylene glycol added in step S2 was 0.27 g.
Comparative example 2
This comparative example prepared a thermally conductive material, which differs from example 1 in that:
(1) in step S1, the mass of the silicon powder is 35 g; corresponding to 110g of grinding beads with a diameter of 0.8mm and 550g of grinding beads with a diameter of 4 mm;
(2) accordingly, the amount of ethylene glycol added in step S2 was 0.58 g.
Comparative example 3
The comparative example prepares a heat conducting material, and comprises the following specific steps:
A1. mixing 25g of silicon powder and 0.42g of ethylene glycol in a ball milling tank; the ball milling tank contains 50g of grinding beads of zirconium oxide, wherein the grinding beads have a diameter of 0.8mm, and 200g of grinding beads have a diameter of 4 mm;
A2. b, ball-milling the mixture obtained in the step A1 at the rotating speed of 800rpm for 5 hours, and then screening out grinding beads;
A3. and B, mixing the mixture obtained in the step A2 with 20g of modified carbon nano tubes, and then carrying out heat treatment at 300 ℃ for 3.5 h.
The preparation process of this example was carried out under nitrogen protection.
Comparative examples 4 to 7 respectively prepare a pouring sealant, and the differences from example 5 are as follows: the thermally conductive material of comparative example 4 is from comparative example 1, the thermally conductive material of comparative example 5 is from comparative example 2, the thermally conductive material of comparative example 6 is from comparative example 3, and the thermally conductive material is not included in comparative example 7.
Test examples
The present experimental example tested the specific surface area of the heat conductive materials prepared in examples 1 to 4 and comparative examples 1 to 3, and the size of the silicon particles therein. Wherein: the specific surface area is measured by BET, the size of the silicon particles is measured by a transmission electron microscope, and 20 particles in a visual field are measured in total, and the average value is obtained. The characterization results are shown in table 1.
TABLE 1 Properties of the thermally conductive materials obtained in examples 1 to 4 and comparative examples 1 to 3
Figure BDA0003492389700000081
Figure BDA0003492389700000091
The results in Table 1 show that the specific surface area of the heat-conductive materials obtained in examples 1 to 4 is 100 to 125m2The grain diameter of the silicon particles is between 2.77 nm and 4.68nm, the silicon particles obtained by grinding in the heat treatment process of the embodiment and the embodiment 4 are fused to a certain extent, so that the grain diameter of the silicon particles is larger, and the specific surface area of the heat conduction material is smaller; in example 3, the grinding aid was not added, and therefore, the grinding was insufficient, the particle diameter was large, and the specific surface area was small, as compared with example 2.
In comparative example 1, the content of silicon particles was < 50%, and thus the specific surface area of the heat conductive material was closer to that of the modified carbon nanotube; in addition, in the process of observing the microscopic morphology by a transmission electron microscope, the modified carbon nano tube is still partially exposed, and the silicon particles do not completely cover the modified carbon nano tube, so that the insulation requirement can not be met.
The proportion of silicon particles in comparative example 2 was > 60%, but the physicochemical properties of the resulting material were similar to those of examples 1 and 4.
In comparative example 3, the particle size of the silicon particles was controlled by ball milling, and the silicon particles were mixed with the modified carbon nanotubes and then heat-treated, and most of the obtained silicon particles were separated from the modified carbon nanotubes without forming a coating.
The test example also tests the performance of the pouring sealant prepared in examples 5 to 8 and comparative examples 4 to 7, and specifically, the obtained pouring sealant is poured into a mold (the size of the mold refers to standard documents of various tests), and is cured for 12 hours at 85 ℃ in an argon protective atmosphere, so as to obtain a test module. And then, carrying out a breaking elongation test according to GB/T1040-92, measuring the thermal conductivity according to ASTM-D-2214, and carrying out a volume resistivity test according to GB/T1692, wherein the test results are shown in Table 2.
TABLE 2 Properties of potting Compounds obtained in examples 5 to 8 and comparative examples 4 to 7
Figure BDA0003492389700000092
The results in Table 2 show that the pouring sealant obtained in the embodiments 5-8 of the invention has excellent heat conductivity and good insulativity; and is equivalent to the comparative example 7 without adding heat conduction material, and the mechanical property and the heat conduction property of the pouring sealant are not obviously reduced.
The heat conduction material adopted in the comparative example 4 is from the comparative example 1, and the modified carbon nano tube is not completely wrapped by the silicon particles, so that a conductive path is formed, and the resistivity of the pouring sealant is obviously reduced; in the comparative example 5, the silicon particles are wrapped too thickly, so that the heat conduction performance of the modified carbon nano tube cannot be fully exerted, and the heat conduction coefficient of the obtained pouring sealant is poor; comparative example 6 is equivalent to using a mixture of modified carbon nanotubes and silicon particles as the heat conductive material, the modified carbon nanotubes form a conductive path, and the insulation of the obtained potting adhesive is the worst.
The embodiments of the present invention have been described in detail, but the present invention is not limited to the embodiments, and various changes can be made without departing from the gist of the present invention within the knowledge of those skilled in the art. Furthermore, the embodiments of the present invention and the features of the embodiments may be combined with each other without conflict.

Claims (10)

1. A thermally conductive material, comprising:
modified carbon nanotubes and silicon particles dispersed on the surface of the modified carbon nanotubes;
the particle size of the silicon particles is 1-5 nm;
the mass of the silicon particles accounts for 50-60% of the mass of the heat conduction material.
2. The heat conductive material of claim 1, wherein the modified carbon nanotubes have an outer diameter of 30 to 50 nm; preferably, the length of the modified carbon nanotube is 1-2 μm.
3. The thermally conductive material of claim 1, wherein the modified carbon nanotubes comprise at least one of carboxyl and hydroxyl groups thereon.
4. The heat conductive material according to any one of claims 1 to 3, wherein the heat conductive material has a specific surface area of 95 to 130m2/g。
5. A preparation method of the heat conduction material according to any one of claims 1 to 4, which comprises mixing and ball milling silicon powder and the modified carbon nanotubes.
6. The preparation method according to claim 5, wherein the diameter of the silicon powder is 500 nm-5 μm.
7. The preparation method according to claim 5, wherein in the ball milling, the diameter of the grinding balls is 0.1-4 mm; preferably, the ball-to-material ratio of the ball mill is 2-20: 1; preferably, the rotation speed of the ball mill is 300-1200 rpm; preferably, the time of the ball milling is 2-24 h.
8. The pouring sealant is characterized by comprising a component A and a component B;
the raw materials for preparing the component A comprise the heat conduction material as claimed in any one of claims 1 to 4 or the heat conduction material prepared by the preparation method as claimed in any one of claims 5 to 7.
9. The pouring sealant according to claim 8, wherein the raw materials for preparing the component A further comprise epoxy resin and organic solvent; preferably, the raw materials for preparing the B component comprise a curing agent.
10. Use of the potting adhesive according to claim 8 or 9 in the production of electronic products.
CN202210101397.8A 2022-01-27 2022-01-27 Heat conducting material and preparation method and application thereof Active CN114456738B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202210101397.8A CN114456738B (en) 2022-01-27 2022-01-27 Heat conducting material and preparation method and application thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202210101397.8A CN114456738B (en) 2022-01-27 2022-01-27 Heat conducting material and preparation method and application thereof

Publications (2)

Publication Number Publication Date
CN114456738A true CN114456738A (en) 2022-05-10
CN114456738B CN114456738B (en) 2023-09-19

Family

ID=81410758

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202210101397.8A Active CN114456738B (en) 2022-01-27 2022-01-27 Heat conducting material and preparation method and application thereof

Country Status (1)

Country Link
CN (1) CN114456738B (en)

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20120021376A (en) * 2010-07-29 2012-03-09 부산대학교 산학협력단 Method for fabrication of si coated multi-wall carbon nano tube for composite materials
CN107353674A (en) * 2017-06-22 2017-11-17 广州中谱检测技术服务有限公司 A kind of preparation method of nano silicon carbon nano-tube hybridization material
CN111455208A (en) * 2020-05-27 2020-07-28 国家电网有限公司 Nano modified aluminum alloy material, preparation method thereof and energy-saving and environment-friendly electric power fitting manufactured by nano modified aluminum alloy material
CN112029240A (en) * 2020-09-07 2020-12-04 吉祥三宝高科纺织有限公司 High-thermal-conductivity polymer carbon nanotube composite material and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20120021376A (en) * 2010-07-29 2012-03-09 부산대학교 산학협력단 Method for fabrication of si coated multi-wall carbon nano tube for composite materials
CN107353674A (en) * 2017-06-22 2017-11-17 广州中谱检测技术服务有限公司 A kind of preparation method of nano silicon carbon nano-tube hybridization material
CN111455208A (en) * 2020-05-27 2020-07-28 国家电网有限公司 Nano modified aluminum alloy material, preparation method thereof and energy-saving and environment-friendly electric power fitting manufactured by nano modified aluminum alloy material
CN112029240A (en) * 2020-09-07 2020-12-04 吉祥三宝高科纺织有限公司 High-thermal-conductivity polymer carbon nanotube composite material and preparation method thereof

Also Published As

Publication number Publication date
CN114456738B (en) 2023-09-19

Similar Documents

Publication Publication Date Title
KR102265034B1 (en) Hexagonal boron nitride powder, its manufacturing method, resin composition, and resin sheet
EP2201079B1 (en) Thermally conductive composition
KR102210618B1 (en) Hexagonal boron nitride powder and its manufacturing method, and composition and heat dissipating material using the same
TW201927689A (en) Hexagonal boron nitride powder and method for producing the same, and composition and heat dissipation material using the same
CN107736085B (en) High-frequency electromagnetic interferes (EMI) composite material
JP6687818B1 (en) Method for producing silicon-containing oxide-coated aluminum nitride particles and silicon-containing oxide-coated aluminum nitride particles
TWI751632B (en) Inorganic particle-dispersed resin composition and method for producing inorganic particle-dispersed resin composition
CN104830031B (en) A kind of epoxy resin composite material and preparation method thereof having both heat conduction and antistatic property
TWI690484B (en) Manufacturing method of glass-coated aluminum nitride particles and manufacturing method of exothermic resin composition containing glass-coated aluminum nitride particles
CN113583388A (en) Heat-conducting epoxy resin composite material and preparation method thereof
CN115011306A (en) Low-density organic silicon pouring sealant and preparation process thereof
CN110845989B (en) Two-component organic silicon pouring sealant and application method thereof
JP6347644B2 (en) Surface-modified silica powder and slurry composition
Suzuki et al. Fabrication of epoxy composites with large-pore sized mesoporous silica and investigation of their thermal expansion
CN114456738B (en) Heat conducting material and preparation method and application thereof
CN114410063A (en) Heat-conducting and insulating epoxy resin composite material and preparation method thereof
CN111479773A (en) Glass-coated aluminum nitride particles, process for producing the same, and heat-radiating resin composition containing the same
CN115595102B (en) Epoxy resin composition glue solution, preparation method thereof, adhesive film and application
JP3434029B2 (en) Epoxy resin composition
JP7249209B2 (en) Epoxy resin composition for casting, electronic component, and method for producing electronic component
CN112980053A (en) Heat-conducting filler of epoxy plastic packaging material, preparation method of heat-conducting filler and epoxy plastic packaging material
Yang et al. Thermal and electrical properties of BNNPs/TiO 2-Epoxy three-phase nanocomposites
JP7438442B1 (en) Boron nitride aggregated particles, sheet member, and method for producing boron nitride aggregated particles
Li et al. Comparative study of anhydride and amine-based underfill materials for flip chip applications
JP6950028B2 (en) Insulating filler and its manufacturing method, insulating material containing the insulating filler and its manufacturing method.

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant