CN110256985B - Epoxy-based electric-conduction heat-conduction adhesive and preparation method thereof - Google Patents

Epoxy-based electric-conduction heat-conduction adhesive and preparation method thereof Download PDF

Info

Publication number
CN110256985B
CN110256985B CN201910573308.8A CN201910573308A CN110256985B CN 110256985 B CN110256985 B CN 110256985B CN 201910573308 A CN201910573308 A CN 201910573308A CN 110256985 B CN110256985 B CN 110256985B
Authority
CN
China
Prior art keywords
epoxy
graphene
epoxy resin
solution
adhesive
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.)
Active
Application number
CN201910573308.8A
Other languages
Chinese (zh)
Other versions
CN110256985A (en
Inventor
孟庆实
韩森森
崔旭
王朔
岳新
马傲
王英波
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.)
Shenyang Aerospace University
Original Assignee
Shenyang Aerospace University
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 Shenyang Aerospace University filed Critical Shenyang Aerospace University
Priority to CN201910573308.8A priority Critical patent/CN110256985B/en
Publication of CN110256985A publication Critical patent/CN110256985A/en
Application granted granted Critical
Publication of CN110256985B publication Critical patent/CN110256985B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/04—Non-macromolecular additives inorganic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J9/00—Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
    • C09J9/02—Electrically-conducting adhesives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/001—Conductive additives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

An epoxy-based electric-conduction heat-conduction adhesive and a preparation method thereof belong to the field of adhesive preparation methods. The preparation method is to prepare the graphene nanosheet with a regular structure, and the graphene nanosheet is mixed with the epoxy adhesive to prepare the epoxy group electric and heat conducting adhesive which is high in strength, high in toughness and excellent in electric and heat conducting performance. The graphene in the adhesive exists in fewer layers instead of aggregates, so that the performance of the epoxy-based electric and heat conductive adhesive can be obviously improved, the preparation method is simple, and the defects of poor toughness, poor electric and heat conductivity and the like of the existing epoxy adhesive can be overcome.

Description

Epoxy-based electric-conduction heat-conduction adhesive and preparation method thereof
Technical Field
The invention relates to the technical field of adhesive preparation methods, in particular to an epoxy-based electric-conduction heat-conduction adhesive and a preparation method thereof.
Background
Epoxy adhesives are widely used in a variety of fields, such as aerospace, automotive, electronics, civilian use, and packaging industries, as one of the most important structural adhesives. However, many of these applications are environmentally harsh and require enhanced epoxy adhesive strength and electrical and thermal conductivity properties to meet the requirements. In the prior art, the method for improving the strength of the epoxy adhesive comprises the following steps: the filler is added into the epoxy adhesive, and the traditional fillers such as metal, ceramic, clay and the like have higher reinforcing capacity, but the materials have high density, poor corrosion resistance and single reinforcing effect, and the high filling content can reduce the mechanical strength and toughness of the adhesive.
Patent 201810883840.5 discloses a macromolecular composite epoxy resin adhesive of single-layer graphene and a preparation method thereof, wherein the method completely avoids the reaggregation of the single-layer graphene by adopting solvation and ensures the single-layer structure. However, the single-layer graphene used in the method is obtained by directly thermally reducing or chemically reducing the single-layer graphene oxide, and the preparation method of the single-layer graphene oxide composite adhesive causes defects to the graphene lamellar structure, reduces regularity, and influences the mechanics and electric and heat conduction enhancement effect of the graphene in an epoxy matrix, so that the obtained single-layer graphene macromolecular composite epoxy resin adhesive has poor mechanical property and electric and heat conduction property.
Disclosure of Invention
Compared with the traditional preparation method of a reinforcing material, the preparation method uses a nano carbon-based filler, is a graphene nanosheet with a regular structure, and is mixed with the epoxy adhesive to prepare the epoxy group electric conduction and heat conduction adhesive with high strength, high toughness and excellent electric conduction and heat conduction performance. According to the invention, the epoxy group electric conduction and heat conduction adhesive compounded by few-layer graphene molecules can be obtained without a complex technology, and the performances of the epoxy group electric conduction and heat conduction adhesive, such as the bonding performance and the like, can be remarkably improved by a very small amount (0.01 wt%) of graphene because the graphene exists in the adhesive in few layers instead of aggregates.
The invention relates to a preparation method of an epoxy-based electric-conduction heat-conduction adhesive, which comprises the following steps:
step 1: thermally expanding the graphene intercalation compound at 650-800 ℃ for 1-2 min to obtain a thermally expanded graphene intercalation compound;
adding acetone capable of immersing the graphene intercalation compound into the graphene intercalation compound subjected to thermal expansion, and ultrasonically stripping for 20-50 min to obtain a graphene nanosheet solution;
step 2: adding acetone into epoxy resin, and uniformly mixing to obtain an epoxy resin acetone solution; the volume consumption of the acetone is the volume consumption capable of fully dissolving the epoxy resin, and preferably, the mass concentration of the epoxy resin in the epoxy resin acetone solution is 0.2-0.5 g/mL;
mixing an epoxy resin acetone solution and a graphene nanosheet solution, and ultrasonically oscillating for 20-60 min to obtain an epoxy/graphene mixed solution; the mixing proportion of the epoxy resin acetone solution and the graphene nanosheet solution is calculated according to the following formula:
M/M ═ k; wherein K is a proportionality coefficient and is 0.5-2;
m is the mass of the graphene nanosheets in the graphene nanosheet solution;
m is the mass of the graphene nanosheet in the graphene nanosheet solution, the mass of the epoxy resin and the mass of a curing agent adopted by the epoxy resin;
wherein, according to the mass ratio, the curing agent: epoxy resin ═ (1-1.3): 3.3;
and step 3: removing acetone and air bubbles in the epoxy/graphene mixed solution to obtain an epoxy/graphene mixture;
and 4, step 4: and adding a curing agent into the epoxy/graphene mixture, and uniformly stirring to obtain the epoxy group electric and heat conductive adhesive.
In the step 1, the ultrasonic power is 90-110W, the ultrasonic work is 2-3 s, and the ultrasonic pause is 1 s.
In the step 1, in the graphene nanosheet solution, the graphene nanosheets are few-layer graphene, and the few-layer graphene is a two-dimensional carbon material formed by stacking 3-5 layers of carbon atoms which are periodically and closely stacked in a hexagonal honeycomb structure in different stacking modes.
In the step 2, the epoxy resin is an epoxy resin capable of being cured by an amine short-molecular-chain curing agent.
In the step 2, the curing agent is a D230 curing agent.
In the step 3, one or a combination of a plurality of modes is adopted according to the acetone content in the epoxy/graphene mixed solution;
the first method comprises the following steps: directly placing the epoxy/graphene mixed solution in a vacuum oven, heating to 70-100 ℃ under the vacuum degree of-0.09 MPa to-0.1 MPa, and drying in vacuum until the quality of the epoxy/graphene mixture is not changed;
and the second method comprises the following steps: stirring and heating the epoxy/graphene mixed solution, wherein the heating temperature is 70-100 ℃, the stirring speed is 300 r/min, and the stirring and heating time is until the quality of the epoxy/graphene mixture is not changed;
and the third is that: and (4) performing reduced pressure rotary evaporation and concentration until the quality of the epoxy/graphene mixture is not changed.
In the step 4, the curing agent is an amine short-molecular-chain curing agent.
The epoxy-based electric-conduction heat-conduction adhesive is prepared by adopting the method.
When the epoxy-based electric and heat conductive adhesive is used, the curing conditions are as follows: curing for 8-12 h at 100-140 ℃.
In the epoxy-based conductive and heat-conductive adhesive, the graphene nanosheets account for 0.5-2.0% of the total mass of the epoxy-based conductive and heat-conductive adhesive in percentage by mass;
after the epoxy group conductive heat-conducting adhesive is cured, the shear strength is 11MPa to 18MPa, and the toughness is 400 to 600J.m2Conductivity of 10-9～10-5S/cm, thermal conductivity of 0.17-0.35 W.m-1K-1。
The epoxy-based electric-conduction heat-conduction adhesive and the preparation method thereof have the beneficial effects that:
according to the invention, the graphene nanosheets with regular structures are mixed with the epoxy resin, and the prepared epoxy-based electric and heat conducting adhesive overcomes the defects of poor toughness, poor electric and heat conductivity and the like of the existing epoxy adhesive.
Drawings
FIG. 1 is a flow chart of a process for preparing an epoxy-based electrically and thermally conductive adhesive according to an embodiment of the present invention;
FIG. 2 is a shear strength curve of an epoxy-based electrically and thermally conductive adhesive prepared according to an embodiment of the present invention;
FIG. 3 is a toughness curve of an epoxy-based electrically and thermally conductive adhesive prepared according to an embodiment of the present invention;
FIG. 4 is a graph of the electrical conductivity of an epoxy-based electrically and thermally conductive adhesive prepared in accordance with an embodiment of the present invention;
FIG. 5 is a heat-conducting property curve of the epoxy-based electrically and thermally conductive adhesive prepared according to the embodiment of the present invention;
fig. 6 is a transmission electron microscope test chart of graphene nanoplatelets in embodiment 1 of the present invention.
Detailed Description
The present invention will be described in further detail with reference to examples.
In the following examples, epoxy resin used was epoxy E-51, a synthetic material of star, south Pole, Jiangsu.
In the following examples, the graphene intercalation compound used is american album carbohydrates, archive 1395.
In the following examples, the curing agent used was hensimei D230.
Example 1
The preparation method of the epoxy-based electric and heat conductive adhesive comprises the following steps of:
step 1: thermally expanding the graphene intercalation compound at 700 ℃ for 1min, then adding acetone, and ultrasonically stripping for 30min to obtain a graphene nanosheet solution; wherein the concentration of the graphene nanosheets in the graphene nanosheet solution is 0.01 g/mL; wherein the ultrasonic power is 100W, the ultrasonic work is 2s, and the pause is 1 s.
The transmission electron microscope analysis test is carried out on the graphene nanosheets in the graphene nanosheet solution, the obtained transmission electron microscope images are shown as a graph (a), a graph (b) and a graph (c) in fig. 6, the structure and atomic scale details of the graphene can be observed from the graph (a), the graph (a) shows transparency, the graphene is proved to be few-layer graphene, and the graphene nanosheets are 3-layer graphene which are regular in structure and free of defects by combining the analysis of the graph (b) and the graph (c).
Step 2: taking epoxy resin, adding acetone to completely dissolve the epoxy resin to obtain an epoxy resin acetone solution; wherein, in the epoxy resin acetone solution, the concentration of the epoxy resin is 0.3 g/mL;
mixing an epoxy resin acetone solution and a graphene nanosheet solution, and continuing to perform ultrasonic treatment for 30min to obtain an epoxy/graphene mixed solution; wherein, according to the mass ratio, the graphene nano sheet: epoxy resin, curing agent and graphene nanosheet are 0.5: 100;
and step 3: heating the epoxy/graphene mixed solution in a vacuum oven at the vacuum degree of-0.09 MPa and the temperature of 100 ℃ to remove acetone and bubbles to obtain an epoxy/graphene mixture;
and 4, step 4: adding an amine short-molecular-chain curing agent D230 into the epoxy/graphene mixture, and uniformly stirring for 2min to obtain an epoxy group electric-conduction and heat-conduction adhesive; wherein, according to the mass ratio, the curing agent: epoxy resin in epoxy/graphene mixture ═ 1: 3.3.
example 2
The preparation method of the epoxy-based electric and heat conductive adhesive is the same as that in example 1, except that:
in the step 2, the mass of the graphene nanosheets is as follows according to the mass ratio: epoxy resin + curing agent + graphene nanoplatelets 0.8: 100.
Example 3
The preparation method of the epoxy-based electric and heat conductive adhesive is the same as that in example 1, except that:
in the step 2, according to the mass ratio, the graphene nanosheet: epoxy resin + curing agent + graphene nanoplate 1.0: 100.
Example 4
The preparation method of the epoxy-based electric and heat conductive adhesive is the same as that in example 1, except that:
in the step 2, according to the mass ratio, the graphene nanosheet: epoxy resin + curing agent + graphene nanoplatelets 1.3: 100.
Example 5
The preparation method of the epoxy-based electric and heat conductive adhesive is the same as that in example 1, except that:
in the step 2, according to the mass ratio, the graphene nanosheet: epoxy resin + curing agent + graphene nanoplatelets at a ratio of 1.5: 100.
Example 6
The preparation method of the epoxy-based electric and heat conductive adhesive is the same as that in example 1, except that:
in the step 2, according to the mass ratio, the graphene nanosheet: epoxy resin + curing agent + graphene nanoplatelets at a ratio of 1.8: 100.
Example 7
The preparation method of the epoxy-based electric and heat conductive adhesive is the same as that in example 1, except that:
in the step 2, according to the mass ratio, the graphene nanosheet: epoxy resin, curing agent and graphene nanosheet are 2.0: 100.
Comparative example
A method for preparing an epoxy resin adhesive,
step i, taking epoxy resin, adding acetone to completely dissolve the epoxy resin to obtain an epoxy resin acetone solution; wherein, in the epoxy resin acetone solution, the concentration of the epoxy resin is 0.3 g/mL;
step ii: adding a D230 curing agent into the epoxy resin acetone solution, uniformly stirring for 2min, and removing acetone to obtain an epoxy resin adhesive; wherein, according to the mass ratio, the curing agent: epoxy resin 1: 3.3.
test example
The epoxy-based conductive and heat-conductive adhesives prepared in examples 1-7 and comparative examples are cured at 130 ℃ for 10h, and then tested by using a method for measuring tensile shear strength of adhesives (rigid material to rigid material) in GB/T7124-2008, and the shear strength of each obtained example is shown in FIG. 2, and from FIG. 2, it can be seen that when the mass fraction of graphene nanosheets in the whole epoxy resin adhesive is 1.0%, the maximum shear strength of the epoxy resin adhesive is close to 16MPa after curing.
The toughness of each of the embodiments obtained by testing the epoxy-based electrically-conductive and thermally-conductive adhesives prepared in examples 1 to 5 after curing is shown in fig. 3, and from fig. 3, it can be seen that the toughness of the cured epoxy resin adhesive is improved as the mass fraction of graphene in the whole epoxy resin adhesive is improved.
After the epoxy-based conductive and heat-conductive adhesives prepared in the embodiments 1 to 5 are cured, tests are carried out, the conductivity of each obtained embodiment is shown in fig. 4, and from fig. 4, it can be obtained that the conductivity of the epoxy-based conductive and heat-conductive adhesive is divided into three stages, namely an initial stage, a rapid growth region and a gentle region, wherein the rapid growth region is 0.5 to 1.0, and the pre-permeation value is 1.08%, along with the improvement of the mass fraction of graphene in the whole epoxy resin adhesive.
The epoxy-based conductive and heat-conductive adhesives prepared in the embodiments 1 to 5 are cured and then tested, the heat-conductive performance of each obtained embodiment is shown in fig. 5, and from fig. 5, it can be obtained that the heat conductivity of the cured epoxy resin adhesive is improved along with the improvement of the mass fraction of graphene in the whole epoxy resin adhesive.
Example 8
A preparation method of an epoxy-based electric and heat conductive adhesive comprises the following steps:
step 1: thermally expanding the graphene intercalation compound at 800 ℃ for 1min to obtain a thermally expanded graphene intercalation compound;
adding acetone capable of immersing the graphene intercalation compound into the thermally expanded graphene intercalation compound, and ultrasonically stripping for 50min at the ultrasonic power of 90W to obtain a graphene nanosheet solution;
the graphene nanosheets in the prepared graphene nanosheet solution are analyzed, and the graphene nanosheets are few-layer graphene, specifically, two-dimensional carbon materials formed by stacking 3-5 layers of carbon atoms with hexagonal honeycomb structures and periodically and closely stacked in different stacking modes.
Step 2: adding acetone into epoxy resin, and uniformly mixing to obtain an epoxy resin acetone solution; wherein, in the epoxy resin acetone solution, the mass concentration of the epoxy resin is 0.2 g/mL;
mixing an epoxy resin acetone solution and a graphene nanosheet solution, and performing ultrasonic oscillation for 40min to obtain an epoxy/graphene mixed solution; the mixing proportion of the epoxy resin acetone solution and the graphene nanosheet solution is calculated according to the following formula:
according to the property of the epoxy resin, determining a curing agent matched with the epoxy resin, and adding and calculating the using amount of the curing agent according to the type and the proportion of the curing agent in the selected epoxy resin, wherein in the embodiment, the curing agent comprises the following components in percentage by mass: epoxy resin 1: 3.3;
according to the following steps:
M/M ═ k; wherein, K is a proportionality coefficient, which is 1.0 in this embodiment;
m is the mass of the graphene nanosheets in the graphene nanosheet solution;
m is the mass of the graphene nanosheet in the graphene nanosheet solution, the mass of the epoxy resin and the mass of a curing agent adopted by the epoxy resin;
and step 3: stirring and heating the epoxy/graphene mixed solution at the heating temperature of 80-100 ℃, the stirring speed of 300 r/min, and the stirring and heating time until the quality of the epoxy/graphene mixture is not changed, removing acetone and air bubbles to obtain an epoxy/graphene mixture;
and 4, step 4: and adding an amine short molecular chain curing agent into the epoxy/graphene mixture, and uniformly stirring to obtain the epoxy group electric-conductive and heat-conductive adhesive.
Example 9
A preparation method of an epoxy-based electric and heat conductive adhesive comprises the following steps:
step 1: thermally expanding the graphene intercalation compound at 650 ℃ for 2min to obtain a thermally expanded graphene intercalation compound;
adding acetone capable of immersing the graphene intercalation compound into the thermally expanded graphene intercalation compound, and ultrasonically stripping for 20min at the ultrasonic power of 90W to obtain a graphene nanosheet solution;
the graphene nanosheets in the prepared graphene nanosheet solution are analyzed, and the graphene nanosheets are few-layer graphene, specifically, two-dimensional carbon materials formed by stacking 3-5 layers of carbon atoms with hexagonal honeycomb structures and periodically and closely stacked in different stacking modes.
Step 2: adding acetone into epoxy resin, and uniformly mixing to obtain an epoxy resin acetone solution; wherein, in the epoxy resin acetone solution, the mass concentration of the epoxy resin is 0.5 g/mL;
mixing an epoxy resin acetone solution and a graphene nanosheet solution, and performing ultrasonic oscillation for 40min to obtain an epoxy/graphene mixed solution; the mixing proportion of the epoxy resin acetone solution and the graphene nanosheet solution is calculated according to the following formula:
according to the property of the epoxy resin, determining a curing agent matched with the epoxy resin, and adding and calculating the using amount of the curing agent according to the type and the proportion of the curing agent in the selected epoxy resin, wherein in the embodiment, the curing agent comprises the following components in percentage by mass: epoxy resin 1.3: 3.3;
according to the following steps:
M/M ═ k; wherein K is a proportionality coefficient, which is 2.0 in this embodiment;
m is the mass of the graphene nanosheets in the graphene nanosheet solution;
m is the mass of the graphene nanosheet in the graphene nanosheet solution, the mass of the epoxy resin and the mass of a curing agent adopted by the epoxy resin;
and step 3: performing reduced pressure rotary evaporation concentration on the epoxy/graphene mixed solution until the quality of the epoxy/graphene mixture is not changed, and removing acetone and air bubbles to obtain an epoxy/graphene mixture;
and 4, step 4: and adding an amine short molecular chain curing agent into the epoxy/graphene mixture, and uniformly stirring to obtain the epoxy group electric-conductive and heat-conductive adhesive.

Claims (8)

1. The preparation method of the epoxy-based electric and heat conducting adhesive is characterized by comprising the following steps:
step 1: thermally expanding the graphene intercalation compound at 650-800 ℃ for 1-2 min to obtain a thermally expanded graphene intercalation compound;
adding acetone capable of immersing the graphene intercalation compound into the graphene intercalation compound subjected to thermal expansion, and ultrasonically stripping for 20-50 min to obtain a graphene nanosheet solution;
the ultrasonic power is 90-110W, the ultrasonic work is 2-3 s, and the ultrasonic pause is 1 s;
in the graphene nanosheet solution, the graphene nanosheets are few-layer graphene, and the few-layer graphene is a two-dimensional carbon material formed by stacking 3-5 layers of carbon atoms which are periodically and closely stacked in a hexagonal honeycomb structure in different stacking modes;
step 2: adding acetone into epoxy resin, and uniformly mixing to obtain an epoxy resin acetone solution; the volume amount of the acetone is the volume amount capable of fully dissolving the epoxy resin; in the epoxy resin acetone solution, the mass concentration of the epoxy resin is 0.2-0.5 g/mL;
mixing an epoxy resin acetone solution and a graphene nanosheet solution, and ultrasonically oscillating for 20-60 min to obtain an epoxy/graphene mixed solution; the mixing proportion of the epoxy resin acetone solution and the graphene nanosheet solution is calculated according to the following formula:
M/M = k; wherein K is a proportionality coefficient and is 0.5-2;
m is the mass of the graphene nanosheets in the graphene nanosheet solution;
m is the mass of the graphene nanosheet in the graphene nanosheet solution, the mass of the epoxy resin and the mass of a curing agent adopted by the epoxy resin;
wherein, according to the mass ratio, the curing agent: epoxy resin = (1 to 1.3): 3.3;
and step 3: removing acetone and air bubbles in the epoxy/graphene mixed solution to obtain an epoxy/graphene mixture;
and 4, step 4: adding a curing agent into the epoxy/graphene mixture, and uniformly stirring to obtain an epoxy group conductive and heat-conducting adhesive;
after the epoxy group conductive heat-conducting adhesive is cured, the shear strength is 11MPa to 18MPa, and the toughness is 400 to 600J.m2Conductivity of 10-9~10-5S/cm, thermal conductivity of 0.17-0.35 W.m-1K-1。
2. The preparation method of the epoxy-based electrically and thermally conductive adhesive according to claim 1, wherein in the step 2, the mass concentration of the epoxy resin in the epoxy resin acetone solution is 0.2-0.5 g/mL.
3. The method for preparing the epoxy-based electrically and thermally conductive adhesive according to claim 1, wherein in the step 2, the curing agent is D230 curing agent.
4. The preparation method of the epoxy-based electrically and thermally conductive adhesive according to claim 1, wherein in the step 3, one or a combination of several of the following ways is adopted according to the acetone content in the epoxy/graphene mixed solution;
the first method comprises the following steps: directly placing the epoxy/graphene mixed solution in a vacuum oven, heating to 70-100 ℃ under the vacuum degree of-0.09 MPa to-0.1 MPa, and drying in vacuum until the quality of the epoxy/graphene mixture is not changed;
and the second method comprises the following steps: stirring and heating the epoxy/graphene mixed solution, wherein the heating temperature is 70-100 ℃, the stirring speed is 300 r/min, and the stirring and heating time is until the quality of the epoxy/graphene mixture is not changed;
and the third is that: and (4) performing reduced pressure rotary evaporation and concentration until the quality of the epoxy/graphene mixture is not changed.
5. An epoxy-based electrically and thermally conductive adhesive, characterized by being prepared by the method of any one of claims 1 to 4.
6. The epoxy-based electrically and thermally conductive adhesive of claim 5, wherein the curing conditions of the epoxy-based electrically and thermally conductive adhesive during use are as follows: curing for 8-12 h at 100-140 ℃.
7. The epoxy-based electric and heat conductive adhesive as claimed in claim 5, wherein the graphene nanosheets account for 0.5-2.0% by mass of the total mass of the epoxy-based electric and heat conductive adhesive.
8. The epoxy-based electrically and thermally conductive adhesive according to claim 5, wherein the shear strength and toughness of the cured epoxy-based electrically and thermally conductive adhesive are respectively 11MPa to 18MPa and 400 to 600J.m2Conductivity of 10-9~10-5S/cm, thermal conductivity of 0.17-0.35 W.m-1K-1。
CN201910573308.8A 2019-06-28 2019-06-28 Epoxy-based electric-conduction heat-conduction adhesive and preparation method thereof Active CN110256985B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201910573308.8A CN110256985B (en) 2019-06-28 2019-06-28 Epoxy-based electric-conduction heat-conduction adhesive and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201910573308.8A CN110256985B (en) 2019-06-28 2019-06-28 Epoxy-based electric-conduction heat-conduction adhesive and preparation method thereof

Publications (2)

Publication Number Publication Date
CN110256985A CN110256985A (en) 2019-09-20
CN110256985B true CN110256985B (en) 2020-11-24

Family

ID=67922776

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201910573308.8A Active CN110256985B (en) 2019-06-28 2019-06-28 Epoxy-based electric-conduction heat-conduction adhesive and preparation method thereof

Country Status (1)

Country Link
CN (1) CN110256985B (en)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110791250B (en) * 2019-10-29 2021-07-16 沈阳航空航天大学 Graphene-aliphatic polyurethane composite material adhesive and application thereof

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8198349B2 (en) * 2008-11-18 2012-06-12 GL Global Technology Operations LLC Self-healing and scratch resistant shape memory polymer system
CN105820514A (en) * 2016-04-08 2016-08-03 泰州巨纳新能源有限公司 Preparation method of high-conductivity graphene-resin composite material

Also Published As

Publication number Publication date
CN110256985A (en) 2019-09-20

Similar Documents

Publication Publication Date Title
Zhang et al. Thermally conductive and insulating epoxy composites by synchronously incorporating Si-sol functionalized glass fibers and boron nitride fillers
CN110872193B (en) Preparation method of high-thermal-conductivity graphene/chopped carbon fiber composite material
Jia et al. A strong and tough polymer–carbon nanotube film for flexible and efficient electromagnetic interference shielding
Gu et al. Thermal conductivities, mechanical and thermal properties of graphite nanoplatelets/polyphenylene sulfide composites
CN110951254A (en) Boron nitride composite high-thermal-conductivity insulating polymer composite material and preparation method thereof
CN110128792B (en) Thermal interface composite material and preparation method and application thereof
EP3623441A1 (en) Thermal interface material, and preparation and application thereof
Chu et al. The cryogenic thermal expansion and mechanical properties of plasma modified ZrW2O8 reinforced epoxy
Dinca et al. Nanocomposites as advanced materials for aerospace industry
Mu et al. Thermal conductivity of 2D nano-structured graphitic materials and their composites with epoxy resins
CN112778703A (en) High-toughness and heat-conducting epoxy resin composite material and preparation method thereof
Ming et al. Bioinspired highly electrically conductive graphene–epoxy layered composites
CN110551908A (en) Preparation method of boron nitride nanosheet reinforced aluminum-based composite material
CN110256985B (en) Epoxy-based electric-conduction heat-conduction adhesive and preparation method thereof
Zaheer et al. A treatise on multiscale glass fiber epoxy matrix composites containing graphene nanoplatelets
CN106565263B (en) A kind of preparation method of carbon nanotube/silicon carbide heat-conductive composite material
CN109265919B (en) 3D heat-conducting composite material and preparation method thereof
CN110964219B (en) Nano cellulose membrane with high thermal conductivity and preparation method thereof
Zhang et al. Graphite tube woven fabric/boron nitride/polymer composite with enhanced thermal conductivity and electric isolation
CN110894338B (en) Controllable deformation accurate regulation and control composite material based on super-elastic network and preparation method and application thereof
Fu et al. Improved dielectric stability of epoxy composites with ultralow boron nitride loading
Khobragade et al. Studies on graphene reinforced Cu base composites prepared by two step thermal processing method
KR101470829B1 (en) Epoxy composites and manufacturing method thereof
Qi et al. Surface treatments of hexagonal boron nitride for thermal conductive epoxy composites
Zhang et al. Surface modification of graphite and its effect on thermal and mechanical properties of graphite-based thermal interface materials

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