CN112280516A - UV-curable epoxy resin heat-conducting adhesive and preparation method thereof - Google Patents
UV-curable epoxy resin heat-conducting adhesive and preparation method thereof Download PDFInfo
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- CN112280516A CN112280516A CN202011174106.5A CN202011174106A CN112280516A CN 112280516 A CN112280516 A CN 112280516A CN 202011174106 A CN202011174106 A CN 202011174106A CN 112280516 A CN112280516 A CN 112280516A
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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
- 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
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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
- 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
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- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/382—Boron-containing compounds and nitrogen
- C08K2003/385—Binary compounds of nitrogen with boron
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- 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
- C08K2201/002—Physical properties
- C08K2201/005—Additives being defined by their particle size in general
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- 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
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- 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
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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Abstract
The invention relates to the technical field of adhesives, in particular to a UV-curable epoxy resin heat-conducting adhesive and a preparation method thereof. The raw materials comprise the following components in parts by weight: 5-15 parts of epoxy resin, 2-8 parts of nano epoxy resin, 2-8 parts of alicyclic epoxy resin, 2-8 parts of reactive diluent, 0.5-1.5 parts of UV initiator, 0.2-1 part of sensitizer, 70-80 parts of inorganic filling material and 0.2-2 parts of dispersant. The UV-curable epoxy resin heat-conducting adhesive provided by the invention can be rapidly cured under the irradiation of a UV curing lamp, so that the defect of poor curing timeliness of the existing heat-conducting adhesive is overcome, the heat conductivity of the material is good, and the use environment requirements of electronic devices such as mobile phones and computers and the like with higher heat dissipation requirements can be particularly met; meanwhile, the epoxy resin heat-conducting adhesive prepared by the method has good weather resistance, strong fatigue resistance and aging resistance and wide application prospect.
Description
Technical Field
The invention relates to the technical field of adhesives, in particular to a UV-curable epoxy resin heat-conducting adhesive and a preparation method thereof.
Background
Ultraviolet (UV) curing is a process of curing and film-forming by using medium and short wavelength (300-800 nm) of UV ultraviolet light and under UV radiation, a photoinitiator in a liquid UV material is stimulated to be changed into free radicals or cations so as to initiate rapid polymerization and crosslinking of a high polymer material (resin) containing active functional groups, and the process is a new environment-friendly technology with low VOC emission which is created in the 60 s of the 20 th century. After the 20 th century and the 80 th era, the UV curing technology is rapidly developed in China and is widely applied to the fields of coatings, printing ink, adhesives and the like. Most of the existing curing modes of the heat-conducting adhesive are curing at normal temperature for more than 24 hours or curing by heating for 30 minutes or even more than 1 hour, and the timeliness is poor. Compared with a thermal curing mode, the UV curing has the advantages of energy conservation, high production efficiency and the like.
With the rapid development of information technology, the circuit density and the load capacity are rapidly increased, and the heat generated by plastic products in the electronic components in the operation must be timely diffused to the environment, otherwise, the electronic components are damaged due to the overhigh local temperature, and even a fire disaster is caused. The prior art generally selects to add high thermal conductive inorganic particles in the epoxy resin composition to improve the thermal conductivity of the resin, but the mechanical properties of the epoxy resin are often negatively affected, so that the application of the epoxy resin is limited.
Based on this, how to prepare a UV-curable epoxy resin thermal conductive adhesive becomes an urgent problem to be solved in the art.
Disclosure of Invention
The UV-curable epoxy resin heat-conducting adhesive provided by the invention can be rapidly cured under the irradiation of a UV curing lamp, so that the defect of poor curing timeliness of the existing heat-conducting adhesive is overcome, the heat conductivity of the material is good, and the use environment requirements of electronic devices such as mobile phones and computers and the like with higher heat dissipation requirements can be particularly met; meanwhile, the epoxy resin heat-conducting adhesive prepared by the method has good weather resistance, strong fatigue resistance and aging resistance and wide application prospect.
The invention provides a UV-curable epoxy resin heat-conducting adhesive which comprises the following raw materials in parts by weight: 5-15 parts of epoxy resin, 2-8 parts of nano epoxy resin, 2-8 parts of alicyclic epoxy resin, 2-8 parts of reactive diluent, 0.5-1.5 parts of UV initiator, 0.2-1 part of sensitizer, 70-80 parts of inorganic filling material and 0.2-2 parts of dispersant.
In a preferred embodiment, the epoxy resin comprises a bisphenol F type epoxy resin and/or a novolac type epoxy resin.
In a preferred embodiment, the nano epoxy resin is a nano aluminum oxide modified epoxy resin.
In a preferred embodiment, the weight ratio of the epoxy resin to the nano-type epoxy resin is (1-4): 1.
in a preferred embodiment, the UV initiator is a cationic initiator.
In a preferred embodiment, the inorganic filler material is alumina and boron nitride; the alumina comprises first alumina and second alumina, and the weight ratio of the first alumina to the second alumina to the boron nitride is (2-6): 1: (1-3).
In a preferred embodiment, the first alumina has a particle size of 8 to 12 μm, the second alumina has a particle size of 0.4 to 1 μm, and the boron nitride has a particle size of 8 to 14 μm.
In a preferred embodiment, the dispersant is a titanate compound.
The invention provides a preparation method of a UV-curable epoxy resin heat-conducting adhesive, which comprises the following specific steps:
s1, weighing 5-15 parts of epoxy resin, 2-8 parts of nano epoxy resin, 2-8 parts of alicyclic epoxy resin, 2-8 parts of active diluent, 0.5-1.5 parts of UV initiator, 0.2-1 part of sensitizer, 70-80 parts of inorganic filling material and 0.2-2 parts of dispersing agent according to parts by weight;
s2, sequentially adding the epoxy resin, the nano epoxy resin, the alicyclic epoxy resin, the reactive diluent, the UV initiator, the sensitizer, the inorganic filling material and the dispersing agent into a material cylinder of the double-planet type dispersing instrument, and stirring at a first stirring speed for 10-20 min; setting the vacuum degree of the material placing cylinder at-0.08 MPa, and stirring at a second stirring speed for 100-150 min.
In a preferred embodiment, the first stirring speed is 40-100r/min, and the second stirring speed is 750-.
Has the advantages that:
most of the existing curing modes of the heat-conducting adhesive are curing at normal temperature for more than 24 hours or curing by heating for 30 minutes or even more than 1 hour, and the timeliness is poor. The invention provides a UV-curable epoxy resin heat-conducting adhesive which can be cured in only about 20s under the irradiation of a 365nm curing lamp with 800 watts, and a cured product has excellent weather resistance and heat conductivity. The invention can especially meet the use environment requirements of mobile phone electronic chips and the like which have higher heat dissipation requirements or are difficult to heat, and has simple and easy process and wide application prospect.
Detailed Description
The invention will be further understood by reference to the following detailed description of preferred embodiments of the invention and the examples included therein. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. To the extent that a definition of a particular term disclosed in the prior art is inconsistent with any definitions provided herein, the definition of the term provided herein controls.
As used herein, a feature that does not define a singular or plural form is also intended to include a plural form of the feature unless the context clearly indicates otherwise. It will be further understood that the term "prepared from …," as used herein, is synonymous with "comprising," including, "comprising," "having," "including," and/or "containing," when used in this specification means that the recited composition, step, method, article, or device is present, but does not preclude the presence or addition of one or more other compositions, steps, methods, articles, or devices. Furthermore, the use of "preferred," "preferably," "more preferred," etc., when describing embodiments of the present application, is meant to refer to embodiments of the invention that may provide certain benefits, under certain circumstances. However, other embodiments may be preferred, under the same or other circumstances. In addition, the recitation of one or more preferred embodiments does not imply that other embodiments are not useful, nor is it intended to exclude other embodiments from the scope of the invention. In addition, the starting materials for the present invention are commercially available unless otherwise specified.
In order to solve the above problems, a first aspect of the present invention provides a UV-curable epoxy resin thermal conductive adhesive, which comprises, by weight: 5-15 parts of epoxy resin, 2-8 parts of nano epoxy resin, 2-8 parts of alicyclic epoxy resin, 2-8 parts of reactive diluent, 0.5-1.5 parts of UV initiator, 0.2-1 part of sensitizer, 70-80 parts of inorganic filling material and 0.2-2 parts of dispersant.
In some preferred embodiments, the epoxy resin comprises a bisphenol F type epoxy resin and/or a novolac type epoxy resin.
In some preferred embodiments, the nano-epoxy resin is a nano-alumina-modified epoxy resin.
The nano aluminum oxide modified epoxy resin can be sold in the market, such as the winning industry group.
The invention discovers that when the nano epoxy resin is added into the raw materials of the epoxy resin heat-conducting adhesive, the heat-conducting property of the adhesive is effectively improved. The surmised reasons are that the nano aluminum oxide modified epoxy resin modifies the surface of the epoxy resin, so that the uniformity and the dispersibility of an epoxy resin curing system are improved, the combination of an inorganic filler and an epoxy resin base material is optimized, the unstable agglomeration among particles in the epoxy resin curing process is inhibited, a four-way and eight-way heat conduction passage is formed in the filling system, and the heat conductivity coefficient of the prepared epoxy resin heat conduction adhesive is obviously improved.
More preferably, the weight ratio of the epoxy resin to the nano-type epoxy resin is (1-4): 1.
the present invention has unexpectedly found that when the weight ratio of the epoxy resin to the nano-type epoxy resin is (1-4): 1, the weather resistance of the prepared epoxy resin heat-conducting adhesive is improved. The suspected reason may be that the weight ratio of the epoxy resin and the nano-type epoxy resin is (1-4): the three-dimensional network structure generated in the 1 time is high in stability, the inorganic rigid particles are orderly filled in a curing system to form a protective layer, and a good slow release effect is achieved on external stress, so that the influence of external environment change on the mechanical property of the epoxy resin composition is weakened, and the weather resistance of the epoxy resin heat-conducting adhesive is improved.
In some preferred embodiments, the cycloaliphatic epoxy resin may be commercially available, for example, from Jiangsutaire chemical Co., Ltd, model number TTA 21P.
In some preferred embodiments, the reactive diluent is an epoxy reactive diluent.
Further preferably, the epoxy reactive diluent comprises at least one of 3-ethyl-3-oxetanemethanol, p-di (oxiranyl) benzene and 1,2,7, 8-diepoxyoctane.
In some preferred embodiments, the UV initiator is a cationic initiator.
The cationic initiator is selected from at least one of CPI-410, CPI-310, available from San-Apro corporation, and Pasteur IRGACURE250, Germany.
The invention discovers that when the cationic initiator is selected as the UV initiator, the UV curing time of the epoxy resin heat-conducting adhesive can be as low as 20 s. The reason may be that the cationic initiator has more excellent solubility in the organic compound, has stronger migration and passing capacity among polymer molecular chains, and active free radicals formed by the cationic initiator absorbing light energy are combined with substances such as alicyclic epoxy resin and the like more quickly, so that the progress of crosslinking and curing reaction is accelerated, and the epoxy resin heat-conducting adhesive can be cured in only 20 seconds under the irradiation of an 800W and 365nm curing lamp.
In some preferred embodiments, the inorganic filler material is alumina and boron nitride; the alumina comprises first alumina and second alumina, and the weight ratio of the first alumina to the second alumina to the boron nitride is (2-6): 1: (1-3).
More preferably, the particle size of the first alumina is 8-12 μm, the particle size of the second alumina is 0.4-1 μm, and the particle size of the boron nitride is 8-14 μm. Both the first alumina having a particle size of 8 to 12 μm and the second alumina having a particle size of 0.4 to 1 μm are commercially available, for example from Yadman commercial (Shanghai) Co. Boron nitride having a particle size of 8-14 μ M is commercially available, for example, from 3M company (Minnesota mining).
The invention discovers that when the inorganic filling material selects the aluminum oxide and the boron nitride in the proportion to act together, the weather resistance of the epoxy resin heat-conducting adhesive is improved to the best. The reason is probably that the aluminum oxide and the boron nitride in the proportion can be well dispersed in the epoxy resin network structure of the system, rigid particles with stable mechanical property are introduced into the epoxy resin composition, so that the damage effect of ultraviolet energy on chemical bonds of body type curing products is inhibited, the mechanical stability of the epoxy resin heat-conducting adhesive after UV irradiation is improved, and the weather resistance of the material is improved.
Although the addition of the aluminum oxide and the boron nitride improves the weather resistance of the epoxy resin heat-conducting adhesive, the UV curing time of the material is slightly prolonged, on one hand, the aluminum oxide and the boron nitride are supposed to be inorganic particles with extremely high surface energy, and are easy to rapidly agglomerate in a system to reduce the uniformity of the system, on the other hand, the compatibility of the aluminum oxide and the boron nitride with an organic compound is poor, and the continuous proceeding of the epoxy resin crosslinking curing reaction is inhibited.
The invention discovers that when the inorganic filling materials are alumina with the particle size of 8-12 mu m, alumina with the particle size of 0.4-1 mu m and boron nitride with the particle size of 8-14 mu m, the thermal conductivity of the epoxy resin heat-conducting adhesive can be improved, and the prepared epoxy resin heat-conducting adhesive can be cured under the UV irradiation of 800W and 365nm without heating. The guess is that when three-level limitation of large, medium and small is carried out on the particle size of the inorganic heat-conducting filling material, the particles with smaller particle sizes are among the particles with larger particle sizes, and the filling particles orderly form heat-conducting passages among the epoxy resin, so that the network chain heat-conducting passages of the epoxy resin heat-conducting adhesive are optimized, and the heat-conducting coefficient of the epoxy resin heat-conducting adhesive is improved.
The present inventors have surprisingly found that when the mass ratio of alumina having a particle size of 8 to 12 μm, alumina having a particle size of 0.4 to 1 μm and boron nitride having a particle size of 8 to 14 μm is (2 to 6): 1: (1-3), the curing time of the epoxy resin heat-conducting adhesive under the irradiation of an 800W, 365nm curing lamp can be kept within 20 s. The conjoint ability of the inorganic heat-conducting filling material and the titanate compound is best under the condition, the density of stable contact points in the system is increased, the inorganic filler can give consideration to both the dispersibility and the filling compact space effect in the epoxy resin network structure, and then the crosslinking and curing of the epoxy resin can be completed in a short time.
In some preferred embodiments, the dispersant is a titanate compound.
The invention discovers that when the dispersant selects a titanate compound, the prepared epoxy resin heat-conducting adhesive has the best performance. The suspected reason is that the titanate compound not only contains alkoxy capable of being coupled with inorganic matters, but also contains reactive groups capable of being crosslinked and cured with unsaturated materials, so that a bridge is formed between the inorganic filling material and the epoxy resin polymer, and the compatibility of substances such as epoxy resin, reactive diluent, inorganic filling material and the like in the system is improved; the migration and passing performance of active free radicals of the UV initiator after UV irradiation is strong, the active free radicals are rapidly combined with substances such as alicyclic epoxy resin and the like, and the components are fully compatible, so that the crosslinking curing reaction can rapidly occur in a relatively stable environment, the curing time of the prepared epoxy resin heat-conducting adhesive under the irradiation of a 800W and 365nm curing lamp is shortest, and the weather resistance and the heat conductivity of the material are optimal.
More preferably, the titanate compound is isopropyl triisostearate (TTS), which is commercially available, for example, from Aomoto Fine Chemicals, CAS number 61417-49-0.
In some preferred embodiments, the sensitizer is a thioxanthone-based compound. More preferably, the thioxanthone compound is 2-isopropyl thioxanthone with CAS number 5495-84-1.
The invention provides a preparation method of a UV-curable epoxy resin heat-conducting adhesive, which comprises the following specific steps:
s1, weighing 5-15 parts of epoxy resin, 2-8 parts of nano epoxy resin, 2-8 parts of alicyclic epoxy resin, 2-8 parts of active diluent, 0.5-1.5 parts of UV initiator, 0.2-1 part of sensitizer, 70-80 parts of inorganic filling material and 0.2-2 parts of dispersing agent according to parts by weight;
s2, sequentially adding the epoxy resin, the nano epoxy resin, the alicyclic epoxy resin, the reactive diluent, the UV initiator, the sensitizer, the inorganic filling material and the dispersing agent into a material cylinder of the double-planet type dispersing instrument, and stirring at a first stirring speed for 10-20 min; setting the vacuum degree of the material placing cylinder at-0.08 MPa, and stirring at a second stirring speed for 100-150 min.
In some preferred embodiments, the first stirring speed is 40-100r/min and the second stirring speed is 750-.
Examples
Example 1.
The embodiment provides a UV-curable epoxy resin heat-conducting adhesive which comprises the following raw materials in parts by weight: 9.5 parts of epoxy resin, 5 parts of nano epoxy resin, 4.5 parts of alicyclic epoxy resin, 5 parts of reactive diluent, 0.6 part of UV initiator, 0.2 part of sensitizer, 75 parts of inorganic filling material and 0.2 part of dispersant.
The epoxy resin is phenolic aldehyde type epoxy resin which is purchased from Shanghai Kaiyn chemical Co., Ltd and has the type of Dow DEN 438.
The nano epoxy resin is purchased from the winning industrial group and has the model number of NANOPOX XP 24/0108.
The cycloaliphatic epoxy resin was purchased from Jiangsu Tetel chemical Co., Ltd, and was model number TTA 21P.
The active diluent is p-di (epoxy ethyl) benzene, and the CAS number is 16832-58-9.
The UV initiator is a cationic initiator, purchased from Pasteur, Germany, and has the model IRGACURE 250.
The sensitizer is 2-isopropyl thioxanthone, and the CAS number is 5495-84-1.
The inorganic filling material is first aluminum oxide, second aluminum oxide and boron nitride; the weight ratio of the first alumina to the second alumina to the boron nitride is 4.5: 1: 2.
the first alumina was purchased from Yadu Ma commercial (Shanghai) Inc. under the model AC 9000.
The second alumina is purchased from Yadu Ma commercial (Shanghai) Inc. and has a model number of AC 2000.
The boron nitride was purchased from 3M company (Minnesota mining, Inc.) and was model CFP 012.
The dispersant was TTS, purchased from Ajinomoto, Japan, CAS number 61417-49-0.
The specific preparation steps of the UV-curable epoxy resin heat-conducting adhesive comprise:
s1, weighing 9.5 parts of epoxy resin, 5 parts of nano epoxy resin, 4.5 parts of alicyclic epoxy resin, 5 parts of active diluent, 0.6 part of UV initiator, 0.2 part of sensitizer, 75 parts of inorganic filling material and 0.2 part of dispersant according to parts by weight;
s2, sequentially adding the epoxy resin, the nano epoxy resin, the alicyclic epoxy resin, the reactive diluent, the UV initiator, the sensitizer, the inorganic filling material and the dispersing agent into a material cylinder of the double-planet type dispersing instrument, and stirring at a first stirring speed for 10 min; setting the vacuum degree of the material placing tank to be-0.08 MPa, and stirring for 120min at a second stirring speed.
The first stirring speed is 50r/min, and the second stirring speed is 1000 r/min.
Example 2.
A UV-curable epoxy resin thermal conductive adhesive, which is implemented in the same manner as in example 1. Except that the nano-type epoxy resin described in the examples was not added.
Example 3.
A UV-curable epoxy resin thermal conductive adhesive, which is implemented in the same manner as in example 1. The difference is that the nano epoxy resin is added with the mark MX125, which is produced in Japan clock Yuan.
Example 4.
A UV-curable epoxy resin thermal conductive adhesive, which is implemented in the same manner as in example 1. The difference is that the UV initiator is a free radical initiator, specifically dicumyl peroxide, and the CAS number is 80-43-3.
Example 5.
A UV-curable epoxy resin thermal conductive adhesive, which is implemented in the same manner as in example 1. The difference is that the inorganic filling material is alumina.
The alumina was purchased from Yadu Ma commercial (Shanghai) Inc. under the model AC 9000.
Performance test method
UV curing time:
the epoxy resin thermal conductive adhesives prepared in the examples and comparative examples were irradiated under an 800W, 365nm UV curing lamp, and the desired curing time was recorded.
Coefficient of thermal conductivity:
the thermal conductivity of the cured product was determined using an LFA467 relaxation resistant laser flash thermal conductivity meter, each sample was tested 5 times, and the results averaged.
Performance test data
TABLE 1 Performance test results of epoxy resin thermally conductive adhesives prepared in examples
| Curing time/s | Coefficient of thermal conductivity/(W.m)-1·K-1) | |
| Example 1 | 20.1 | 1.59 |
| Example 2 | 20 | 1.15 |
| Example 3 | 20 | 1.08 |
| Example 4 | Not cured | \ |
| Example 5 | 18.9 | 1.22 |
Finally, it is pointed out that the foregoing examples are illustrative only, serving to explain some of the characteristics of the process according to the invention. The appended claims are intended to claim as broad a scope as is contemplated, and the examples presented herein are merely illustrative of selected implementations in accordance with all possible combinations of examples. Accordingly, it is applicants' intention that the appended claims are not to be limited by the choice of examples illustrating features of the invention. Also, where numerical ranges are used in the claims, subranges therein are included, and variations in these ranges are also to be construed as possible being covered by the appended claims.
Claims (10)
1. The UV-curable epoxy resin heat-conducting adhesive is characterized by comprising the following raw materials in parts by weight: 5-15 parts of epoxy resin, 2-8 parts of nano epoxy resin, 2-8 parts of alicyclic epoxy resin, 2-8 parts of reactive diluent, 0.5-1.5 parts of UV initiator, 0.2-1 part of sensitizer, 70-80 parts of inorganic filling material and 0.2-2 parts of dispersant.
2. The UV-curable epoxy resin thermal conductive adhesive according to claim 1, wherein the epoxy resin comprises bisphenol F type epoxy resin and/or novolac type epoxy resin.
3. The UV-curable epoxy resin heat-conducting adhesive is characterized in that the nano epoxy resin is a nano aluminum oxide modified epoxy resin.
4. The UV-curable epoxy resin heat-conducting adhesive is characterized in that the weight ratio of the epoxy resin to the nano epoxy resin is (1-4): 1.
5. the UV-curable epoxy resin thermal conductive adhesive according to claim 1, wherein the UV initiator is a cationic initiator.
6. The UV-curable epoxy resin thermal conductive adhesive according to claim 1, wherein the inorganic filler material is aluminum oxide and boron nitride;
the alumina comprises first alumina and second alumina;
the weight ratio of the first alumina to the second alumina to the boron nitride is (2-6): 1: (1-3).
7. The UV-curable epoxy resin heat-conducting adhesive according to claim 6, wherein the particle size of the first aluminum oxide is 8-12 μm, the particle size of the second aluminum oxide is 0.4-1 μm, and the particle size of the boron nitride is 8-14 μm.
8. The UV-curable epoxy resin thermal conductive adhesive according to claim 1, wherein the dispersant is a titanate compound.
9. The preparation method of the UV-curable epoxy resin heat-conducting adhesive according to any one of claims 1 to 8, which comprises the following specific steps:
s1, weighing 5-15 parts of epoxy resin, 2-8 parts of nano epoxy resin, 2-8 parts of alicyclic epoxy resin, 2-8 parts of active diluent, 0.5-1.5 parts of UV initiator, 0.2-1 part of sensitizer, 70-80 parts of inorganic filling material and 0.2-2 parts of dispersing agent according to parts by weight;
s2, sequentially adding the epoxy resin, the nano epoxy resin, the alicyclic epoxy resin, the reactive diluent, the UV initiator, the sensitizer, the inorganic filling material and the dispersing agent into a material cylinder of the double-planet type dispersing instrument, and stirring at a first stirring speed for 10-20 min; setting the vacuum degree of the material placing cylinder at-0.08 MPa, and stirring at a second stirring speed for 100-150 min.
10. The method as claimed in claim 9, wherein the first stirring speed is 40-100r/min, and the second stirring speed is 750-1200 r/min.
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| CN114989730A (en) * | 2021-11-03 | 2022-09-02 | 深圳市撒比斯科技有限公司 | Expansion type UV cross-linking low-stress adhesive and preparation method thereof |
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| CN1962799A (en) * | 2006-11-09 | 2007-05-16 | 上海大学 | Low-viscosity heat-conductive adhesive and process for preparing same |
| CN101597420A (en) * | 2008-06-03 | 2009-12-09 | 横滨橡胶株式会社 | Highly heat-conductive epoxy resin composition |
| CN106010398A (en) * | 2016-05-24 | 2016-10-12 | 黑龙江省科学院石油化学研究院 | Cationic ultraviolet-deep-curing adhesive and preparation method thereof |
| CN108003823A (en) * | 2017-09-08 | 2018-05-08 | 烟台信友新材料股份有限公司 | A kind of preparation method that may extend away cured UV-LED cationic curings adhesive |
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2020
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1962799A (en) * | 2006-11-09 | 2007-05-16 | 上海大学 | Low-viscosity heat-conductive adhesive and process for preparing same |
| CN101597420A (en) * | 2008-06-03 | 2009-12-09 | 横滨橡胶株式会社 | Highly heat-conductive epoxy resin composition |
| CN106010398A (en) * | 2016-05-24 | 2016-10-12 | 黑龙江省科学院石油化学研究院 | Cationic ultraviolet-deep-curing adhesive and preparation method thereof |
| CN108003823A (en) * | 2017-09-08 | 2018-05-08 | 烟台信友新材料股份有限公司 | A kind of preparation method that may extend away cured UV-LED cationic curings adhesive |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114989730A (en) * | 2021-11-03 | 2022-09-02 | 深圳市撒比斯科技有限公司 | Expansion type UV cross-linking low-stress adhesive and preparation method thereof |
| CN114989730B (en) * | 2021-11-03 | 2023-08-11 | 深圳市撒比斯科技有限公司 | Expansion type UV cross-linked low-stress adhesive and preparation method thereof |
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| CN112280516B (en) | 2023-04-18 |
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