CN111334044B - Organic silicone gel for precise electronic component encapsulation and use method thereof - Google Patents
Organic silicone gel for precise electronic component encapsulation and use method thereof Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 25
- 238000005538 encapsulation Methods 0.000 title claims abstract description 17
- 229920001296 polysiloxane Polymers 0.000 title claims description 12
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 41
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 41
- 239000010703 silicon Substances 0.000 claims abstract description 41
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000012530 fluid Substances 0.000 claims description 27
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 15
- 229910021389 graphene Inorganic materials 0.000 claims description 8
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- 229910052681 coesite Inorganic materials 0.000 claims description 7
- 229910052906 cristobalite Inorganic materials 0.000 claims description 7
- 239000000377 silicon dioxide Substances 0.000 claims description 7
- 229910052682 stishovite Inorganic materials 0.000 claims description 7
- 229910052905 tridymite Inorganic materials 0.000 claims description 7
- VTYYLEPIZMXCLO-UHFFFAOYSA-L calcium carbonate Substances [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 6
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- 238000002156 mixing Methods 0.000 claims description 5
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- 238000003756 stirring Methods 0.000 claims description 2
- 239000000499 gel Substances 0.000 abstract description 46
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 9
- 229910052782 aluminium Inorganic materials 0.000 abstract description 9
- 239000004593 Epoxy Substances 0.000 abstract description 8
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- 239000000463 material Substances 0.000 description 12
- 238000002360 preparation method Methods 0.000 description 8
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- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 2
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- AKYHKWQPZHDOBW-UHFFFAOYSA-N (5-ethenyl-1-azabicyclo[2.2.2]octan-7-yl)-(6-methoxyquinolin-4-yl)methanol Chemical compound OS(O)(=O)=O.C1C(C(C2)C=C)CCN2C1C(O)C1=CC=NC2=CC=C(OC)C=C21 AKYHKWQPZHDOBW-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- JNTYLPFZLSURCZ-UHFFFAOYSA-L C(C)(=O)O[Zn]Br Chemical compound C(C)(=O)O[Zn]Br JNTYLPFZLSURCZ-UHFFFAOYSA-L 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 239000001576 FEMA 2977 Substances 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- REYJJPSVUYRZGE-UHFFFAOYSA-N Octadecylamine Chemical compound CCCCCCCCCCCCCCCCCCN REYJJPSVUYRZGE-UHFFFAOYSA-N 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- 229910018557 Si O Inorganic materials 0.000 description 1
- 229910002808 Si–O–Si Inorganic materials 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
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- 150000008049 diazo compounds Chemical class 0.000 description 1
- NAPSCFZYZVSQHF-UHFFFAOYSA-N dimantine Chemical compound CCCCCCCCCCCCCCCCCCN(C)C NAPSCFZYZVSQHF-UHFFFAOYSA-N 0.000 description 1
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- WBJINCZRORDGAQ-UHFFFAOYSA-N ethyl formate Chemical compound CCOC=O WBJINCZRORDGAQ-UHFFFAOYSA-N 0.000 description 1
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- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
- 229960003110 quinine sulfate Drugs 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 239000004945 silicone rubber Substances 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 150000003512 tertiary amines Chemical class 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Images
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
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Abstract
The invention discloses an organic silicon gel for precise electronic component encapsulation and a using method thereof, relating to the technical field of electronic component protection in the electronic industry, wherein the organic silicon gel comprises a component A and a component B, wherein the component A is organic silicon gel, and the component B is solvent-free nanofluid; the component A accounts for 100 parts by weight, and the component B accounts for 0.5-10 parts by weight. The application method is that 100 parts of the component A and 0.5 to 10 parts of the component B are stirred and mixed evenly, and then the mixture is cured for 24 to 96 hours at room temperature. Various performance indexes of the silica gel can meet the encapsulation requirement of precise electronic components. I.e. viscosity at 25 ℃ is 2200 MPa.s-2500 MPa.s; the shear strength reaches 0.2-0.5MPa (aluminum and aluminum) and 0.2-0.5MPa (3240 epoxy plate and 3240 epoxy plate); linear expansion coefficient less than or equal to 3.0 x 10‑4℃‑1。
Description
Technical Field
The invention relates to the technical field of electronic component protection in the electronic industry, in particular to an organic silicon gel for precise electronic component encapsulation and a using method thereof.
Background
Electronic encapsulation is that liquid rubber material is filled into devices with electronic elements and circuits mechanically or manually and is solidified into thermosetting polymer insulating material with excellent performance under normal temperature or heating condition. The electronic device can strengthen the integrity of the electronic device and improve the resistance to external impact and vibration; the insulation between internal elements and circuits is improved, and the miniaturization and the light weight of devices are facilitated; the direct exposure of elements and circuits is avoided, and the waterproof and moisture-proof performances of the device are improved.
The addition type organic silicon gel has unique excellent performance, takes Si-O-Si as a main chain, and the bond energy of the Si-O is high and reaches 422.5kJ/mol, becauseThe stability is very good, the silicone oil chain is of a spiral structure and is very soft, and the viscosity is-40-200OThe C can keep better mechanical property and performance stability, and has no by-product in the curing process, so the C is commonly used for encapsulation protection of precise electronic components. However, the problems of poor adhesion performance and high thermal expansion coefficient exist, interface delamination between the silicone gel and an adhesion object under the action of high temperature often occurs, and a large pressure is caused to each component of the electronic component under the structural constraint, so that the electronic component is deformed or damaged, and therefore, how to effectively increase the adhesion performance of the silicone gel and reduce the thermal expansion coefficient becomes the key for solving the problems.
Currently, there are two main methods for the study of the adhesion performance of silicone gel, first, the treatment of the substrate surface. The main surface modification methods at present are: physical mechanical methods, chemical oxidation methods, plasma treatment, flame methods, surface coating treatments, corona methods, and the like; secondly, the self-bonding improvement is carried out on the addition type silicon rubber formula, and two main modes are as follows: one is to add a tackifier with active groups in the formula; the other method is to change the molecular structure of the base material to make the molecular chain have active groups. For complex precision electromechanical products, due to the fact that the complex precision electromechanical products are multiple in component types and complex in structure, the problem of low efficiency exists when the first treatment method is adopted for the surfaces of the components in the encapsulation structure, and multiple surface modification methods can be combined aiming at different base material objects, so that the realizability is poor. The second method is to add an active group tackifier to a silicone rubber formula or introduce an active group into a chain segment structure, wherein the introduction of the active group has a certain influence on the curing behavior of the material, and generally requires driving the reaction at a relatively high temperature, and the high temperature may cause the high-temperature damage of electronic components.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the invention provides the organic silicon gel for the encapsulation of the precise electronic components, and aims to solve the problem that the adhesion property and the thermal expansion coefficient of the silicon gel cannot meet the encapsulation requirement of the precise electronic components in the prior art. The invention is based on the existing commercial silicon gel material formula, by directly introducing the solvent-free nano fluid which is in a flowing state at room temperature, the thermal expansion coefficient of the silicon gel material can be effectively reduced and the bonding strength of the silicon gel material can be increased on the basis of not obviously influencing the viscosity of the silicon gel material formula.
In order to solve the problems in the prior art, the invention is realized by the following technical scheme:
an organic silicon gel for precise electronic component encapsulation is characterized in that: the solvent-free nano-fluid comprises a component A and a component B, wherein the component A is organic silicon gel, and the component B is solvent-free nano-fluid; the component A accounts for 100 parts by weight, and the component B accounts for 0.5-10 parts by weight.
Further preferably, the component B is 0.5 to 5 parts.
The organosilicon gel of the component A is selected from one or two of GN-502 and GN-522.
The solvent-free nano fluid used in the component B is solvent-free TiO2Nanofluid, solventless CaCO3Nanofluid, solventless SiO2A nanofluid, a solvent-free ZnO nanofluid, a solvent-free carbon black nanofluid, a solvent-free graphene nanofluid, and a solvent-free carbon nanotube nanofluid.
The solvent-free nanofluids consist of flexible organic chains with nanoparticles (organic or inorganic particles) as core, grafted to the nanoparticle surface (see fig. 1). The organic chains can be single-layer coronary layers or multiple layers (such as a coronary layer and a neck layer), and the agglomeration of the nano particles is effectively prevented due to the blocking effect of the flexible organic chains. By increasing the grafting density of the organic chains, a liquid-like substance can be obtained which is homogeneous under the microscope and the entire system can be regarded as a single component. Meanwhile, the organic chain grafted to the surface of the nano-particle can enhance the compatibility and the dispersibility of the nano-particle, and is different from the traditional colloidal suspension in that the solvent-free nano-fluid is completely solvent-free and has zero vapor pressure, the nano-fluid has the characteristics of good thermal stability and single dispersion, particularly, the core and the surface oligomer of the nano-fluid have designability, and the nano-fluid can be introduced into an organic silicon gel system to fully exert various excellent performances of the nano-particle, thereby being beneficial to improving the bonding performance of the organic silicon gel and reducing the linear expansion coefficient of the organic silicon gel. The project obtains the high-adhesion and low-expansion-coefficient organic silicon gel for encapsulating the precise electronic components and the using method thereof by utilizing the designability of the core-shell structure of the solvent-free nano fluid, scientific experimental design and matching research with the components of the organic silicon gel.
The invention also provides a use method of the organic silicon gel for precise electronic component encapsulation, and the organic silicon gel is cured by the method, so that various performance indexes of the organic silicon gel can meet the encapsulation requirement of precise electronic components. Namely 2200 mPas-2500 mPas with the viscosity at 25 ℃; the shear strength reaches 0.2-0.5MPa (aluminum and aluminum) and 0.2-0.5MPa (3240 epoxy plate and 3240 epoxy plate); linear expansion coefficient less than or equal to 3.0 x 10-4 ℃-1。
A use method of organic silicon gel for precise electronic component encapsulation is characterized in that: stirring and mixing 100 parts of the component A and 0.5-10 parts of the component B uniformly, and curing for 24-96 h at room temperature.
As a preferable technical scheme of the invention, 100 parts of the component A and 0.5-5 parts of the component B are stirred and mixed uniformly, and then the mixture is cured for 36-60 h at room temperature.
Compared with the prior art, the invention has the beneficial technical effects that:
1. the invention is based on the existing commercial silicon gel material formula, by directly introducing the solvent-free nano fluid which is in a flowing state at room temperature, the thermal expansion coefficient of the silicon gel material can be effectively reduced on the basis of not obviously reducing the viscosity of the silicon gel material formula, and meanwhile, the bonding strength of the silicon gel material is increased.
2. The performance indexes of the organic silicon gel are as follows: viscosity: at 25 ℃ in the range of 2200mPa ∙ s to 2500mPa ∙ s, (2) shear strength: 0.2-0.5MPa (aluminum and aluminum), 0.2-0.5MPa (3240 epoxy plate and 3240 epoxy plate), (4) linear expansion coefficient less than or equal to 3.0 × 10-4 ℃-1。
Drawings
Fig. 1 is a schematic view of a solvent-free nanofluid.
Detailed Description
The technical solution of the present invention is further described in detail with reference to the following examples.
The invention discloses an organic silicon gel for precise electronic component encapsulation, which comprises a component A and a component B, wherein the component A is organic silicon gel, and the component B is solvent-free nanofluid; the component A accounts for 100 parts by weight, and the component B accounts for 0.5-10 parts by weight.
The specific application is shown in the following table 1:
table 1 shows the compounding ratio of the component A to the component B and the performance index of the obtained silicone gel.
Through the above examples 1-6, after the components a and B are mixed at room temperature, the viscosity of the mixed silica gel is tested by using a viscosity tester, and the viscosity test results of the different ratios in the examples 1-6 are shown in the table above; after mixing component A and component B in the proportions of examples 1 to 6 described above, they were cured at room temperature, and their shear strengths were measured by adhesion between aluminum plates and adhesion between resin plates, respectively, and the results of the measurements are shown in the above table. Testing the linear expansion coefficient of the cured silicone gel by a linear expansion coefficient tester, wherein the viscosity is measured by a rotational viscometer at room temperature of 25 ℃; the shear strength is measured by a universal testing machine according to the GB/T7124-86 adhesive tensile shear strength test standard; the linear expansion coefficient is obtained according to a GB/T1036-89 plastic linear expansion coefficient measuring method; the specific test results are shown in table 1 above.
In the present application, a set of comparative experiments was also proposed, i.e. replacing component B of the present application with nanoparticles and performing a performance test on the silica gel after mixing component a and the nanoparticles, the test method being consistent with the above test method. The experimental results obtained are shown in table 2 below:
table 2 shows the ratio of component A to nanoparticles and the performance index of the obtained silica gel.
As can be seen from the above tables 1 and 2, the viscosity of the solvent-free nano fluid is obviously reduced, the shear strength is obviously improved, and the linear expansion coefficient is obviously reduced compared with the solid nano particles.
The solvent-free nanofluids consist of flexible organic chains with nanoparticles (organic or inorganic particles) as core, grafted to the nanoparticle surface (see fig. 1). The organic chains can be single-layer coronary layers or multiple layers (such as a coronary layer and a neck layer), and the agglomeration of the nano particles is effectively prevented due to the blocking effect of the flexible organic chains. By increasing the grafting density of the organic chains, a liquid-like substance can be obtained which is homogeneous under the microscope and the entire system can be regarded as a single component. Meanwhile, the organic chain grafted to the surface of the nano-particle can enhance the compatibility and the dispersibility of the nano-particle, and is different from the traditional colloidal suspension in that the solvent-free nano-fluid is completely solvent-free and has zero vapor pressure, the nano-fluid has the characteristics of good thermal stability and single dispersion, particularly, the core and the surface oligomer of the nano-fluid have designability, and the nano-fluid can be introduced into an organic silicon gel system to fully exert various excellent performances of the nano-particle, thereby being beneficial to improving the bonding performance of the organic silicon gel and reducing the linear expansion coefficient of the organic silicon gel. The project obtains the high-adhesion and low-expansion stress organic silicon gel for encapsulating the precise electronic component and the preparation method thereof by utilizing the designability of the core-shell structure of the solvent-free nano fluid, scientific experimental design and matching research with the components of the organic silicon gel.
The silicone gel of component A is a combination of one or more of GN-502 and GN-522, and is cured at room temperature.
The solvent-free nano fluid used in the component B is solvent-free TiO2Nanofluid, solventless CaCO3Nanofluid, solventless SiO2A nanofluid, a solvent-free ZnO nanofluid, a solvent-free carbon black nanofluid, a solvent-free graphene nanofluid, and a solvent-free carbon nanotube nanofluid.
In this example, solvent-free nano TiO2The fluid preparation method comprises the following steps: hydroxylating surface of nano TiO2Grafted with quaternized silane coupling agent, and then ion-exchanged with polyoxyethylene functionalized organic long chain.
Solvent-free CaCO3The preparation method of the nano-fluid comprises the following steps of (Li Q and other J Am Chem Soc, 2009, 131 (26): 9148-9149): under specific chemical conditions, the number of hydroxyl groups on the surface of the nano fluid is increased, and then the solvent-free calcium carbonate nano fluid can be prepared by adopting a silane coupling agent grafting technology.
Solventless SiO2The preparation method of the nanofluid comprises the following steps: preparing solid SiO with different grain diameters by using absolute ethyl alcohol, ammonia water, deionized water, methanol and tetraethoxysilane at room temperature by adopting a Stober method2Nanometer microsphere, wherein KH560 is used to graft polyether amine (monoamine, diamine or triamine) on SiO2Surface or first in SiO2The surface of the particles is treated by an acidic silane coupling agent, then is neutralized by NaOH to form salt, after the reaction is carried out for 24 hours at 70 ℃, sodium ions are removed by a particle exchange column and are fully protonated, the obtained product and alkaline PEG functionalized tertiary amine are subjected to acid-base reaction to prepare the solvent-free SiO2A nanofluid.
The preparation method of the solvent-free ZnO nanofluid comprises the following steps: firstly, NaOH and ZnCl are used2Reaction to prepare Zn (OH)2Then reacting with bromoacetic acid to obtain bromozinc acetate, then reacting with N, N-dimethyl octadecyl amine to obtain corresponding quaternary ammonium salt, then carrying out anion exchange with quinine sulfate to obtain zinc ionic liquid, and finally reacting with LiOH to obtain ZnO ionic liquid, namely the solvent-free ZnO nanofluid.
The preparation method of the solvent-free carbon black nanofluid comprises the following steps: firstly, carrying out strong acid oxidation treatment on original carbon black, then grafting by using a silane coupling agent DC5700 to obtain carbon black organic ionic salt, and finally carrying out ion exchange with PEG functionalized nitrate to prepare the solvent-free carbon black nano fluid with liquid-like behavior.
The preparation method of the solvent-free graphene nanofluid comprises the following steps: the method comprises the steps of grafting diazonium salt to the surface of graphene by utilizing a spontaneous transfer mechanism from graphene surface electrons to the diazonium salt to obtain sulfonated graphene, and exchanging flexible long-chain ions with graphene ions to obtain diazo compound grafting solvent-free graphene fluid.
The preparation method of the solvent-free carbon nanotube nanofluid comprises the following steps: the solvent-free carbon nano tube nano fluid is prepared by carrying out acid-base reaction on octadecylamine polyoxyethylene ether and an acid-oxidized carbon nano tube or by grafting polyether amine (monoamine, diamine or triamine) on the surface of the carbon nano tube by using a KH560 coupling agent.
In this embodiment, a use method of the organic silicon gel for precise electronic component potting is further provided, and the organic silicon gel is cured by the method, so that various performance indexes of the organic silicon gel can meet the potting requirement of precise electronic components. Namely the viscosity is 2200 to 2500 mPa.s at the temperature of 25 ℃; the shear strength reaches 0.2-0.5MPa (aluminum and aluminum) and 0.2-0.5MPa (3240 epoxy plate and 3240 epoxy plate); linear expansion coefficient less than or equal to 3.0 x 10-4 ℃-1。
A method for preparing organic silicon gel for encapsulating precise electronic components includes mixing 100 parts of component A and 0.5-10 parts of component B uniformly, and curing at room temperature for 24-96 h. In this case, component A is selected from one or a combination of GN-502 and GN-522.
As a preferable technical scheme of the invention, 100 parts of the component A and 0.5-5 parts of the component B are stirred and mixed uniformly, and then cured for 36-60 h at room temperature; in this case, component A is selected from one or a combination of GN-502 and GN-522.
Claims (6)
1. The room temperature curing organic silicon gel for encapsulating the precise electronic components is characterized in that: the solvent-free nano-fluid comprises a component A and a component B, wherein the component A is organic silicon gel, and the component B is solvent-free nano-fluid; the component A accounts for 100 parts by weight, and the component B accounts for 0.5-10 parts by weight.
2. The room temperature curing silicone gel for precise electronic component potting of claim 1, wherein: the component B is 0.5-5 parts.
3. The room-temperature-curing silicone gel for potting precision electronic components as claimed in claim 1 or 2, wherein: the organosilicon gel of the component A is selected from one or two of GN-502 and GN-522.
4. The room temperature curing silicone gel for precise electronic component potting of claim 1, wherein: the solvent-free nano fluid used in the component B is solvent-free TiO2Nanofluid, solventless CaCO3Nanofluid, solventless SiO2A nanofluid, a solvent-free ZnO nanofluid, a solvent-free carbon black nanofluid, a solvent-free graphene nanofluid, and a solvent-free carbon nanotube nanofluid.
5. The use method of the room temperature curing silicone gel for the encapsulation of the precise electronic components, according to any one of claims 1 to 4, is characterized in that: stirring and mixing 100 parts of the component A and 0.5-10 parts of the component B uniformly, and curing for 24-96 h at room temperature.
6. The use method of the room temperature curing organic silicon gel for the encapsulation of the precise electronic component, according to claim 5, is characterized in that: after 100 parts of the component A and 0.5-5 parts of the component B are stirred and mixed uniformly, curing is carried out for 36-60 h at room temperature.
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