CN102964983B - Silicon hybrid composite coating electronic adhesive and preparation method thereof - Google Patents
Silicon hybrid composite coating electronic adhesive and preparation method thereof Download PDFInfo
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Abstract
The invention provides a silicon hybrid composite coating electronic adhesive and a preparation method thereof. The preparation method comprises the following steps: under the action of acid catalysts which are respectively added in multiple steps, performing catalytic reaction on ethyl orthosilicate, PDMS (polydimethylsiloxane) and methyltriethoxysilane to form sol A; and compounding the sol A and chitosan to form the novel silicon hybrid composite coating electronic adhesive. The prepared coating electronic adhesive has favorable comprehensive properties; a coated film formed by the coating electronic adhesive has excellent hydrophobicity, favorable stain resistance and corrosion resistance, high adhesive force onto a coated substrate, high refracting index, fine mechanical property and good oxygen barrier property; and the preparation method is simple in preparation technique, easy to control in technical process and low in cost.
Description
Technical field
The present invention relates to a kind of organic inorganic hybridization silicon materials, be specifically related to a kind of hydrophobic type organic/inorganic silicon hybrid composite coated electronic pastes.
Background technology
Along with the development of the new high-tech industry such as novel material, advanced equipment manufacturing, higher requirement can be it is also proposed to unicircuit and the qualitative of electron device.Integrated circuit package is to pollutent and sensitivity thereof, and surface contamination even can badly influence assembly property, easily causes short circuit etc. because of adsorption of dust and moisture.Electron device surface-coated protecting materials is adopted to be the reliable scheme avoided Similar Problems to occur and extend the electron device life-span.Material for surface-coated must have good over-all properties, and energy and circuit board surface well attach, have high-insulativity can avoid puncturing or short circuit between circuit; There is the performances such as excellent electrical insulating property, resistant of high or low temperature, Inverter fed motor, radiation hardness, humidity and water resisting property, resistance to ozone, weather-resistant, stain resistant and resistance to chemical attack; The coating waste water performance had and the coating process of automatization, can adapt to the board production of high cleaning and automatization.
Organosilicon material has high-insulativity can avoid puncturing or short circuit between circuit; There is the performances such as excellent electrical insulating property, resistant of high or low temperature, Inverter fed motor, resistance to ozone; because it possesses these high-performance and advantage; Ying Te Do in vehicle electric field comes into one's own; Application Areas in automotive electronics is also more and more wider, as protection engine control module, spark coil and ignition module, power system module, breaking system module, exhaust gas measuring module, power-supply system, lighting system, various sensor, junctor etc.But, the organosilicon coating electronic pastes ubiquity film-forming properties of current preparation is poor, solidification value is high (being generally 150 ~ 200 DEG C), and the defect such as the sticking power of film to base material is poor, and its solvent resistance and physical strength also Shortcomings, make it apply and be subject to a definite limitation.There is provided a kind of good over-all properties that has, the coating electronic pastes not only having good thermotolerance, weathering resistance, hydrophobicity, a mechanical property and smear levelling property becomes the technical problem being badly in need of at present solving.
Sol-gel (sol-gel) method is considered to the method preparing transparent film of great potential.Sol-gel chemistry in sol gel processing grows up on the basis of alkoxide compound chemistry, namely alkoxide compound (presoma) is under the existence of acid (alkali) catalyzer, obtains highly cross-linked inorganic polymeric product through hydrolysis-condensation reaction (formation of adjoint colloidal sol and gel).The present invention prepares a kind of silicon hybridization composite coated electronic pastes with excellent over-all properties by sol-gel method.
Summary of the invention
The object of the invention is to the deficiency making up prior art existence, a kind of preparation method of silicon hybridization composite coated electronic pastes is provided, coating electronic pastes good combination property prepared by it, the film that this coating electronic pastes is formed has superpower hydrophobic performance, simultaneously resistance to soiling and good corrosion resistance, to smear substrate strong adhesion, specific refractory power is high, mechanical property is good, and has good oxygen-barrier property, and this preparation method preparation technology is simple, technological process is easy to control, and cost is low.
Another object of the present invention is the silicon hybridization composite coated electronic pastes providing a kind of preparation method mentioned above to obtain.
The present invention is for realizing its object, and the preparation method of the silicon hybridization composite coated electronic pastes provided, comprises the steps:
(1) mass concentration adding 20 ~ 40 weight parts in advance in flask is the ethanolic soln of 20% ~ 40%;
(2) prepare teos solution, wherein tetraethoxy weight part is 40-60, and dehydrated alcohol weight part is 100, is added drop-wise to by described teos solution in the flask of step (1), stirs after 10 minutes, is warming up to 55 ~ 60 DEG C;
(3) slowly acid catalyst A is dripped, until the pH value of mixing solutions is 3.5 ~ 4.5 in flask;
(4) in flask, add the PDMS(polydimethylsiloxane of 10 ~ 20 weight parts), the Union carbide A-162 of 2 ~ 5 weight parts and the silane coupling agent of 1 ~ 5 weight part, continue stirring 20 ~ 40min;
(5) in flask, be slowly added dropwise to acid catalyst B, until the pH value of mixing solutions is 2.5 ~ 3.0 in flask, insulation continues reaction 1 ~ 2h;
(6) in flask, the silane coupling agent of 2 ~ 6 weight parts is added dropwise to, insulated and stirred 1 hour, obtained Sol A;
(7) preparing mass concentration is the chitosan solution of 1%, and the Sol A that it is obtained with step (6) mixes by the volume ratio of 1 ~ 3:10, and being placed in temperature is that the water bath with thermostatic control of 55 ~ 70 DEG C is heated, and stirring 3 ~ 5h, namely obtains transparent silicon hybridization composite coated electronic pastes.
The preparation method of described silicon hybridization composite coated electronic pastes, the acid catalyst A described in step (3) is mass ratio is the hydrochloric acid of 8:0.5 ~ 2 and the acid catalyst of hydrofluoric acid composition, and the acid catalyst B in step (5) is hydrochloric acid soln.Thisly arrange in pairs or groups cleverly, make hydrolysis rate very fast, shorten colloidal sol formation time, and can obtain stable sol system, not easily occurring being separated, there is cleavage phenomenon in the film avoiding follow-up obtained coating electronic pastes to be formed; And obtained hybrid inorganic-organic silicon coating electronic pastes has very stable Si-O-Si cross-linked network, not easily occur that solvent is assembled and cause being separated.
The preparation method of described silicon hybridization composite coated electronic pastes, the weight proportion of the PDMS described in step (4) and Union carbide A-162 is 5:1.PDMS and Union carbide A-162 is added ,-the CH of introducing in this ratio
3quantity is moderate, defines the cross-linked network with chemical bonds in system, has the hybrid inorganic-organic network of smooth densification.Give mechanical property and the optical characteristics of hybrid material excellence simultaneously, and make the hybrid silicon of formation coating electronic pastes have better thermostability, solvent resistance and hydrophobicity.
The preparation method of described silicon hybridization composite coated electronic pastes, the volume ratio of described chitosan solution and Sol A is 2:10.Add chitosan solution in this ratio, obtained composite coated electronic pastes outward appearance more homogeneous transparent, coating electronic pastes to the strong adhesion of base material, and film and oxygen-barrier property better.
The preparation method of described silicon hybridization composite coated electronic pastes, the silane coupling agent described in step (4) is KH560.
The preparation method of described silicon hybridization composite coated electronic pastes, the silane coupling agent described in step (6) is KH-570.Add KH-570 in reaction system and effectively can improve phase interface, be conducive to two-phase in reaction system and be uniformly dispersed.
The invention provides the silicon hybridization composite coated electronic pastes that a kind of preparation method as described above obtains.
The invention provides technical scheme and there is following beneficial effect:
Preparation method of the present invention each component compatibility in preparation process is good, not easily occurs being separated, and ensure that the obtained hybrid silicon colloidal sol transparency is good, product stability is good, and spreading property is good, easily forms smooth film; And effectively reduce the surface energy of polysiloxane, there is splendid hydrophobicity, improve the resistance to bond of obtained product.Catalyzer adopts two step addition manners, more effectively ensure that the hybrid silicon sol size formed is evenly distributed, the cross-linked network that the Si-O-Si keyed jointing forming good stability is formed, not easily occur the gathering of large size sol particles, can also speed of reaction be ensured simultaneously, raise the efficiency.
The silicon hybridization composite coated electronic pastes high comprehensive performance that preparation method provided by the invention obtains, good heat resistance, hydrophobicity are strong, film-forming properties is good, and refractive index is up to more than 1.7.
Embodiment
Below in conjunction with embodiment, technical scheme of the present invention is further described:
Embodiment 1
A kind of silicon hybridization composite coated electronic pastes, its preparation adopts following steps to carry out:
(1) mass concentration adding 20 weight parts in advance in flask is the ethanolic soln of 20%;
(2) prepare the teos solution with dehydrated alcohol preparation, wherein tetraethoxy weight part is 40, and dehydrated alcohol weight part is 100, is added drop-wise to by described teos solution in the flask of step (1), stirs after 10 minutes, is warming up to 55 DEG C;
(3) acid catalyst of the hydrochloric acid that mass ratio is 8:0.5 and hydrofluoric acid composition is slowly dripped, until the pH value of mixing solutions is 3.5 in flask;
(4) in flask, add the silane coupling agent KH560 of the PDMS of 10 weight parts, the Union carbide A-162 of 2 weight parts and 1 weight part, continue to stir 20min;
(5) in flask, be slowly added dropwise to hydrochloric acid soln, until the pH value of mixing solutions is 2.5 in flask, insulation continues reaction 1h;
(6) in flask, the Silane coupling reagent KH-570 of 2 weight parts is added dropwise to, insulated and stirred 1 hour, obtained Sol A;
(7) getting appropriate chitosan, to be dissolved in volume fraction be in the aqueous acetic acid of 0.5%, at the uniform velocity be stirred to and dissolve completely, suction filtration, obtained quality solubility is the chitosan solution of 1%, Sol A obtained with step (6) for chitosan solution is mixed by the volume ratio of 1:10, being placed in temperature is that the water bath with thermostatic control of 55 DEG C is heated, and stirs 3h, namely obtained transparent silicon hybridization composite coated electronic pastes;
(8) after the product of step (7) at room temperature being placed 24h, get and be coated on totally smooth slide glass in right amount, vibration allows its natural levelling, drying at room temperature 1h, continue at 90 DEG C of dry 3h, be cooled to the film that room temperature obtains silicon hybridization composite coated electronic pastes, carry out performance test to this film, testing method and test result see table 1.
Embodiment 2
A kind of silicon hybridization composite coated electronic pastes, its preparation adopts following steps to carry out:
(1) mass concentration adding 40 weight parts in advance in flask is the ethanolic soln of 40%;
(2) prepare the teos solution with dehydrated alcohol preparation, wherein tetraethoxy weight part is 60, and dehydrated alcohol weight part is 100, is added drop-wise to by described teos solution in the flask of step (1), stirs after 10 minutes, is warming up to 60 DEG C;
(3) acid catalyst of the hydrochloric acid that mass ratio is 8:1 and hydrofluoric acid composition is slowly dripped, until the pH value of mixing solutions is 4.5 in flask;
(4) in flask, add the silane coupling agent KH560 of the PDMS of 20 weight parts, the Union carbide A-162 of 5 weight parts and 5 weight parts, continue to stir 40min;
(5) in flask, be slowly added dropwise to hydrochloric acid soln, until the pH value of mixing solutions is 3.0 in flask, insulation continues reaction 2h;
(6) in flask, the Silane coupling reagent KH-570 of 6 weight parts is added dropwise to, insulated and stirred 1 hour, obtained Sol A;
(7) taking appropriate chitosan is dissolved in aqueous acetic acid, at the uniform velocity be stirred to and dissolve completely, suction filtration, obtained volume ratio is the chitosan solution of mass concentration 1%, Sol A obtained with step (6) for chitosan solution is mixed by the volume ratio of 3:10, being placed in temperature is that the water bath with thermostatic control of 70 DEG C is heated, and stirs 5h, namely obtained transparent silicon hybridization composite coated electronic pastes;
(8) after the product of step (7) at room temperature being placed 24h, get and be coated on totally smooth slide glass in right amount, vibration allows its natural levelling, drying at room temperature 1h, continue at 90 DEG C of dry 3h, be cooled to the film that room temperature obtains hybrid inorganic-organic silicon coating electronic pastes, carry out performance test to this film, testing method and test result see table 1.
Embodiment 3
A kind of silicon hybridization composite coated electronic pastes, its preparation adopts following steps to carry out:
(1) mass concentration adding 30 weight parts in advance in flask is the ethanolic soln of 30%;
(2) prepare the teos solution with dehydrated alcohol preparation, wherein tetraethoxy weight part is 50, and dehydrated alcohol weight part is 100, is added drop-wise to by described teos solution in the flask of step (1), stirs after 10 minutes, is warming up to 60 DEG C;
(3) acid catalyst of the hydrochloric acid that mass ratio is 8:2 and hydrofluoric acid composition is slowly dripped, until the pH value of mixing solutions is 4 in flask;
(4) in flask, add the silane coupling agent KH560 of the PDMS of 15 weight parts, the Union carbide A-162 of 3 weight parts and 3 weight parts, continue to stir 30min,
(5) in flask, be slowly added dropwise to hydrochloric acid soln, until the pH value of mixing solutions is 2.7 in flask, insulation continues reaction 1.5h,
(6) in flask, the Silane coupling reagent KH-570 of 4 weight parts is added dropwise to, insulated and stirred 1 hour, obtained Sol A.
(7) taking appropriate chitosan is dissolved in aqueous acetic acid, at the uniform velocity be stirred to and dissolve completely, suction filtration, obtained mass concentration is the chitosan solution of 1%, Sol A obtained with step (6) for chitosan solution is mixed by the volume ratio of 2:10, being placed in temperature is that the water bath with thermostatic control of 60 DEG C is heated, and stirs 4h, namely obtained transparent silicon hybridization composite coated electronic pastes.
(8) after the product of step (7) at room temperature being placed 24h, get and be coated on totally smooth slide glass in right amount, vibration allows its natural levelling, drying at room temperature 1h, continue at 90 DEG C of dry 3h, be cooled to the film that room temperature obtains hybrid inorganic-organic silicon coating electronic pastes, carry out performance test to this film, testing method and test result see table 1.
Table 1
The above, it is only preferred embodiment of the present invention, not any pro forma restriction is done to the present invention, therefore all contents not departing from technical solution of the present invention, according to technical spirit of the present invention to any simple modification made for any of the above embodiments, equivalent variations and modification, all still belong in the scope of technical solution of the present invention.
Claims (6)
1. a preparation method for silicon hybridization composite coated electronic pastes, is characterized in that, comprises the steps:
(1) mass concentration adding 20 ~ 40 weight parts in advance in flask is the ethanolic soln of 20% ~ 40%;
(2) prepare teos solution, wherein tetraethoxy weight part is 40-60, and dehydrated alcohol weight part is 100, is added drop-wise to by described teos solution in the flask of step (1), stirs after 10 minutes, is warming up to 55 ~ 60 DEG C;
(3) slowly acid catalyst A is dripped, until the pH value of mixing solutions is 3.5 ~ 4.5 in flask;
(4) in flask, add the silane coupling agent of the PDMS of 10 ~ 20 weight parts, the Union carbide A-162 of 2 ~ 5 weight parts and 1 ~ 5 weight part, continue stirring 20 ~ 40min;
(5) in flask, be slowly added dropwise to acid catalyst B, until the pH value of mixing solutions is 2.5 ~ 3.0 in flask, insulation continues reaction 1 ~ 2h;
(6) in flask, the silane coupling agent of 2 ~ 6 weight parts is added dropwise to, insulated and stirred 1 hour, obtained Sol A;
(7) preparing mass concentration is the chitosan solution of 1%, the Sol A that it is obtained with step (6) mixes by the volume ratio of 1 ~ 3:10, being placed in temperature is that the water bath with thermostatic control of 55 ~ 70 DEG C is heated, and stirs 3 ~ 5h, namely obtained transparent silicon hybridization composite coated electronic pastes;
Wherein, the acid catalyst A described in step (3) is mass ratio is the hydrochloric acid of 8:0.5 ~ 2 and the acid catalyst of hydrofluoric acid composition, and the acid catalyst B in step (5) is hydrochloric acid soln.
2. the preparation method of silicon hybridization composite coated electronic pastes according to claim 1, is characterized in that, the weight proportion of the PDMS described in step (4) and Union carbide A-162 is 5:1.
3. the preparation method of silicon hybridization composite coated electronic pastes according to claim 1, is characterized in that, the chitosan solution in step (7) and the volume ratio of Sol A are 2:10.
4. the preparation method of silicon hybridization composite coated electronic pastes according to claim 1, is characterized in that, the silane coupling agent described in step (4) is KH560.
5. the preparation method of silicon hybridization composite coated electronic pastes according to claim 1, is characterized in that, the silane coupling agent described in step (6) is KH-570.
6. the silicon hybridization composite coated electronic pastes that obtains of the preparation method as described in any one of Claims 1 to 5.
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