CN113597088A - Circuit material, preparation method and circuit board thereof - Google Patents
Circuit material, preparation method and circuit board thereof Download PDFInfo
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- CN113597088A CN113597088A CN202110832260.5A CN202110832260A CN113597088A CN 113597088 A CN113597088 A CN 113597088A CN 202110832260 A CN202110832260 A CN 202110832260A CN 113597088 A CN113597088 A CN 113597088A
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K1/00—Printed circuits
- H05K1/02—Details
- H05K1/09—Use of materials for the conductive, e.g. metallic pattern
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/10—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern
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Abstract
The application relates to the field of circuit board production and manufacturing, and particularly discloses a circuit material, a preparation method and a circuit board thereof; a circuit material comprises a flexible conductive metal layer, a PET film and an adhesive layer arranged between the flexible conductive metal layer and the PET film, wherein the thickness of the adhesive layer is 0.4-1 mm; the adhesive layer is made of an adhesive, and the adhesive is made of the following raw materials in parts by weight: 80-120 parts of hydroxyl-terminated polydimethylsiloxane, 2-7 parts of ethyl orthosilicate, 2-7 parts of catalyst and 5-15 parts of coated titanium dioxide; the preparation method comprises the following steps: coating an adhesive between the flexible conductive metal layer and the PET film, and curing the adhesive to form an adhesive layer at 40-55 ℃ to obtain a finished circuit material; a circuit board made of a circuit material; the adhesive has good flexibility, cohesiveness and transparency, so that the substrate has good flexibility, processability and appearance.
Description
Technical Field
The application relates to the field of circuit board production and manufacturing, in particular to a circuit material, a preparation method and a circuit board thereof.
Background
The circuit board is also called as a PCB board or a printed circuit board, is an important electronic component, is a support body of an electronic component, and is also a carrier for electrical connection of the electronic component.
The circuit board is divided into a rigid circuit board and a flexible circuit board, the flexible circuit board is made of polyimide or polyester film as a base material and has the advantages of light weight and good bending performance, an adhesive used in the preparation process of the flexible circuit board needs to have good flexibility and cohesiveness, and the polyester film has good transparency and light transmittance, so that the surface condition of the flexible circuit board can be observed conveniently, and therefore the adhesive needs to have good transparency.
Since epoxy resin has good high temperature resistance, epoxy resin is often used as an adhesive for circuit boards, and although it has good transparency and adhesiveness, it has poor flexibility after curing and is not suitable for flexible circuit boards.
Therefore, it is urgently needed to prepare a substrate for a flexible circuit board, and the substrate has better flexibility, processability and appearance performance by utilizing better flexibility, cohesiveness and transparency of an adhesive on the substrate.
Disclosure of Invention
In order to prepare a substrate applied to a flexible circuit board, wherein an adhesive on the substrate has better flexibility and good transparency, so that the substrate has better flexibility and the surface performance of the substrate is convenient to observe, the application provides a circuit material, a preparation method and a circuit board thereof.
In a first aspect, the present application provides a circuit material, which adopts the following technical scheme:
a circuit material comprises a flexible conductive metal layer, a PET film and an adhesive layer arranged between the flexible conductive metal layer and the PET film, wherein the thickness of the adhesive layer is 0.4-1 mm;
the adhesive layer is made of an adhesive, and the adhesive is made of the following raw materials in parts by weight:
80-120 parts of hydroxyl-terminated polydimethylsiloxane, 2-7 parts of ethyl orthosilicate, 2-7 parts of catalyst and 5-15 parts of coated titanium dioxide.
By adopting the technical scheme, the hydroxyl-terminated polydimethylsiloxane, the tetraethoxysilane and the catalyst are matched to ensure that the adhesive has better flexibility and elasticity after being cured, and then the coated titanium dioxide is matched to improve the cohesive force of the adhesive by utilizing the coated titanium dioxide so as to improve the viscosity of the adhesive.
When the prepared adhesive is used for bonding the flexible conductive metal layer and the PET film, the good viscosity of the adhesive is utilized, so that the bonding effect of the flexible conductive metal layer and the PET film is good, and the processing performance of the finished circuit material is improved; and the finished product circuit material has better flexibility by utilizing the better flexibility of the adhesive; meanwhile, the good transparency of the adhesive is matched with the good transparency of the PET film, so that the adhesion effect of the PET film on the surface of the flexible conductive metal layer can be observed conveniently, and the finished circuit material has good apparent performance.
In a second aspect, the present application provides a method for preparing a circuit material, which adopts the following technical scheme:
a method of making a circuit material comprising the steps of:
coating the adhesive on the surface of the flexible conductive metal layer, then covering the surface of the adhesive with a PET film, placing the adhesive at 40-55 ℃, and curing the adhesive to form an adhesive layer to obtain the finished product circuit material.
By adopting the technical scheme, the curing of the adhesive can be accelerated in the environment of 40-50 ℃, so that the processing efficiency of the finished circuit material is improved, the bonding effect among the raw materials of the circuit material is improved, and the processing performance of the circuit material is improved.
Preferably, the coated titanium dioxide is prepared by the following method:
i, weighing titanium dioxide, soaking in water, stirring, and taking out the titanium dioxide to obtain water-absorbing titanium dioxide; then spraying chitosan membrane liquid on the surface of the water-absorbing titanium dioxide, wherein the weight ratio of the water-absorbing titanium dioxide to the chitosan membrane liquid is 1:0.4-0.8, drying the chitosan membrane liquid to form a chitosan membrane, and scattering to obtain a coating material;
II, soaking the coating material in water for 20-35min, and then draining the surface moisture of the coating material to prepare a water-absorbing coating material; and spraying gelatin solution on the surface of the water-absorbing coating material, wherein the weight ratio of the water-absorbing coating material to the gelatin solution is 1:0.1-0.5, and drying the gelatin solution to form a gelatin film to prepare the coated titanium dioxide.
By adopting the technical scheme, the titanium dioxide is placed in water for soaking and stirring, the moisture absorption effect of the titanium dioxide is utilized to enable the pores inside the titanium dioxide to absorb moisture, then the chitosan film liquid is sprayed on the surface of the titanium dioxide, and the titanium dioxide after water absorption is coated by utilizing the better bonding effect of the chitosan film liquid, so that the coating material is prepared.
Soaking the coating material in water, making the chitosan film gradually absorb water and expand by utilizing the good water absorption effect of the chitosan film, draining the water on the surface of the chitosan film after the chitosan film absorbs water, spraying gelatin solution on the surface of the coating material, and coating the coating material by utilizing the good viscosity of the gelatin solution to prepare the coated titanium dioxide.
The PET membrane and the flexible conductive metal layer are attached to adhesive layer surface both sides respectively, and the two all have better isolated effect, can isolate moisture and adhesive contact in the external environment, and the adhesive needs to utilize the moisture in the external environment to realize the solidification admittedly.
When the coated titanium dioxide is used as a raw material of the adhesive, because the chitosan film can absorb water which is several times of the self weight, part of water in the chitosan film is matched with the residual water in the gelatin film, so that the gelatin film is gradually dissolved at the temperature of 40-55 ℃; after the gelatin film is dissolved, the residual moisture in the chitosan film which absorbs water and expands is gradually released, the moisture in the pores of the titanium dioxide is also gradually released, the moisture released into the adhesive can promote the curing of the adhesive, so that the adhesive can still be cured through the moisture to form an elastomer even under the condition that the surface of the adhesive is not contacted with the external environment, and the formed adhesive layer has better flexibility and elasticity.
The gelatin solution after the gelatin film is dissolved has better viscosity, so that the titanium dioxide particles can be better bonded in the adhesive, namely, the titanium dioxide is bound in the adhesive by using the gelatin solution after the dissolution around the titanium dioxide particles, and a network binding structure is formed on the surface of the titanium dioxide, so that the titanium dioxide can be firmly filled in the adhesive, the strength of the adhesive is improved, and the viscosity of the adhesive can be improved.
Preferably, the gelatin solution is prepared by the following method:
weighing 3-4.2 parts by weight of gelatin particles and 45.5-50.2 parts by weight of water, mixing, stirring for 25-35min at room temperature, stirring in a water bath at 40-52 ℃ until the gelatin particles are completely dissolved, adding 0.2-3.4 parts by weight of glutaraldehyde aqueous solution, stirring, standing, and defoaming to obtain the gelatin solution.
By adopting the technical scheme, after the gelatin solution formed by the gelatin particles under the crosslinking action of glutaraldehyde is solidified to form the gelatin film, the formed gelatin film has better tensile strength, so that the surface gelatin film is not easy to puncture in the stirring process of the coated titanium dioxide, the coating effect of the coated titanium dioxide is ensured, and the processability of the finished product adhesive is improved.
Preferably, in the process of soaking the titanium dioxide in water in the step I, the titanium dioxide is firstly stirred at the rotating speed of 500-1200r/min for 12-20min, and then ultrasonic dispersion is carried out for 3-8 min.
By adopting the technical scheme, in the stirring process of the titanium dioxide, the titanium dioxide is enabled to absorb water with larger content in the pores inside the titanium dioxide, and the subsequent ultrasonic dispersion is matched to prevent the titanium dioxide from agglomerating, so that the titanium dioxide is uniformly dispersed, and the pores at all positions on the surface of the titanium dioxide can be contacted with water, thereby improving the water absorption effect of the titanium dioxide; during the curing process of the adhesive, the curing of the adhesive is facilitated.
Preferably, in the step I, the chitosan membrane liquid is sprayed on the surface of the water-absorbing titanium dioxide within 1-4min, and the water-absorbing titanium dioxide is stirred at the rotating speed of 350-800 r/min.
By adopting the technical scheme, the spraying time of the chitosan film liquid and the stirring speed in the spraying process are limited, so that the chitosan film liquid is uniformly connected with the surface of the titanium dioxide, and the film coating effect on the surface of the titanium dioxide is improved.
Preferably, the raw materials of the adhesive also comprise 3-7 parts of coated silk, and the coated silk is prepared by adopting the following method: placing silk fibers in water for soaking and absorbing water, taking out the silk fibers, and draining the surface water to obtain the water-absorbing silk; and then spraying gelatin solution on the surface of the water-absorbing silk, wherein the weight ratio of the water-absorbing silk to the gelatin solution is 1:0.2-0.6, and drying the gelatin solution to form a gelatin film to obtain the coated silk.
Through adopting above-mentioned technical scheme, utilize the higher water absorption on silk surface for silk absorbs a large amount of moisture after soaking, when the adhesive was solidified under the condition of 40-55 ℃, the gelatin membrane in the diolame silk absorbed moisture in the silk gradually, made the gelatin membrane dissolve gradually, utilized the better bonding effect of gelatin solution, made the bonding that silk can be firm in the adhesive, thereby improved the intensity of adhesive when improving the adhesive pliability.
After the silk is exposed in the adhesive, the water molecules are dispersed in the adhesive by utilizing the flow guiding effect of the silk surface on the water molecules, so that the curing of the adhesive is promoted.
Preferably, the catalyst is diethylaminomethyltriethoxysilane.
By adopting the technical scheme, the curing of the adhesive is promoted, and the adhesive has better flexibility while the curing efficiency of the adhesive is improved.
Preferably, the adhesive is prepared by the following method:
and weighing hydroxyl-terminated polydimethylsiloxane and tetraethoxysilane, mixing and stirring, adding the catalyst and the coated titanium dioxide, and continuously stirring and mixing to obtain the adhesive.
By adopting the technical scheme, the hydroxyl-terminated polydimethylsiloxane is firstly mixed with the tetraethoxysilane, so that the hydroxyl-terminated polydimethylsiloxane is dispersed in the tetraethoxysilane solvent, and then the catalyst and the coated titanium dioxide are added, so that the damage of the adhesive to the surface film structure of the coated titanium dioxide in the preparation process is reduced, and the curing effect of the adhesive is ensured.
In a third aspect, the present application provides a circuit board, which adopts the following technical solution:
a circuit board is made of circuit materials.
By adopting the technical scheme, the prepared circuit board has better flexibility.
In summary, the present application has the following beneficial effects:
1. the better viscosity of the adhesive is utilized, so that the bonding effect of the flexible conductive metal layer and the PET film is good, and the processing performance of the finished circuit material is improved; and the finished product circuit material has better flexibility by utilizing the better flexibility of the adhesive; meanwhile, the good transparency of the adhesive is matched with the good transparency of the PET film, so that the adhesion effect of the PET film on the surface of the flexible conductive metal layer can be observed conveniently, and the finished circuit material has good apparent performance.
2. The titanium dioxide, the chitosan film and the gelatin film are matched, and partial water in the chitosan film is matched with residual water in the gelatin film to promote the gelatin film to be gradually dissolved at the temperature of 40-55 ℃; after the gelatin film is dissolved, the residual moisture in the chitosan film which absorbs water and expands is gradually released, the moisture in the pores of the titanium dioxide is also gradually released, the moisture released into the adhesive can promote the curing of the adhesive, so that the adhesive can still be cured through the moisture to form an elastomer even under the condition that the surface of the adhesive is not contacted with the external environment, and the formed adhesive layer has better flexibility and elasticity.
3. The chitosan film has good water permeability effect, and can release the moisture absorbed by the chitosan film in an expansion way, and the moisture in the titanium dioxide can also be released, so that the released moisture can promote the curing of the adhesive in the circuit material.
Detailed Description
The present application will be described in further detail with reference to examples.
Preparation example of gelatin solution
Gelatin granules in the following raw materials were purchased from biogelatin, Inc. of Purpurent, Binzhou; other raw materials and equipment are all sold in the market.
Preparation example 1: the gelatin solution is prepared by the following method:
weighing 375g of gelatin particles, mixing with 4850g of deionized water, stirring at 150r/min for 30min at room temperature, and stirring at 500r/min in a 45 ℃ constant-temperature water bath until the gelatin particles are completely dissolved; then adding 260g of glutaraldehyde aqueous solution with volume fraction of 0.5%, stirring at the rotating speed of 500r/min for 3min, and standing for 30 min; then 10g of methyl silicone oil is added to continue stirring for 2min, and then standing for 20min to prepare the gelatin solution.
Preparation example 2: the gelatin solution is prepared by the following method:
weighing 300g of gelatin particles, mixing with 4550g of deionized water, stirring at the rotation speed of 150r/min for 25min at room temperature, and then stirring at the rotation speed of 500r/min at the constant-temperature water bath condition of 40 ℃ until the gelatin particles are completely dissolved; then 20g of glutaraldehyde water solution with volume fraction of 0.5 percent is added, and the mixture is stirred for 3min at the rotating speed of 500r/min and then stands for 30 min; then 10g of methyl silicone oil is added to continue stirring for 2min, and then standing for 20min to prepare the gelatin solution.
Preparation example 3: the gelatin solution is prepared by the following method:
weighing 420g of gelatin particles, mixing with 5020g of deionized water, stirring at the rotation speed of 150r/min for 35min at room temperature, and stirring at the rotation speed of 500r/min in a thermostatic water bath at 52 ℃ until the gelatin particles are completely dissolved; then 340g of glutaraldehyde aqueous solution with volume fraction of 0.5 percent is added, and the mixture is stirred for 3min at the rotating speed of 500r/min and then stands for 30 min; then 10g of methyl silicone oil is added to continue stirring for 2min, and then standing for 20min to prepare the gelatin solution.
Preparation example of Chitosan Membrane liquid
Chitosan in the following raw materials was purchased from grand humidity biotechnology limited to Chengdu; other raw materials and equipment are all sold in the market.
Preparation example 4: the chitosan film liquid is prepared by the following method:
weighing 0.5kg of chitosan, placing the chitosan in 25kg of acetic acid solution with the mass fraction of 2%, and standing for 12 hours to prepare a chitosan solution; weighing 6.5kg of chitosan solution with the mass fraction of 2%, adding 0.2kg of glutaraldehyde solution with the mass fraction of 2%, and stirring for 45min under the condition of 500r/min to obtain the chitosan membrane solution.
Preparation example of coated Silk
The silk fiber in the following raw materials is purchased from Suzhou silk fibroin Biotechnology Limited; other raw materials and equipment are all sold in the market.
Preparation example 5: the coated silk is prepared by the following method:
weighing 10kg of silk fiber, placing in 150kg of water, soaking for 40min, and stirring at a rotating speed of 150r/min in the soaking process; after soaking, filtering silk fibers, draining surface water, and making the silk fibers not drip water to obtain water-absorbing silk; and then weighing 4kg of the gelatin solution prepared in the preparation example 1, spraying the gelatin solution on the surface of 10kg of water-absorbing silk within 3min, stirring the water-absorbing silk at the rotating speed of 200r/min in the spraying process, drying the water-absorbing silk at the temperature of 24 ℃ until the gelatin solution on the surface of the water-absorbing silk is formed into a film, preparing a semi-finished product, and crushing the semi-finished product to pass through a 60-mesh sieve to prepare the coated silk.
Preparation example 6: the coated silk is prepared by the following method:
weighing 10kg of silk fiber, placing in 150kg of water, soaking for 40min, and stirring at a rotating speed of 150r/min in the soaking process; after soaking, filtering silk fibers, draining surface water, and making the silk fibers not drip water to obtain water-absorbing silk; and then weighing 2kg of the gelatin solution prepared in the preparation example 1, spraying the gelatin solution on the surface of 10kg of water-absorbing silk within 3min, stirring the water-absorbing silk at the rotating speed of 200r/min in the spraying process, drying the water-absorbing silk at the temperature of 24 ℃ until the gelatin solution on the surface of the water-absorbing silk is formed into a film, preparing a semi-finished product, and crushing the semi-finished product to pass through a 60-mesh sieve to prepare the coated silk.
Preparation example 7: the coated silk is prepared by the following method:
weighing 10kg of silk fiber, placing in 150kg of water, soaking for 40min, and stirring at a rotating speed of 150r/min in the soaking process; after soaking, filtering silk fibers, draining surface water, and making the silk fibers not drip water to obtain water-absorbing silk; and then 6kg of gelatin solution prepared in preparation example 1 is weighed and sprayed on the surface of 10kg of water-absorbing silk within 3min, in the spraying process, the water-absorbing silk is stirred at the rotating speed of 200r/min and then dried at the temperature of 24 ℃ until the gelatin solution on the surface of the water-absorbing silk is formed into a film, a semi-finished product is prepared, and the semi-finished product is crushed to pass through a 60-mesh sieve, so that the coated silk is prepared.
Preparation example of coated titanium dioxide
Titanium dioxide in the following raw materials is purchased from Hebei Leilicai energy-saving technology Limited, model R-940, and the particle size is 50-100 μm; other raw materials and equipment are all sold in the market.
Preparation example 8: the coated titanium dioxide is prepared by the following method:
i, weighing 5kg of titanium dioxide, soaking the titanium dioxide in 50kg of water, firstly stirring for 16min at the rotating speed of 1000r/min, then carrying out ultrasonic dispersion for 5min, and filtering to obtain the titanium dioxide for water absorption; then weighing 6kg of chitosan membrane liquid prepared in preparation example 4, spraying the chitosan membrane liquid on the surface of 10kg of water-absorbing titanium dioxide, wherein in the spraying process, the chitosan membrane liquid prepared in preparation example 4 is sprayed on the surface of the water-absorbing titanium dioxide within 3min, the water-absorbing titanium dioxide is stirred at the rotating speed of 550r/min, the chitosan membrane liquid prepared in preparation example 4 is dried to form a chitosan membrane, a semi-finished product is prepared, and the semi-finished product is scattered to prepare a coating material;
II, weighing 10kg of coating material, soaking in 200kg of water for 28min, continuously stirring at the rotating speed of 1000r/min in the soaking process, filtering out the coating material after soaking is finished, and draining the surface moisture of the coating material to prepare a water-absorbing coating material; 3kg of the gelatin solution prepared in preparation example 1 is weighed and sprayed on the surface of 10kg of water-absorbing coating material, and in the spraying process, the water-absorbing coating material is stirred at the rotating speed of 500r/min for 2 min; then drying the mixture at room temperature until gelatin solution on the surface of the water-absorbing coating material forms a film, and then crushing the film and sieving the film with a 80-mesh sieve to obtain the coated titanium dioxide.
Preparation example 9: the coated titanium dioxide is prepared by the following method:
i, weighing 5kg of titanium dioxide, soaking the titanium dioxide in 50kg of water, firstly stirring the titanium dioxide at a rotating speed of 500r/min for 20min, then ultrasonically dispersing the titanium dioxide for 8min, and filtering the titanium dioxide to obtain water-absorbing titanium dioxide; then weighing 4kg of chitosan membrane liquid prepared in preparation example 4, spraying the chitosan membrane liquid on the surface of 10kg of water-absorbing titanium dioxide, wherein in the spraying process, the chitosan membrane liquid prepared in preparation example 4 is sprayed on the surface of the water-absorbing titanium dioxide within 1min, the water-absorbing titanium dioxide is stirred at the rotating speed of 800r/min, the chitosan membrane liquid prepared in preparation example 4 is dried to form a chitosan membrane, a semi-finished product is prepared, and the semi-finished product is scattered to prepare a coating material;
II, weighing 10kg of coating material, soaking in 200kg of water for 20min, continuously stirring at the rotating speed of 1000r/min in the soaking process, filtering out the coating material after soaking is finished, and draining the surface moisture of the coating material to prepare a water-absorbing coating material; weighing 1kg of the gelatin solution prepared in preparation example 1, and spraying the gelatin solution on the surface of 10kg of the water-absorbing coating material, wherein in the spraying process, the water-absorbing coating material is stirred at the rotating speed of 500r/min, and the spraying time is 2 min; then drying the mixture at room temperature until gelatin solution on the surface of the water-absorbing coating material forms a film, and then crushing the film and sieving the film with a 80-mesh sieve to obtain the coated titanium dioxide.
Preparation example 10: the coated titanium dioxide is prepared by the following method:
i, weighing 5kg of titanium dioxide, soaking the titanium dioxide in 50kg of water, firstly stirring for 12min at the rotating speed of 1200r/min, then carrying out ultrasonic dispersion for 3min, and filtering to obtain the titanium dioxide for water absorption; then weighing 8kg of chitosan membrane liquid prepared in preparation example 4, spraying the chitosan membrane liquid on the surface of 10kg of water-absorbing titanium dioxide, wherein in the spraying process, the chitosan membrane liquid prepared in preparation example 4 is sprayed on the surface of the water-absorbing titanium dioxide within 4min, the water-absorbing titanium dioxide is stirred at the rotating speed of 350r/min, the chitosan membrane liquid prepared in preparation example 4 is dried to form a chitosan membrane, a semi-finished product is prepared, and the semi-finished product is scattered to prepare a coating material;
II, weighing 10kg of coating material, soaking in 200kg of water for 35min, continuously stirring at the rotating speed of 1000r/min in the soaking process, filtering out the coating material after soaking is finished, and draining the surface moisture of the coating material to prepare a water-absorbing coating material; 5kg of the gelatin solution prepared in preparation example 1 is weighed and sprayed on the surface of 10kg of water-absorbing coating material, and in the spraying process, the water-absorbing coating material is stirred at the rotating speed of 500r/min for 2 min; then drying the mixture at room temperature until gelatin solution on the surface of the water-absorbing coating material forms a film, and then crushing the film and sieving the film with a 80-mesh sieve to obtain the coated titanium dioxide.
Preparation example 11: the difference between this preparation and preparation 8 is that:
the gelatin solution prepared in preparation example 2 was used.
Preparation example 12: the difference between this preparation and preparation 8 is that:
the gelatin solution prepared in preparation example 3 was used.
Preparation example of adhesive
The hydroxy-terminated polydimethylsiloxane in the following raw materials is purchased from silicone rubber powder produced by a processing plant for carrying mineral products in Lingshu county, the specification is 800 meshes, and the state is transparent;
preparation example 13: the adhesive is prepared by the following method:
100kg of hydroxyl-terminated polydimethylsiloxane and 5kg of ethyl orthosilicate are weighed and mixed, stirred for 10min at the rotating speed of 500r/min, then 5kg of diethylaminomethyl triethoxysilane and 10kg of coated titanium dioxide prepared in preparation example 8 are added, and stirring and mixing are continued for 8min, so that the adhesive is prepared.
Preparation example 14: the adhesive is prepared by the following method:
weighing 80kg of hydroxyl-terminated polydimethylsiloxane and 2kg of ethyl orthosilicate, mixing, stirring at the rotating speed of 500r/min for 10min, then adding 2kg of diethylaminomethyl triethoxysilane and 5kg of the coated titanium dioxide prepared in preparation example 8, and continuously stirring and mixing for 8min to obtain the adhesive.
Preparation example 15: the adhesive is prepared by the following method:
120kg of hydroxyl-terminated polydimethylsiloxane and 7kg of ethyl orthosilicate are weighed and mixed, stirred for 10min at the rotating speed of 500r/min, then 7kg of diethylaminomethyl triethoxysilane and 15kg of coated titanium dioxide prepared in preparation example 8 are added, and stirring and mixing are continued for 8min, so that the adhesive is prepared.
Preparation example 16: the difference between this preparation and preparation 13 is that:
the coated titanium dioxide prepared in preparation example 9 is selected as the coated titanium dioxide.
Preparation example 17: the difference between this preparation and preparation 13 is that:
the coated titanium dioxide prepared in preparation example 10 is selected as the coated titanium dioxide.
Preparation example 18: the difference between this preparation and preparation 13 is that:
the coated titanium dioxide prepared in preparation example 11 is selected as the coated titanium dioxide.
Preparation example 19: the difference between this preparation and preparation 13 is that:
the coated titanium dioxide prepared in preparation example 12 is selected as the coated titanium dioxide.
Preparation example 20: the difference between this preparation and preparation 13 is that:
5kg of diethylaminomethyltriethoxysilane, 10kg of the coated titanium dioxide prepared in preparation example 8 and 5kg of the coated silk prepared in preparation example 5 were added, and the mixture was stirred and mixed for 8min to obtain an adhesive.
Preparation example 21: the difference between the present preparation example and preparation example 20 is that:
the weight of the coated silk is 3 kg.
Preparation example 22: the difference between the present preparation example and preparation example 20 is that:
the weight of the coated silk is 7 kg.
Preparation example 23: the difference between the present preparation example and preparation example 20 is that:
the coated silk prepared in preparation example 6 was used as the coated silk.
Preparation example 24: the difference between the present preparation example and preparation example 20 is that:
the coated silk prepared in preparation example 7 was used as the coated silk.
Examples
The copper foil of the following raw materials was purchased from Shanghai Xin Ye-Mao metal products Co., Ltd; PET films were purchased from kunshan hui electronic ltd; other raw materials and equipment are all sold in the market.
Example 1: a circuit material comprising:
comprises a copper foil, a PET film and an adhesive layer arranged between the copper foil and the PET film; the adhesive layer was made of the adhesive prepared in preparation example 13; the thickness of the adhesive layer is 0.6 mm;
the preparation method comprises the following steps:
the adhesive prepared in preparation example 13 was coated on the surface of a copper foil, and then a PET film was coated on the surface of the adhesive, and the adhesive was cured at 45 ℃ to form an adhesive layer, thereby obtaining a finished circuit material.
Example 2: the present embodiment is different from embodiment 1 in that:
the thickness of the adhesive layer is 0.4 mm;
the adhesive prepared in preparation example 13 was coated on the surface of a copper foil, and then a PET film was coated on the surface of the adhesive, and the adhesive was cured at 40 ℃ to form an adhesive layer, thereby obtaining a finished circuit material.
Example 3: the present embodiment is different from embodiment 1 in that:
the thickness of the adhesive layer is 1 mm;
the adhesive prepared in preparation example 13 was coated on the surface of a copper foil, and then a PET film was coated on the surface of the adhesive, which was then placed at 55 ℃, and the adhesive was cured to form an adhesive layer, to obtain a finished circuit material.
Example 4: the present embodiment is different from embodiment 1 in that:
the adhesive prepared in preparation example 14 was used as the adhesive.
Example 5: the present embodiment is different from embodiment 1 in that:
the adhesive prepared in preparation example 15 was used as the adhesive.
Example 6: the present embodiment is different from embodiment 1 in that:
the adhesive prepared in preparation example 16 was used as the adhesive.
Example 7: the present embodiment is different from embodiment 1 in that:
the adhesive prepared in preparation example 17 was used as the adhesive.
Example 8: the present embodiment is different from embodiment 1 in that:
the adhesive prepared in preparation example 18 was used as the adhesive.
Example 9: the present embodiment is different from embodiment 1 in that:
the adhesive prepared in preparation example 19 was used as the adhesive.
Example 10: the present embodiment is different from embodiment 1 in that:
the adhesive prepared in preparation example 20 was used as the adhesive.
Example 11: the present embodiment is different from embodiment 1 in that:
the adhesive prepared in preparation example 21 was used as the adhesive.
Example 12: the present embodiment is different from embodiment 1 in that:
the adhesive prepared in preparation example 22 was used as the adhesive.
Example 13: the present embodiment is different from embodiment 1 in that:
the adhesive prepared in preparation example 23 was used as the adhesive.
Example 14: the present embodiment is different from embodiment 1 in that:
the adhesive prepared in preparation 24 was used as the adhesive.
Example 15: the present embodiment is different from embodiment 1 in that:
the adhesive prepared in preparation example 13 was coated on the surface of a copper foil, and then a PET film was coated on the surface of the adhesive, which was then placed at 25 ℃, and the adhesive was cured to form an adhesive layer, to obtain a finished circuit material.
Example 16: the present embodiment is different from embodiment 1 in that:
the preparation process of the coated titanium dioxide comprises the following steps:
i, weighing 5kg of titanium dioxide, soaking the titanium dioxide in 50kg of water, firstly stirring for 16min at the rotating speed of 1000r/min, then carrying out ultrasonic dispersion for 5min, and filtering to obtain the titanium dioxide for water absorption; and then 6kg of chitosan membrane liquid prepared in preparation example 4 is weighed and sprayed on the surface of 10kg of water-absorbing titanium dioxide, in the spraying process, the chitosan membrane liquid prepared in preparation example 4 is sprayed on the surface of the water-absorbing titanium dioxide within 3min, the water-absorbing titanium dioxide is stirred at the rotating speed of 550r/min, the chitosan membrane is formed after the chitosan membrane liquid prepared in preparation example 4 is dried, a semi-finished product is prepared, and the coated titanium dioxide is prepared after the semi-finished product is scattered.
Example 17: the present embodiment is different from embodiment 1 in that:
the preparation process of the coated titanium dioxide comprises the following steps:
i, weighing 3kg of the gelatin solution prepared in the preparation example 1, spraying the gelatin solution on the surface of 10kg of water-absorbing titanium dioxide, and stirring the water-absorbing titanium dioxide at the rotating speed of 500r/min for 2min in the spraying process; then drying the titanium dioxide powder at room temperature until gelatin solution on the surface of the water-absorbing titanium dioxide powder forms a film, and then crushing and sieving the film by a 80-mesh sieve to obtain the coated titanium dioxide powder.
Example 18: the present embodiment is different from embodiment 1 in that:
II, weighing 3kg of the gelatin solution prepared in the preparation example 1, spraying the gelatin solution on the surface of 10kg of coating material, and stirring the coating material at the rotating speed of 500r/min for 2min in the spraying process; then drying the mixture at room temperature until gelatin solution on the surface of the coating material forms a film, and then crushing the film and sieving the film with a 80-mesh sieve to obtain the coated titanium dioxide.
Example 19: the present embodiment is different from embodiment 1 in that:
i, weighing 6kg of chitosan membrane liquid prepared in preparation example 4, spraying the chitosan membrane liquid on the surface of 10kg of titanium dioxide, wherein in the spraying process, the chitosan membrane liquid prepared in preparation example 4 is sprayed on the surface of the titanium dioxide within 3min, the titanium dioxide is stirred at the rotating speed of 550r/min, the chitosan membrane liquid prepared in preparation example 4 is dried to form a chitosan membrane, a semi-finished product is prepared, and the semi-finished product is scattered to prepare a coating material;
example 20: the present embodiment is different from embodiment 1 in that:
the flexible conductive metal layer is aluminum foil, and the catalyst is dibutyl tin dilaurate.
Application example:
a circuit board can be prepared using any one of embodiments 1-20.
Comparative example
Comparative example 1: this comparative example differs from example 1 in that:
the adhesive was a commercially available epoxy adhesive available from QI chen New Material Co., Ltd, available in Dongguan, model E-40 FL.
Comparative example 2: this comparative example differs from example 1 in that:
the adhesive is commercially available silica gel adhesive, which is purchased from Taizhou easy-to-stick electronic technology Co., Ltd, model YZ-5860 organic silicon special adhesive.
Comparative example 3: this comparative example differs from example 1 in that:
the raw materials of the adhesive are not added with the coated titanium dioxide.
Performance test
1. Determination of curing time
Adhesives were prepared by the preparation methods of examples 1 to 20, respectively, and then circuit materials were prepared using the adhesives prepared in examples 1 to 20 and comparative examples 1 to 3, respectively, and the adhesive complete curing time thereof was recorded.
2. Viscosity measurement
The preparation methods of the examples 1 and 4 to 20 are respectively adopted to prepare the adhesives, the adhesives are placed at 45 ℃ for 30min, and then the viscosities of the adhesives prepared in the examples 1 to 20 and the adhesives prepared in the comparative examples 1 to 3 are respectively detected by GB/T2794-2013 adhesive viscosity measurement and a single-cylinder rotary viscometer method.
3. Determination of uneven tensile test
Preparing adhesives by adopting the preparation methods of the examples 1, 10-12, 15-20 and the comparative examples 1-3 respectively, coating the prepared adhesives between an iron block and a copper foil with the thickness of 1cm, standing for 20 hours at the temperature of 25 ℃, and removing the residual adhesive on the surface to prepare a sample; the equipment adopts a universal TSE104B microcomputer controlled electronic universal testing machine and a WZTC103A adhesive stretching clamp; and (3) loading the sample into a tension clamp, keeping the distance between the clamping positions at the two ends of the sample to be 200mm, keeping the distance difference between the edge of the iron block and the clamping positions at the two ends to be not more than 0.5mm, loading at the speed of 10mm/min until the sample is damaged, and recording the tensile strength.
4. Flexibility assay
The adhesive was prepared by the preparation methods of examples 1 and 10 to 12, respectively, and the adhesive was placed on the surface of a glass plate to form a film having a thickness of 2mm, to prepare a sample having a length of 4cm and a width of 2cm, and the two ends of the sample were respectively abutted against the two ends of the sample with a thumb and a forefinger, and then folded in half in the direction of approaching each other, and when the sample was folded in half to the maximum (the sample was folded in half again to cause a break or crack), the distance between the two ends of the sample was recorded.
5. Measurement of transparency
Respectively adopting the preparation methods of example 1 and comparative example 1 to prepare the adhesive, placing the adhesive on the surface of a glass plate for casting to form a film with the film thickness of 0.2mm, scoring the transparency of the adhesive, wherein the transparency is full-transparency 10 points → the transparency is poor 0 point
TABLE 1 Performance test Table
As can be seen by combining example 1 and table 1, the curing time of the adhesive prepared in example 1 is short, which indicates that under the insulation effect of the copper foil and the PET film, although moisture in the external environment cannot promote the curing of the adhesive, the coated titanium dioxide inside the adhesive can promote the curing of the adhesive, so that the adhesive has short curing time; and the prepared adhesive has better viscosity, toughness, flexibility and transparency.
Combining example 1 and examples 2-3 with table 1, it can be seen that examples 2-3 differ from example 1 in curing time, indicating that different heat curing temperatures and adhesive thicknesses have an effect on the curing time of the adhesive.
Combining examples 1 and 4-5 and table 1, it can be seen that the raw material ratio of the adhesive has an effect on the cure time, viscosity, tensile strength of the finished adhesive.
Combining example 1 and examples 6-7 and table 1, it can be seen that the thickness of the chitosan film and the gelatin film coated on the surface of titanium dioxide has an influence on the curing time, viscosity, tensile strength and flexibility of the finished adhesive, the gelatin solution generated after the gelatin film is dissolved can increase the viscosity of the adhesive when the gelatin film is coated with a thicker gelatin film, but has an influence on the flexibility, and the curing time of the adhesive when the gelatin film is coated with a thinner gelatin film.
Combining example 1 and examples 8-9 with table 1, it can be seen that the process of preparing the gelatin solution has an effect on the cure time, viscosity, tensile strength of the finished adhesive.
Combining example 1 and examples 10-12 with Table 1, it can be seen that the addition of coated silk to the adhesive raw materials of examples 10-12 resulted in slightly longer curing time for the adhesives of examples 10-12 than example 1, higher viscosity than example 1, higher tensile strength than example 1, but slightly less flexibility than example 1; the addition of the coated silk is illustrated, under the condition of heating and curing, the gelatin film gradually absorbs the moisture in the coated silk, so that the gelatin film is dissolved, the gelatin solution has good viscosity, the viscosity of the adhesive can be improved, and the gelatin solution is cured and matched with the good flexibility of the silk, so that the tensile strength of the adhesive can be improved.
Combining example 1 and examples 13-14 with table 1, it can be seen that examples 13-14 use different coated silks whose preparation method has an effect on the properties of the finished adhesive.
Combining example 1 with examples 15-20 and table 1, it can be seen that the adhesive of example 15 cures at 25 ℃, and the adhesive prepared in example 15 cures longer than in example 1 compared to example 1; the curing under the condition of proper heating temperature can promote the gelatin film on the surface of the coated titanium dioxide to absorb the moisture in the chitosan film, thereby promoting the dissolution of the gelatin film, leading the moisture absorbed in the chitosan film and the moisture in the titanium dioxide to be matched with the catalyst, promoting the curing of the adhesive, even if the surface of the adhesive is blocked by the copper foil and the PET film and can not be contacted with the water molecules in the external environment, the adhesive can be still cured, and the required curing time is shorter.
Example 16 during the preparation of the coated titanium dioxide, the surface of the titanium dioxide is not coated with a gelatin film, compared with example 1, the curing time of the adhesive prepared in example 16 is longer than that of example 1, the viscosity of the adhesive is lower than that of example 1, and the tensile strength of the adhesive is lower than that of example 1; the coating of the surface gelatin film of the titanium dioxide is illustrated, the water required for dissolving the surface gelatin film is the partial water absorbed by the chitosan film, and the residual water of the chitosan film and the partial water in the titanium dioxide are the water required for adhesive curing, so that the adhesive curing is promoted; and the viscosity of the adhesive is increased after the gelatin film is dissolved, and the gelatin solution can increase the connection effect of the titanium dioxide and the adhesive, improve the density and further improve the tensile strength of the adhesive.
Example 17 during the preparation of coated titanium dioxide, the chitosan film is not coated on the surface of titanium dioxide, compared to example 1, the curing time of the adhesive prepared in example 17 is longer than that of example 1, the viscosity is lower than that of example 1, and the tensile strength is lower than that of example 1; the chitosan film is not coated, the gelatin film is not easy to dissolve, and the moisture in the titanium dioxide is not easy to release, so that the adhesive is not easy to cure; namely, the better water absorption effect of the chitosan film is utilized to be matched with the gelatin film, so that the curing time of the adhesive can be shortened, and the viscosity and the tensile strength of the adhesive are improved.
Example 18 during the preparation of the coated titanium dioxide, the chitosan film does not absorb water, compared with example 1, the curing time of the adhesive prepared in example 18 is longer than that of example 1, the viscosity of the adhesive is lower than that of example 1, and the tensile strength of the adhesive is lower than that of example 1; the explanation shows that the chitosan film can load water with the mass several times or even tens times of the chitosan film by utilizing the good water absorption effect of the chitosan film, the water is supplied to the gelatin film to be dissolved, the viscosity of the adhesive is improved, and the residual water is matched with the catalyst, so that the adhesive can still be cured even if the adhesive is not contacted with the external environment.
Example 19 during the preparation of the coated titanium dioxide, the titanium dioxide raw material did not absorb water, and compared to example 1, the curing time of the adhesive prepared in example 19 was longer than that of example 1, the viscosity was lower than that of example 1, and the tensile strength was lower than that of example 1; it is shown that the moisture absorbed by the titanium dioxide can promote the curing of the adhesive and has an influence on the viscosity and tensile strength of the adhesive.
Example 20 during the preparation of the adhesive, the flexible conductive metal layer was aluminum foil and the catalyst was dibutyl tin dilaurate, compared to example 1, the differences between the parameters were not very different, which indicates that different raw materials have an effect on the properties of the finished adhesive.
Combining example 1 and comparative examples 1-3 with table 1, it can be seen that comparative example 1 uses a commercially available epoxy adhesive, and compared to example 1, the adhesive prepared in comparative example 1 has a significantly lower clarity score than example 1 and a longer cure time than example 1; the epoxy resin adhesive is selected to prepare the circuit material, so that the apparent performance of the finished circuit material is easily influenced.
Comparative example 2 a commercially available silicone adhesive was used, and the curing time of the adhesive prepared in comparative example 2 was significantly longer than that of example 1 compared to example 1, which indicates that the conventional silicone adhesive needs to contact with water molecules in the external environment during the curing process to promote the curing of the silicone adhesive, and the conventional silicone adhesive cannot continuously contact with water molecules in the environment after the copper foil and the PET film block the adhesive, thereby affecting the curing.
Comparative example 3 the binder raw material is not added with coated titanium dioxide, compared with example 1, the curing time of the binder prepared in comparative example 3 is longer than that of example 1, which shows that the coated titanium dioxide can promote the curing of the binder under the condition that the copper foil and the PET film block the contact of the binder and water molecules in the environment.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (10)
1. A circuit material is characterized by comprising a flexible conductive metal layer, a PET film and an adhesive layer arranged between the flexible conductive metal layer and the PET film, wherein the thickness of the adhesive layer is 0.4-1 mm;
the adhesive layer is made of an adhesive, and the adhesive is made of the following raw materials in parts by weight:
80-120 parts of hydroxyl-terminated polydimethylsiloxane, 2-7 parts of ethyl orthosilicate, 2-7 parts of catalyst and 5-15 parts of coated titanium dioxide.
2. A method of making a circuit material according to claim 1, comprising the steps of:
coating the adhesive on the surface of the flexible conductive metal layer, then covering the surface of the adhesive with a PET film, placing the adhesive at 40-55 ℃, and curing the adhesive to form an adhesive layer to obtain the finished product circuit material.
3. The method of claim 2, wherein: the coated titanium dioxide is prepared by the following method:
i, weighing titanium dioxide, soaking in water, stirring, and taking out the titanium dioxide to obtain water-absorbing titanium dioxide; then spraying chitosan membrane liquid on the surface of the water-absorbing titanium dioxide, wherein the weight ratio of the water-absorbing titanium dioxide to the chitosan membrane liquid is 1:0.4-0.8, drying the chitosan membrane liquid to form a chitosan membrane, and scattering to obtain a coating material;
II, soaking the coating material in water for 20-35min, and then draining the surface moisture of the coating material to prepare a water-absorbing coating material; and spraying gelatin solution on the surface of the water-absorbing coating material, wherein the weight ratio of the water-absorbing coating material to the gelatin solution is 1:0.1-0.5, and drying the gelatin solution to form a gelatin film to prepare the coated titanium dioxide.
4. The method of claim 3, wherein the gelatin solution is prepared by the following method:
weighing 3-4.2 parts by weight of gelatin particles and 45.5-50.2 parts by weight of water, mixing, stirring for 25-35min at room temperature, stirring in a water bath at 40-52 ℃ until the gelatin particles are completely dissolved, adding 0.2-3.4 parts by weight of glutaraldehyde aqueous solution, stirring, standing, and defoaming to obtain the gelatin solution.
5. The method as claimed in claim 3, wherein the titanium pigment is first stirred at a rotation speed of 500-1200r/min for 12-20min and then ultrasonically dispersed for 3-8min during the soaking process in water in step I.
6. The method for preparing a circuit material as claimed in claim 3, wherein the chitosan solution is sprayed on the surface of the water-absorbing titanium dioxide within 1-4min in the step I, and the water-absorbing titanium dioxide is stirred at a rotation speed of 350-800 r/min.
7. The method for preparing a circuit material according to claim 2, wherein the adhesive raw material further comprises 3-7 parts by weight of coated silk, and the coated silk is prepared by the following method:
placing silk fibers in water for soaking and absorbing water, taking out the silk fibers, and draining the surface water to obtain the water-absorbing silk; and then spraying gelatin solution on the surface of the water-absorbing silk, wherein the weight ratio of the water-absorbing silk to the gelatin solution is 1:0.2-0.6, and drying the gelatin solution to form a gelatin film to obtain the coated silk.
8. The method of claim 1, wherein the catalyst is diethylaminomethyltriethoxysilane.
9. The method of claim 1, wherein the adhesive is prepared by the following method:
and weighing hydroxyl-terminated polydimethylsiloxane and tetraethoxysilane, mixing and stirring, adding the catalyst and the coated titanium dioxide, and continuously stirring and mixing to obtain the adhesive.
10. A circuit board made from a material comprising the circuit material of any one of claims 1-9.
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