阅读说明：本技术 一种石英晶振用胶粘剂及其制备方法 (Adhesive for quartz crystal oscillator and preparation method thereof ) 是由 刘佳林 焦柯嘉 何阳 殷文钢 于 2021-08-25 设计创作，主要内容包括：本发明提供了一种石英晶振用胶粘剂,包括下述原料：载体树脂、催化剂、附着剂、流动剂、防沉剂、稳定剂、导电粉体；所述载体树脂由下述原料组成乙烯基硅树脂和/或液体硅橡胶和/或硅油,氢化树脂。本发明的有益效果为：本发明所述的石英晶振用胶粘剂能够在高温条件下固化,固化后具有较高的柔韧性,在各种金属、石英、陶瓷上具有良好的剪切强度,同时能够承受较高的温度而不发生性质变化。该胶粘剂应用于石英晶振上为点胶工艺,点胶时胶点圆润,无拉胶堵塞针管现象。(The invention provides an adhesive for quartz crystal oscillators, which comprises the following raw materials: carrier resin, catalyst, adhesive, flowing agent, anti-settling agent, stabilizing agent and conductive powder; the carrier resin is vinyl silicon resin and/or liquid silicon rubber and/or silicon oil and hydrogenated resin which are prepared from the following raw materials. The invention has the beneficial effects that: the adhesive for the quartz crystal oscillator can be cured at high temperature, has higher flexibility after being cured, has good shearing strength on various metals, quartz and ceramics, and can bear higher temperature without property change. The adhesive is applied to a quartz crystal oscillator and is a glue dispensing process, glue dispensing points are smooth, and the phenomenon that a needle tube is blocked by glue drawing is avoided.)

1. The adhesive for quartz crystal oscillators is characterized by comprising the following raw materials in parts by weight: 12-15 parts of carrier resin, 0.01-0.1 part of catalyst, 0.5-1 part of adhesive, 4-9 parts of flowing agent, 0.3-0.5 part of anti-settling agent, 0.01-0.1 part of stabilizer and 75-85 parts of conductive powder;

the carrier resin is vinyl silicon resin and/or liquid silicon rubber and/or silicon oil and hydrogenated resin which are prepared from the following raw materials.

2. The adhesive for quartz crystal oscillators as claimed in claim 1, wherein the catalyst is a platinum-based catalyst; the platinum catalyst is platinic chloride, a complex of platinic chloride and alcohol, aldehyde and ketone, a platinum divinyl tetramethyl disiloxane complex and a platinum-vinyl siloxane complex.

3. The adhesive for quartz crystal oscillators of claim 1, wherein the adhesive is a silane coupling agent, a titanate coupling agent, an aluminate coupling agent or a rare earth coupling agent.

4. The adhesive according to claim 1, wherein the flowable agent is white kerosene, heptane, octane, undecane, dodecane, cyclohexanone, isophorone, dibasic acid ester or dibasic alcohol ester.

5. The adhesive for quartz crystal oscillators as defined in claim 1, wherein the anti-settling agent is polyethylene wax, polyamide wax or fumed silica.

6. The adhesive according to claim 1, wherein the stabilizer is a radical absorbent or a metal chelating agent, the radical absorbent is benzoquinone, hydroquinone or hydroquinone monomethyl ether, and the metal chelating agent is ethylenediaminetetraacetic acid, oxalic acid, acetylacetone or o-aminophenol.

7. The adhesive for quartz crystal oscillators as defined in claim 1, wherein the conductive powder is at least one of pure silver powder, silver-nickel powder, silver-copper powder, silver-aluminum powder, silver-plated glass powder, and nickel-carbon powder.

8. A method for preparing the adhesive for the quartz crystal oscillator according to any one of claims 1 to 7, characterized by comprising the following steps:

(1) sequentially adding vinyl silicone resin and/or liquid silicone rubber and/or silicone oil, a catalyst and an anti-settling agent into a stirring device, premixing for 10min at the temperature of 35-45 ℃, adding a stabilizer and hydrogenated resin, stirring and mixing for 25-35min to prepare an adhesive carrier;

(2) adding the adhesive, the flowing agent and the conductive powder into the adhesive carrier, putting the mixture into a stirrer, stirring for 15-25min, and putting the mixture into a three-roll grinder, and uniformly grinding to obtain the adhesive for quartz crystal oscillators.

9. The method for preparing the adhesive for the quartz crystal oscillator according to claim 8, wherein in the step (2), the fineness of the adhesive for the quartz crystal oscillator is 5 to 25 um.

Technical Field

The invention relates to the field of adhesives, and particularly relates to an adhesive for quartz crystal oscillators and a preparation method thereof.

Background

The crystal oscillator generally refers to a crystal oscillator, some electronic devices need an ac signal with highly stable frequency, and the LC oscillator has poor stability and easily drifts frequency. A highly stable signal can be generated by using a quartz crystal as a special element in an oscillator, which is called a crystal oscillator.

With the development of industry, the trend of crystal oscillators is continuously toward miniaturization, flaking and high precision, the sizes thereof are continuously reduced, the frequency intervals are also continuously shortened, and the hardness of the epoxy adhesives used for the crystal oscillators in the past is high, so that the epoxy adhesives are not suitable for the smaller crystal oscillators.

Disclosure of Invention

The invention aims to provide an adhesive which has good flexibility and conductivity on a quartz crystal oscillator chip.

In order to achieve the purpose, the invention adopts the following technical scheme:

an adhesive for quartz crystal oscillators comprises the following raw materials in parts by weight: 12-15 parts of carrier resin, 0.01-0.1 part of catalyst, 0.5-1 part of adhesive, 4-9 parts of flowing agent, 0.3-0.5 part of anti-settling agent, 0.01-0.1 part of stabilizer and 75-85 parts of conductive powder;

the carrier resin is vinyl silicon resin and/or liquid silicon rubber and/or silicon oil and hydrogenated resin which are prepared from the following raw materials in parts by weight.

The adhesive is a novel resin type adhesion promoter and has special effect on the anti-dropping property of the coating. Has wider solubility, and can improve the adhesion of various coating systems such as: water paint, UV gloss oil, metal baking paint, etc.

The flow agents are of various types, and the different types of plastic flow agents can greatly improve the melt index of various plastics through corresponding chemical and physical actions in plastic molding processing. Under dynamic or static conditions, the surface tension can be reduced, the wetting property can be improved, and the leveling effect can be improved.

The anti-settling agent is a rheological control agent of the coating, so that the coating has thixotropy and greatly improved viscosity.

The stabilizer can increase the stability of solution, colloid, solid and mixture, and can slow down reaction, maintain chemical balance, reduce surface tension, and prevent light, thermal decomposition or oxidative decomposition.

The carrier resin, the vinyl silicon resin, the liquid silicon rubber and the hydrogenated resin contained in the adhesive for the quartz crystal oscillator generate a crosslinking reaction between Si-H bonds and vinyl groups of the vinyl silicon resin under the action of the catalyst, but the adhesive has insufficient bonding strength due to a polymerization reaction generated by chelation through a platinum catalyst, and can be decomposed at high temperature, so that the phenomenon that gas escapes from the inside of the adhesive during the packaging of the quartz crystal oscillator is seriously influenced, and the impedance of the adhesive is increased.

The method strengthens the crosslinking reaction by adjusting the contents of the catalyst and the carrier resin, and ensures the catalytic degree of Si-H and vinyl and the hardness of colloid.

The above adhesive for quartz crystal oscillators, as a preferred embodiment, is a platinum catalyst; the platinum catalyst is platinic chloride, a complex of platinic chloride and alcohol, aldehyde and ketone, a platinum divinyl tetramethyl disiloxane complex and a platinum-vinyl siloxane complex.

As a preferred embodiment, the adhesive for quartz crystal oscillators is a silane coupling agent, a titanate coupling agent, an aluminate coupling agent or a rare earth coupling agent.

In the above adhesive for quartz crystal oscillators, as a preferred embodiment, the flowing agent is white kerosene, heptane, octane, undecane, dodecane, cyclohexanone, isophorone, dibasic acid ester or dibasic alcohol ester.

The above adhesive for quartz crystal oscillators is preferably polyethylene wax, polyamide wax or fumed silica.

As a preferred embodiment, the stabilizer is a radical absorbent or a metal chelating agent, the radical absorbent is benzoquinone, hydroquinone or hydroquinone monomethyl ether, and the metal chelating agent is ethylenediamine tetraacetic acid, oxalic acid, acetylacetone or o-aminophenol.

As a preferred embodiment, the conductive powder is at least one of pure silver powder, silver-nickel powder, silver-copper powder, silver-aluminum powder, silver-plated glass powder and nickel-carbon powder.

In a second aspect of the application, a preparation method of the adhesive for the quartz crystal oscillator is provided, which comprises the following steps:

(1) sequentially adding vinyl silicone resin and/or liquid silicone rubber and/or silicone oil, a catalyst and an anti-settling agent into a stirring device, premixing for 10min at the temperature of 35-45 ℃, adding a stabilizer and hydrogenated resin, stirring and mixing for 25-35min to prepare an adhesive carrier;

(2) adding the adhesive, the flowing agent and the conductive powder into the adhesive carrier, putting the mixture into a stirrer, stirring for 15-25min, and putting the mixture into a three-roll grinder, and uniformly grinding to obtain the adhesive for quartz crystal oscillators.

In the above preparation method of the adhesive for quartz crystal oscillators, as a preferred embodiment, in the step (2), the fineness of the adhesive for quartz crystal oscillators is 5-25 um.

The invention has the beneficial effects that: the adhesive for the quartz crystal oscillator can be cured at high temperature, has higher flexibility after being cured, has good shearing strength on various metals, quartz and ceramics, and can bear higher temperature without property change. The adhesive is applied to a quartz crystal oscillator and is a glue dispensing process, glue dispensing points are smooth, and the phenomenon that a needle tube is blocked by glue drawing is avoided.

Detailed Description

In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below. It is to be understood that the described embodiments are merely a few embodiments of the invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the examples given herein without any inventive step, are within the scope of the present invention.

Example 1

An adhesive for quartz crystal oscillators comprises the following raw materials in parts by weight: 12 parts of carrier resin, 0.01 part of catalyst, 0.5 part of adhesive, 4 parts of flow agent, 0.3 part of anti-settling agent, 0.01 part of stabilizer and 75 parts of conductive powder;

the carrier resin comprises vinyl silicone resin, silicone oil and hydrogenated resin;

the catalyst is platinic chloride; the adhesive is a silane coupling agent; the flowing agent is white kerosene; the anti-settling agent is polyethylene wax; the stabilizer is hydroquinone monomethyl ether; the conductive powder is silver nickel powder.

The preparation method of the adhesive for the quartz crystal oscillator comprises the following steps:

(1) sequentially adding vinyl silicone resin, silicone oil, a catalyst and an anti-settling agent into a stirring device, premixing for 10min at the temperature of 35 ℃, adding a stabilizer and hydrogenated resin, stirring and mixing for 35min to prepare an adhesive carrier;

(2) adding the adhesive, the flowing agent and the conductive powder into the adhesive carrier, placing the mixture into a stirrer, stirring for 15min, and placing the mixture into a three-roll grinder, and uniformly grinding to obtain the adhesive with the fineness of 5um for the quartz crystal oscillator.

Example 2

An adhesive for quartz crystal oscillators comprises the following raw materials in parts by weight: 13 parts of carrier resin, 0.05 part of catalyst, 0.8 part of adhesive, 7 parts of flow agent, 0.4 part of anti-settling agent, 0.05 part of stabilizer and 80 parts of conductive powder;

the carrier resin comprises vinyl silicone resin, liquid silicone rubber and hydrogenated resin;

the catalyst is platinic chloride; a solid platinum catalyst supported on an alumina carrier;

the adhesive is a titanate coupling agent; the flow agent is undecane; the anti-settling agent is polyamide wax; the stabilizer is ethylene diamine tetraacetic acid; the conductive powder is silver powder of 1-5 um.

The preparation method of the adhesive for the quartz crystal oscillator comprises the following steps:

(1) sequentially adding vinyl silicone resin, liquid silicone rubber, a catalyst and an anti-settling agent into a stirring device, premixing for 10min at the temperature of 45 ℃, adding a stabilizer and hydrogenated resin, stirring and mixing for 25min to prepare an adhesive carrier;

(2) adding the adhesive, the flowing agent and the conductive powder into the adhesive carrier, putting the adhesive, the flowing agent and the conductive powder into a stirrer, stirring for 20min, putting the mixture into a three-roll grinder, and grinding uniformly to obtain the adhesive with the fineness of 15um for the quartz crystal oscillator.

Example 3

An adhesive for quartz crystal oscillators comprises the following raw materials in parts by weight: 15 parts of carrier resin, 0.1 part of catalyst, 1 part of adhesive, 9 parts of flow agent, 0.5 part of anti-settling agent, 0.1 part of stabilizer and 85 parts of conductive powder;

the carrier resin comprises vinyl silicon resin and hydrogenated resin which are prepared from the following raw materials;

the catalyst is a platinum-vinylsiloxane complex; the adhesive is a rare earth coupling agent;

the flow agent is glycol ester; the anti-settling agent is fumed silica; the stabilizer is o-aminophenol; the conductive powder is silver-plated glass powder.

The preparation method of the adhesive for the quartz crystal oscillator comprises the following steps:

(1) sequentially adding vinyl silicone resin, a catalyst and an anti-settling agent into a stirring device, premixing for 10min at the temperature of 40 ℃, adding a stabilizer and hydrogenated resin, stirring and mixing for 30min to prepare an adhesive carrier;

(2) adding the adhesive, the flowing agent and the conductive powder into the adhesive carrier, putting the adhesive, the flowing agent and the conductive powder into a stirrer, stirring for 25min, putting the mixture into a three-roll grinder, and grinding uniformly to obtain the adhesive with the fineness of 25um for the quartz crystal oscillator.

Comparative example 1

The adhesive of comparative example 1 differs from example 1 in that: the weight part of the conductive powder of the adhesive in the comparative example 1 is 60 weight parts.

Comparative example 2

The adhesive of comparative example 2 differs from example 2 in that: the weight part of the conductive powder of the adhesive in the comparative example 2 is 100 parts.

Comparative example 3

The adhesive of comparative example 3 differs from example 3 in that: the weight part of the adhesive carrier resin described in comparative example 3 was 20 parts by weight.

The performance research of the adhesive for quartz crystal oscillators of the invention comprises the following steps:

TABLE 1 Properties of the adhesive for quartz crystal oscillators according to the present invention

As can be seen from table 1: under the same condition, the addition of the conductive powder with different proportions can obviously influence the conductivity and the viscosity of the adhesive, and the addition of the conductive powder is preferably 75-85; the proportion of carrier resin also affects the bulk properties of the adhesive at the same powder addition level.

The above description is only a preferred embodiment of the present application and is not intended to limit the present application, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.