CN116239866A - Insulating protection material, preparation method and preparation method of insulating protection layer - Google Patents

Abstract

The invention provides an insulation protection material, a preparation method and a preparation method of an insulation protection layer. The insulation protection material comprises: amino epoxy resin, polyurethane, polyimide, dicyandiamide, acrylic acid, methacrylic acid isocyanate ethyl ester, acetone, butanol and isopropanol. Using isocyanoethyl methacrylate as a cross-linking agent, the amino epoxy resin is ring-opened and cured into a network structure, and the elasticity and impact resistance of the insulating protective layer can be improved through polyurethane, and the polyimide Improve the mechanical strength of the insulating protective layer and improve the protection performance. Therefore, the above insulation protection material has the characteristics of high versatility and high protection.

Description

Insulation protection material, preparation method and preparation method of insulation protection layer

technical field

The invention relates to the technical field of semiconductors, in particular to an insulation protection material, a preparation method and a preparation method of an insulation protection layer.

Background technique

In the manufacturing process of devices in integrated circuits, it is necessary to prepare an insulating protective layer on the surface of the device to protect the device and prevent the device from being affected by the external environment, such as water vapor, dust, conductive ions, electromagnetic radiation and other factors, so as to ensure that the circuit has good performance. electrical properties. At present, the commonly used materials for preparing the insulating protective layer are silicon dioxide, borophosphosilicate glass, aluminum oxide, silicon nitride, polysilicon and polyimide, etc., and different materials are used for protection according to the characteristics of the dielectric layer. The versatility is poor, and the uniformity of the insulating protective layer obtained by the spin coating process is poor when the structure is complex, and the front and back semiconductor devices can only be completed in two steps, resulting in low production efficiency and long preparation time. long.

Contents of the invention

The invention provides an insulating protection material, a preparation method and a preparation method of an insulating protection layer to solve the problem that the preparation material of the current insulation protection layer is determined according to the characteristics of the dielectric layer, and the versatility is poor, and the insulation protection layer prepared by the spin coating process The layer can only be prepared on one side, resulting in poor uniformity, low preparation efficiency, and long preparation time.

In a first aspect, the present invention provides an insulating protective material, including: amino epoxy resin, polyurethane, polyimide, dicyandiamide, acrylic acid, isocyanoethyl methacrylate, acetone, butanol and isocyanate propanol,

Wherein, the acetone is used as the diluent of the amino epoxy resin;

The isocyanoethyl methacrylate is used for polymerization with the amino epoxy resin to generate a polymer;

The polyimide and the dicyandiamide are used for a copolymerization reaction with the polymer to generate a copolymer, and an intermediate product is generated during the copolymerization reaction;

The butanol and the isopropanol are used for chain extension of the polyurethane to generate a polyurethane prepolymer;

The polyurethane prepolymer is used to react with the intermediate product to obtain the target product.

In the second aspect, the present invention also provides a method for preparing an insulating and protective material, which is used to prepare the insulating and protective material as described in the first aspect above, including:

Mix amino epoxy resin, polyurethane, polyimide, dicyandiamide, acrylic acid, isocyanoethyl methacrylate, acetone, butanol and isopropanol at a temperature of 60-75°C , to obtain a mixture, and to stir said mixture;

Based on the mixture, an initial solvent is obtained;

adjusting the pH value of the initial solvent to the target pH range to obtain the target solvent;

Stir the target solvent to obtain the target product.

Optionally, the range of the target pH value is: 5.5-6.5.

In the third aspect, the present invention also provides a method for preparing an insulating protective layer, which is used to prepare an insulating protective layer using the insulating protective material described in the first aspect above, including:

immersing the wafer connected to the negative pole of the power supply and the electrode connected to the positive pole of the power supply into the insulating protection material;

controlling the voltage of the power supply to prepare an insulating protective layer on the surface of the wafer.

Optionally, the area ratio of the wafer to the electrode is 1:5˜1:2.

Optionally, the method for preparing the insulating protective layer also includes:

adjusting the temperature of the insulating protection material;

Stir the insulating protection material.

Optionally, the controlling the voltage of the power supply includes:

The voltage of the power supply is controlled by a rectifier.

Optionally, the method for preparing the insulating protective layer also includes:

taking out the wafer from the insulating protection material, and putting it into the first cleaning chamber for rinsing;

When the rinsing time reaches a preset rinsing time, the wafer is taken out.

Optionally, the method for preparing the insulating protective layer also includes:

Putting the wafer into the second cleaning chamber and flipping it for rinsing;

When the immersion time reaches the preset immersion time, the liquid in the second cleaning chamber is emptied, and the wafer is spin-dried in the second cleaning chamber.

Optionally, the method for preparing the insulating protective layer also includes:

The wafer is taken out and baked in an oven to cure the insulating protective layer.

It can be seen from the above technical solutions that the present invention provides an insulating protection material, a preparation method and a preparation method of an insulating protection layer. The insulating protection material includes: amino epoxy resin, polyurethane, polyimide, dicyandiamide, acrylic acid , isocyanoethyl methacrylate, acetone, butanol and isopropanol. Since the preparation material of the current insulating protective layer is determined according to the characteristics of the dielectric layer, there is a problem of poor versatility, and the insulating protective layer prepared by the spin coating process can only be prepared on one side, resulting in relatively poor uniformity of the protective layer. Poor, low preparation efficiency and long preparation time. In the embodiment of the present application, isocyanoethyl methacrylate is used as a crosslinking agent to make the amino epoxy resin ring-opened and cured into a network structure, and the polyurethane can improve the elasticity and impact resistance of the insulating protective layer. The mechanical strength of the insulating protective layer is improved by polyimide, and the protection performance is improved. Therefore, the above insulation protection material has the characteristics of high versatility and high protection.

Description of drawings

In order to illustrate the technical solution of the present application more clearly, the accompanying drawings that need to be used in the embodiments will be briefly introduced below. Obviously, for those of ordinary skill in the art, on the premise of not paying creative work, there are also Additional figures can be derived from these figures.

Fig. 1 is a schematic flow chart of the preparation method of the insulating protection material provided by the embodiment of the present application;

FIG. 2 is a schematic flowchart of a method for preparing an insulating protective layer provided in an embodiment of the present application.

Detailed ways

The embodiments will be described in detail hereinafter, examples of which are illustrated in the accompanying drawings. When the following description refers to the accompanying drawings, the same numerals in different drawings refer to the same or similar elements unless otherwise indicated. The implementations described in the following examples do not represent all implementations consistent with this application. These are merely examples of systems and methods consistent with aspects of the present application as recited in the claims. In the several embodiments provided in the embodiments of the present application, it should be understood that the disclosed device and method may also be implemented in other ways, and the device embodiments described below are only exemplary.

The embodiment of the present application provides an insulating protection material, including: amino epoxy resin, polyurethane, polyimide, dicyandiamide, acrylic acid, isocyanoethyl methacrylate, acetone, butanol and isocyanate propanol,

Wherein, above-mentioned acetone is used as the diluent of above-mentioned amino epoxy resin;

The above-mentioned isocyanoethyl methacrylate is used for polymerizing with the above-mentioned amino epoxy resin to generate a polymer;

The above-mentioned polyimide and the above-mentioned dicyandiamide are used for a copolymerization reaction with the above-mentioned polymer to form a copolymer, and an intermediate product is generated during the above-mentioned copolymerization reaction;

The above-mentioned butanol and the above-mentioned isopropanol are used for the chain extension of the above-mentioned polyurethane to generate a polyurethane prepolymer;

The above polyurethane prepolymer is used to react with the above intermediate product to obtain the target product.

Exemplarily, the above-mentioned intermediate product is a tertiary amine containing an alcoholic hydroxyl group.

Using acetone as the diluent of the amino epoxy resin, the viscosity of the low amino epoxy resin can be reduced, and isocyanoethyl methacrylate is used as the crosslinking agent to make the amino epoxy resin ring-opened and cured into a network structure. Urethane can improve the elasticity and impact resistance of the insulating protective layer. When dicyandiamide is used as the curing agent of amino epoxy resin alone, the required curing temperature is about 150-170°C. Therefore, adding polyimide As a curing agent, the required curing temperature can be adjusted, the heating time can be shortened, and the heating cost can be saved. In addition, the mechanical strength of the insulating protective layer can be improved by adding polyimide, and the protective performance can be improved, which in turn can improve the universality of the insulating protective material. sex and practicality.

As shown in Figure 1, the embodiment of the present application also provides a method for preparing an insulating and protecting material, which is used to prepare the above-mentioned insulating and protecting material, and the method includes:

Step S110. Mix amino epoxy resin, polyurethane, polyimide, dicyandiamide, acrylic acid, isocyanoethyl methacrylate, acetone, butanol and isopropanol, obtain the mixture, and stir the above mixture.

Exemplarily, the above mixture may be stirred at a rotational speed of 800 rpm for 3 hours, so as to fully react various components in the above mixture.

Step S120, based on the above mixture, obtain an initial solvent.

Exemplarily, ethylene glycol monobutyl ether may be added to the mixture to obtain the aforementioned initial solvent.

Step S130, adjusting the pH value of the initial solvent to the target pH value range to obtain the target solvent.

Exemplarily, deionized water, acetic acid, etc. may be added to the initial solvent to adjust the pH value of the initial solvent and provide a suitable reaction environment for the initial solvent.

Step S140, stirring the above target solvent to obtain the target product.

Exemplarily, it can be fully stirred for about half an hour to promote the reaction of the initial solvent and increase the reaction rate.

The insulating protection material prepared according to the above method has good insulating performance and wrapping performance, and can also reduce preparation difficulty, save preparation cost, and increase preparation speed.

According to some embodiments, the range of the target pH value is: 5.5-6.5.

By adjusting the pH value of the initial solvent to the target pH value range, a suitable reaction environment can be provided for the initial solvent, which can neutralize the insulating protection material for ionization, and prevent the pH value of the initial solvent from being too high, resulting in precipitation of the insulating protection material , affecting the electrodeposition performance of the insulating protection material, which in turn can improve the adsorption capacity of the insulating protection material, and can also prevent the pH value of the initial solvent from being too low and causing corrosion, so that the insulating protection material can only be used for applications with strong corrosion resistance Scenarios, improve the practicability of insulation protection materials.

As shown in Figure 2, the embodiment of the present application also provides a method for preparing an insulating protective layer, which is used to prepare an insulating protective layer from the above insulating protective material, which is characterized in that it includes:

Step S210, immersing the wafer connected to the negative pole of the power supply and the electrode connected to the positive pole of the power supply into the above-mentioned insulating protection material.

Exemplarily, the wafer to be prepared with an insulating protective layer can be adsorbed by a vacuum chuck, and the wafer can be immersed in the insulating protective material liquid by controlling the mechanical arm. The above-mentioned electrode has high stability and does not interact with the insulating protective material. The metal electrode for the reaction, for example, the above-mentioned electrode can be a platinum disk electrode.

Step S220, controlling the voltage of the above-mentioned power source to prepare an insulating protection layer on the surface of the above-mentioned wafer.

Exemplarily, when the above power is turned on, a reaction occurs at the anode: 2H ₂ Oe ^- =O ₂ ↑+4H ⁺ , and a reaction occurs at the cathode: H ₂ 0+e ^- =H ₂ ↑+OH ^- ,R- NH ⁺ +OH ^- = RN + H ₂ 0, wherein RN is the above-mentioned insulating protection material.

The preparation of the insulating protective layer by electrophoresis can improve the uniformity and smoothness of the insulating protective layer, improve the protective performance, improve the adhesion of the insulating protective layer, enhance the bonding between the insulating protective layer and the wafer, and prevent the insulating protective layer fall off.

According to some embodiments, the area ratio of the wafer to the electrode is 1:5˜1:2.

According to I=US/rL, when the material of the electrode is determined, the resistivity of the electrode is constant, and the thickness of the electrode is constant, a certain voltage is applied to the electrode, and the current through the electrode increases with the increase of the cross-sectional area of the electrode. The larger, that is, the more electricity passing through the cross-sectional area of the electrode per unit time. Therefore, the preparation rate can be controlled by controlling the area of the electrode.

According to some embodiments, the above method for preparing an insulating protective layer further includes:

Regulate the temperature of the above-mentioned insulation protection material;

Stir the above insulation protection material.

Exemplarily, the temperature of the insulating and protecting material can be controlled between 30°C and 40°C, and the above insulating and protecting material can be stirred at a speed of 120 rpm.

Stirring the insulating protection material can increase the preparation rate. At the same time, when the temperature rises, the viscosity of the insulating protection material decreases, the ion movement speed of the insulating protection material accelerates, and the preparation rate of the insulating protection layer is improved. In addition, since the reaction will be accompanied by an exothermic process, the temperature of the insulating protective material will be too high, which may lead to the acceleration of the ion movement rate of hydrogen ions and impurity ions, resulting in defects on the surface of the insulating protective layer, affecting the insulating protective layer. Preparation quality. Therefore, controlling the temperature of the insulating protection material can improve the preparation quality of the insulating protection layer and increase the preparation rate.

According to some embodiments, the above-mentioned controlling the voltage of the above-mentioned power supply includes:

The voltage of the above power supply is controlled by a rectifier.

Exemplarily, the voltage change cycle can be set by the rectifier, for example, the voltage change cycle can be divided into 4 sections by the rectifier, wherein, the voltage of the first segment is 80V, and the duration is 15 seconds; the voltage of the second segment is 180V, and the duration is 15 seconds; the third stage voltage is 280V, the duration is 30 seconds; the fourth stage voltage is 360V, the duration is 30 seconds.

When the thickness of the insulating protective layer increases, the ionization speed at the wafer will be affected to a certain extent. Therefore, the gradual increase of the voltage controlled by the rectifier can adjust the preparation speed through the rectifier according to the thickness of the insulating protective layer, and can also prevent excessive instantaneous voltage. cause the wafer to be broken down. The use of a rectifier can simplify the voltage control process, and it is convenient to adjust the magnitude and duration of the voltage according to information such as the type of wafer to be prepared for the insulating protective layer, thereby improving the preparation efficiency of the insulating protective layer and improving the convenience and practicability of the preparation method .

According to some embodiments, the above method for preparing an insulating protective layer further includes:

taking out the above-mentioned wafer from the above-mentioned insulation protection material, and putting it into the first cleaning chamber for rinsing;

When the rinsing time reaches the preset rinsing time, the above-mentioned wafer is taken out.

Exemplarily, the aforementioned preset flushing time may be a flushing time determined according to the viscosity of the insulating protection material. The flushing rate can be adjusted by the pressure of the flushing water stream.

Rinsing with running water can improve the rinsing efficiency and save the cleaning time of the wafer.

According to some embodiments, the above method for preparing an insulating protective layer further includes:

Put the above-mentioned wafer into the second cleaning chamber and turn it over for immersion;

When the immersion time reaches the preset immersion time, the liquid in the above-mentioned second cleaning chamber is emptied, and the above-mentioned wafer is dried in the above-mentioned second cleaning chamber, thereby improving the preparation efficiency of the insulating protective layer and the efficiency of the preparation method. practicality.

After the rinsing is completed, the wafer is further flipped and dipped to improve the cleaning quality, save water, and save cleaning costs, thereby improving the preparation efficiency of the insulating protective layer and the practicability of the preparation method.

According to some embodiments, the above method for preparing an insulating protective layer further includes:

The above-mentioned wafer is taken out and baked in an oven to cure the above-mentioned insulating protective layer.

After baking in an oven, the wafer can be further dried to increase the drying rate, thereby improving the preparation efficiency of the insulating protective layer and the practicability of the preparation method.

In summary, the above embodiments are only used to illustrate the technical solutions of the present application, rather than to limit them; although the present application has been described in detail with reference to the foregoing embodiments, those of ordinary skill in the art should understand that: it can still The technical solutions described in the foregoing embodiments are modified, or some of the technical features are replaced equivalently; and these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the spirit and scope of the technical solutions of the embodiments of the present application.

Claims (10)

1. The insulation protection material is characterized in that, including: amino epoxy resin, polyurethane, polyimide, dicyandiamide, acrylic acid, isocyanoethyl methacrylate, acetone, butanol and isopropanol , Wherein, the acetone is used as the diluent of the amino epoxy resin; The isocyanoethyl methacrylate is used for polymerization with the amino epoxy resin to generate a polymer; The polyimide and the dicyandiamide are used for a copolymerization reaction with the polymer to generate a copolymer, and an intermediate product is generated during the copolymerization reaction; The butanol and the isopropanol are used for chain extension of the polyurethane to generate a polyurethane prepolymer; The polyurethane prepolymer is used to react with the intermediate product to obtain the target product. 2. The preparation method of insulating protection material, is used for preparing insulating protection material as claimed in claim 1, is characterized in that, comprises: Mix amino epoxy resin, polyurethane, polyimide, dicyandiamide, acrylic acid, isocyanoethyl methacrylate, acetone, butanol and isopropanol at a temperature of 60-75°C , to obtain a mixture, and to stir said mixture; Based on the mixture, an initial solvent is obtained; adjusting the pH value of the initial solvent to the target pH range to obtain the target solvent; Stir the target solvent to obtain the target product. 3 . The method for preparing insulating and protective materials according to claim 2 , wherein the range of the target pH value is: 5.5-6.5. 4. The method for preparing an insulating protective layer is used to prepare an insulating protective layer using the insulating protective material as claimed in claim 1, characterized in that, comprising: immersing the wafer connected to the negative pole of the power supply and the electrode connected to the positive pole of the power supply into the insulating protection material; controlling the voltage of the power supply to prepare an insulating protective layer on the surface of the wafer. 5 . The method for preparing an insulating protective layer according to claim 4 , wherein an area ratio of the wafer to the electrode is 1:5˜1:2. 6. The insulating protection layer preparation method as claimed in claim 4, is characterized in that, also comprises: adjusting the temperature of the insulating protection material; Stir the insulating protection material. 7. The method for preparing an insulating protective layer according to claim 4, wherein said controlling the voltage of said power supply comprises: The voltage of the power supply is controlled by a rectifier. 8. The method for preparing an insulating protective layer as claimed in claim 4, further comprising: taking out the wafer from the insulating protection material, and putting it into the first cleaning chamber for rinsing; When the rinsing time reaches a preset rinsing time, the wafer is taken out. 9. The insulating protection layer preparation method as claimed in claim 9, is characterized in that, also comprises: Putting the wafer into the second cleaning chamber and flipping it for rinsing; When the immersion time reaches the preset immersion time, the liquid in the second cleaning chamber is emptied, and the wafer is spin-dried in the second cleaning chamber. 10. The method for preparing an insulating protective layer as claimed in claim 9, further comprising: The wafer is taken out and baked in an oven to cure the insulating protection layer.

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