阅读说明：本技术 一种含多羟基有机物的防氧化液制备方法及应用 (Preparation method and application of anti-oxidation liquid containing polyhydroxy organic matter ) 是由 王又容 程先忠 于 2021-08-04 设计创作，主要内容包括：本发明公开了一种含多羟基有机物的防氧化液制备方法及应用,涉及铜箔表面处理技术领域。所述铜箔防氧化液包括多羟基有机物、无机成膜助剂、有机/无机酸和蒸馏水。其中,所述多羟基有机物的浓度为1～12g/L,所述无机成膜助剂的浓度为2～10g/L,所述有机/无机酸的浓度为1～6g/L。本发明所提供的防氧化液不含六价铬等重金属离子、无需水洗、操作简便、能耗低、安全环保,能显著提高铜箔耐高温防氧化的效果,是一种绿色防氧化液。(The invention discloses a preparation method and application of an anti-oxidation liquid containing polyhydroxy organic matters, and relates to the technical field of copper foil surface treatment. The copper foil anti-oxidation liquid comprises polyhydroxy organic matters, inorganic film-forming auxiliaries, organic/inorganic acid and distilled water. The concentration of the polyhydroxy organic matter is 1-12 g/L, the concentration of the inorganic film-forming aid is 2-10 g/L, and the concentration of the organic/inorganic acid is 1-6 g/L. The anti-oxidation liquid provided by the invention does not contain heavy metal ions such as hexavalent chromium and the like, does not need washing, is simple and convenient to operate, low in energy consumption, safe and environment-friendly, can obviously improve the high-temperature-resistant anti-oxidation effect of the copper foil, and is a green anti-oxidation liquid.)

1. The anti-oxidation liquid containing the polyhydroxy organic matter is characterized by comprising the polyhydroxy organic matter, an inorganic film forming aid, organic/inorganic acid and distilled water, wherein the concentration of the polyhydroxy organic matter is 1-12 g/L, the concentration of the film forming aid is 2-10 g/L, and the concentration of the organic/inorganic acid is 1-6 g/L.

2. The method for preparing the anti-oxidation liquid containing polyhydroxy organic compound according to claim 1, comprising the steps of:

step 1: adding 1-12 g of polyhydroxy organic matter into 500 ml of distilled water, stirring by using a stirrer, and mixing and dissolving to obtain solution A;

step 2: adding 2-10 g of inorganic film-forming aid into 300 ml of distilled water, stirring by using a stirrer, and mixing and dissolving to obtain a solution B;

and step 3: dissolving 1-6 g of organic/inorganic acid in 200 ml of distilled water, and stirring for 1 hour at 25 ℃ to obtain a solution C;

and 4, step 4: adding the solution B into the solution A, stirring for 0.5 hour by a stirrer, adding the solution C, and continuously stirring for 0.5 hour to obtain the anti-oxidation solution containing the polyhydroxy organic matters.

3. The method for preparing the anti-oxidation liquid containing the polyhydroxy organic substance according to claim 1, wherein the polyhydroxy organic substance in the step 1 is one or two of sodium tannate, hydroxypropyl chitosan, carboxymethyl cellulose, tannic acid and sodium alginate, and the mass concentration of the polyhydroxy organic substance in the anti-oxidation liquid is 1-12 g/L.

4. The method for preparing the anti-oxidation liquid containing the polyhydroxy organic compound according to claim 1, wherein the inorganic film-forming aid in the step 2 comprises one or two of a sodium silicate sol (mass concentration 400 g/L), a silica sol (mass concentration 400 g/L), a graphene oxide dispersion liquid (mass concentration 12g/L) and an aluminum trioxide sol (mass concentration 250 g/L), and the mass concentration of the film-forming aid in the anti-oxidation liquid is 2 to 10 g/L.

5. The method for preparing the antioxidation liquid containing polyhydroxy organic substance according to claim 1, characterized in that the organic/inorganic acid in the step 3 is one of acetic acid, oxalic acid and phosphoric acid, and the mass concentration of the organic/inorganic acid in the antioxidation liquid is 1-6 g/L.

6. The method for preparing the anti-oxidation liquid containing the polyhydroxy organic compound according to claim 1, wherein the stirring speed in the step 1 is 600-1200 rpm, the stirring temperature is 30-60 ℃, and the stirring time is 6-12 hours.

7. The method for preparing the anti-oxidation liquid containing the polyhydroxy organic compound according to claim 1, wherein the stirring speed in the step 2 is 600-1200 rpm, the stirring temperature is 25-35 ℃, and the stirring time is 1-3 hours.

8. An application of an anti-oxidation liquid containing polyhydroxy organic matters in copper foil anti-oxidation.

Technical Field

The invention relates to the technical field of copper foil surface treatment, in particular to a preparation method and application of an anti-oxidation liquid containing polyhydroxy organic matters.

Background

At present, various surface treatment techniques play an important role in the oxidation corrosion prevention of metal engineering materials. In particular, chemical conversion coating technology has become an indispensable surface treatment process before the use of metal products and equipment. However, the carcinogenic effect of hexavalent chromium on humans has been banned or greatly limited. Therefore, some non-hexavalent chromium, green and environmentally friendly surface treatment technologies are attracting increasing attention in the commercial industry. Most commercial metal surface coatings are inorganic films, the formation of which typically involves the deposition of metal salts or oxides on the metal surface. Although the thickness and surface morphology of the deposit are controlled by the reaction parameters, the film-forming mechanism has certain technical defects. The organic film forming agent is introduced, the organic film is prepared on the metal surface by a molecular self-assembly method, and meanwhile, the advantages of the electrodeless nano material are combined, so that a uniform and compact organic-inorganic anti-oxidation composite film is formed on the metal surface, and the organic film forming agent has greater advantages. The applicant finds the high temperature resistance and oxidation resistance of the polyhydroxy organic compound composite film in the electrolytic copper foil. Therefore, the invention discloses a preparation method of polyhydroxy-containing organic-inorganic antioxidant liquid, which mainly solves the problem of high temperature resistance and oxidation resistance of electrolytic copper foil.

Disclosure of Invention

Aiming at the defects of the prior art, the invention provides a preparation method and application of an anti-oxidation liquid containing polyhydroxy organic matters, which meet the anti-oxidation requirement of electrolytic copper foil under the condition of high temperature. In order to achieve the purpose, the invention is realized by the following technical scheme:

an anti-oxidation liquid containing polyhydroxy organic matter comprises the following components: the organic film forming agent comprises a polyhydroxy organic matter, an inorganic film forming auxiliary agent, an organic/inorganic acid and distilled water, wherein the concentration of the polyhydroxy organic matter is 1-12 g/L, the concentration of the inorganic film forming auxiliary agent is 2-10 g/L, and the concentration of the organic/inorganic acid is 1-6 g/L.

The preparation method of the anti-oxidation liquid containing the polyhydroxy organic matter comprises the following steps:

step 1: weighing 1-12 g of polyhydroxy organic matter, adding into 500 ml of distilled water, stirring by using a stirrer, and uniformly mixing to obtain solution A.

Step 2: weighing 2-10 g of inorganic film-forming additive, adding into 300 ml of distilled water, stirring by using a stirrer, and uniformly mixing to obtain solution B.

And step 3: weighing 1-6 g of organic/inorganic acid, dissolving in 200 ml of distilled water, and stirring at 25 ℃ for 1 hour to obtain solution C.

And 4, adding the solution B into the solution A, stirring for 0.5 hour by using a stirrer, adding the solution C, and continuously stirring for 0.5 hour to prepare the anti-oxidation solution.

In the step 1, the polyhydroxy organic matter is one or two of sodium tannate, hydroxypropyl chitosan, carboxymethyl cellulose, tannic acid and sodium alginate, and the mass concentration of the polyhydroxy organic matter in the prepared anti-oxidation liquid is 1-12 g/L.

In the step 2, the inorganic film-forming aid comprises one or two of sodium silicate sol (with the mass concentration of 400 g/L), silicon dioxide sol (with the mass concentration of 400 g/L), graphene oxide dispersion liquid (with the mass concentration of 12g/L) and aluminum trioxide sol (with the mass concentration of 250 g/L) which are mixed, and the mass concentration of the inorganic film-forming aid in the prepared anti-oxidation liquid is 2-10 g/L.

In the step 3, the organic/inorganic acid is one of acetic acid, oxalic acid and phosphoric acid, and the mass concentration of the organic/inorganic acid in the prepared anti-oxidation liquid is 1-6 g/L.

In the step 1, the stirring speed is 600-1200 rpm, the stirring temperature is 30-60 ℃, and the stirring time is 6-12 hours.

In the step 2, the stirring speed is 600-1200 rpm, the stirring temperature is 25-35 ℃, and the stirring time is 1-3 hours.

Advantageous effects

The invention aims to provide preparation and application of anti-oxidation liquid containing polyhydroxy organic matters, the method realizes the purposes of no heavy metal ions, low energy consumption and no washing for anti-oxidation, and the anti-oxidation temperature can reach 180 ℃ for 30 minutes. The polyhydroxy organic matter is used as an organic film forming agent, and is easier to self-assemble with copper to form a film on the surface of the copper foil due to more hydrophilic groups to form a stable organic matter anti-oxidation layer. In addition, the polyhydroxy organic matters are easy to complex with exposed copper on the surface of the copper foil, and can generate a composite film with silica sol, sodium silicate sol, graphene oxide or aluminum trioxide sol, so that the high-temperature resistance and oxidation resistance of the film are further improved.

Detailed Description

Example 1

The anti-oxidation liquid containing polyhydroxy organic matter comprises the following components: the mass concentration of sodium tannate was 1g/L, the mass concentration of silica sol (mass concentration 400 g/L) was 2g/L, and the mass concentration of phosphoric acid was 1 g/L.

Step 1: weighing 1g of sodium tannate, adding the sodium tannate into 500 ml of distilled water, stirring by a stirrer at the stirring speed of 600rpm and the stirring temperature of 30 ℃ for 6 hours, and uniformly mixing to obtain solution A.

Step 2: weighing 2g of silica sol (the mass concentration is 400 g/L), adding the silica sol into 300 ml of distilled water, stirring the mixture by a stirrer at the stirring speed of 600rpm and the stirring temperature of 25 ℃ for 1 hour, and uniformly mixing the mixture to obtain solution B.

And step 3: 1g of phosphoric acid was weighed, dissolved in 200 ml of distilled water, and stirred at 25 ℃ for 1 hour to obtain solution C.

And 4, step 4: adding the solution B into the solution A, stirring for 0.5 hour, adding the solution C, and continuously stirring for 0.5 hour to prepare the anti-oxidation solution.

And (3) testing the oxidation performance of the copper foil, namely soaking the treated electrolytic copper foil with the thickness of 1.5cm by 6.0cm into an antioxidant for 8 seconds, then drying the electrolytic copper foil by hot air at the temperature of 80 ℃, then placing the electrolytic copper foil into an oven, setting the temperature at 180 ℃, baking the electrolytic copper foil for 15 minutes and 30 minutes respectively, and observing the oxidation discoloration condition of the electrolytic copper foil.

Example 2

The anti-oxidation liquid containing polyhydroxy organic matter comprises the following components: the mass concentration of sodium tannate was 12g/L, the mass concentration of silica sol (mass concentration 400 g/L) was 10g/L, and the mass concentration of phosphoric acid was 6 g/L.

Step 1: weighing 12g of sodium tannate, adding the sodium tannate into 500 ml of distilled water, stirring by a stirrer at the stirring speed of 1200rpm and the stirring temperature of 60 ℃ for 12 hours, and uniformly mixing to obtain solution A.

Step 2: weighing 10g of silica sol (with the mass concentration of 400 g/L), adding into 300 ml of distilled water, stirring by a stirrer at the stirring speed of 1200rpm at the stirring temperature of 35 ℃ for 3 hours, and uniformly mixing to obtain solution B.

And step 3: 6g of phosphoric acid was weighed, dissolved in 200 ml of distilled water, and stirred at 25 ℃ for 1 hour to obtain solution C.

And 4, adding the solution B into the solution A, stirring for 0.5 hour, adding the solution C, and continuously stirring for 0.5 hour to prepare the anti-oxidation solution.

And (3) testing the oxidation performance of the copper foil, namely soaking the treated electrolytic copper foil with the thickness of 1.5cm by 6.0cm into an antioxidant for 8 seconds, then drying the electrolytic copper foil by hot air at the temperature of 80 ℃, then placing the electrolytic copper foil into an oven, setting the temperature at 180 ℃, baking the electrolytic copper foil for 15 minutes and 30 minutes respectively, and observing the oxidation discoloration condition of the electrolytic copper foil.

Example 3

The anti-oxidation liquid containing polyhydroxy organic matter comprises the following components: the mass concentration of sodium tannate was 6g/L, the mass concentration of silica sol (mass concentration 400 g/L) was 6g/L, and the mass concentration of phosphoric acid was 4 g/L.

Step 1: weighing 6g of sodium tannate, adding the sodium tannate into 500 ml of distilled water, stirring by a stirrer at the stirring speed of 900rpm, the stirring temperature of 45 ℃ and the stirring time of 9 hours, and uniformly mixing to obtain solution A.

Step 2: weighing 6g of silica sol (with the mass concentration of 400 g/L), adding the silica sol into 300 ml of distilled water, stirring by using a stirrer at the stirring speed of 900rpm at the stirring temperature of 30 ℃ for 2 hours, and uniformly mixing to obtain solution B.

And step 3: 4g of phosphoric acid was weighed, dissolved in 200 ml of distilled water, and stirred at 25 ℃ for 1 hour to obtain solution C.

And 4, step 4: adding the solution B into the solution A, stirring for 0.5 hour, adding the solution C, and continuously stirring for 0.5 hour to prepare the anti-oxidation solution.

And (3) testing the oxidation performance of the copper foil, namely soaking the treated electrolytic copper foil with the thickness of 1.5cm by 6.0cm into an antioxidant for 8 seconds, then drying the electrolytic copper foil by hot air at the temperature of 80 ℃, then placing the electrolytic copper foil into an oven, setting the temperature at 180 ℃, baking the electrolytic copper foil for 15 minutes and 30 minutes respectively, and observing the oxidation discoloration condition of the electrolytic copper foil.

Example 4

The anti-oxidation liquid containing polyhydroxy organic matter comprises the following components: the mass concentration of hydroxypropyl chitosan is 3g/L, the mass concentration of sodium silicate sol (mass concentration 400 g/L) is 6g/L, and the mass concentration of graphene oxide dispersion liquid (mass concentration 12g/L) is 4g/L, and the mass concentration of acetic acid is 6 g/L.

Step 1: weighing 3g of hydroxypropyl chitosan, adding the hydroxypropyl chitosan into 500 ml of distilled water, stirring by using a stirrer at the stirring speed of 1200rpm, the stirring temperature of 60 ℃ and the stirring time of 12 hours, and uniformly mixing to obtain a solution A.

Step 2: weighing 6g of sodium silicate sol (with the mass concentration of 400 g/L) and 4g of graphene oxide dispersion liquid (with the mass concentration of 12g/L), adding the mixture into 300 ml of distilled water, stirring the mixture by using a stirrer at the stirring speed of 1000rpm and the stirring temperature of 25 ℃ for 1 hour, and uniformly mixing the mixture to obtain solution B.

And step 3: 6g of acetic acid was weighed out and dissolved in 200 ml of distilled water to obtain solution C at 25 ℃.

And 4, adding the solution B into the solution A, stirring for 0.5 hour, adding the solution C, and continuously stirring for 0.5 hour to prepare the anti-oxidation solution.

And (3) testing the oxidation performance of the copper foil, namely soaking the treated electrolytic copper foil with the thickness of 1.5cm by 6.0cm into an antioxidant for 8 seconds, then drying the electrolytic copper foil by hot air at the temperature of 80 ℃, then placing the electrolytic copper foil into an oven, setting the temperature at 180 ℃, baking the electrolytic copper foil for 15 minutes and 30 minutes respectively, and observing the oxidation discoloration condition of the electrolytic copper foil.

Example 5

The anti-oxidation liquid containing polyhydroxy organic matter comprises the following components: the mass concentration of the carboxymethyl cellulose is 1g/L, the mass concentration of the graphene oxide dispersion liquid (mass concentration is 12g/L) is 10g/L, and the mass concentration of the oxalic acid is 2 g/L.

Step 1: weighing 1g of carboxymethyl cellulose, adding the carboxymethyl cellulose into 500 ml of distilled water, stirring by using a stirrer at the stirring speed of 900rpm and the stirring temperature of 50 ℃ for 10 hours, and uniformly mixing to obtain a solution A.

Step 2: weighing 10g of graphene oxide dispersion liquid (with the mass concentration of 12g/L), adding the graphene oxide dispersion liquid into 300 ml of distilled water, stirring the mixture by using a stirrer at the stirring speed of 600rpm and the stirring temperature of 30 ℃ for 2 hours, and uniformly mixing the mixture to obtain a solution B.

And step 3: 2g of oxalic acid was weighed, dissolved in 200 ml of distilled water, and stirred at 25 ℃ for 1 hour to obtain solution C.

And 4, step 4: adding the solution B into the solution A, stirring for 0.5 hour, adding the solution C, and continuously stirring for 0.5 hour to prepare the anti-oxidation solution.

And (3) testing the oxidation performance of the copper foil, namely soaking the treated electrolytic copper foil with the thickness of 1.5cm by 6.0cm into an antioxidant for 8 seconds, then drying the electrolytic copper foil by hot air at the temperature of 80 ℃, then placing the electrolytic copper foil into an oven, setting the temperature at 180 ℃, baking the electrolytic copper foil for 15 minutes and 30 minutes respectively, and observing the oxidation discoloration condition of the electrolytic copper foil.

Example 6

The anti-oxidation liquid containing polyhydroxy organic matter comprises the following components: the mass concentration of tannic acid is 9g/L, the mass concentration of the aluminum trioxide sol (the mass concentration is 250 g/L) is 2g/L, and the mass concentration of acetic acid is 3 g/L.

Step 1: weighing 9g of tannic acid, adding the tannic acid into 500 ml of distilled water, stirring by using a stirrer at the stirring speed of 700rpm and the stirring temperature of 30 ℃ for 6 hours, and uniformly mixing to obtain solution A.

Step 2: weighing 2g of aluminum trioxide sol (the mass concentration is 250 g/L), adding the aluminum trioxide sol into 300 ml of distilled water, stirring by using a stirrer at the stirring speed of 800rpm and the stirring temperature of 25 ℃ for 3 hours, and uniformly mixing to obtain a solution B.

And step 3: 3g of acetic acid was weighed, dissolved in 200 ml of distilled water, and stirred at 25 ℃ for 1 hour to obtain solution C.

And 4, step 4: adding the solution B into the solution A, stirring for 0.5 hour, adding the solution C, and continuously stirring for 0.5 hour to prepare the anti-oxidation solution.

And (3) testing the oxidation performance of the copper foil, namely soaking the treated electrolytic copper foil with the thickness of 1.5cm by 6.0cm into an antioxidant for 8 seconds, then drying the electrolytic copper foil by hot air at the temperature of 80 ℃, then placing the electrolytic copper foil into an oven, setting the temperature at 180 ℃, baking the electrolytic copper foil for 15 minutes and 30 minutes respectively, and observing the oxidation discoloration condition of the electrolytic copper foil.

Example 7

The anti-oxidation liquid containing polyhydroxy organic matter comprises the following components: the mass concentration of sodium alginate is 12g/L, the mass concentration of silica sol (mass concentration 400 g/L) is 3g/L, the mass concentration of graphene oxide dispersion liquid (mass concentration 12g/L) is 6g/L, and the mass concentration of phosphoric acid is 5 g/L.

Step 1: weighing 12g of sodium alginate, adding into 500 ml of distilled water, stirring with a stirrer at 1200rpm and 60 ℃ for 10 hours, and uniformly mixing to obtain solution A.

Step 2: weighing 3g of silica sol (with the mass concentration of 400 g/L) and 6g of graphene oxide dispersion (with the mass concentration of 12g/L), adding into 300 ml of distilled water, stirring by using a stirrer at the stirring speed of 700rpm at the stirring temperature of 30 ℃ for 3 hours, and uniformly mixing to obtain solution B.

And step 3: 5g of phosphoric acid was weighed, dissolved in 200 ml of distilled water, and stirred at 25 ℃ for 1 hour to obtain solution C.

And 4, step 4: adding the solution B into the solution A, stirring for 0.5 hour, adding the solution C, and continuously stirring for 0.5 hour to prepare the anti-oxidation solution.

And (3) testing the oxidation performance of the copper foil, namely soaking the treated electrolytic copper foil with the thickness of 1.5cm by 6.0cm into an antioxidant for 8 seconds, then drying the electrolytic copper foil by hot air at the temperature of 80 ℃, then placing the electrolytic copper foil into an oven, setting the temperature at 180 ℃, baking the electrolytic copper foil for 15 minutes and 30 minutes respectively, and observing the oxidation discoloration condition of the electrolytic copper foil.

Example 8

The anti-oxidation liquid containing polyhydroxy organic matter comprises the following components: the mass concentration of tannic acid is 5g/L, the mass concentration of sodium alginate is 1g/L, the mass concentration of aluminum trioxide sol is 4g/L, the mass concentration of graphene oxide dispersion liquid is 5g/L, and the mass concentration of oxalic acid is 4 g/L.

Step 1: weighing 5g of sodium tannate and 1g of sodium alginate, adding into 500 ml of distilled water, stirring with a stirrer at the stirring speed of 1000rpm and the stirring temperature of 60 ℃ for 12 hours, and uniformly mixing to obtain solution A.

Step 2: weighing 4g of aluminum trioxide sol (with the mass concentration of 250 g/L) and 5g of graphene oxide dispersion (with the mass concentration of 12g/L), adding the mixture into 300 ml of distilled water, stirring the mixture by using a stirrer at the stirring speed of 1000rpm and the stirring temperature of 30 ℃ for 3 hours, and uniformly mixing the mixture to obtain solution B.

And step 3: 4g of oxalic acid was weighed, dissolved in 200 ml of distilled water, and stirred at 25 ℃ for 1 hour to obtain solution C.

And 4, step 4: adding the solution B into the solution A, stirring for 0.5 hour, adding the solution C, and continuously stirring for 0.5 hour to prepare the anti-oxidation solution.

And (3) testing the oxidation performance of the copper foil, namely soaking the treated electrolytic copper foil with the thickness of 1.5cm by 6.0cm into an antioxidant for 8 seconds, then drying the electrolytic copper foil by hot air at the temperature of 80 ℃, then placing the electrolytic copper foil into an oven, setting the temperature at 180 ℃, baking the electrolytic copper foil for 15 minutes and 30 minutes respectively, and observing the oxidation discoloration condition of the electrolytic copper foil.

Comparative example 1

The copper foil anti-oxidation liquid comprises the following components: no polyhydroxy organic matter, the mass concentration of the silica sol is 2g/L, and the mass concentration of the phosphoric acid is 1 g/L.

Step 1: 500 ml of distilled water was designated as solution A.

Step 2: weighing 2g of silica sol (the mass concentration is 400 g/L), adding the silica sol into 300 ml of distilled water, stirring the mixture by a stirrer at the stirring speed of 600rpm and the stirring temperature of 25 ℃ for 1 hour, and uniformly mixing the mixture to obtain solution B.

And step 3: 1g of phosphoric acid was weighed, dissolved in 200 ml of distilled water, and stirred at 25 ℃ for 1 hour to obtain solution C.

And 4, step 4: adding the solution B into the solution A, stirring for 0.5 hour, adding the solution C, and continuously stirring for 0.5 hour to prepare the anti-oxidation solution.

And (3) testing the oxidation performance of the copper foil, namely soaking the treated electrolytic copper foil with the thickness of 1.5cm by 6.0cm into an antioxidant for 8 seconds, then drying the electrolytic copper foil by hot air at the temperature of 80 ℃, then placing the electrolytic copper foil into an oven, setting the temperature at 180 ℃, baking the electrolytic copper foil for 15 minutes and 30 minutes respectively, and observing the oxidation discoloration condition of the electrolytic copper foil.

Comparative example 2

The copper foil anti-oxidation liquid comprises the following components: the mass concentration of the sodium tannate is 1g/L, the mass concentration of the inorganic film-forming assistant is 1g/L, and the mass concentration of the phosphoric acid is 1 g/L.

Step 1: weighing 1g of sodium tannate, adding the sodium tannate into 500 ml of distilled water, stirring by a stirrer at the stirring speed of 600rpm and the stirring temperature of 30 ℃ for 6 hours, and uniformly mixing to obtain solution A.

Step 2: and 300 ml of distilled water is used as the solution B.

And step 3: 1g of phosphoric acid was weighed and dissolved in 200 ml of distilled water at 25 ℃ to obtain solution C.

And 4, adding the solution B into the solution A, stirring for 0.5 hour, adding the solution C, and continuously stirring for 0.5 hour to prepare the anti-oxidation solution.

And (3) testing the oxidation performance of the copper foil, namely soaking the treated electrolytic copper foil with the thickness of 1.5cm by 6.0cm into an antioxidant for 8 seconds, then drying the electrolytic copper foil by hot air at the temperature of 80 ℃, then placing the electrolytic copper foil into an oven, setting the temperature at 180 ℃, baking the electrolytic copper foil for 15 minutes and 30 minutes respectively, and observing the oxidation discoloration condition of the electrolytic copper foil.

Comparative example 3

The copper foil anti-oxidation liquid comprises the following components: the mass concentration of sodium tannate was 1g/L, the mass concentration of silica sol (mass concentration 400 g/L) was 2g/L, and no organic/inorganic acid was present.

Step 1: weighing 1g of sodium tannate, adding the sodium tannate into 500 ml of distilled water, stirring by a stirrer at the stirring speed of 600rpm and the stirring temperature of 30 ℃ for 6 hours, and uniformly mixing to obtain solution A.

Step 2: weighing 2g of silica sol (the mass concentration is 400 g/L), adding the silica sol into 300 ml of distilled water, stirring the mixture by a stirrer at the stirring speed of 600rpm and the stirring temperature of 25 ℃ for 1 hour, and uniformly mixing the mixture to obtain solution B.

And step 3: the volume of distilled water was designated as volume C.

And 4, adding the solution B into the solution A, stirring for 0.5 hour, adding the solution C, and continuously stirring for 0.5 hour to prepare the anti-oxidation solution.

And (3) testing the oxidation performance of the copper foil, namely soaking the treated electrolytic copper foil with the thickness of 1.5cm by 6.0cm into an antioxidant for 8 seconds, then drying the electrolytic copper foil by hot air at the temperature of 80 ℃, then placing the electrolytic copper foil into an oven, setting the temperature at 180 ℃, baking the electrolytic copper foil for 15 minutes and 30 minutes respectively, and observing the oxidation discoloration condition of the electrolytic copper foil.

The copper foil oxidation resistance test data of each example and comparative example are shown in the following table 1:

TABLE 1 test results of copper foil oxidation resistance

As can be seen from comparative examples 1-3, the lack of the polyhydroxy organic film forming agent, the lack of the inorganic film forming aid or the lack of the organic/inorganic acid can cause the reduction of the high-temperature anti-oxidation function of the copper foil. The oxidation resistance is reduced by the lack of a polyhydroxy organic film forming agent, the lack of an organic/inorganic acid and the lack of a film forming aid in sequence.