阅读说明：本技术 一种多功能铜清洗剂及其制备方法 (Multifunctional copper cleaning agent and preparation method thereof ) 是由 张丹 刘帅 郑磊 聂宜苹 季静怡 于 2019-11-25 设计创作，主要内容包括：本发明公开了一种多功能铜清洗剂及其制备方法,属于助剂技术领域。本发明多功能铜清洗剂由如下原料组成：酒石酸15-20份,柠檬酸钠10-20份,聚丁二酸丁二醇脂5-10份,木质素磺酸钠3-8份,天然油酯10-20份,十二烷基磺酸钠5-10份,酒石酸钠5-10份,十二烷基硫酸钠5-10份,月桂酸3-8份,乳酸2-3份,失水山梨醇脂肪酸酯3-8份,丁基羟基茴香醚3-5份,茶多酚2-3份,水30-50份。本发明的多功能铜清洗剂制造工艺简单易操作,原料价格低廉易获得,且无毒无害,多种原料相互配合在快速去除铜锈的同时还可以达到抛光的效果,给予铜件意想不到的光亮感,并且有一定的防腐蚀功能,对基材无损伤。(The invention discloses a multifunctional copper cleaning agent and a preparation method thereof, and belongs to the technical field of auxiliaries. The multifunctional copper cleaning agent comprises the following raw materials: 15-20 parts of tartaric acid, 10-20 parts of sodium citrate, 5-10 parts of polybutylene succinate, 3-8 parts of sodium lignosulfonate, 10-20 parts of natural oil ester, 5-10 parts of sodium dodecyl sulfate, 5-10 parts of sodium tartrate, 5-10 parts of sodium dodecyl sulfate, 3-8 parts of lauric acid, 2-3 parts of lactic acid, 3-8 parts of sorbitan fatty acid ester, 3-5 parts of butyl hydroxy anisole, 2-3 parts of tea polyphenol and 30-50 parts of water. The multifunctional copper cleaning agent disclosed by the invention is simple and easy to operate in manufacturing process, low in price and easy to obtain raw materials, is non-toxic and harmless, can achieve a polishing effect while rapidly removing copper rust by matching multiple raw materials, gives unexpected brightness to a copper part, has a certain anti-corrosion function, and does not damage a base material.)

1. The multifunctional copper cleaning agent is characterized by comprising, by mass, 15-20 parts of a pH regulator, 10-20 parts of sodium citrate, 5-10 parts of sodium tartrate, 5-10 parts of a surfactant, 3-8 parts of a penetrating agent, 10-20 parts of an anionic surfactant, 2-3 parts of a solubilizer and 5-10 parts of an antioxidant.

2. The multifunctional copper cleaner according to claim 1, wherein the pH regulator is a mixture of tartaric acid, lauric acid and lactic acid.

3. The multifunctional copper cleaning agent as claimed in claim 2, wherein the cleaning agent comprises 15-20 parts of tartaric acid, 3-8 parts of lauric acid and 2-3 parts of lactic acid.

4. The multifunctional copper cleaner according to claim 1, wherein the surfactant is a mixture of polybutylene succinate, sodium lignosulfonate, natural oil ester, sodium dodecylsulfate and sorbitan fatty acid ester.

5. The multifunctional copper cleaning agent according to claim 4, wherein the multifunctional copper cleaning agent comprises 5-10 parts of polybutylene succinate, 3-8 parts of sodium lignosulfonate, 10-20 parts of natural oil ester, 5-10 parts of sodium dodecyl sulfate and 3-8 parts of sorbitan fatty acid ester.

6. The multifunctional copper cleaning agent according to claim 1, wherein the antioxidant is a compound of butyl hydroxyanisole and tea polyphenol, 3-5 parts of butyl hydroxyanisole and 2-3 parts of tea polyphenol.

7. The multifunctional copper cleaning agent as claimed in claim 1, further comprising water 30-50 parts.

8. The multifunctional copper cleaning agent according to claim 1, wherein the natural oil is one or more of coconut oil, lanolin and peanut oil.

9. A preparation method of the multifunctional copper cleaning agent as claimed in any one of claims 1 to 8, characterized by comprising the following steps:

(1) adding 10-20 parts of natural oil ester into a reaction kettle, raising the temperature to 60-80 ℃, adding 30-50 parts of water after the natural oil ester is molten, stirring for 20-30 minutes at 500 revolutions per minute;

(2) when the temperature in the step (1) is reduced to 25-30 ℃, adding 3-8 parts of sodium lignosulphonate, 3-8 parts of sorbitan fatty acid ester, 5-10 parts of sodium tartrate, 3-8 parts of lauric acid, 2-3 parts of lactic acid, and stirring for 10 minutes at 500-1000 r/min;

(3) when the temperature in the step (2) is reduced to room temperature, 5-10 parts of sodium dodecyl sulfate, 3-5 parts of butyl hydroxy anisole and 2-3 parts of tea polyphenol are added, and the mixture is stirred for 10 minutes at the speed of 500 revolutions per minute;

(4) continuously adding 10-20 parts of sodium citrate, 5-10 parts of succinic acid succinate, 5-10 parts of sodium dodecyl sulfate, 15-20 parts of tartaric acid and 1000 revolutions per minute into the step (3), and stirring for 10-20 minutes; discharging and packaging to obtain the finished product.

10. Use of the copper cleaner according to any one of claims 1 to 8 in the industrial removal of oil stains and patina on metal surfaces.

Technical Field

The invention relates to a multifunctional copper cleaning agent and a preparation method thereof, belonging to the technical field of auxiliaries.

Background

With the continuous reduction of the feature size of integrated circuit devices and the continuous increase of the wafer size, copper chemical cleaning is receiving more and more attention as the only practical technology capable of realizing global planarization of chips at present in order to improve the reliability and service life of the devices. The copper chemical cleaning process mainly comprises two stages of polishing and cleaning, and the cleaning procedure is used as the final treatment step of various copper wafers and plays a role in playing a role. However, in the related reports of copper cleaning in the past, relatively few descriptions are provided for the cleaning part. At present, most of copper cleaning agents on the market are organic type copper cleaning agents, and although the copper rust and oil stains on the surface of a copper part are removed to a certain degree, the organic type copper cleaning agents are particularly troublesome in subsequent treatment, easily pollute the environment and are high in treatment cost.

Therefore, the copper cleaning agent is produced by transportation, can remove various oil stains and copper rust, does not damage a substrate, has a certain polishing effect, is easy to treat, and has little environmental pollution.

Disclosure of Invention

In order to solve the problems, tartaric acid, lauric acid and lactic acid are adopted in the multifunctional copper cleaning agent, and the three weak acids are matched with each other to provide a pH adjusting effect, so that a weak acid condition is provided for a solution to accelerate the activation of the surface of a copper workpiece, and meanwhile, the multifunctional copper cleaning agent also has weak corrosivity on copper rust to accelerate the removal of the rust on the surface of the copper; the multifunctional copper cleaning agent disclosed by the invention adopts natural grease as an emulsifier, so that oil stains on the surface of copper are dispersed, and the effect of quickly removing the oil stains is achieved; the multifunctional copper cleaning agent provided by the invention adopts butyl hydroxy anisole, tea polyphenol and butyl hydroxy anisole, and has certain oxidation resistance and corrosion resistance effects.

The first purpose of the invention is to provide a multifunctional copper cleaning agent, which comprises, by mass, 15-20 parts of a pH regulator, 10-20 parts of sodium citrate, 5-10 parts of sodium tartrate, 5-10 parts of a surfactant, 3-8 parts of a penetrant, 10-20 parts of an anionic surfactant, 2-3 parts of a solubilizer and 5-10 parts of an antioxidant.

The second purpose of the invention is to provide a preparation method of the multifunctional copper cleaning agent, which comprises the following steps:

(1) adding 10-20 parts of natural oil ester into a reaction kettle, raising the temperature to 60-80 ℃, adding water and stirring when the natural oil ester is molten;

(2) when the temperature in the step (1) is reduced to 25-30 ℃, adding 3-8 parts of sodium lignosulphonate, 3-8 parts of sorbitan fatty acid ester, 5-10 parts of sodium tartrate, 3-8 parts of lauric acid and 2-3 parts of lactic acid, and uniformly mixing;

(3) when the temperature in the step (2) is reduced to room temperature, adding 5-10 parts of sodium dodecyl sulfate, 3-5 parts of butyl hydroxy anisole and 2-3 parts of tea polyphenol, and uniformly mixing;

(4) continuously adding 10-20 parts of sodium citrate, 5-10 parts of poly (butylene succinate), 5-10 parts of sodium dodecyl sulfate and 15-20 parts of tartaric acid into the step (3), and uniformly mixing; discharging and packaging to obtain the finished product.

In one embodiment of the invention, the pH regulator is a mixture of tartaric acid, lauric acid and lactic acid, 15-20 parts of tartaric acid, 3-8 parts of lauric acid and 2-3 parts of lactic acid.

In one embodiment of the invention, the surfactant is a mixture of polybutylene succinate, sodium lignosulfonate, natural oil ester, sodium dodecyl sulfate and sorbitan fatty acid ester.

In one embodiment of the invention, the composition comprises 5-10 parts of polybutylene succinate, 3-8 parts of sodium lignosulfonate, 10-20 parts of natural oil ester, 5-10 parts of sodium dodecyl sulfate and 3-8 parts of sorbitan fatty acid ester.

In one embodiment of the invention, the antioxidant is a compound of butyl hydroxy anisol and tea polyphenol, 3-5 parts of butyl hydroxy anisol and 2-3 parts of tea polyphenol.

In one embodiment of the invention, the multifunctional copper cleaning agent further comprises 30-50 parts of water.

In one embodiment of the invention, the natural oil is one or more of coconut oil, lanolin and peanut oil.

In one embodiment of the present invention, the method specifically includes:

(1) adding 10-20 parts of natural oil ester into a reaction kettle, raising the temperature to 60-80 ℃, adding 30-50 parts of water after the natural oil ester is molten, stirring for 20-30 minutes at 500 revolutions per minute;

(2) when the temperature in the step (1) is reduced to 25-30 ℃, adding 3-8 parts of sodium lignosulphonate, 3-8 parts of sorbitan fatty acid ester, 5-10 parts of sodium tartrate, 3-8 parts of lauric acid, 2-3 parts of lactic acid, and stirring for 10 minutes at 500-1000 r/min;

(3) when the temperature in the step (2) is reduced to room temperature, 5-10 parts of sodium dodecyl sulfate, 3-5 parts of butyl hydroxy anisole and 2-3 parts of tea polyphenol are added, and the mixture is stirred for 10 minutes at the speed of 500 revolutions per minute;

(4) continuously adding 10-20 parts of sodium citrate, 5-10 parts of succinic acid succinate, 5-10 parts of sodium dodecyl sulfate, 15-20 parts of tartaric acid and 1000 revolutions per minute into the step (3), and stirring for 10-20 minutes; discharging and packaging to obtain the finished product.

The third purpose of the invention is to provide a copper cleaning agent prepared by the preparation method.

The fourth purpose of the invention is to provide the application of the copper cleaning agent in the industry for removing oil stains and patina on metal surfaces.

The invention has the beneficial effects that:

(1) the multifunctional copper cleaning agent can wash rust and oil stains on the surface of copper, can also provide certain characteristics of acid, alkali and salt corrosion resistance for copper workpieces, and enables the copper workpieces to become bright and have certain polishing effect, thereby being the multifunctional copper cleaning agent.

(2) The tartaric acid, the lauric acid and the lactic acid are adopted in the multifunctional copper cleaning agent, and the three weak acids are matched with each other to provide a pH adjusting effect, so that a weak acid condition is provided for a solution to accelerate the activation of the surface of a copper workpiece, and meanwhile, the multifunctional copper cleaning agent also has weak corrosivity on copper rust to accelerate the removal of the rust on the surface of copper.

(3) The multifunctional copper cleaning agent disclosed by the invention adopts natural grease as an emulsifier, so that oil stains on the surface of copper are dispersed, and the effect of quickly removing the oil stains is achieved.

(4) The multifunctional copper cleaning agent adopts butyl hydroxy anisole, tea polyphenol and butyl hydroxy anisole which have certain oxidation resistance and corrosion resistance effects, the tea polyphenol is generally used for oxidation resistance on food, the butyl hydroxy anisole and the tea polyphenol are mixed together in a ratio of 3:1 in the multifunctional copper cleaning agent, the salt spray resistance time can reach 14h, and the multifunctional copper cleaning agent has good oxidation resistance and corrosion resistance effects.

Drawings

FIG. 1 shows the effect of the present invention, (a) is a copper device before processing, and (b) is a copper device after processing.

Detailed Description

The following description of the preferred embodiments of the present invention is provided for the purpose of better illustrating the invention and is not intended to limit the invention thereto.

1. Experimental sample (copper device): the copper piece is a common rusty greasy dirt copper sheet.

2. The oil stain removal rate test method comprises the following steps: the method for detecting the surface oil stain mainly comprises the following steps: visual inspection, wiping, optical microscopy. Whether the copper part contains oil stains can be seen by looking at the copper part with eyes and wiping with paper, and the cleanliness of the surface of the workpiece can be seen by an optical microscope.

3. Surface patina content/patina removal rate: calculating according to the oil stain area on the copper surface; surface patina content (initial oil stain area-post-removal oil stain area)/initial oil stain area.

4. Salt spray test: the time to rust was observed under 5% salt spray conditions. The salt spray test for 1 day corresponds to 1 month in the natural environment.