Production process method of electronic-grade cleaning agent in integrated circuit industry

Abstract

The invention belongs to the technical field of electronic chemicals in the integrated circuit industry, and particularly relates to a production process method of an electronic-grade cleaning agent. Comprising the following steps: S1, filtering an alcohol amine solvent through a filter element for later use; the method comprises the following steps: S1, adding part of ultrapure water into a storage tank, adding part of alcohol amine solvent, and adding part of solid additive into the storage tank, so as to form a cycle; the whole batch is fed in three periods, and stirring is started in the feeding process. The dissolvability of the solid raw material is improved by utilizing the dissolution heat release of the organic solvent dissolved in the aqueous solution. And step 2, further, after all the raw materials are added, starting circulation overnight. And step 3 and step 4, further, filtering after complete circulation, and sampling and detecting. The invention provides a production process of an electronic-grade cleaning agent in the integrated circuit industry, which can effectively shorten the production period, improve the granularity index quality of a system and prolong the service life of a filter element.

Description

Technical Field

[0001] The present invention belongs to the technical field of electronic chemicals in the integrated circuit industry, and specifically relates to a production process method of an electronic-grade cleaning agent. Background Art

[0002] Electronic chemicals are indispensable consumables for integrated circuit manufacturing. According to their uses, electronic chemicals can be divided into two categories: general chemicals and functional chemicals. General chemicals are mainly high-purity solvents, such as phosphoric acid, sulfuric acid, hydrofluoric acid, hydrogen peroxide, isopropyl alcohol, NMP, etc.; functional chemicals refer to formulated or compounded chemicals that achieve special functions through compounding methods and meet special process requirements in manufacturing, mainly including developers, stripping solutions, cleaning agents, etching solutions, etc.

[0003] Electronic grade cleaning agents are very important materials in the integrated circuit industry. About 1 / 3 of the chip manufacturing process is the cleaning step, and the quality of the cleaning agent determines the yield of the chip. According to different categories, cleaning agents can be used to remove metal ions, particle size, post-etching residues or post-CMP residues.

[0004] Cleaning agents are compound formulated chemicals based on organic systems. Due to their many ingredients, poor solubility of some solid raw materials and complex systems, they are difficult to produce, have low efficiency and are costly. Summary of the invention

[0005] The present invention provides a production process for an electronic-grade cleaning agent for the integrated circuit industry, which can effectively shorten the production cycle, improve the quality of the system particle size index and increase the service life of a filter element.

[0006] The original production process of cleaning agent: Step 1, feeding (liquid first, then solid); Step 2, stirring and circulation; Step 3, filtering; Step 4, testing and filling. There are problems such as slow solid dissolution, long production cycle, poor particle size index and short filter life. The steps of the present invention are as follows: step 1, filtering and feeding liquid raw materials, and adding solids in batches during the liquid feeding process; step 2, circulation; step 3, filtering; step 4, testing and filling.

[0007] Specific: Step 1, filtering the alcohol amine solvent through a filter element for later use; Step 1: Add some ultrapure water, then some alcohol amine solvent, and then some solid additives into the storage tank, and this is a cycle. The whole batch of materials is added in three cycles, and stirring is turned on during the feeding process. The dissolution heat of the organic solvent in the aqueous solution is used to improve the solubility of the solid raw material.

[0008] The mass ratio of the ultrapure water, the alcohol amine and the solid additive is 800-1000:100-300:100-300.

[0009] Step 2: After all the raw materials are added, the circulation is started overnight to mix all the raw material components.

[0010] Step 3 and step 4: further, filtering and sampling for testing after the circulation is complete.

[0011] In the step 1, the filter element is selected from any one of PP, HDPE or Nylon, and the pore size of the selected filter element is preferably 0.2-0.5 μm.

[0012] The alcoholamine described in step 1 is selected from any one or more combinations of ethanolamine, N-methylethanolamine, monoethanolamine, diethanolamine, triethanolamine, 3-propanolamine, isopropanolamine, cyclohexeneimine, triethylenediamine, morpholine, acrylamide and dimethylacetamide.

[0013] In the step 2, the solid additive is one or more of catechol, resorcinol, gallic acid, pyrogallic acid, tannic acid, 4-mercaptopyridine, L-cysteine, tetrabutylammonium bromide and hydroxyethylidene diphosphonic acid.

[0014] The three-cycle material adding method is to add ultrapure water, alcohol amine solvent and solid additive at least three times to perform cyclic material adding to achieve uniform mixing of the materials.

[0015] The stirring speed is 50-100rpm, and the feeding speed of the added materials is 60-100L / min.

[0016] The present invention has the following beneficial effects: Effect 1: Filtering the liquid raw materials in advance can reduce the particulate impurities in the liquid raw materials, increase the particle size level of the final product, and increase the service life and use cost of the filter element.

[0017] Effect 2: Cross-feeding of solid and liquid raw materials in batches can utilize the heat of dissolution to dissolve the solids and shorten the dissolution time of the solid raw materials.

[0018] Effect three: The stirring step after feeding can be removed, which can shorten the production time and improve the production efficiency.

[0019] The present invention provides a production process method for an electronic-grade cleaning agent, which can shorten production time, improve product quality, and reduce filter elements. The process method is simple and easy to operate, and has good application prospects in the production field of semiconductor formula chemicals. DETAILED DESCRIPTION

[0020] The present invention is described in detail below in conjunction with specific embodiments. This embodiment is implemented based on the technical solution of the present invention, and provides a detailed implementation method and a specific operation process, but the protection scope of the present invention is not limited to the following embodiments.

[0021] Example 1 Step 1: Use Nylon filter element to filter the liquid raw material.

[0022] In the embodiment of the present invention, the selected filter element pore size is 0.2-0.5 μm, and the filter element membrane material is PP or Nylon.

[0023] Step 2: Add some ultrapure water to the storage tank, then add 1 / 3 of the mass of monoethanolamine, morpholine and dimethylacetamide (volume ratio of 3:2:2) mixed organic solvent required by the total formula, and then add 1 / 3 of the mass of pyrogallic acid and hydroxyethylidene diphosphonic acid (mass ratio of 3:2) mixed solid additives required by the total formula, and stir for 60 minutes at a stirring speed of 100 rpm, which is one cycle. The whole batch of materials is added in three cycles. The dissolution heat of the organic solvent dissolved in the aqueous solution is used to improve the solubility of the solid raw materials.

[0024] The mass ratio of the ultrapure water, the organic solvent and the solid additive is 900:200:100.

[0025] Step 2: After all the raw materials are added, the circulation is started overnight to mix the components.

[0026] In the embodiment of the present invention, the cycle time is 12 hours.

[0027] Step 3: Further, after the circulation is complete, the product is filtered and sampled for testing.

[0028] The original production process is: Step 1, adding organic solvent to ultrapure water, and then adding all solid raw materials; Step 2: Start the cycle for 36 hours; Step three: filtering; step three: sampling and testing.

[0029] Example 2 The method and steps are the same as those in Example 1, except that the solid additive is a mixture of catechol and hydroxyethylidene diphosphonic acid (in a mass ratio of 3:2).

[0030] Example 3 The method and steps are the same as those in Example 1, except that the solid additive is a mixture of catechol and L-cysteine ​​(mass ratio is 3:2).

[0031] Example 4 The method and steps are the same as those in Example 1, except that the solid additive is a mixture of catechol and 4-mercaptopyridine (mass ratio is 3:2).

[0032] Example 5 The method and steps are the same as those in Example 1, except that the solid additive is a mixture of tannic acid and hydroxyethylidene diphosphonic acid (in a mass ratio of 3:2).

[0033] Example 6 The method and steps are the same as those in Example 1, except that the solid additive is a mixture of L-cysteine ​​and hydroxyethylidene diphosphonic acid (in a mass ratio of 3:2).

[0034] Comparison of production time of electronic grade cleaning agents

[0035] The original production process takes about 56 hours for one batch, while the production process of the present invention takes 32 hours, and the production cycle of one batch is reduced by about 24 hours.

[0036] Comparison of particle size effects of electronic grade cleaning agents

[0037] The production process of the present invention has a great improvement on the particle size level of the cleaning agent, and the particle size index of different particle sizes is significantly improved. The reason is that the liquid raw material is filtered in advance to remove a large part of the particle impurities, and the change in the solid feeding method also makes the solid dissolve more completely, so that the particle index level in the cleaning agent product is better.

[0038] The particle size of the cleaning agent mainly comes from the solid raw materials, but the solid raw materials used in the production of cleaning agents have poor solubility, so the particle size of the cleaning agent has always been a very important technical indicator. By adding in batches, the solubility of the solid raw materials can be improved by using the heat of dissolution. In addition, adding in batches makes it difficult for the solid raw materials to sink to the bottom and clump, which further improves the dissolution effect and makes the various components mixed more evenly.

[0039] Filter element service life comparison

[0040] Sites ABC are respectively located at the sampling points after the three-stage filter element.

[0041] The production process of the present invention also greatly improves the service life of the filter element of the cleaning agent production device. The reason is that the particle size level is greatly reduced and the solid raw materials are completely dissolved, so that the service life of the filter element at different points of the production device is greatly improved.

[0042] The above embodiments describe the preferred implementation of the present invention, but the present invention is not limited thereto. Within the technical concept of the present invention, the technical solution of the present invention can be subjected to a variety of simple modifications, including the combination of various technical features in any other manner, and these simple modifications and combinations should also be regarded as the contents disclosed by the present invention and belong to the protection scope of the present invention. Therefore, the protection scope of the patent of the present invention shall be subject to the attached claims.

Claims

1. A production process of electronic grade cleaning agent for integrated circuit industry, characterized in that: The steps include: Step 1, filtering the alcohol amine solvent through a filter element for later use; Step 2: Add ultrapure water into the storage tank, then add an organic solvent such as an alcohol amine, an amide or an alicyclic amine, and then add a solid additive, and start stirring during the feeding process; Step 3: After all the raw materials are added, the circulation is started overnight to mix all the raw material components. Step 4: Filter and take samples for testing after the circulation is complete.

2. The production process of electronic grade cleaning agent for integrated circuit industry according to claim 1, characterized in that: In step 1, the filter element is selected from any one of PP, HDPE or Nylon filter elements, and the pore size of the selected filter element is preferably 0.2-0.5 μm.

3. The production process of electronic grade cleaning agent for integrated circuit industry according to claim 1, characterized in that: The alcoholamine described in step 1 is selected from any one or more combinations of ethanolamine, N-methylethanolamine, monoethanolamine, diethanolamine, triethanolamine, 3-propanolamine, isopropanolamine, cyclohexeneimine, triethylenediamine, morpholine, acrylamide and dimethylacetamide.

4. The production process of electronic grade cleaning agent for integrated circuit industry according to claim 1, characterized in that: In the step 2, the solid additive is one or more of catechol, resorcinol, gallic acid, pyrogallic acid, tannic acid, 4-mercaptopyridine, L-cysteine, tetrabutylammonium bromide and hydroxyethylidene diphosphonic acid.

5. The production process of electronic grade cleaning agent for integrated circuit industry according to claim 1, characterized in that: In the step 2, materials are added in batches for mixing.

6. The production process of electronic grade cleaning agent for integrated circuit industry according to claim 5, characterized in that: The method of adding materials in batches is to add ultrapure water, alcoholamine solvent and solid additives at least three times to cyclically add materials to achieve uniform mixing of materials.

7. The production process of electronic grade cleaning agent for integrated circuit industry according to claim 6, characterized in that: The stirring speed is 50-100rpm, and the feeding speed of the added materials is 60-100L / min.

8. The production process of electronic grade cleaning agent for integrated circuit industry according to claim 1, characterized in that: Cycle overnight in step 3.

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