CMP polishing solution for stainless steel fine polishing orange peel removal and preparation method thereof

Abstract

The invention relates to the technical field of stainless steel polishing abrasives, in particular to a CMP polishing solution for stainless steel fine polishing orange peel removal and a preparation method thereof.The polishing solution is prepared from 1%-20% Wt of abrasives, 0.1%-10% Wt of oxidizing agents, 0.1%-10% Wt of chelating agents, 1%-20% Wt of humectants, 0.1%-10% Wt of corrosion inhibitors and the balance water. The content of the brightening agent is 0.1%-10% Wt, the balance is deionized water, the pH value of the polishing solution is 2-5, the polishing rate is 1 micron / min, and the optimal surface roughness Sa can reach 2 nm or below. According to the polishing solution for stainless steel fine polishing, the pH value of the slurry is 2-5, the polishing rate is 1 micron / min, the optimal surface roughness Sa can reach 2 nm or below, the polished surface is free of orange peel, the surface precision is high, the polishing solution is high in universality to used equipment, the used raw materials are easy to treat, no pollution is caused to the environment, the production process is simple and convenient, and industrialization is easy.

Description

Technical Field

[0001] The present invention relates to the technical field of stainless steel polishing abrasives, and specifically to a CMP polishing liquid for removing orange peel during the fine polishing of stainless steel and a preparation method thereof. Background Art

[0002] Stainless steel is short for corrosion-resistant stainless steel. Steel types that are resistant to weak corrosive media such as air, steam, and water or have corrosion resistance are called stainless steel; while steel types that are resistant to chemical corrosive media (chemical etching such as acids, alkalis, and salts) are called acid-resistant steel. According to the definition in GB / T20878-2007, stainless steel is mainly characterized by corrosion resistance and oxidation resistance, and the chromium content is at least 10.5%, and the maximum carbon content does not exceed 1.2%. Stainless steel materials have good corrosion resistance, high temperature resistance, and wear resistance, and are also malleable with a beautiful smooth surface, and are widely used in industry and daily life.

[0003] Since the patent on chemical polishing of stainless steel appeared in the early 1940s, numerous scholars at home and abroad have conducted in-depth and extensive research on the polishing technology of stainless steel surfaces. The main polishing methods include: mechanical polishing, chemical polishing, electrolytic polishing, and chemical mechanical polishing, etc. The slurry pH value of conventional stainless steel polishing liquids is basically acidic, and the polishing effect can reach the best under acidic conditions. In current stainless steel polishing technology, the most difficult problem to overcome is the orange peel problem that appears on the surface after polishing. The reason is that surface wrinkles are caused by the wear of the polishing pad during the polishing process, or under the action of abrasives, oxidants, and chelating agents, the mechanical action and chemical action do not match. This problem is currently one of the most difficult problems to overcome in the stainless steel field. Summary of the Invention

[0004] Aiming at the deficiencies of the prior art, the present invention provides a CMP polishing liquid for removing orange peel during the fine polishing of stainless steel and a preparation method thereof, so as to solve the problems of orange peel on the surface after stainless steel polishing, slow polishing rate, and high requirements for equipment by the slurry in the prior art.

[0005] In order to achieve the above object, the following technical solutions are provided:

[0006] A CMP polishing liquid for removing orange peel during the fine polishing of stainless steel, characterized in that the polishing liquid is composed of the following raw materials: the abrasive content is 1%-20% Wt, the oxidant content is 0.1%-10% Wt, the chelating agent content is 0.1%-10% Wt, the humectant content is 1%-20% Wt, the corrosion inhibitor content is 0.1%-10% Wt, the brightening agent content is 0.1%-10% Wt, and the balance is deionized water. And the pH of the polishing liquid is 2-5, the polishing rate is 1um / min, and the optimal surface roughness Sa can reach below 2nm.

[0007] Preferably, the abrasive is one or more of silica, alumina, cerium oxide, zirconium oxide, silicon carbide, manganese dioxide, and chromium oxide.

[0008] Preferably, the oxidizing agent is one or more of potassium permanganate, potassium manganate, potassium ferrate, potassium periodate, potassium iodate, hydrogen peroxide, and persulfates such as potassium persulfate.

[0009] Preferably, the chelating agent is one or more of citric acid, glycine, malic acid, ethylenediaminetetraacetic acid, disodium ethylenediaminetetraacetate, nitrilotriacetic acid, and tetrasodium hydroxyethylidene diphosphonate.

[0010] Preferably, the humectant is one or more of polyglycerol-10, glycerol, butanediol, ethylene glycol, polyethylene glycol, propylene glycol, sorbitol, and xylitol.

[0011] Preferably, the corrosion inhibitor is one or more of sodium silicate, tolylthiourea, propyl sulfide, benzotriazole, dipentylamine, formaldehyde, and p-thiocresol.

[0012] Preferably, the brightening agent is one or more of thiourea, aluminum nitrate, benzalacetone, nonylphenol polyoxyethylene ether, anhydrous sodium silicate, sodium dodecylsulfonate, and butynediol.

[0013] A method for preparing a CMP polishing liquid for precision polishing of stainless steel to remove orange peel, characterized by comprising the following steps:

[0014] Step 1: Weigh 0.1%-10% Wt of the oxidizing agent, 0.1%-10% Wt of the chelating agent, 0.1%-10% Wt of the corrosion inhibitor, and 0.1%-10% Wt of the brightening agent, add them to 45%-90% of deionized water, and stir evenly.

[0015] Step 2: Weigh 1%-20% Wt of the humectant and add it to the solution obtained in Step 1, and stir evenly.

[0016] Step 3: Weigh 1%-20% Wt of the abrasive and add it to the solution obtained in Step 2, stir evenly, perform ball milling by a planetary ball mill, and filter through a 400-mesh stainless steel sieve.

[0017] Step 4: Stir the abrasive slurry solution obtained in Step 3 evenly, with a pH of 2-5, to obtain the polishing liquid for precision polishing of stainless steel to remove orange peel.

[0018] The beneficial effects of the present invention are as follows: The polishing liquid for precision polishing of stainless steel of the present invention has a slurry pH of 2-5, a polishing rate of 1 um / min, the optimal surface roughness Sa can reach below 2 nm, there is no orange peel on the surface after polishing, the surface precision is high, the polishing liquid has high versatility for the equipment used, the raw materials used are easy to handle, there is no pollution to the environment, the production process is simple, and it is easy to industrialize. Description of the Drawings

[0019] Figure 1 This is the 1# surface roughness picture in Embodiment 1 of the present invention;

[0020] Figure 2 This is the 2# surface roughness picture in Embodiment 1 of the present invention;

[0021] Figure 3 This is the 3# surface roughness picture in Embodiment 1 of the present invention;

[0022] Figure 4 This is the 4# surface roughness picture in Embodiment 2 of the present invention;

[0023] Figure 5 This is the 5# surface roughness picture in Embodiment 2 of the present invention;

[0024] Figure 6 This is the 6# surface roughness picture in Embodiment 2 of the present invention;

[0025] Figure 7 This is the 7# surface roughness picture in Embodiment 3 of the present invention;

[0026] Figure 8 This is the 8# surface roughness picture in Embodiment 3 of the present invention;

[0027] Figure 9 This is the 9# surface roughness picture in Embodiment 3 of the present invention;

[0028] Figure 10 This is the 10# surface roughness picture in Embodiment 4 of the present invention;

[0029] Figure 11 This is the 11# surface roughness picture in Embodiment 4 of the present invention;

[0030] Figure 12 This is the 12# surface roughness picture in Embodiment 4 of the present invention;

[0031] Figure 13 This is the 13# surface roughness picture in Embodiment 5 of the present invention;

[0032] Figure 14 This is the 14# surface roughness picture in Embodiment 5 of the present invention;

[0033] Figure 15 This is the 15# surface roughness picture in Embodiment 5 of the present invention;

[0034] Figure 16 This is the 16# surface roughness picture in Embodiment 6 of the present invention;

[0035] Figure 17 It is the surface roughness picture of No. 17 in Embodiment 6 of the present invention;

[0036] Figure 18 It is the surface roughness picture of No. 18 in Embodiment 6 of the present invention;

[0037] Figure 19 It is the surface roughness picture in Embodiment 7 of the present invention;

[0038] Figure 20 It is the comparison of orange peel before and after polishing the stainless steel parts of the present invention. Detailed implementation manners

[0039] Next, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.

[0040] The prepared stainless steel fine polishing and orange peel removing polishing liquid, and all embodiments are compared and tested according to the following conditions and polishing parameters:

[0041]

[0042]

[0043] Embodiment 1

[0044] The stainless steel polishing liquid prepared in this embodiment has the following preparation method:

[0045] Step 1: Weigh 5% Wt of potassium iodate, 5% Wt of citric acid, 5% Wt of propyl sulfide, and 5% Wt of thiourea, add them to 70% deionized water, and stir evenly;

[0046] Step 2: Weigh 10% Wt of polyglycerol-10 and add it to the solution in Step 1, and stir evenly;

[0047] Step 3: Weigh 1% of abrasive and add it to the solution obtained in Step 2 as No. 1, weigh 10% of abrasive and add it to the solution obtained in Step 2 as No. 2, weigh 10% of abrasive and add it to the solution obtained in Step 2 as No. 3 (the abrasive is uniformly pre-tested with 0.2um silicon carbide first), stir evenly, perform ball milling through a planetary ball mill, and filter with a 400-mesh stainless steel sieve;

[0048] Step 4: Stir the abrasive slurry solution obtained in Step 3 evenly, with a pH of 2-5, to obtain the stainless steel fine polishing and orange peel removing polishing liquid.

[0049] The results show that: for Sample 1 of Example 1, the removal rate is 0.2 um / min and the surface roughness Sa is 5.266 nm; for Sample 2, the removal rate is 0.9 μm / min and the surface roughness Sa is 1.906 nm; for Sample 3, the removal rate is 2.1 μm / min and the surface roughness Sa is 5.004 nm.

[0050] Example 2

[0051] The stainless steel polishing solution prepared in this example is prepared by the following method:

[0052] Step 1: Weigh 0.1% Wt of Oxidant 4#; weigh 5% Wt of Oxidant 5#; weigh 10% Wt of Oxidant 6# (the oxidant is uniformly tried with hydrogen peroxide first), 5% Wt of glycine, 5% Wt of benzotriazole, 5% Wt of aluminum nitrate, and add them to 65% deionized water, and stir evenly;

[0053] Step 2: Weigh 10% Wt of glycerol and add it to the solution obtained in Step 1, and stir evenly;

[0054] Step 3: Weigh 10% Wt of silicon dioxide and add it to the solution obtained in Step 2, stir evenly, perform ball milling with a planetary ball mill, and filter through a 400-mesh stainless steel sieve;

[0055] Step 4: Stir the abrasive slurry solution obtained in Step 3 evenly, with a pH of 2 - 5, to obtain the stainless steel fine polishing solution for removing orange peel.

[0056] The results show that: for Sample 4# of Example 2, the removal rate is 0.3 um / min and the surface roughness Sa is 3.2 nm; for Sample 5#, the removal rate is 0.7 μm / min and the surface roughness Sa is 3.215 nm; for Sample 6#, the removal rate is 0.6 μm / min and the surface roughness Sa is 3.851 nm.

[0057] Example 3

[0058] The stainless steel polishing solution prepared in this example is prepared by the following method:

[0059] Step 1: Weigh 5% Wt of potassium permanganate, weigh 0.1% Wt of Chelating Agent 7#; weigh 5% Wt of Chelating Agent 8#; weigh 10% Wt of Chelating Agent 9# (the chelating agent is uniformly tried with malic acid first), 5% Wt of tolylthiourea, 5% Wt of nonylphenol polyoxyethylene ether, and add them to 45 - 90% deionized water, and stir evenly;

[0060] Step 2: Weigh 10% Wt of butanediol and add it to the solution obtained in Step 1, and stir evenly;

[0061] Step 3: Weigh 10% Wt of cerium oxide and add it to the solution obtained in Step 2. Stir evenly, perform ball milling using a planetary ball mill, and filter through a 400-mesh stainless steel sieve;

[0062] Step 4: Stir the abrasive slurry solution obtained in Step 3 evenly until the pH is 2 - 5 to obtain the stainless steel fine polishing anti-orange peel polishing liquid.

[0063] The results show that: for sample 7# in Example 3, the removal rate is 0.6 um / min and the surface roughness Sa is 3.179 nm; for sample 8#, the removal rate is 0.7 μm / min and the surface roughness Sa is 3.274 nm; for sample 9#, the removal rate is 0.6 μm / min and the surface roughness Sa is 3.116 nm.

[0064] Example 4

[0065] The preparation method of the stainless steel polishing liquid prepared in this example is as follows:

[0066] Step 1: Weigh 5% Wt of potassium manganate, 5% Wt of ethylenediaminetetraacetic acid, weigh 0.1% Wt of corrosion inhibitor 10#; weigh 5% Wt of corrosion inhibitor 11#; weigh 10% Wt of corrosion inhibitor 12# (the corrosion inhibitor is uniformly tried with dipentylamine first), 5% Wt of benzylideneacetone, and add them to 65% deionized water, and stir evenly;

[0067] Step 2: Weigh 10% Wt of ethylene glycol and add it to the solution in Step 1, and stir evenly;

[0068] Step 3: Weigh 10% Wt of zirconia and add it to the solution obtained in Step 2. Stir evenly, perform ball milling using a planetary ball mill, and filter through a 400-mesh stainless steel sieve;

[0069] Step 4: Stir the abrasive slurry solution obtained in Step 3 evenly until the pH is 2 - 5 to obtain the stainless steel fine polishing anti-orange peel polishing liquid.

[0070] The results show that: for sample 10# in Example 4, the removal rate is 0.4 um / min and the surface roughness Sa is 5.319 nm; for sample 11#, the removal rate is 0.5 μm / min and the surface roughness Sa is 4.107 nm; for sample 12#, the removal rate is 0.45 μm / min and the surface roughness Sa is 6.196 nm.

[0071] Example 5

[0072] The preparation method of the stainless steel polishing liquid prepared in this example is as follows:

[0073] Step 1: Weigh 5% Wt of potassium ferrate, 5% Wt of disodium ethylenediaminetetraacetate, 5% Wt of formaldehyde, and 0.1% Wt of brightener No. 13; weigh 5% Wt of brightener No. 14; weigh 10% Wt of brightener No. 15 (the brightener is uniformly tried with sodium dodecyl sulfonate first), and add them to 65% deionized water and stir evenly.

[0074] Step 2: Weigh 10% Wt of polyethylene glycol and add it to the solution in Step 1, and stir evenly.

[0075] Step 3: Weigh 10% Wt of silicon carbide micropowder and add it to the solution obtained in Step 2, stir evenly, perform ball milling with a planetary ball mill, and filter through a 400-mesh stainless steel sieve.

[0076] Step 4: Stir the abrasive slurry solution obtained in Step 3 evenly, with a pH of 2 - 5, to obtain the stainless steel fine polishing anti-orange peel polishing liquid.

[0077] The results show that: for sample No. 10 in Example 5, the removal rate is 5.2 um / min, and the surface roughness Sa is 17.105 nm; for sample No. 11, the removal rate is 5.4 μm / min, and the surface roughness Sa is 16.603 nm; for sample No. 12, the removal rate is 5.6 μm / min, and the surface roughness Sa is 17.747 nm.

[0078] Example 6

[0079] The preparation method of the stainless steel polishing liquid prepared in this example is as follows:

[0080] Step 1: Weigh 5 Wt of potassium persulfate, 5% Wt of tetrasodium hydroxyethylidene diphosphonate, 5% Wt of p-thiocresol, 5% Wt of butynediol, add them to 65% deionized water, and stir evenly.

[0081] Step 2: Weigh 1% Wt of humectant No. 16; weigh 10% Wt of humectant No. 17; weigh 20% Wt of humectant No. 18 (the humectant is uniformly tried with propylene glycol first) and add them to the solution in Step 1, and stir evenly.

[0082] Step 3: Weigh 10% Wt of silicon carbide and add it to the solution obtained in Step 2, stir evenly, perform ball milling with a planetary ball mill, and filter through a 400-mesh stainless steel sieve.

[0083] Step 4: Stir the abrasive slurry solution obtained in Step 3 evenly, with a pH of 2 - 5, to obtain the stainless steel fine polishing anti-orange peel polishing liquid.

[0084] The results show that: for sample 16# of Example 6, the removal rate is 0.8 um / min and the surface roughness Sa is 11.767 nm; for sample 17#, the removal rate is 0.7 μm / min and the surface roughness Sa is 10.430 nm; for sample 18#, the removal rate is 0.8 μm / min and the surface roughness Sa is 10.458 nm.

[0085] Example 7

[0086] The stainless steel polishing liquid prepared in this example is prepared by the following method:

[0087] Step 1: Weigh 5Wt of potassium periodate, 5%Wt of nitrilotriacetic acid, 5%Wt of benzotriazole, and 5%Wt of anhydrous sodium silicate, add them to 65% of deionized water, and stir evenly.

[0088] Step 2: Weigh 10%Wt of sorbitol and add it to the solution obtained in Step 1, and stir evenly.

[0089] Step 3: Weigh 10%Wt of alumina and add it to the solution obtained in Step 2, stir evenly, perform ball milling with a planetary ball mill, and filter through a 400-mesh stainless steel sieve.

[0090] Step 4: Stir the abrasive slurry obtained in Step 3 evenly, with a pH of 2 - 5, to obtain the stainless steel fine polishing liquid for removing orange peel.

[0091] The results show that: for the samples of Example 6, the removal rate is 1 um / min and the surface roughness Sa is 1.7 nm.

[0092] The comparative test data of the examples are as follows:

[0093]

[0094]

[0095] Comparative Examples and Analysis of Test Results: Combining the three samples of Example 1, it can be clearly seen that as the abrasive addition amount gradually increases, the polishing rate gradually increases, and the surface roughness shows a curve of first decreasing and then increasing. The optimal abrasive addition amount is selected as 10%; combining the three samples of Example 2, it can be seen that as the oxidant content gradually increases, the polishing rate first increases and then decreases, and the change in the Sa value of the surface roughness is not significant. The optimal oxidant addition amount is selected as 5%; for the three samples of Example 3, it can be seen that as the chelating agent content gradually increases, the polishing rate first increases and then decreases, and the change in the Sa value of the surface roughness is not significant. Therefore, the optimal chelating agent addition amount is selected as 5%; for the three samples of Example 4, it can be seen that as the corrosion inhibitor content gradually increases, the polishing rate first increases and then decreases, and the Sa value of the surface roughness first decreases and then increases. Therefore, the optimal corrosion inhibitor addition amount is selected as 5%; for the three samples of Example 5, it can be seen that as the brightening agent content gradually increases, the polishing rate changes little, and the Sa value of the surface roughness first decreases and then increases. Therefore, the optimal brightening agent addition amount is selected as 5%; in the three samples of Example 6, it can be seen that as the humectant content increases, it has little effect on the polishing rate and surface roughness. Therefore, the optimal humectant addition amount is selected as 1%; for the analysis of the abrasive type, the polishing rate of silicon carbide micropowder is the fastest, but scratches will appear. The polishing rates of zirconia, etc. can meet the requirements, but the surface roughness is high. Considering both the bonding rate and surface roughness, alumina is the best choice for the abrasive; comprehensively comparing the 19 samples, the sample with the best performance is Sample 19, Example 7, with a polishing rate MRR of 1 μm / min, a surface roughness Sa of 1.7 nm, and the orange peel problem can be quickly removed after polishing.

[0096] For those skilled in the art, it is obvious that the present invention is not limited to the details of the above exemplary embodiments, and without departing from the spirit or basic characteristics of the present invention, the present invention can be implemented in other specific forms. Therefore, from any point of view, the embodiments should be regarded as exemplary and non-limiting. The scope of the present invention is defined by the appended claims rather than the above description. Therefore, all changes falling within the meaning and scope of the equivalent elements of the claims are intended to be included in the present invention. Any reference signs in the claims should not be regarded as limiting the claims involved.

Claims

1. A CMP polishing liquid for removing orange peel in the fine polishing of stainless steel, characterized in that, The polishing liquid is composed of the following raw materials: the abrasive content is 1%-20% Wt, the oxidant content is 0.1%-10% Wt, the chelating agent content is 0.1%-10% Wt, the humectant content is 1%-20% Wt, the corrosion inhibitor content is 0.1%-10% Wt, the brightening agent content is 0.1%-10% Wt, and the balance is deionized water. The pH of the polishing liquid is 2-5, the polishing rate is 1 um / min, and the surface roughness Sa is less than 2 nm.

2. The CMP polishing liquid for removing orange peel in the fine polishing of stainless steel according to claim 1, wherein: The abrasive is one or more of silica, alumina, cerium oxide, zirconium oxide, silicon carbide, manganese dioxide, and chromium oxide.

3. The CMP polishing liquid for removing orange peel in the fine polishing of stainless steel according to claim 1, wherein: The oxidant is one or more of potassium permanganate, potassium manganate, potassium ferrate, potassium periodate, potassium iodate, hydrogen peroxide, and persulfates such as potassium persulfate.

4. A CMP polishing liquid for removing orange peel in the fine polishing of stainless steel according to claim 1, characterized in that: The chelating agent is one or more of citric acid, glycine, malic acid, ethylenediaminetetraacetic acid, disodium ethylenediaminetetraacetate, nitrilotriacetic acid, and tetrasodium hydroxyethylidene diphosphonate.

5. A CMP polishing liquid for removing orange peel in the fine polishing of stainless steel according to claim 1, characterized in that: The humectant is one or more of polyglycerol-10, glycerol, butanediol, ethylene glycol, polyethylene glycol, propylene glycol, sorbitol, and xylitol.

6. The CMP polishing liquid for precisely polishing stainless steel to remove orange peel according to claim 1, wherein: The corrosion inhibitor is one or more of sodium silicate, tolylthiourea, propyl sulfide, benzotriazole, dipentylamine, formaldehyde, and p-thiocresol.

7. A CMP polishing liquid for removing orange peel in the fine polishing of stainless steel according to claim 1, characterized in that: The brightening agent is one or more of thiourea, aluminum nitrate, benzalacetone, nonylphenol polyoxyethylene ether, anhydrous sodium silicate, sodium dodecylsulfonate, and butynediol.

8. A preparation method of a CMP polishing liquid for removing orange peel in the fine polishing of stainless steel, characterized in that, It includes the following steps: Step (1): Weigh 0.1%-10% Wt of the oxidant, 0.1%-10% Wt of the chelating agent, 0.1%-10% Wt of the corrosion inhibitor, and 0.1%-10% Wt of the brightening agent, add them to 45%-90% of deionized water, and stir evenly. Step (2): Weigh 1%-20% Wt of the humectant and add it to the solution in step (1), and stir evenly. Step (3): Weigh 1%-20% Wt of the abrasive and add it to the solution obtained in step (2), stir evenly, perform ball milling by a planetary ball mill, and filter through a 400-mesh stainless steel sieve. Step (4): Stir the abrasive slurry solution obtained in step (3) evenly, with a pH of 2-5, to obtain the stainless steel fine polishing liquid for removing orange peel.

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