CN101724347A - Chemical mechanical polishing solution - Google Patents
Chemical mechanical polishing solution Download PDFInfo
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- CN101724347A CN101724347A CN200810201030A CN200810201030A CN101724347A CN 101724347 A CN101724347 A CN 101724347A CN 200810201030 A CN200810201030 A CN 200810201030A CN 200810201030 A CN200810201030 A CN 200810201030A CN 101724347 A CN101724347 A CN 101724347A
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Abstract
The invention discloses a chemical mechanical polishing solution which comprises abrasive grains, an oxidizing agent, water and a methyl benzoxazole compound shown as the formula 1, wherein R1 and R2 are individually C1-C4 alkyl groups; and the methyl (CH3) on a benzene ring is any methyl with substituted hydrogen. The chemical mechanical polishing solution can better protect the surface of copper, reduce the generation of corrosion defects and effectively reduce edge over etching (EOE) phenomena of a barrier layer in a polishing process. The formula 1 is disclosed in the specification.
Description
Technical field
The present invention relates to a kind of polishing fluid, be specifically related to a kind of chemical mechanical polishing liquid.
Background technology
In unicircuit is made, the standard of interconnection technique is improving, along with interconnection increase of the number of plies and dwindling of technology characteristics size, requirement to the silicon chip surface planeness is also more and more higher, if there is not the ability of planarization, create complicated on semiconductor crystal wafer and intensive structure is very limited, cmp method CMP is exactly the effective means that can realize the whole silicon wafer planarization.
Along with dwindling of IC device feature size, in the CMP (Chemical Mechanical Polishing) process of blocking layer depression and corrosive are required just to appear suddenly out, simultaneously, edge excessive erosion (EOE) phenomenon has also received concern as the new defective that produces in the technological process.EOE is also referred to as brave tooth, canine tooth and edge crack etching, and the generation of this phenomenon is because the corrosion of copper pattern edge place dielectric materials causes.Owing in the CMP (Chemical Mechanical Polishing) process on blocking layer, can remove dielectric materials and side force is arranged; so the abrasion at dielectric layer edge takes place through regular meeting; this has just caused the edge excessive erosion, may have a negative impact when the edge excessive erosion is serious, and it will become a potential problem.So will be in glossing this phenomenon be reduced to bottom line or with its elimination.
Among the publication WO2008004579, disclose and in polishing process, utilized triazole class compounds protection dielectric substance layer, prevented from dielectric substance layer, to produce the cave because of excessive polishing.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of chemical mechanical polishing liquid in order to overcome edge excessive erosion (EOE) problem that occurs in the barrier polishing process.Chemical mechanical polishing liquid of the present invention can better protecting copper surface, reduces the generation of corrosion default, and can effectively reduce edge excessive erosion (EOE) phenomenon that occurs at copper pattern edge place in the barrier polishing process.
Chemical mechanical polishing liquid of the present invention comprises abrasive grain, oxygenant, water and methyl benzotriazazole compounds as shown in Equation 1;
Wherein, R
1And R
2Alone be C
1-C
4Alkyl; Methyl (CH in the formula 1 on the phenyl ring
3) methyl that has been substituted for any one hydrogen on the phenyl ring.
Described methyl benzotriazazole compounds as shown in Equation 1 is metal inhibitor in the present invention, and is preferable in the formula 1, R
1=methyl, R
2=ethyl; Or R
1=methyl, R
2=propyl group; Or R
1=methyl, R
2=butyl; Or R
1=ethyl, R
2=propyl group; Or R
1=methyl, R
2=methyl; Or R
1=ethyl, R
2=ethyl; Or R
1=propyl group, R
2=propyl group; Or R
1=butyl, R
2=butyl; Better, R
1=methyl, R
2=methyl; Or R
1=ethyl, R
2=ethyl; Or R
1=propyl group, R
2=propyl group; Or R
1=butyl, R
2=butyl.
What the content of described methyl benzotriazazole compounds as shown in Equation 1 was preferable is massfraction 0.1%~1%.Why select 0.1%~1% this scope to be because: when the content of inhibiter less than 0.1% the time, the removal speed of Cu can not be controlled preferably, when content greater than 1% the time, the stability of solution can be affected again.What content was better is 0.15%~0.3%, and in this content range, polishing fluid can better protection copper surface, reduces the generation of corrosion default, and can more effectively reduce edge excessive erosion (EOE) phenomenon that occurs in the barrier polishing process.
Abrasive grain of the present invention is the abrasive grain of this area routine, preferable be selected from silicon-dioxide (as silica sol particles), aluminum oxide, cerium oxide and the polymer beads one or more, better is silica sol particles, what the content of described abrasive grain was preferable is massfraction 5%~20%, and better is massfraction 5~10%; That the particle diameter of described abrasive grain is preferable is 20~120nm, and that better is 20~80nm.
Among the present invention, described oxygenant is the oxygenant of this area routine, can be superoxide, S
2O
6 2-Metal-salt, S
2O
8 2-Metal-salt, KIO
3And KMnO
4In one or more, wherein superoxide can be hydrogen peroxide (H
2O
2), in peroxidation organic acid and the peroxidation mineral acid one or more.Wherein, S
2O
6 2-Metal-salt and S
2O
8 2-Metal-salt be in the chemical field this type of conventional metal-salt, can be ammonium salt or sylvite etc.
In the described oxygenant, best is hydrogen peroxide; What the content of oxygenant was preferable is massfraction 0.3%~1.0%, and better is 0.5%~1.0%.
What the pH value of chemical mechanical polishing liquid of the present invention was preferable is 2~4, and better is 2~3.The pH regulator agent can be various acid and/or alkali, as potassium hydroxide, ammoniacal liquor or nitric acid etc., pH regulator to desirable value is got final product.
Chemical mechanical polishing liquid of the present invention can also comprise some conventional additives of this area, as sterilant, mould inhibitor, wetting agent or dispersion agent etc.
Among the present invention, what described water was preferable is deionized water.The content of described water is the massfraction 100% of supplying polishing fluid.
Chemical mechanical polishing liquid of the present invention can be made by following method: with the mentioned component uniform mixing, adopt the pH regulator agent to adjust the pH value to desirable value then.
Agents useful for same of the present invention and raw material are all commercially available to be got.
Positive progressive effect of the present invention is:
Chemical mechanical polishing liquid of the present invention with as shown in Equation 1 methyl benzotriazazole compounds as metal inhibitor; has excellent corrosion mitigating effect; in polishing process, well protected copper (Cu) surface, by control Cu removal speed effectively reduced occur in the barrier polishing process depression and edge excessive erosion (EOE) phenomenon.
Description of drawings
Fig. 1 is the diagrammatic cross-section of edge excessive erosion (EOE) phenomenon, edge excessive erosion (EOE) is made up of the abrasion of dielectric substance layer and Cu crack etching, wherein, Cu crack etching is meant the damaged bench height of Cu line edge material, and the medium layer abrasion is meant the damaged bench height in medium layer edges of regions place.
Fig. 2 polishes the log (electric current/A)~electromotive force/V figure of blank Cu wafer for the polishing fluid that contains different inhibiter among the effect embodiment 1.
Fig. 3 contains the removal rate diagram of the polishing fluid of different inhibiter to blank Cu wafer among the effect embodiment 1.
Fig. 4 polishes the log (electric current/A)~electromotive force/V figure of blank Cu wafer for the polishing fluid that has different inhibiter content among the effect embodiment 2.
Fig. 5 has the removal rate diagram of the polishing fluid of different inhibiter content to blank Cu wafer among the effect embodiment 2;
Fig. 6 is the polishing fluid that has different inhibiter among the effect embodiment 3 diagrammatic cross-section after to the silicon-dioxide testing wafer polishing of sputter tantalum blocking layer/electro-coppering.
Fig. 7 has the removal rate diagram of the polishing fluid of different abrasive concentrations to blank Cu wafer and blank TEOS wafer among the effect embodiment 4.
Fig. 8 has the removal rate diagram of the polishing fluid of different PH to blank Cu wafer and blank TEOS wafer among the effect embodiment 5.
Embodiment
Further specify the present invention with embodiment below, but the present invention is not limited.
Table 1 has provided the polishing fluid of embodiment 1~4, and by wherein filling a prescription, with the simple uniform mixing of each composition, water is supplied the mass percent 100% of polishing fluid, adopts rare nitric acid or potassium hydroxide to regulate pH afterwards, can make each polishing fluid.Wherein, 1,3-dihydroxymethyl-5,5-methyl hydantoin are sterilant.
The polishing fluid of table 1 embodiment 1-4
Wherein, the 1-N described in the embodiment 1, N (methylol hydroxyethyl) methylamino--methyl benzotriazazole is:
The 1-N described in 2 is executed in enforcement, and N (methylol hydroxypropyl) methylamino--methyl benzotriazazole is:
1-N described in the embodiment 3, N (methylol hydroxyl butyl) methylamino--methyl benzotriazazole is:
1-N described in the embodiment 4, N (hydroxyethyl hydroxypropyl) methylamino--methyl benzotriazazole is:
Following is effect embodiment 1-effect embodiment 5, presses the wherein prescription of each polishing fluid, and with the simple uniform mixing of each composition, water is supplied the mass percent 100% of polishing fluid, adopts rare nitric acid to regulate pH afterwards, can make each polishing fluid.
Effect embodiment 1:
Polishing fluid 1: silica sol particles (particle diameter 45nm): 7%, 1-N, N (dihydroxymethyl) methylamino--methyl benzotriazazole: 0.15%, H
2O
2: 0.1%, PH=3.0;
1-N in the polishing fluid 1, the structural formula of N (dihydroxymethyl) methylamino--methyl benzotriazazole is:
Polishing fluid 2: silica sol particles (particle diameter 45nm): 7%, benzotriazole: 0.15%, H
2O
2: 0.1%, PH=3.0;
Polishing fluid 3: silica sol particles (particle diameter 45nm): 7%, 5-sulfydryl-3-amino-1,2,4 triazoles: 0.15%, H
2O
2: 0.1%, PH=3.0;
Polishing fluid 4: silica sol particles (particle diameter 45nm): 7%, 3-amino-1,2,4 triazoles: 0.15%, H
2O
2: 0.1%, PH=3.0;
Polishing fluid 5: silica sol particles (particle diameter 45nm): 7%, 4-amino-1,2,4 triazoles: 0.15%, H
2O
2: 0.1%, PH=3.0;
Polishing material: blank Cu wafer, polishing condition: 1.5psi, polishing disk rotating speed 70rpm, polishing fluid flow velocity 200ml/min, polishing pad Politex, Logitech PM5 Polisher.
Test condition and method: on CHI600B electrochemical workstation (Shanghai occasion China instrument company), carry out the electrochemical research test, with the platinum electrode is that supporting electrode, saturated calomel electrode are that reference electrode and copper electrode are working electrode, sweep limit-1.0~1.5V, scanning result are as shown in Figure 2.Obtain corrosion current and calculate static etch rate by carrying software analysis, as shown in table 2; Contain polishing speed such as the table 3 and shown in Figure 3 of the polishing fluid of different inhibiter to Cu.
The corrosion current of table 2 polishing fluid 1~5 and static etch rate
The Cu polishing speed of table 3 polishing fluid 1~5
Conclusion: as can be seen by table 3 and Fig. 3, with employing 1-N, N (dihydroxymethyl) methylamino--methyl benzotriazazole is compared as inhibiter (polishing fluid 1), when inhibiter is 5-sulfydryl-3-amino-1,2,4 triazoles (polishing fluid 3), 3-amino-1,2,4 triazoles (polishing fluid 4), 4-amino-1,2, during 4 triazoles (polishing fluid 5), polishing fluid has higher Cu polishing speed, thereby produces the defective of saucerization easily in polishing process.
Effect embodiment 2:
Polishing fluid 6: silica sol particles (particle diameter 45nm): 7%, 1-N, N (dihydroxymethyl) methylamino--methyl benzotriazazole: 0.05%, H
2O
2: 0.1%, PH=3.0;
Polishing fluid 7: silica sol particles (particle diameter 20nm): 7%, 1-N, N (dihydroxymethyl) methylamino--methyl benzotriazazole: 0.10%, H
2O
2: 0.1%, PH=3.0;
Polishing fluid 8: silica sol particles (particle diameter 30nm): 7%, 1-N, N (dihydroxymethyl) methylamino--methyl benzotriazazole: 0.15%, H
2O
2: 0.1%, PH=3.0;
Polishing fluid 9: silica sol particles (particle diameter 80nm): 7%, 1-N, N (dihydroxymethyl) methylamino--methyl benzotriazazole: 0.20%, H
2O
2: 0.1%, PH=3.0;
Polishing fluid 10: silica sol particles (particle diameter 120nm): 7%, 1-N, N (dihydroxymethyl) methylamino--methyl benzotriazazole: 0.30%, H
2O
2: 0.1%, PH=3.0;
Polishing material: blank Cu wafer, polishing condition: 1.5psi, polishing disk rotating speed 70rpm, polishing fluid flow velocity 200ml/min, polishing pad Politex, Logitech PM5 Polisher.
1-N described in the above polishing fluid 6-10, N (dihydroxymethyl) methylamino--methyl benzotriazazole structural formula is:
Test condition and method: on CHI600B electrochemical workstation (Shanghai occasion China instrument company), carry out the electrochemical research test, with the platinum electrode is that supporting electrode, saturated calomel electrode are that reference electrode and copper electrode are working electrode, sweep limit-1.0~1.5V, scanning result are as shown in Figure 4.Obtain corrosion current and calculate static etch rate by carrying software analysis, as shown in table 4; Contain polishing speed such as the table 5 and shown in Figure 5 of the polishing fluid of different content inhibiter to Cu.
The corrosion current of table 4 polishing fluid 6~10 and static etch rate
The Cu polishing speed of table 5 polishing fluid 6~10
Conclusion: along with the increase of inhibiter consumption, the polishing speed of Cu reduces, but the Cu polishing speed is constant substantially after the inhibiter consumption is higher than 0.15%.Associative list 4 can be seen simultaneously, and along with the increase of inhibiter consumption, polishing fluid also reduces gradually to the erosion rate of Cu.
Effect embodiment 3:
Polishing fluid 11: silica sol particles (particle diameter 45nm): 7%, 1-N, N (dihydroxy ethyl) methylamino--methyl benzotriazazole (as follows): 0.15%, H
2O
2: 0.5%, PH=3.0;
Polishing fluid 12: silica sol particles (particle diameter 45nm): 7%, 3-amino-1,2,4 triazoles: 0.15%, H
2O
2: 0.1%, PH=3.0;
Polishing fluid 13: silica sol particles (particle diameter 45nm): 7%, benzotriazole: 0.15%, H
2O
2: 0.5%, PH=3.0;
Polishing material: blank Cu wafer, blank TEOS wafer, the silicon-dioxide testing wafer of sputter tantalum blocking layer/electro-coppering; Polishing condition: 1.5psi, polishing disk rotating speed 70rpm, polishing pad Politex, polishing fluid flow velocity 200ml/min, Logitech LP50 Polisher.Topography measurement: scanning atomic force microscope (AFM), experimental result such as table 6 and shown in Figure 6:
In the table 6, it is the result who draws by blank testing Cu wafer that Cu removes speed; It is the result who draws by blank testing TEOS wafer that TEOS removes speed; Depression, Cu seam etching and TEOS abrasion are the results who draws by the silicon-dioxide testing wafer of testing sputter tantalum blocking layer/electro-coppering; Wherein, depression, Cu seam etching and TEOS abrasive data are the data that polishing drew after a minute.
The influence of 11~13 pairs of edge excessive erosion of table 6 polishing fluid (EOE)
Conclusion:, make each polishing fluid obtain proximate blank Cu wafer and remove speed earlier by using the hydrogen peroxide of different concns.The silicon-dioxide testing wafer of sputter tantalum blocking layer/electro-coppering is owing to figuratum reason; so it is inequality with the polishing removal speed that blank wafer obtained that polishing fluid polishes the removal speed of this wafer acquisition; by Fig. 6 and table 6 as can be seen; it is inequality that polishing fluid polishes the wafer topography that the silicon-dioxide testing wafer of sputter tantalum blocking layer/electro-coppering obtained; polishing fluid 11 adopts 1-N; N (dihydroxy ethyl) methylamino--methyl benzotriazazole compounds as the metal inhibitor better protecting Cu surface; revised the saucerization that the Cu surface produces, made 720 before polishing
Reduce to 444
Also reduced simultaneously the corrosion situation at Cu edge, Cu seam etching only is 69
This has reduced edge excessive erosion (EOE) phenomenon, has obtained wafer topography preferably.
Effect embodiment 4:
Polishing fluid 14: silica sol particles (particle diameter 45nm): 2%, 1-N, N (dihydroxymethyl) methylamino--methyl benzotriazazole: 0.15%, H
2O
2: 0.5%, PH=3.0;
Polishing fluid 15: silica sol particles (particle diameter 45nm): 5%, 1-N, N (dihydroxymethyl) methylamino--methyl benzotriazazole: 0.15%, H
2O
2: 0.5%, PH=3.0;
1-N described in the above polishing fluid 14,15, N (dihydroxymethyl) methylamino--methyl benzotriazazole structural formula is:
Polishing fluid 16: silica sol particles (particle diameter 45nm): 7%, 1-N, N (dihydroxy ethyl) methylamino--methyl benzotriazazole: 0.15%, H
2O
2: 0.5%, PH=3.0;
1-N described in the polishing fluid 16, N (dihydroxy ethyl) methylamino--methyl benzotriazazole structural formula is:
Polishing fluid 17: silica sol particles (particle diameter 45nm): 10%, 1-N, N (dihydroxymethyl) methylamino--methyl benzotriazazole: 0.15%, H
2O
2: 0.5%, PH=3.0;
1-N described in the polishing fluid 17, N (dihydroxymethyl) methylamino--methyl benzotriazazole structural formula is:
Polishing fluid 18: silica sol particles (particle diameter 45nm): 15%, 1-N, N (dihydroxypropyl) methylamino--methyl benzotriazazole: 0.15%, H
2O
2: 0.5%, PH=3.0;
1-N described in the polishing fluid 18, the structural formula of N (dihydroxypropyl) methylamino--methyl benzotriazazole is:
Polishing fluid 19: silica sol particles (particle diameter 45nm): 20%, 1-N, N (dihydroxy butyl) methylamino--methyl benzotriazazole: 0.15%, H
2O
2: 0.5%, PH=3.0;
1-N described in the polishing fluid 19, the structural formula of N (dihydroxy butyl) methylamino--methyl benzotriazazole is:
Polishing material: blank Cu wafer, blank TEOS wafer, the silicon-dioxide testing wafer of sputter tantalum blocking layer/electro-coppering; Polishing condition: 1.5psi, polishing disk rotating speed 70rpm, polishing pad Politex, polishing fluid flow velocity 200ml/min, Logitech LP50 Polisher.Topography measurement: scanning atomic force microscope (AFM), experimental result such as table 7 and shown in Figure 7:
In the table 7, it is the result who draws by blank testing Cu wafer that Cu removes speed; It is the result who draws by blank testing TEOS wafer that TEOS removes speed; Depression, Cu seam etching and TEOS abrasion are the results who draws by the silicon-dioxide testing wafer of testing sputter tantalum blocking layer/electro-coppering; Wherein, depression, Cu seam etching and TEOS abrasive data are the data that polishing drew after a minute.
The influence of 14~19 pairs of edge excessive erosion of table 7 polishing fluid (EOE)
Conclusion: along with the increase of abrasive grain concentration, polishing fluid increases the removal speed of TEOS, and when abrasive concentration increased to 7%, the removal speed of Cu was constant substantially, and Cu seam etching increases gradually.From the result of table 7, abrasive material content is 5~10% o'clock, and polishing fluid shows moderate polishing speed and lower Cu seam etching.
Effect embodiment 5:
Polishing fluid 20: silica sol particles (particle diameter 45nm): 7%, 1-N, N (dihydroxymethyl) methylamino--methyl benzotriazazole: 0.15%, H
2O
2: 0.5%, PH=2.0;
Polishing fluid 21: silica sol particles (particle diameter 45nm): 7%, 1-N, N (dihydroxymethyl) methylamino--methyl benzotriazazole: 0.15%, H
2O
2: 0.5%, PH=3.0;
Polishing fluid 22: silica sol particles (particle diameter 45nm): 7%, 1-N, N (dihydroxymethyl) methylamino--methyl benzotriazazole: 0.15%, H
2O
2: 0.5%, PH=4.0;
Polishing fluid 23: silica sol particles (particle diameter 45nm): 7%, 1-N, N (dihydroxymethyl) methylamino--methyl benzotriazazole: 0.15%, H
2O
2: 0.5%, PH=5.0;
Polishing fluid 24: silica sol particles (particle diameter 45nm): 7%, 1-N, N (dihydroxymethyl) methylamino--methyl benzotriazazole: 0.15%, H
2O
2: 0.5%, PH=7.0;
1-N described in the above-mentioned polishing fluid 20-24, the structural formula of N (dihydroxymethyl) methylamino--methyl benzotriazazole is:
Polishing material: blank Cu wafer, blank TEOS wafer, the silicon-dioxide testing wafer of sputter tantalum blocking layer/electro-coppering; Polishing condition: 1.5psi, polishing disk rotating speed 70rpm, polishing pad Politex, polishing fluid flow velocity 200ml/min, Logitech LP50 Polisher.Topography measurement: scanning atomic force microscope (AFM), experimental result such as table 8 and shown in Figure 8; In the table 8, it is the result who draws by blank testing Cu wafer that Cu removes speed; It is the result who draws by blank testing TEOS wafer that TEOS removes speed; Depression, Cu seam etching and TEOS abrasion are the results who draws by the silicon-dioxide testing wafer of testing sputter tantalum blocking layer/electro-coppering; Wherein, depression, Cu seam etching and TEOS abrasive data are the data that polishing drew after a minute.
The influence of 20~24 pairs of edge excessive erosion of table 8 polishing fluid (EOE)
Conclusion: along with the increase of pH value, polishing fluid descends to the removal speed of TEOS, and the removal speed influence of Cu is little, and polishing fluid will produce higher depression and lower Cu seam etching.Therefore from table 8 and Fig. 8 as seen, what the pH of polishing fluid was preferable is 2~4, and better is 2~3.
Claims (11)
1. chemical mechanical polishing liquid, it is characterized in that: it comprises abrasive grain, oxygenant, water and methyl benzotriazazole compounds as shown in Equation 1;
Formula 1
Wherein, R
1And R
2Alone be C
1-C
4Alkyl; Methyl in the formula 1 on the phenyl ring is the methyl that any one hydrogen has been substituted on the phenyl ring.
2. chemical mechanical polishing liquid as claimed in claim 1 is characterized in that: in the described methyl benzotriazazole compounds as shown in Equation 1, and R
1=methyl, R
2=ethyl; Or R
1=methyl, R
2=propyl group; Or R
1=methyl, R
2=butyl; Or R
1=ethyl, R
2=propyl group; Or R
1=methyl, R
2=methyl; Or R
1=ethyl, R
2Ethyl; Or R
1=propyl group, R
2=propyl group; Or R
1=butyl, R
2Butyl.
3. chemical mechanical polishing liquid as claimed in claim 1 is characterized in that: the massfraction of described methyl benzotriazazole compounds as shown in Equation 1 is 0.1%~1%.
4. chemical mechanical polishing liquid as claimed in claim 3 is characterized in that: the massfraction of described methyl benzotriazazole compounds as shown in Equation 1 is 0.15%~0.3%.
5. chemical mechanical polishing liquid as claimed in claim 1 is characterized in that: described abrasive grain is selected from one or more in silicon-dioxide, aluminum oxide, cerium oxide and the polymer beads.
6. chemical mechanical polishing liquid as claimed in claim 1 is characterized in that: the content of described abrasive grain is massfraction 5%~20%.
7. chemical mechanical polishing liquid as claimed in claim 1 is characterized in that: the particle diameter of described abrasive grain is 20~120nm.
8. chemical mechanical polishing liquid as claimed in claim 1 is characterized in that: described oxygenant is superoxide, S
2O
6 2-Metal-salt, S
2O
8 2-Metal-salt, KIO
3And KMnO
4In one or more.
9. chemical mechanical polishing liquid as claimed in claim 8 is characterized in that: described superoxide is one or more in hydrogen peroxide, peroxidation organic acid and the peroxidation mineral acid.
10. chemical mechanical polishing liquid as claimed in claim 1 is characterized in that: the content of described oxygenant is massfraction 0.3%~1.0%.
11. chemical mechanical polishing liquid as claimed in claim 1 is characterized in that: the pH value of described chemical mechanical polishing liquid is 2~4.
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CN104152906A (en) * | 2014-07-22 | 2014-11-19 | 清华大学 | Polishing solution for machining ultra-smooth stainless steel surface and application of polishing solution |
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