CN114940866B - Chemical mechanical polishing liquid for silicon wafer, preparation method and application thereof - Google Patents
Chemical mechanical polishing liquid for silicon wafer, preparation method and application thereof Download PDFInfo
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- CN114940866B CN114940866B CN202210756342.0A CN202210756342A CN114940866B CN 114940866 B CN114940866 B CN 114940866B CN 202210756342 A CN202210756342 A CN 202210756342A CN 114940866 B CN114940866 B CN 114940866B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B37/00—Lapping machines or devices; Accessories
- B24B37/04—Lapping machines or devices; Accessories designed for working plane surfaces
- B24B37/042—Lapping machines or devices; Accessories designed for working plane surfaces operating processes therefor
- B24B37/044—Lapping machines or devices; Accessories designed for working plane surfaces operating processes therefor characterised by the composition of the lapping agent
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention provides a chemical mechanical polishing solution for a silicon wafer, a preparation method and application, wherein the polishing solution comprises the following components in percentage by mass: 5% -15% of high-purity silica sol, 0.01% -0.5% of viscosity regulator, 0.1% -0.5% of pH regulator, 0.001% -0.05% of surfactant and the balance of water. The viscosity of the polishing liquid can be effectively improved by the viscosity regulator, a thicker pressure film is formed during polishing, and the number of defects and the roughness of the surface of the wafer are reduced.
Description
Technical Field
The invention relates to the technical field of Chemical Mechanical Polishing (CMP), in particular to a chemical mechanical polishing solution for a silicon wafer, a preparation method and application thereof.
Background
Semiconductor technology has evolved rapidly over the last few decades, with silicon wafers from 50mm to 300mm being ever larger, and the critical dimensions of electronic devices being continually shrinking. As device dimensions are gradually reduced and the depth of focus of optical lithography equipment is reduced, the requirements of integrated circuit fabrication processes on the surface of silicon wafers are consequently increased to the nanometer level, and the flatness of the surface of silicon wafers will directly relate to the performance quality of chips.
The surface processing process flow of the silicon wafer comprises the steps of silicon single crystal ingot cutting, orientation, barreling, corrosion, slicing, grinding disc, chamfering, chemical thinning, polishing, cleaning and detection. Polishing is the final process for preparing a silicon wafer with complete crystal lattice and undamaged surface, and becomes a crucial step in the semiconductor device manufacturing technology. At present, the requirements on the polishing quality of silicon wafers are higher and higher, such as extremely strict requirements and control on metal impurity contamination and particles on the surface of a polishing sheet, because the breakdown characteristics, interface states and minority carrier lifetime are seriously affected by the particles and the metal impurity contamination on the surface of the polishing sheet, and particularly, the surface effect type MOS large-scale integrated circuit is greatly affected.
Therefore, the finish polishing of the silicon wafer has an important meaning for improving the surface quality thereof. It is required to improve the surface flatness of the silicon wafer in a short time and reduce surface defects. Patent CN101693813a discloses a silicon-based polishing liquid, the composition of which only comprises high-purity silica sol, a pH regulator, a surfactant and water, and the example proves that the best surface quality cannot be obtained by only adding the surfactant. Patent CN113881347a discloses a chemical mechanical polishing solution, which is compounded by abrasive materials with different appearances, so that the polishing rate of a silicon wafer is improved and the scratch of the silicon wafer is reduced. However, the polymeric ellipsoidal abrasive used in the patent has no stable mature technology at present and has certain limitations. Patent CN112175524a discloses a sapphire polishing composition in which the thickener acts to increase the friction between the polishing liquid and the wafer, thereby increasing the polishing rate, which is in stark contrast to the viscosity modifier of the present patent. Patent US20210332264A1 discloses a polishing composition which uses two viscosity modifiers to act as suspending particles to ensure the stability of the polishing solution, but has little effect on reducing the number of defects and roughness on the wafer surface.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to design the chemical mechanical polishing liquid for the silicon wafer, which can effectively improve the viscosity of the polishing liquid through a viscosity regulator, inhibit the removal rate of the silicon wafer and reduce the surface defects.
The invention further aims at providing a preparation method of the chemical mechanical polishing liquid.
It is a further object of the present invention to provide the use of such a chemical mechanical polishing liquid.
In order to achieve the above object, the present invention adopts the following technical scheme:
the chemical mechanical polishing solution for the silicon wafer comprises the following components in percentage by mass: 5 to 15 percent of high-purity silica sol, 0.01 to 0.5 percent of viscosity regulator, 0.1 to 0.5 percent of pH regulator, 0.001 to 0.05 percent of surfactant and the balance of water.
In a specific embodiment, the high purity silica sol has a metal ion content of less than 0.1ppm and a primary particle size of 10 to 50nm.
In a specific embodiment, the viscosity modifier is selected from any one or a combination of at least two of carboxymethyl starch, carboxyethyl starch, hydroxyethyl starch, and hydroxypropyl starch, preferably hydroxypropyl starch.
In a specific embodiment, the pH adjustor is selected from any of potassium hydroxide, ammonium hydroxide, tetramethylammonium hydroxide, tetraethylammonium hydroxide, preferably tetramethylammonium hydroxide.
In a specific embodiment, the surfactant is selected from fatty alcohol polyoxyethylene ethers, for example any one selected from the group consisting of AEO3, AEO5, AEO7, AEO9, E1006, E1306, preferably E1006.
In a specific embodiment, the pH of the chemical mechanical polishing solution for silicon wafers ranges from 10 to 11, and the pH after 10 to 30 times dilution ranges from 10 to 11.
The invention also provides a preparation method of the chemical mechanical polishing solution for the silicon wafer, which comprises the following steps:
1) Uniformly mixing high-purity silica sol and half of water to obtain dispersion;
2) And (2) uniformly mixing the viscosity regulator, the pH regulator, the surfactant and the rest half of water, adding the mixture into the dispersion liquid in the step (1), and fully and uniformly mixing to obtain the chemical mechanical polishing liquid for the silicon wafer.
The use method of the chemical mechanical polishing liquid for the silicon wafer can be used for polishing after being diluted by 10-30 times by water (preferably ultrapure water), and all the polishing liquid meets the chemical mechanical polishing requirement for the silicon wafer.
The chemical mechanical polishing liquid is applied to chemical mechanical polishing of silicon wafers or wafers taking silicon as a substrate.
The chemical mechanical polishing liquidSuitable polishing conditions are: silicon wafer diameter 200 or 300mm, polishing pad POLYPAS 27NX series, polishing pressure 100-200 g/cm 2 The polishing temperature is 25-30 ℃, the rotation speed of the polishing head and the polishing disk is 10-30 rpm, the polishing time is 1-10 min, the flow rate of the fine polishing liquid is 1-5L/min, and the consumption of the fine polishing liquid per unit area is 5-20 mL/cm 2 。
In one specific application, the polishing conditions are, for example: polishing table type SPEEDFAM or EBARA, silicon wafer diameter 200mm, polishing pad POLYPAS 275NX, polishing pressure 150g/cm 2 The polishing temperature is 27 ℃, the rotation speed of the polishing head and the polishing disk is 30rpm, the polishing time is 6min, the flow rate of the polishing liquid is 3L/min, and the consumption of the polishing liquid per unit area is 16mL/cm 2 The polishing solution can not be recycled.
Compared with the prior art, the technical scheme of the invention has the beneficial effects that:
1) In the chemical mechanical polishing solution for the silicon wafer, the adopted viscosity modifier (such as hydroxypropyl starch) has a polyhydroxy structure, can form hydrogen bonds with surrounding water molecules, and improves the fluid volume of the viscosity modifier, thereby achieving the thickening effect.
2) According to the chemical mechanical polishing solution for the silicon wafer, in the polishing process, the viscosity of the polishing solution is high, the fluidity is poor, the formed pressure film is thicker, and the removal rate of the silicon wafer can be inhibited. Meanwhile, silicon dioxide nano particles in the polishing liquid are prevented from contacting with the wafer, particle residues and surface scratches are reduced, and the number of defects on the surface of the wafer and the surface roughness are reduced.
Drawings
FIG. 1 is a plot of viscosity versus hydroxypropyl starch concentration for a chemical mechanical polishing solution for silicon wafers according to the present invention.
Fig. 2 is a photograph of a silicon wafer under an atomic force microscope after polishing according to example 10 of the present invention.
Detailed Description
The following examples will further illustrate the method provided by the present invention for a better understanding of the technical solution of the present invention, but the present invention is not limited to the examples listed but should also include any other known modifications within the scope of the claims of the present invention.
The main raw material source information adopted by the embodiment of the invention is as follows:
high-purity silica sol: the PL series silica sol is purchased from the Japanese FUSO company, and the primary particle size is 10-50 nm;
viscosity modifier: all purchased from Shanghai Bohr chemical Co., ltd;
other reagents were common raw materials purchased in the market unless otherwise specified.
Examples 1 to 10
The chemical mechanical polishing solution for preparing the silicon wafer comprises the following raw material components except water in the formula, wherein the composition of the raw material components is shown in a table 1, the balance is ultrapure water, and the sum of the mass percentages of the raw material components is 100 percent:
1) Taking high-purity silica sol, adding half of water under the stirring condition for dilution, uniformly mixing, and dispersing;
2) And (2) uniformly mixing the viscosity regulator, the pH regulator, the surfactant and the rest half of water, adding the mixture into the dispersion liquid in the step (1), and fully and uniformly mixing to obtain the chemical mechanical polishing liquid for the silicon wafer.
Table 1 raw material compositions of the chemical mechanical polishing solutions for silicon wafers of examples 1 to 10
Comparative example 1
With reference to the formulation and preparation method of example 10, except that hydroxypropyl starch (viscosity modifier) and E1006 (fatty alcohol-polyoxyethylene ether surfactant) were not added to the formulation, other operating conditions and parameters were kept unchanged, and a fine polishing liquid was prepared at a pH of 10.5.
Comparative example 2
With reference to the formulation and preparation method of example 10, except that hydroxypropyl starch (viscosity modifier) was not added to the formulation, other operating conditions and parameters remained unchanged, and a polishing solution was prepared, with a pH of 10.5.
Comparative example 3
Referring to the formulation and preparation method of example 10, except that E1006 (fatty alcohol polyoxyethylene ether surfactant) was not added to the formulation, other operating conditions and parameters were kept unchanged, and a polishing solution was prepared, with a pH of 10.5.
Comparative example 4
With reference to the formulation and preparation method of example 10, the only difference is that hydroxypropyl starch (viscosity modifier) in the formulation is replaced by hydroxypropyl cellulose of equal molar mass, and other operating conditions and parameters are kept unchanged, so that a fine polishing liquid with a pH of 10.5 is prepared.
Comparative example 5
Referring to the formulation and preparation method of example 10, except that E1006 (fatty alcohol polyoxyethylene ether surfactant) in the formulation was replaced with polyethylene glycol PEG600 of equal molar mass, other operating conditions and parameters were kept unchanged, and a polishing solution was prepared at pH 10.5.
Comparative example 6
With reference to the formulation and preparation method of example 10, the only difference is that the hydroxypropyl starch in the formulation is replaced by hydroxyethyl cellulose as a viscosity regulator used in patents US20210332264A1 and CN112175524a, and other operating conditions and parameters are kept unchanged, so that a polishing solution is prepared, and the pH is 10.5.
Examples 1 to 10 and comparative examples 1 to 6 were used for preparing polishing solutions:
the diameter of the silicon wafer used was 200mm, which is supplied by Shandong's raw Crystal electronic technologies Co.
Each polishing solution is diluted by ultrapure water for 20 times and then used, the pH value after dilution is 10-11, and the solid content is 0.25-0.75%.
The polishing conditions were as follows: the polisher station was a japanese Speedfam 36GPAW single-sided polisher with four polishing heads, each capable of polishing a 200mm diameter silicon wafer.
The polishing pad was a POLYPAS 275NX. Polishing pressure 150g/cm 2 The polishing pad temperature was 27 ℃, the rotational speed of the polishing head and the polishing disk was 30/30rpm, the polishing time was 6min, the flow rate of the polishing liquid was 3L/min, and the amount of the polishing liquid per unit area was 16mL/cm 2 。
The statistics of the surface defect count of the silicon wafer in the polishing liquid of the present invention in comparative examples 1 to 6 and examples 1 to 10 are shown in Table 2.
Number of surface defects of silicon wafer: defects of 32nm or more on the wafer surface and the coordinates of the defects are detected by a defect detection device Surfscan SP 2. Then, the defects in the detected defect coordinates are observed by scanning electron microscope SEM, and the defect number is counted. The number of defects was evaluated by taking the number of defects of the silicon wafer polished in comparative example 1 as a relative value of 100. The lower the relative value of the defect number is, the more preferable, and 30 or less is preferable.
Silicon wafer surface roughness: and detecting by using an atomic force microscope AFM, randomly selecting a line passing through the center of a circle on the surface of the wafer, and calculating the arithmetic average value of each point in the outline to obtain the line roughness Ra.
Table 2 comparative examples 1 to 5 and examples 1 to 10 were polished for the number of surface defects and surface roughness of silicon wafers
| Sequence number | Number of surface defects of silicon wafer (relative value) | Surface roughness Ra/nm of silicon wafer |
| Comparative example 1 | 100 | 1.30 |
| Comparative example 2 | 81 | 0.771 |
| Comparative example 3 | 63 | 0.637 |
| Comparative example 4 | 45 | 0.543 |
| Comparative example 5 | 75 | 0.723 |
| Comparative example 6 | 49 | 0.566 |
| Example 1 | 29 | 0.336 |
| Example 2 | 23 | 0.263 |
| Example 3 | 25 | 0.230 |
| Example 4 | 13 | 0.190 |
| Example 5 | 18 | 0.136 |
| Example 6 | 20 | 0.143 |
| Example 7 | 14 | 0.152 |
| Example 8 | 11 | 0.164 |
| Example 9 | 15 | 0.184 |
| Example 10 | 8 | 0.123 |
In contrast to example 10, comparative example 1 contained only the pH adjustor, comparative example 2 did not contain the viscosity adjustor, and comparative example 3 did not contain the fatty alcohol-polyoxyethylene ether surfactant. As can be seen from Table 2, the addition of any one of the viscosity modifier and the fatty alcohol-polyoxyethylene ether surfactant can reduce the number of surface defects to some extent, but the optimum effect is not achieved. For analysis of the reason, comparative example 1 contained only the pH adjuster, the alkaline auxiliary agent and the high purity silica sol directly contacted the wafer, and the surface defects were large due to chemical etching and particle residue. In comparative examples 2 and 3, only the viscosity modifier or the fatty alcohol-polyoxyethylene ether surfactant is used, the surface of the wafer or the high-purity silica sol cannot be comprehensively protected, the surface defects can be improved to a certain extent, and the best effect is not achieved yet. In comparative examples 4 and 6, the viscosity modifier was replaced with a cellulose material having a similar structure but a higher hydroxyl group content, and the cellulose material was a natural polymer material, and the origin and structure thereof were not determined. The viscosity modifier used in the patent can be synthesized by a chemical method, and the content of the exposed hydroxyl is controlled. In particular, the higher hydroxyl content of hydroxyethyl cellulose or hydroxypropyl cellulose is more tightly combined with the surface of the wafer, so that more surface residues are caused, and the cleaning is difficult. The fatty alcohol-polyoxyethylene ether surfactant in comparative example 5 was replaced with a surfactant of similar structure, but without a hydrophobic end, because of the lack of a long carbon chain structure, the high purity silica sol could not be effectively protected. In summary, the wafer surface defect and roughness after polishing using the comparative example are high and cannot meet the polishing requirements.
Examples 1 to 10 use a viscosity modifier and a fatty alcohol-polyoxyethylene ether surfactant together, and further reduce the number of defects and roughness of the wafer surface. The reason is analyzed, as shown in figure 1, the hydroxypropyl starch used in the patent can effectively improve the viscosity of the polishing liquid by controlling the addition amount. The viscosity of the polishing solution is increased, the fluidity is poor, the formed pressure film is thicker, the contact of silicon dioxide nano particles in the polishing solution with a wafer is prevented, the surface of the wafer is effectively protected, and the fatty alcohol polyoxyethylene ether surfactant is effectively protected for the formation of high-purity silica sol due to a hydrophobic structure. Therefore, the relative value of the number of defects on the wafer surface is below 30. Fig. 2 is a photograph of the silicon wafer polished in example 10 under an atomic force microscope, and the line roughness test has randomness, so that the surface roughness of the wafers in examples 1 to 10 in table 2 is slightly different, but the results all meet the polishing requirements.
In conclusion, the viscosity regulator can effectively improve the viscosity of the polishing solution, form a thicker pressure film during polishing, and reduce the number of defects and roughness of the wafer surface. The polishing solution can optimally reduce the relative value of the defect number of the wafer surface to below 10, and the surface roughness reaches 0.123nm.
While the present invention has been described in detail through the foregoing description of the preferred embodiment, it should be understood that the foregoing description is not to be considered as limiting the invention. Those skilled in the art will appreciate that certain modifications and adaptations of the invention are possible and can be made under the guidance of the present specification. Such modifications and adaptations are intended to be within the scope of the present invention as defined in the appended claims.
Claims (12)
1. The chemical mechanical polishing solution for the silicon wafer is characterized by comprising the following components in percentage by mass: 5% -15% of high-purity silica sol, 0.01% -0.5% of viscosity regulator, 0.1% -0.5% of pH regulator, 0.001% -0.05% of surfactant and the balance of water;
the viscosity regulator is at least one selected from carboxymethyl starch, carboxyethyl starch, hydroxyethyl starch and hydroxypropyl starch; the surfactant is fatty alcohol polyoxyethylene ether.
2. The chemical mechanical polishing liquid according to claim 1, wherein the content of metal ions in the high-purity silica sol is less than 0.1ppm, and the primary particle size is 10-50 nm.
3. The chemical mechanical polishing liquid according to claim 1, wherein the viscosity modifier is hydroxypropyl starch.
4. The chemical mechanical polishing liquid according to claim 1, wherein the pH adjustor is any one selected from the group consisting of potassium hydroxide, ammonium hydroxide, tetramethylammonium hydroxide, and tetraethylammonium hydroxide.
5. The chemical mechanical polishing liquid of claim 4, wherein the pH adjustor is tetramethylammonium hydroxide.
6. The chemical mechanical polishing liquid according to claim 1, wherein the surfactant is any one of AEO3, AEO5, AEO7, AEO9, E1006, E1306.
7. The chemical mechanical polishing liquid of claim 6, wherein the surfactant is E1006.
8. The chemical mechanical polishing liquid according to any one of claims 1 to 7, wherein the pH of the polishing liquid is 10 to 11.
9. The chemical mechanical polishing liquid according to any one of claims 1 to 7, wherein the polishing is performed after 10 to 30 times dilution with water, and the pH after dilution is 10 to 11.
10. The method for preparing the chemical mechanical polishing liquid for the silicon wafer according to any one of claims 1 to 9, which is characterized by comprising the following steps:
1) Uniformly mixing high-purity silica sol and half of water to obtain a dispersion liquid;
2) And (2) uniformly mixing the viscosity regulator, the pH regulator, the surfactant and the rest half of water, adding the mixture into the dispersion liquid in the step (1), and fully and uniformly mixing to obtain the chemical mechanical polishing liquid for the silicon wafer.
11. Use of the chemical mechanical polishing solution for silicon wafers according to any one of claims 1 to 9 or the chemical mechanical polishing solution prepared by the preparation method according to claim 10 in chemical mechanical polishing of silicon wafers.
12. The use of a chemical mechanical polishing liquid for silicon wafers according to claim 11, wherein the polishing conditions in use are: silicon wafer diameter is 200 or 300mm, polishing pressure is 100-200 g/cm 2 The polishing temperature is 25-30 ℃, the rotation speed of the polishing head and the polishing disk is 10-30 rpm, the polishing time is 1-10 min, the polishing liquid flow rate is 1-5L/min, and the consumption of the polishing liquid per unit area is 5-20 mL/cm 2 。
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| CN113549400A (en) * | 2021-08-10 | 2021-10-26 | 万华化学集团电子材料有限公司 | Method for improving cyclic utilization rate of polishing solution and silicon wafer polishing method |
| CN115244659A (en) * | 2020-03-13 | 2022-10-25 | 福吉米株式会社 | Polishing composition and polishing method |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20210332264A1 (en) * | 2020-04-23 | 2021-10-28 | Fujimi Corporation | Novel polishing vehicles and compositions with tunable viscosity |
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| US6429133B1 (en) * | 1999-08-31 | 2002-08-06 | Micron Technology, Inc. | Composition compatible with aluminum planarization and methods therefore |
| CN101693813A (en) * | 2009-09-01 | 2010-04-14 | 永州皓志稀土材料有限公司 | Silicon-based fine polishing liquid |
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