CN113549399B - Chemical mechanical polishing composition suitable for rough polishing of silicon wafer and application thereof - Google Patents
Chemical mechanical polishing composition suitable for rough polishing of silicon wafer and application thereof Download PDFInfo
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- CN113549399B CN113549399B CN202110883514.6A CN202110883514A CN113549399B CN 113549399 B CN113549399 B CN 113549399B CN 202110883514 A CN202110883514 A CN 202110883514A CN 113549399 B CN113549399 B CN 113549399B
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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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02002—Preparing wafers
- H01L21/02005—Preparing bulk and homogeneous wafers
- H01L21/02008—Multistep processes
- H01L21/0201—Specific process step
- H01L21/02013—Grinding, lapping
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Abstract
The invention discloses a chemical mechanical polishing composition suitable for rough polishing of a silicon wafer and application thereof. The diazo group in the compound containing the diazo group in the polishing composition has a unit of positive charge and has a synergistic effect with the grinding particles with the charges on the surface, so that the high-speed removal of silicon by the polishing composition is realized.
Description
Technical Field
The invention relates to the technical field of chemical mechanical polishing, in particular to a chemical mechanical polishing composition suitable for rough polishing of a silicon wafer and application thereof.
Technical Field
The increase in chip demand presents new challenges to the improvement of production efficiency throughout the industry chain. Semiconductor substrates, such as silicon wafers, required for the fabrication of chips are subjected to a Chemical Mechanical Polishing (CMP) process to obtain surface quality and thickness deviations that meet the use requirements. The improvement of the CMP efficiency is beneficial to improving the chip productivity and reducing the production cost.
The CMP of silicon wafers mainly comprises steps of rough polishing and fine polishing. Rough polishing is mainly used for removing micron-sized scratches generated on the surface of a silicon wafer in the previous process, and reducing the surface roughness of the silicon wafer to a nanometer scale, and requires that a polishing composition provides a removal rate of about 1-2 μm/min. The finish polishing is used to improve the surface quality of the silicon wafer, reduce the roughness of the silicon wafer surface to angstrom level, and reduce the total thickness deviation to micron level, requiring the polishing composition to provide a removal rate of about 1000-. Under mature process conditions, the improvement in CMP efficiency results primarily from the improvement in the performance of the polishing composition for rough polishing.
The silicon wafer polishing solution mainly comprises grinding particles, a rate accelerator, a pH value regulator, a complexing agent, water, a corrosion inhibitor, a bactericide, a dispersing agent and the like. In the chemical mechanical polishing of the silicon wafer, the grinding particles play a small role in the removal of the silicon wafer, a key component determining the removal capacity of the polishing solution on the silicon wafer is a rate accelerator, and the rough polishing of the silicon wafer is more prone to pursuing the high-speed removal of the silicon wafer. Therefore, the silicon wafer rough polishing solution formula is designed by taking the rate accelerator as a core.
US3170273A mentions that low molecular weight aliphatic amines are a very efficient silicon wafer polishing rate accelerator, but amines increase particle defects of the substrate and generate polishing haze. CN102477261B and US8273142B2 mention organic carboxylic acids as rate promoters, but their rate-enhancing effect is limited. CN111378369A takes one or more of piperazine, ethanolamine and diethylenetriamine as a speed accelerator, and the composition polishes the silicon wafer with better surface quality but lower speed. The quaternary ammonium salts or bases mentioned in US4462188A are very effective rate accelerators but require high levels of such materials to achieve the desired polishing rate compared to other types of rate accelerators, but such materials are toxic and are not suitable for use in formulations in excess. Therefore, there is still a need to improve the components of the polishing solution from the viewpoint of chemical formulation to overcome the aforementioned drawbacks of the prior art.
Disclosure of Invention
In order to solve the problems of the prior art, the invention provides a chemical mechanical polishing composition suitable for rough polishing of silicon wafers, and the polishing composition can realize high-speed removal of silicon.
Another object of the present invention is to provide the use of such a chemical-mechanical polishing composition suitable for rough polishing of silicon wafers in chemical-mechanical polishing.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the chemical mechanical polishing composition comprises abrasive particles, a compound containing a diazo group, a pH value regulator, a complexing agent and deionized water.
In a preferred embodiment, the chemical mechanical polishing composition comprises the following components in percentage by mass: 0.1 to 10 weight percent of grinding particles, 0.01 to 5 weight percent of compound containing diazo groups, 0.01 to 0.5 weight percent of pH value regulator, 0.01 to 0.1 weight percent of complexing agent and the balance of deionized water.
In a specific embodiment, the abrasive particles are selected from one or more of silica, zirconia, ceria, alumina, silicon carbide particles; preferably, the abrasive particles are silica.
In a specific embodiment, the silica abrasive particles are silica sols prepared by any one of elemental silica method, ion exchange method, and sol-gel method.
In a particular embodiment, the abrasive particles have a size of 10 to 300nm, preferably 30 to 90 nm.
In a specific embodiment, the diazo group-containing compound is selected from one or more of diazobenzene hydroxide, diazobenzene nitrate, diazobenzene sulfonic acid, diazobenzene chloride, mercapto diazonium salt, diazobenzene sulfonate, preferably diazobenzene nitrate or diazobenzene sulfonic acid.
In a particular embodiment, the pH of the polishing solution is in the range of 9 to 12, preferably 9.5 to 11.
In a specific embodiment, the pH adjuster is selected from one or more of tetramethylammonium hydroxide, tetraethylammonium hydroxide, tetrabutylammonium hydroxide, ethanolamine, diethanolamine, triethanolamine, piperazine, aniline, azole compounds, potassium hydroxide, sodium hydroxide, guanidine compounds, alkali metal alkoxides, preferably any of tetraethylammonium hydroxide, ethanolamine, triazole, potassium hydroxide, guanidine carbonate, more preferably tetraethylammonium hydroxide or guanidine carbonate.
In a specific embodiment, the complexing agent is selected from one or more of ethylenediaminetetraacetic acid, disodium ethylenediaminetetraacetate, sodium ethylenediaminetetramethylenephosphate, oxalic acid, acetic acid, citric acid, malonic acid, nitrilotriacetic acid, ethylenediaminetetramethylenephosphonic acid, aminotrimethylenephosphonic acid, preferably any of oxalic acid, citric acid or ethylenediaminetetraacetic acid, more preferably oxalic acid.
In another aspect, the foregoing chemical mechanical polishing composition is used in chemical mechanical polishing.
Compared with the prior art, the invention has the following beneficial effects:
the polishing composition is added with the compound containing the diazo group, wherein the diazo group in the compound containing the diazo group has a unit positive charge and has a synergistic effect with the grinding particles with the charges on the surface, so that the high-speed removal of silicon by the polishing composition is realized, the removal rate can be about 5 times of that of the traditional polishing solution at most, and the polishing composition is particularly suitable for a silicon wafer rough polishing process.
Detailed Description
The following examples will further illustrate the method provided by the present invention in order to better understand the technical solution of the present invention, but the present invention is not limited to the listed examples, and should also include any other known modifications within the scope of the claims of the present invention.
A chemical mechanical polishing composition suitable for rough polishing of silicon wafers comprises the following components in percentage by mass: 0.1 to 10 weight percent of grinding particles, 0.01 to 5 weight percent of compound containing diazo groups, 0.01 to 0.5 weight percent of pH value regulator, 0.01 to 0.1 weight percent of complexing agent and the balance of deionized water.
The abrasive particles are selected from silicon oxide, silicon carbide, aluminum oxide, zirconium oxide, and cerium oxide, and preferably are silicon oxide particles. The preparation method of the silicon oxide grinding particles is any one of a simple substance silicon method, an ion exchange method and a sol-gel method, and is not limited at all, and the specific preparation method can refer to the prior art and can also be directly purchased from the market for corresponding grinding materials. Actually, the used silicon oxide abrasive particles are silica sol in which silicon oxide is dissolved in water, and negative charges on the surface of the silica sol can interact with positive charges of a unit of diazo group in the unique compound containing the diazo group, so that the absolute value of the Zeta potential on the surface of the silica sol is reduced, the like charge repulsion effect of the particles and the surface of a silicon wafer is reduced, the friction force between the abrasive particles and the silicon wafer in the polishing process is increased, and the removal rate is improved. In addition, the abrasive particles have a size of 10 to 300nm, including but not limited to 20nm, 50nm, 75nm, 100nm, 120nm, 150nm, 180nm, 200nm, 230nm, 250nm, 270nm, 285nm, 300nm, preferably 30 to 90nm, and are too large to cause scratches on the surface of the silicon wafer and too small to achieve high removal rates.
The diazo group-containing compound in the invention is selected from one or more of diazobenzene hydroxide, diazobenzene sulfonic acid, diazobenzene chloride, diazobenzene sulfate, sulfhydryl diazonium salt and diazobenzene nitrate, and is preferably diazobenzene nitrate and diazobenzene sulfonic acid. The diazo group in the diazo group-containing compound has a unit of positive charge and generates a synergistic effect with the grinding particles with the charges on the surface, so that the high-speed removal of silicon by the polishing composition is realized. In the present invention, the mass ratio of the diazo group-containing compound to the abrasive particles is preferably 1:10 to 1:1, and in this range, the synergistic effect of the two is more significant.
The pH value regulator is selected from one or more of tetramethylammonium hydroxide, tetraethylammonium hydroxide, tetrabutylammonium hydroxide, ethanolamine, diethanolamine, triethanolamine, piperazine, aniline, azole compounds, potassium hydroxide, sodium hydroxide, guanidine compounds and alkali metal alkoxide, preferably any one of tetraethylammonium hydroxide, ethanolamine, triazole, potassium hydroxide and guanidine carbonate, and more preferably tetraethylammonium hydroxide or guanidine carbonate. The pH adjustor can be added in an amount of 0.01 wt.% to 0.5 wt.% of the weight of the polishing composition, specifically, the pH of the polishing composition can be adjusted by the pH adjustor to a pH of about 9 to about 12, including, but not limited to, about 9, about 9.5, about 10, about 10.5, about 11, about 11.5, about 12, preferably, the pH of the polishing composition can be adjusted to a pH of about 9.5 to about 11, within which the polishing composition of the invention is more suitable for use in the rough polishing of silicon wafers.
The complexing agent is selected from one or more of ethylene diamine tetraacetic acid, ethylene diamine tetraacetic acid disodium, ethylene diamine tetraacetic acid dipotassium, oxalic acid, citric acid, malonic acid, nitrilotriacetic acid, ethylene diamine tetramethylene phosphonic acid, ethylene diamine tetramethylene sodium phosphate and aminotrimethylene phosphonic acid, preferably oxalic acid, citric acid and ethylene diamine tetraacetic acid, and more preferably oxalic acid. The complexing agent is added in an amount of 0.01 wt.% to 0.1 wt.% of the mass of the polishing composition, including, for example and without limitation, 0.01 wt.%, 0.02 wt.%, 0.03 wt.%, 0.04 wt.%, 0.05 wt.%, 0.06 wt.%, 0.07 wt.%, 0.08 wt.%, 0.09 wt.%, 0.1 wt.%. The addition of the complexing agent in the polishing composition is beneficial to complexing free metal ions in the polishing solution, the metal ion pollution on the surface of the polished silicon wafer is reduced, the polishing rate is reduced due to excessive addition, and the complexing effect cannot be achieved due to too little addition.
The polishing composition has the advantages that the diazo group compound is added, and the components are matched with each other, so that the silicon wafer removal rate is greatly improved, the production efficiency is improved, and the polishing composition is particularly suitable for the rough polishing process of the silicon wafer.
Preparation of polishing solution
And (4) diluting the raw materials. In the preparation process of the polishing solution, when the content of the chemical additive among the silica sol particles is too high, the local charge density and the ion concentration among the silica sol particles are increased rapidly, so that the originally unstable charge balance among the silica sol particles is broken, and a part of nano-scale silica sol particles can be agglomerated into micron-scale large particles. Commercial silica sols typically have a solids content of 20 to 40 wt.%, and therefore, dilution is required before mixing the silica sol with the additives. The dilution factor of the silica sol and the chemical additive in the polishing solution formulation of the embodiment of the present invention is 2 times and 10 times, and the dilution factor is not particularly limited. In the present invention, the following substances are all in a diluted state.
A mixed solution of silica sol and diazo compound is prepared. The silica sol is added dropwise to the aqueous diazo compound solution, and the mixture is stirred while being added dropwise at a stirring speed of, for example, 100rpm for, for example, 20min to obtain solution A. The stirring speed and stirring time in the preparation of the solution A are not particularly limited, and other speeds and times can be used as long as uniform dispersion is ensured.
Adding other chemical auxiliary agents. The other additives described in the examples were added to the solution A, and the order of addition of the components is not particularly limited. Stirring was carried out while dropping at a stirring speed of, for example, 100rpm for, for example, 20min to obtain solution B. The stirring speed and stirring time in the preparation of the solution B are not particularly limited, and other speeds and times can be used as long as uniform dispersion is ensured.
And making up the rest deionized water into the solution B. Stirring was carried out while adding water at a stirring speed of, for example, 100rpm for, for example, 20min to obtain a polishing liquid. Likewise, other speeds and times are possible, as long as uniform dispersion is ensured.
Filtration
The preparation process of the polishing solution inevitably generates aggregates with large particle size, the additive can also contain impurities, and the silicon wafer is easily scratched by foreign matters in the polishing process, so that the silicon wafer is removed by using a filtering process. The filtration method may be reduced pressure filtration, pressure filtration or centrifugal filtration, and preferably pressure filtration is used. The filter pore size is typically taken to be a nominal value, provided by the manufacturer. The filtration can be completed by using a filter with a single pore size, and the multi-stage filtration can also be realized by using filters with different pore sizes in series. The scheme adopts two-stage filtration, and the pore diameter of the first filter is preferably 3-20 μm, preferably 5-10 μm. The pore size of the second filter is preferably 0.1 to 1 μm. The large filter pore size increases production efficiency and filter life, but the larger the number of large particles, the smaller the filter pore size. The material and structure of the filter are not particularly limited. Examples of filter materials include cellulose, nylon, polyethersulfone, polypropylene, polycarbonate, polytetrafluoroethylene, preferably polytetrafluoroethylene. Examples of filter structures include depth filters, pleated filters and membrane filters, preferably pleated filters.
Polishing of
In the following examples, the instruments and parameters used in the polishing of silicon wafer substrate materials were as follows:
in the following examples, the parameters of the silicon wafers used for polishing were as follows:
according to the polishing parameters provided by this patent, the Removal Rate (RR) is calculated as follows: wherein the wafer size is in inches and Δ m is the difference in mass of the silicon wafer before and after CMP in milligrams.
Unless otherwise specified, materials, instruments and reagents used in the examples of the present invention and comparative examples were obtained commercially.
Examples
The types and contents of substances added to the polishing liquid formulations used in the examples and comparative examples are shown in table 1, and the balance is deionized water.
TABLE 1 materials ratios of examples and comparative examples
Compared with the comparative example 1, after the diazobenzene sulfonic acid is added into the polishing solution, the removal rate of silicon is obviously increased, and the removal rate is increased by nearly 6 times.
As can be seen from comparison of comparative examples 2-3 with examples 2-3, when no diazo compound component is present in the polishing solution, the silicon oxide content in the polishing solution has a smaller influence on the removal rate of the silicon wafer, and after the diazo compound is added to the polishing solution, the removal rates obtained by polishing solutions with different silicon oxide contents are obviously different. In conclusion, the diazo compounds have a synergistic effect with the silica sol particles.
Comparing the comparative example 4 with the example 4, if the content ratio of the diazo compound to the silicon oxide in the polishing solution is too high, a good silicon wafer removal rate cannot be achieved; comparative example 5 compared to example 4, the polishing slurry had too low a diazo compound to silica content ratio to give a similarly poor wafer removal rate.
While the present invention has been described in detail with reference to the preferred embodiments, it should be understood that the above description should not be taken as limiting the invention. It will be appreciated by those skilled in the art that modifications or adaptations to the invention may be made in light of the teachings of the present specification. Such modifications or adaptations are intended to be within the scope of the present invention as defined in the claims.
Claims (16)
1. A chemical mechanical polishing composition suitable for roughly polishing a silicon wafer comprises abrasive particles, a compound containing a diazo group, a pH value regulator, a complexing agent and deionized water; the weight percentage of each component is as follows: 0.1-10 wt% of grinding particles, 0.01-5 wt% of a compound containing diazo groups, 0.01-0.5 wt% of a pH value regulator, 0.01-0.1 wt% of a complexing agent and the balance of deionized water; the mass ratio of the diazo group-containing compound to the abrasive particles is 1:10-1: 1; the abrasive particles are selected from one or more of silicon oxide, zirconium oxide, cerium oxide, aluminum oxide and silicon carbide particles.
2. The chemical mechanical polishing composition of claim 1, wherein the abrasive particles are silica.
3. The chemical mechanical polishing composition of claim 2, wherein the silica abrasive particles are silica sols prepared by any one of elemental silica method, ion exchange method, and sol gel method.
4. The chemical mechanical polishing composition according to claim 1 or 2, wherein the abrasive particles have a size of 10 to 300 nm.
5. The chemical mechanical polishing composition of claim 4, wherein the abrasive particles have a size of 30nm to 90 nm.
6. The chemical mechanical polishing composition of claim 1, wherein the diazo group containing compound is selected from one or more of the group consisting of diazobenzene hydroxide, diazobenzene nitrate, diazobenzene sulfonic acid, diazobenzene chloride, mercapto diazonium salt, diazobenzene sulfonate.
7. The chemical mechanical polishing composition of claim 6, wherein the diazonium group-containing compound is diazobenzene nitrate or diazobenzene sulfonic acid.
8. The chemical-mechanical polishing composition of claim 1, wherein the polishing composition has a pH of 9 to 12.
9. The chemical-mechanical polishing composition of claim 8, wherein the polishing composition has a pH of 9.5 to 11.
10. The chemical mechanical polishing composition of claim 1, wherein the pH adjusting agent is selected from one or more of tetramethylammonium hydroxide, tetraethylammonium hydroxide, tetrabutylammonium hydroxide, ethanolamine, diethanolamine, triethanolamine, piperazine, aniline, azole compounds, potassium hydroxide, sodium hydroxide, guanidine compounds, and alkali metal alkoxides.
11. The chemical mechanical polishing composition of claim 10, wherein the pH adjusting agent is selected from any one of tetraethylammonium hydroxide, ethanolamine, triazole, potassium hydroxide, guanidine carbonate.
12. The chemical mechanical polishing composition of claim 11, wherein the pH adjusting agent is selected from the group consisting of tetraethylammonium hydroxide and guanidine carbonate.
13. The chemical mechanical polishing composition of claim 1, wherein the complexing agent is selected from one or more of ethylenediaminetetraacetic acid, disodium ethylenediaminetetraacetate, sodium ethylenediaminetetramethylenephosphate, oxalic acid, acetic acid, citric acid, malonic acid, nitrilotriacetic acid, ethylenediaminetetramethylenephosphonic acid, aminotrimethylenephosphonic acid.
14. The chemical mechanical polishing composition of claim 13, wherein the complexing agent is selected from any of oxalic acid, citric acid, or ethylenediaminetetraacetic acid.
15. The chemical-mechanical polishing composition of claim 14, wherein the complexing agent is oxalic acid.
16. Use of the chemical mechanical polishing composition of any one of claims 1 to 15 in chemical mechanical polishing.
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| CN115851134A (en) * | 2022-10-27 | 2023-03-28 | 万华化学集团电子材料有限公司 | High-precision silicon wafer polishing composition and application thereof |
| CN115851136A (en) * | 2022-12-02 | 2023-03-28 | 博力思(天津)电子科技有限公司 | Recyclable silicon wafer chemical mechanical polishing solution |
| CN117050661B (en) * | 2023-06-21 | 2024-05-17 | 湖北兴福电子材料股份有限公司 | Green monocrystalline silicon coarse polishing solution |
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| CN103080256A (en) * | 2010-09-08 | 2013-05-01 | 巴斯夫欧洲公司 | Aqueous polishing composition and process for chemically mechanically polishing substrates containing silicon oxide dielectric and polysilicon films |
| CN109743878A (en) * | 2016-09-21 | 2019-05-10 | 日立化成株式会社 | Suspension and grinding method |
| CN111423819A (en) * | 2020-04-17 | 2020-07-17 | 深圳市朗纳研磨材料有限公司 | Polishing solution and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103080256A (en) * | 2010-09-08 | 2013-05-01 | 巴斯夫欧洲公司 | Aqueous polishing composition and process for chemically mechanically polishing substrates containing silicon oxide dielectric and polysilicon films |
| CN109743878A (en) * | 2016-09-21 | 2019-05-10 | 日立化成株式会社 | Suspension and grinding method |
| CN111423819A (en) * | 2020-04-17 | 2020-07-17 | 深圳市朗纳研磨材料有限公司 | Polishing solution and preparation method thereof |
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