CN112029417A - Polishing composition for silicon carbide CMP and preparation method thereof - Google Patents
Polishing composition for silicon carbide CMP and preparation method thereof Download PDFInfo
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- CN112029417A CN112029417A CN202011059655.8A CN202011059655A CN112029417A CN 112029417 A CN112029417 A CN 112029417A CN 202011059655 A CN202011059655 A CN 202011059655A CN 112029417 A CN112029417 A CN 112029417A
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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
Abstract
The invention discloses a preparation method of a polishing composition for silicon carbide CMP, which is prepared by the following steps: adding a dispersing agent, an accelerator, a pH buffering agent, a wetting agent and a complexing agent into water, stirring uniformly, adding an abrasive, adding a defoaming agent, adjusting the pH value of the solution by using a pH regulator, and aging. The polishing solution of the invention is adopted to carry out CMP on the silicon carbide wafer, and has better removal rate and surface smoothness, and the roughness can reach below 0.2 nm. The polishing composition is a good silicon carbide wafer polishing agent, can replace a hard abrasive composition, improves roughness and smoothness, and is green and environment-friendly.
Description
Technical Field
The invention relates to the field of Chemical Mechanical Polishing (CMP), in particular to a polishing composition for silicon carbide CMP and a preparation method thereof.
Background
Silicon carbide materials are applied to the semiconductor industry and precision optical devices due to the characteristics of high hard bone, good thermal conductivity, good wear resistance, large forbidden bandwidth and the like, and meanwhile, the surface materials are difficult to process and process, and the surface materials need to be ultra-smooth and ultra-clean during modern high technology, so that the only industrialized technology for realizing the global flat surface is chemical mechanical polishing, and excellent rough and flat surface can be obtained through polishing, so that the semiconductor application becomes possible, and a good foundation is laid for terminal applications such as LED illumination, high-frequency devices, even future mobile terminals, notebook computers and the like.
Much research has been carried out in the field of polishing of silicon carbide, and since the inertness of the silicon carbide surface makes the removal of the silicon carbide surface require surface activation by chemical action, the use of more hard abrasives, such as diamond particles and alumina particles, causes ultra-high hardness, causes scratches and surface defects during polishing, and finally affects the surface roughness.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides a polishing composition for silicon carbide CMP, which comprises the following components in percentage by mass:
0.05 to 5 percent (preferably 0.1 to 2 percent) of dispersant,
0.05 to 5 percent of accelerant,
0.1 to 1 percent of pH buffering agent,
0.005 to 0.1 percent of wetting agent,
0.01 to 5 percent (preferably 0.2 to 2 percent) of complexing agent,
5 to 40 percent (preferably 10 to 30 percent) of abrasive,
0.01 to 0.1 percent (preferably 0.02 to 0.05 percent) of defoaming agent,
0.5 to 1.0 percent of pH regulator,
the balance being deionized water.
Preferably, the dispersant is polystyrene maleic anhydride and derivatives thereof.
Preferably, the dispersant is sulfonated styrene maleic anhydride copolymer (SMA).
Preferably, the accelerator is an oxidizing agent, including peroxides, overflowing compounds, halogen acids, perhalogenated acids, and nitro compounds.
Preferably, the oxidant is selected from one or more of perchloric acid, potassium perchlorate, potassium chlorate, sodium chlorate, periodic acid, potassium periodate, sodium periodate, iodic acid, potassium iodate, hydrogen peroxide, ozone, potassium persulfate, ammonium persulfate, sodium persulfate, potassium nitrate, sodium nitrate and ammonium nitrate.
Preferably, the pH buffering agent is a hydrogen phosphate and phosphate conjugate system.
Preferably, the wetting agent is an acetylenic diol polyether.
Preferably, the complexing agent is selected from one or more of butane-2-phosphonate-1, 2, 4-tricarboxylic acid (PBTC), aminotrimethylene phosphonic Acid (ATMP), Ethylene Diamine Tetra Methylene Phosphonic Acid (EDTMPA), Diethylene Triamine Penta Methylene Phosphonic Acid (DTPMPA), polyamino polyether methylene Phosphonic Acid (PAPEMP), hydroxy ethylidene diphosphonic acid (HDPE).
Preferably, the complexing agent is selected from one or more of aliphatic monobasic acid, aliphatic dibasic acid, aliphatic polycarboxylic acid, acetic acid, oxalic acid, citric acid, tartaric acid, malic acid, malonic acid, succinic acid and tetraethyl oxalic acid.
Preferably, the water is deionized water.
Preferably, the abrasive is silicon dioxide, the abrasive is spherical, spindle-shaped or chain-shaped, and the particle size is 60-150 nm (preferably 80-120 nm).
Preferably, the defoamer is a modified polysiloxane defoamer.
Preferably, the pH adjuster is a 50% potassium hydroxide solution.
The invention also provides a preparation method of the polishing composition for silicon carbide CMP, which comprises the steps of sequentially adding a dispersing agent, an accelerator, a pH buffering agent, a wetting agent and a complexing agent into deionized water, stirring uniformly, adding a silica sol abrasive, adding a defoaming agent, adjusting the pH value of the solution to 11-13 (the pH value is preferably 12.5) by using a pH regulator, and aging for 30-60 minutes (preferably 20 minutes).
The invention has the advantages and beneficial effects that: the polishing composition for silicon carbide CMP is used for CMP of silicon carbide wafers by the polishing solution, has good removal rate and surface smoothness, and the roughness can reach below 0.2 nm. The polishing solution is a good silicon carbide wafer polishing agent, can replace a hard abrasive composition, improves roughness and smoothness, and is green and environment-friendly.
The hardness of the silicon oxide abrasive is less than that of diamond particles and aluminum oxide abrasives, the silicon oxide abrasive has certain advantages in the fine polishing stage of silicon carbide, and the surface quality can be improved while a certain grinding rate is ensured by matching with additives such as an accelerant and an oxidant.
The CMP polishing solution containing silicon oxide provided by the invention can obtain a higher polishing rate, and simultaneously has no scratch, no organic matter residue and better roughness under the matching of proper granularity and special additives.
The polishing solution of the invention has the following characteristics:
1) the invention adopts the combination of a special complexing agent, a wetting agent, a dispersing agent and an accelerating agent, and is matched with a nanometer silicon oxide abrasive, so that the polishing efficiency of silicon carbide is higher, and the polished surface has no scratch, dots and organic matter residues.
2) The polishing solution disclosed by the invention has a special washing-assistant component, so that the residual particles after polishing are easy to clean and remove, and an ideal surface finish is obtained.
3) The polishing solution is a green environment-friendly polishing agent.
4) The invention solves the problem that the traditional hard abrasive such as diamond liquid, alumina and the like damages the surface of the wafer, obtains high polishing efficiency and obtains an ideal surface.
5) The surface of the polished polishing solution is easy to clean, and the problem of particle residue is solved.
Detailed Description
The following further describes embodiments of the present invention with reference to examples. The following examples are only for illustrating the technical solutions of the present invention more clearly, and the protection scope of the present invention is not limited thereby.
The invention provides a polishing composition for silicon carbide CMP, which is prepared by the following method: sequentially adding 0.05-5 parts by weight (preferably 0.1-2 parts by weight) of dispersing agent, 0.1-5 parts by weight of accelerator, 0.5-1 part by weight of pH buffering agent, 0.005-0.1 part by weight of wetting agent and 0.01-5 parts by weight (preferably 0.2-2 parts by weight) of complexing agent into 5-40 parts by weight (preferably 10-30 parts by weight) of silica sol abrasive under stirring, adding 0.01-0.1 part by weight (preferably 0.02-0.05 part by weight) of defoaming agent, adjusting the pH value of the solution to 11-13 (preferably 12.5) by using 0.5-1.0 part by weight of pH regulator, diluting the solution to a required amount by using water, and aging for 30-60 minutes (preferably 20 minutes);
the dispersant is polystyrene maleic anhydride and derivatives thereof, preferably sulfonated styrene maleic anhydride copolymer (SMA);
the accelerant is an oxidant comprising peroxide, overflowing compound, halogen acid, perhalogenated acid and nitro compound; the oxidant can be one or more selected from perchloric acid, potassium perchlorate, potassium chlorate, sodium chlorate, periodic acid, potassium periodate, sodium periodate, iodic acid, potassium iodate, hydrogen peroxide, ozone, potassium persulfate, ammonium persulfate, sodium persulfate, potassium nitrate, sodium nitrate and ammonium nitrate;
the pH buffering agent is a hydrogen phosphate and phosphate conjugated system;
the wetting agent can be selected from acetylene glycol polyether;
the complexing agent can be selected from one or more of 2-phosphonic acid butane-1, 2, 4-tricarboxylic acid (PBTC), amino trimethylene phosphonic Acid (ATMP), Ethylene Diamine Tetra Methylene Phosphonic Acid (EDTMPA), diethylenetriamine pentamethylene phosphonic acid (DTPMPA), polyamino polyether methylene Phosphonic Acid (PAPEMP), hydroxy ethylidene diphosphonic acid (HDPE);
the complexing agent can also be selected from one or more of aliphatic monobasic acid, aliphatic dibasic acid, aliphatic polybasic carboxylic acid, acetic acid, oxalic acid, citric acid, tartaric acid, malic acid, malonic acid, succinic acid and tetraethyl oxalic acid;
the abrasive is silicon dioxide, the abrasive is spherical, spindle-shaped or chain-shaped, and the particle size is 60-150 nm (preferably 80-120 nm);
the defoaming agent can be a polyether defoaming agent;
the pH regulator can be 50% potassium hydroxide solution.
The specific embodiment of the invention is as follows:
example 1
0.1 part by weight of sulfonated SMA and 0.1 part by weight of H2O22 parts by weight of potassium hydrogen phosphate-potassium phosphate, 0.01 part by weight of acetylene glycol polyether and 0.01 part by weight of PBTC are sequentially added into 10 parts by weight of silicon dioxide solution under stirring, 0.01 part by weight of polyether defoaming agent is added, then 0.5 part by weight of potassium hydroxide is used for adjusting the pH value of the solution to 12, and the solution is aged for 40 minutes to prepare the polishing solution.
Example 2
0 is added.1 part by weight of sulfonated SMA, 0.1 part by weight of H2O2And 2 parts by weight of potassium hydrogen phosphate-potassium phosphate, 0.01 part by weight of acetylene glycol polyether and 0.5 part by weight of PBTC, and sequentially adding 10 parts by weight of silicon dioxide, 0.01 part by weight of a polyether defoaming agent, adjusting the pH value of the solution to 12 by using 0.5 part by weight of potassium hydroxide, and aging for 40 minutes to obtain the polishing solution.
Example 3
0.1 part by weight of sulfonated SMA and 0.1 part by weight of H2O22 parts by weight of potassium hydrogen phosphate-potassium phosphate, 0.1 part by weight of acetylene glycol polyether and 0.5 part by weight of PBTC, and then 10 parts by weight of silicon dioxide is sequentially added under stirring, 0.01 part by weight of polyether defoamer is added, and then 0.5 part by weight of potassium hydroxide is used to adjust the pH value of the solution to 12, and the solution is aged for 40 minutes to prepare the polishing solution.
Example 4
1.0 part by weight of sulfonated SMA and 0.1 part by weight of H2O22 parts by weight of potassium hydrogen phosphate-potassium phosphate, 0.1 part by weight of acetylene glycol polyether and 0.5 part by weight of PBTC, and then 10 parts by weight of silicon dioxide is sequentially added under stirring, 0.01 part by weight of polyether defoamer is added, and then 0.5 part by weight of potassium hydroxide is used to adjust the pH value of the solution to 12, and the solution is aged for 40 minutes to prepare the polishing solution.
Example 5
1.0 part by weight of sulfonated SMA and 0.5 part by weight of H2O22 parts by weight of potassium hydrogen phosphate-potassium phosphate, 0.1 part by weight of acetylene glycol polyether and 0.5 part by weight of PBTC, and then 10 parts by weight of silicon dioxide is sequentially added under stirring, 0.01 part by weight of polyether defoamer is added, and then 0.5 part by weight of potassium hydroxide is used to adjust the pH value of the solution to 12, and the solution is aged for 40 minutes to prepare the polishing solution.
Example 6
1.0 part by weight of sulfonated SMA and 0.5 part by weight of H2O2And 2 parts by weight of potassium hydrogen phosphate-potassium phosphate, 0.1 part by weight of acetylene glycol polyether and 0.5 part by weight of PBTC, and sequentially adding 15 parts by weight of silicon dioxide, then adding 0.01 part by weight of a polyether defoaming agent, adjusting the pH value of the solution to 12 by using 0.5 part by weight of potassium hydroxide, and aging for 40 minutes to obtain the polishing solution.
The use method of the polishing solution comprises the following steps: the polishing solution prepared by the invention is added into a charging barrel, the proper stirring speed and flow are controlled, the polishing is started, and the polishing pad adopts Suba600 or IC1000 and the like, and the pressure is 2-3 psi.
The polishing effect of the polishing solution obtained in embodiments 1 to 6 of the present invention on silicon carbide wafers is shown in the following table:
from the polishing effect, in the formula, the content of the complexing agent is increased, the grinding efficiency of the silicon carbide can be improved, the content of the wetting agent and the dispersing agent is increased, the roughness and TTV of the surface can be improved, and the content of the oxidizing agent can also improve the grinding rate to a certain extent and improve the TTV at the same time.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the technical principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (14)
1. A polishing composition for silicon carbide CMP is characterized by comprising the following components in percentage by mass:
0.05 to 5 percent of dispersant,
0.1 to 1.0 percent of accelerant,
0.5 to 1.0 percent of pH buffering agent,
0.005 to 0.1 percent of wetting agent,
0.01 to 5 percent of complexing agent,
5 to 40 percent of abrasive material,
0.01 to 0.1 percent of defoaming agent,
0.1 to 1.0 percent of pH regulator,
the balance being deionized water.
2. The polishing composition for silicon carbide CMP according to claim 1, wherein the dispersant is polystyrene maleic anhydride and a derivative thereof.
3. The polishing composition for silicon carbide CMP according to claim 1, wherein the dispersant is sulfonated styrene maleic anhydride copolymer (SMA).
4. The polishing composition for silicon carbide CMP according to claim 1, wherein the accelerator is an oxidizing agent.
5. The polishing composition for silicon carbide CMP according to claim 4, wherein the oxidizing agent is one or more selected from perchloric acid, potassium perchlorate, potassium chlorate, sodium chlorate, periodic acid, potassium periodate, sodium periodate, iodic acid, potassium iodate, hydrogen peroxide, ozone, potassium persulfate, ammonium persulfate, sodium persulfate, potassium nitrate, sodium nitrate, and ammonium nitrate.
6. The polishing composition for silicon carbide CMP according to claim 1, wherein the pH buffer is a hydrogen phosphate salt and a phosphate salt conjugated system.
7. The polishing composition for silicon carbide CMP according to claim 1, wherein the wetting agent is an acetylenic diol polyether.
8. The polishing composition for silicon carbide CMP according to claim 1, wherein the complexing agent is selected from one or more of butane-2-phosphonate-1, 2, 4-tricarboxylic acid (PBTC), aminotrimethylenephosphonic Acid (ATMP), ethylenediaminetetramethylenephosphonic acid (EDTMPA), diethylenetriaminepentamethylenephosphonic acid (DTPMPA), polyaminopolyetherylmethylenephosphonic acid (papempp), hydroxyethylidene-diphosphonic acid (HDPE).
9. The polishing composition for silicon carbide CMP according to claim 1, wherein the complexing agent is selected from one or more of the group consisting of a monobasic aliphatic acid, a dibasic aliphatic acid, a polybasic aliphatic carboxylic acid, acetic acid, oxalic acid, citric acid, tartaric acid, malic acid, malonic acid, succinic acid, and tetraethyl oxalic acid.
10. The polishing composition for silicon carbide CMP according to claim 1, wherein the water is deionized water.
11. The polishing composition for silicon carbide CMP according to claim 1, wherein the abrasive is silica, and the abrasive is spherical, spindle-shaped, or chain-shaped, and has a particle size of 60 to 150 nm.
12. The polishing composition for silicon carbide CMP according to claim 1, wherein the antifoaming agent is a polyether antifoaming agent.
13. The polishing composition for silicon carbide CMP according to claim 1, wherein the pH adjustor is potassium hydroxide.
14. The method for preparing a polishing composition for silicon carbide CMP according to any one of claims 1 to 13, wherein a dispersant, an accelerator, a pH buffer, a wetting agent, and a complexing agent are added to water, an abrasive is added after stirring uniformly, an antifoaming agent is added, the pH of the solution is adjusted to 11 to 12.5 with a pH adjuster, and aging is carried out for 30 to 60 minutes.
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Cited By (3)
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| CN114108065A (en) * | 2021-12-30 | 2022-03-01 | 左毛毛 | Aluminum alloy processing technology |
| WO2022143719A1 (en) * | 2020-12-30 | 2022-07-07 | 安集微电子科技（上海）股份有限公司 | Chemical-mechanical polishing solution and use method therefor |
| CN115011254A (en) * | 2022-06-09 | 2022-09-06 | 纳芯微电子(河南)有限公司 | Chemical mechanical polishing solution for glass wafer and preparation method and application thereof |
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| CN115011254A (en) * | 2022-06-09 | 2022-09-06 | 纳芯微电子(河南)有限公司 | Chemical mechanical polishing solution for glass wafer and preparation method and application thereof |
| CN115011254B (en) * | 2022-06-09 | 2024-03-12 | 纳芯微电子(河南)有限公司 | Chemical mechanical polishing solution for glass wafer and preparation method and application thereof |
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