CN115124927A - Green chemical mechanical polishing solution for silicon carbide crystals - Google Patents

Green chemical mechanical polishing solution for silicon carbide crystals Download PDF

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Publication number
CN115124927A
CN115124927A CN202210838534.6A CN202210838534A CN115124927A CN 115124927 A CN115124927 A CN 115124927A CN 202210838534 A CN202210838534 A CN 202210838534A CN 115124927 A CN115124927 A CN 115124927A
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silicon carbide
polishing
polishing solution
concentration
chemical mechanical
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CN202210838534.6A
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金洙吉
杨辉鹏
沈煜
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Dalian University of Technology
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Dalian University of Technology
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09GPOLISHING COMPOSITIONS; SKI WAXES
    • C09G1/00Polishing compositions
    • C09G1/02Polishing compositions containing abrasives or grinding agents

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Mechanical Treatment Of Semiconductor (AREA)
  • Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)

Abstract

The green chemical mechanical polishing solution for the silicon carbide crystals is a green, efficient and high-quality chemical mechanical polishing solution for the silicon carbide crystals, comprises hydrogen peroxide, aluminum oxide, sodium bicarbonate, a dispersing agent and deionized water, and is used for chemically and mechanically polishing the silicon carbide crystals. Wherein the concentration of the hydrogen peroxide is 20 wt% -30 wt%, the concentration of the aluminum oxide is 3 wt% -8 wt%, the molar ratio of the hydrogen peroxide to the sodium bicarbonate is 5-20, the concentration of the dispersing agent is 0.5 wt% to 5 wt%, and the balance is deionized water. After the polishing solution is used for polishing the silicon carbide crystal, an ultra-smooth surface with the surface roughness of 0.081nm can be obtained with the material removal rate of 132 nm/h. In addition, the polishing solution is different from other traditional polishing solutions containing strong acid, strong base and heavy metal ions, contains various components and reaction products which have no pollution to the environment, can solve the problems of difficult treatment and high treatment cost of polishing waste liquid in the industrial production process, reduces the production cost, and is beneficial to large-scale industrial production.

Description

Green chemical mechanical polishing solution for silicon carbide crystals
Technical Field
The invention belongs to the technical field of ultraprecise processing of superhard materials, and relates to a green high-quality silicon carbide crystal chemical mechanical polishing solution.
Background
The semiconductor industry is an important development field of the industry integration and transformation innovation of China, and common semiconductor materials comprise silicon, germanium, gallium arsenide and the like. Silicon carbide crystals, which are typical third-generation semiconductor materials, have the advantages of high thermal conductivity, high breakdown field strength, high electron drift rate, large forbidden band width and the like. Due to the characteristics of high efficiency, high temperature and high frequency, silicon carbide crystals are very important in fields with extremely strict requirements on temperature and efficiency. The method is widely applied to photovoltaic industry, new energy automobile motor controllers, PFC/power supplies and the like.
The service performance of the components is influenced by the processing quality and precision of the silicon carbide crystal. Therefore, a high quality of the processed surface is a necessary requirement for silicon carbide crystals as substrate materials. Chemical mechanical polishing is a technology for realizing the ultra-smooth processing of the crystal surface through the synergistic action of mechanical removal and chemical corrosion, and is the only method for realizing the global planarization of the silicon carbide crystal at present. The polishing liquid is a key factor determining the polishing quality. In addition, domestic polishing solutions often contain strong acid, strong base and heavy metal ions. The polishing waste liquid can cause serious pollution to the environment. The neutralization of strong acid and strong base in the polishing waste liquid and the removal of heavy metal ions increase the treatment cost of the waste liquid. Therefore, the development of the green, high-efficiency and high-quality chemical mechanical polishing solution for the silicon carbide crystals has important practical significance for breaking foreign monopoly and realizing the localization of the semiconductor industry.
Disclosure of Invention
In order to solve the problems of poor quality of a processed surface, low efficiency, environmental pollution and the like of a silicon carbide crystal in the traditional chemical mechanical polishing process, the invention provides the chemical mechanical polishing solution for the silicon carbide crystal, and the green, high-efficiency and high-quality chemical mechanical polishing of the silicon carbide crystal is realized.
In order to achieve the purpose, the invention adopts the technical scheme that:
the chemical mechanical polishing solution for the green and high-quality silicon carbide crystals comprises hydrogen peroxide, alumina abrasive particles, sodium bicarbonate, a dispersing agent and deionized water. Wherein: the concentration of the hydrogen peroxide is 20 to 30 weight percent; the grain diameter of the alumina abrasive grain is 0.03-1 μm, and the concentration is 3-8 wt%; the molar ratio of the hydrogen peroxide to the sodium bicarbonate is 5-20; the concentration of the dispersant is 0.5 to 3 weight per thousand. The weight percentage of the deionized water is 62-87%. The polishing solution is dripped to polish silicon carbide crystals.
Further, the dispersing agent is one or more of polyethylene glycol, glycerol, ethanol and HPMA.
And (3) mixing the components at room temperature, uniformly stirring, and oscillating in ultrasonic equipment for 10min to obtain the polishing solution.
The invention has the following effects and benefits:
1) the invention activates hydrogen peroxide through sodium bicarbonate, so that a large amount of ROS (reactive oxygen species) is generated in the polishing solution. ROS has strong oxidizability, and can oxidize the surface of the silicon carbide to form a soft oxide layer on the surface. And finally, removing the oxide layer under the action of the abrasive particles to form an ultra-smooth surface.
2) Compared with the traditional polishing solution, the surface roughness of the polished silicon carbide crystal is reduced, and the material removal rate is improved.
3) The pH of the polishing solution is neutral, and the reaction product of the hydrogen peroxide as the oxidant and the sodium bicarbonate as the active agent is mainly CO 2 、O 2 、H 2 O, no pollution to the environment and environmental protection.
4) The polishing waste liquid does not need special treatment, and the abrasive particles can be discharged after being filtered, so that the waste liquid treatment cost is reduced, and the economic requirement of industrial production is met.
Drawings
FIG. 1 is a graph showing the measurement of the surface roughness profile of a polished silicon carbide crystal silicon surface using a ZygoNewView 9000 white light interferometer of the present invention. The results show a surface roughness of 0.267nm and a material removal rate of 70 nm/h.
FIG. 2 is a graph showing the measurement of the surface roughness profile of a polished silicon carbide crystal silicon surface using a ZygoNewView 9000 white light interferometer of the present invention. The results show that the surface roughness is 0.225nm and the material removal rate is 89 nm/h.
FIG. 3 is a graph showing the measurement of the surface roughness profile of a polished silicon carbide crystal silicon surface using a ZygoNewView 9000 white light interferometer of the present invention. The results show a surface roughness of 0.081nm and a material removal rate of 132 nm/h.
Detailed Description
The invention is further illustrated by the following specific examples, which should not be construed as limiting the scope of the invention.
The polishing sample piece is a silicon surface of the silicon carbide crystal, and the size of the polishing sample piece is 1cm multiplied by 1 cm. The three silicon carbide crystal samples are uniformly adhered to the carrier plate. The used polishing machine is a UNIPOL-1200S automatic grinding polishing machine, the rotation speed of a polishing disc is set to be 70rpm, the polishing pressure is set to be 0.03MPa, the rotation speed of the polishing disc is 70r/min, the polishing pad is a polyurethane polishing pad with the phi of 300mm, the flow of polishing liquid is 10ml/min, and the polishing time is 60 min.
After polishing, the surface roughness was measured using a ZygoNewView 9000 white light interferometer. The scan range is 10 μm × 10 μm.
Example 1:
polishing solution: the concentration of hydrogen peroxide is 10 wt%, the concentration of alumina abrasive particles is 3 wt%, the particle size is 1 mu m, the molar ratio of hydrogen peroxide to sodium bicarbonate is 5, the weight percentage of deionized water is 87%, and the concentration of dispersing agent HPMA is 0.5 wt%. After mixing, stirring evenly and oscillating for 10min in an ultrasonic device.
The surface roughness of the silicon surface of the polished silicon carbide crystal is 0.267nm (see the attached figure 1), and the material removal rate is 70 nm/h.
Example 2:
polishing solution: the concentration of hydrogen peroxide is 20 wt%, the concentration of alumina is 5 wt%, the particle size is 0.5 μm, the molar ratio of hydrogen peroxide to sodium bicarbonate is 20, the weight percentage of deionized water is 75%, and the concentration of the dispersant glycerol is 2 wt%. After mixing, stirring evenly and oscillating for 10min in an ultrasonic device.
The surface roughness of the silicon surface of the polished silicon carbide crystal is 0.225nm (see the attached figure 2), and the material removal rate is 89 nm/h.
Example 3:
polishing solution: the concentration of hydrogen peroxide is 30 wt%, the concentration of aluminum oxide is 8 wt%, the particle size is 0.03nm, the molar ratio of hydrogen peroxide to sodium bicarbonate is 10, the weight percentage of deionized water is 62%, and the concentration of dispersant polyethylene glycol is 5 wt%. After mixing, stirring evenly and oscillating for 10min in an ultrasonic device.
The surface roughness of the silicon surface of the polished silicon carbide crystal is 0.081nm (shown in figure 3), and the material removal rate is 132 nm/h. Namely, after the polishing liquid is used for polishing the silicon carbide crystal, an ultra-smooth surface with the surface roughness of 0.081nm can be obtained with the material removal rate of 132 nm/h.
The above-mentioned embodiments only represent the embodiments of the present invention, but they should not be understood as the limitation of the scope of the present invention, and it should be noted that those skilled in the art can make several variations and modifications without departing from the spirit of the present invention, and these all fall into the protection scope of the present invention.

Claims (3)

1. The green and high-quality chemical mechanical polishing solution for the silicon carbide crystals can be used for polishing the silicon carbide crystals by dripping the polishing solution, and is characterized in that the components of the polishing solution comprise hydrogen peroxide, alumina abrasive particles, sodium bicarbonate, a dispersing agent and deionized water;
the concentration of the hydrogen peroxide is 20 to 30 weight percent; the concentration of the alumina is 3 to 8 weight percent; the molar ratio of the hydrogen peroxide to the sodium bicarbonate is 5-20; the concentration of the dispersant is 0.5 to 3 weight per thousand; the balance being deionized water.
2. The chemical mechanical polishing solution for green and high quality silicon carbide crystals according to claim 1, wherein the alumina abrasive grains have a grain size of 0.03 to 1 μm.
3. The chemical mechanical polishing solution for green and high-quality silicon carbide crystals according to claim 1, wherein the dispersant is one or more of polyethylene glycol, glycerol, ethanol and HPMA.
CN202210838534.6A 2022-07-18 2022-07-18 Green chemical mechanical polishing solution for silicon carbide crystals Pending CN115124927A (en)

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Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2010040280A1 (en) * 2008-10-10 2010-04-15 安集微电子(上海)有限公司 Chemical-mechanical polishing liquid
CN102533124A (en) * 2010-12-31 2012-07-04 上海硅酸盐研究所中试基地 Polishing solution for silicon carbide substrate
CN104835731A (en) * 2015-05-05 2015-08-12 山东天岳晶体材料有限公司 Quick polishing method for large-dimension 4H,6H-SiC wafer
CN105773399A (en) * 2016-03-29 2016-07-20 清华大学 Polishing solution, polishing machine and polishing method
CN107880784A (en) * 2017-12-04 2018-04-06 苏州市宽道模具机械有限公司 A kind of high-performance polishing fluid and preparation method thereof
CN109554119A (en) * 2018-11-02 2019-04-02 山东天岳先进材料科技有限公司 A kind of stability-enhanced silicon carbide chemical mechanical polishing liquid of pH and its application
CN111073520A (en) * 2019-12-25 2020-04-28 苏州纳迪微电子有限公司 Polishing powder for polishing silicon carbide wafer, preparation method thereof and polishing solution
WO2021135805A1 (en) * 2019-12-31 2021-07-08 安集微电子(上海)有限公司 Chemical-mechanical polishing liquid and use thereof in copper polishing
CN114654380A (en) * 2022-04-07 2022-06-24 大连理工大学 Electrochemical mechanical polishing method for silicon carbide wafer

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2010040280A1 (en) * 2008-10-10 2010-04-15 安集微电子(上海)有限公司 Chemical-mechanical polishing liquid
CN102533124A (en) * 2010-12-31 2012-07-04 上海硅酸盐研究所中试基地 Polishing solution for silicon carbide substrate
CN104835731A (en) * 2015-05-05 2015-08-12 山东天岳晶体材料有限公司 Quick polishing method for large-dimension 4H,6H-SiC wafer
CN105773399A (en) * 2016-03-29 2016-07-20 清华大学 Polishing solution, polishing machine and polishing method
CN107880784A (en) * 2017-12-04 2018-04-06 苏州市宽道模具机械有限公司 A kind of high-performance polishing fluid and preparation method thereof
CN109554119A (en) * 2018-11-02 2019-04-02 山东天岳先进材料科技有限公司 A kind of stability-enhanced silicon carbide chemical mechanical polishing liquid of pH and its application
CN111073520A (en) * 2019-12-25 2020-04-28 苏州纳迪微电子有限公司 Polishing powder for polishing silicon carbide wafer, preparation method thereof and polishing solution
WO2021135805A1 (en) * 2019-12-31 2021-07-08 安集微电子(上海)有限公司 Chemical-mechanical polishing liquid and use thereof in copper polishing
CN114654380A (en) * 2022-04-07 2022-06-24 大连理工大学 Electrochemical mechanical polishing method for silicon carbide wafer

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