CN115433522B - Chemical mechanical polishing solution and polishing method thereof - Google Patents
Chemical mechanical polishing solution and polishing method thereof Download PDFInfo
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- CN115433522B CN115433522B CN202211171861.7A CN202211171861A CN115433522B CN 115433522 B CN115433522 B CN 115433522B CN 202211171861 A CN202211171861 A CN 202211171861A CN 115433522 B CN115433522 B CN 115433522B
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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
- B24B1/00—Processes of grinding or polishing; Use of auxiliary equipment in connection with such processes
- B24B1/04—Processes of grinding or polishing; Use of auxiliary equipment in connection with such processes subjecting the grinding or polishing tools, the abrading or polishing medium or work to vibration, e.g. grinding with ultrasonic frequency
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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
- Y02P70/10—Greenhouse gas [GHG] capture, material saving, heat recovery or other energy efficient measures, e.g. motor control, characterised by manufacturing processes, e.g. for rolling metal or metal working
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Abstract
The embodiment of the invention discloses a chemical mechanical polishing solution and a polishing method thereof, wherein the silicon dioxide particles are 20-50wt%; 1-10wt% of alkaline corrosive agent; fenton reagent, 1-10wt%; complexing agent, 0.1-1wt%; 0.01-1wt% of a dispersant; the Fenton reagent comprises ferrous sulfate and hydrogen peroxide. According to the invention, the formula and the composition of the polishing solution are optimized, the Fenton reagent is added in the polishing solution, and the removal efficiency of the polishing solution is improved by utilizing the oxidizing property of the Fenton reagent; the chelating agent and ferrous ions in the Fenton reagent are added into the polishing solution to generate chelate under alkaline conditions, so that the Fenton reagent is prevented from losing efficacy; according to the invention, during the polishing process, the polishing solution is subjected to ultrasonic treatment, on one hand, ferrous ions are slowly released to form Fenton reagent with hydrogen peroxide, and on the other hand, oxidation free radicals are continuously and stably generated. The hydrogen peroxide is added in a continuous dropwise manner, so that the decomposition of the hydrogen peroxide and other components in the polishing solution under the ultrasonic condition is reduced, the performance reduction of the polishing solution is avoided, and the stability of the removal efficiency of the polishing solution is maintained.
Description
Technical Field
The invention relates to the technical field of chemical mechanical polishing, in particular to chemical mechanical polishing solution and a polishing method thereof.
Background
The polishing of hard and brittle materials such as silicon, silicon carbide, gallium nitride and the like faces two challenges of improving the removal rate and the surface quality. Typically, polishing performance is improved by adding mechanical or chemical action: in the aspect of mechanical action, large-particle-size particles or particles with large hardness such as aluminum oxide, silicon carbide and the like are mainly used for increasing and removing; in terms of chemical action, the selective catalysis, electrochemistry and other means are effective means for improving polishing performance by assisting in enhancing the corrosion rate of the surface material. However, the single action change may break the balance of the polishing system, causing deterioration in removal efficiency or surface quality, such as scratches caused by hard particles, corrosion caused by chemical action, and the like. In addition, the reported chemical assistance effect on the removal efficiency increase is not satisfactory for inert materials such as silicon carbide and gallium nitride.
Ultrasonic-assisted machining is used in hard and brittle material grinding, cutting processes to improve the kerf or post-grinding surface quality, but the action of the ultrasonic reduces the force of the abrasive tool/particles against the surface of the material to be machined, resulting in reduced removal rates. Ultrasonic waves create alternating high and low pressures in a liquid, creating small vacuum bubbles during the low pressure cycle, which collapse rapidly during the high pressure cycle, a phenomenon known as cavitation. At the moment of collapse of cavitation bubbles, high temperature (more than 5000 ℃) and high pressure (50-100 MPa) are generated. The water vapor in the cavitation bubbles (gas phase) is cracked into OH free radicals, H free radicals and the like at high temperature and high pressure. The free radicals generated by cavitation are oxides required for the polishing chemical reaction of hard brittle materials. Fenton's reagent has been used in polishing solutions for materials such as silicon carbide due to its strong oxidizing property. Studies have shown that the oxidizing properties of Fenton's reagent are further enhanced in an ultrasound environment. However, the strong oxidizing property under ultrasonic conditions risks decomposing the chemical components in the polishing liquid.
Disclosure of Invention
The technical problem to be solved by the embodiment of the invention is to provide a chemical mechanical polishing solution and a polishing method thereof, which exert the advantage of oxidizing performance of the polishing solution due to the Fenton reagent under the assistance of ultrasound and solve the problem of chemical component failure in the strong oxidizing polishing solution under the ultrasound condition.
In order to solve the technical problems, the embodiment of the invention provides a chemical mechanical polishing solution, which comprises the following components in percentage by weight:
silica particles, 20-50wt%;
1-10wt% of alkaline corrosive agent;
fenton reagent, 1-10wt%;
complexing agent, 0.1-1wt%;
0.01-1wt% of a dispersant;
the Fenton reagent comprises ferrous sulfate and hydrogen peroxide.
Correspondingly, the embodiment of the invention also provides a polishing method of the chemical mechanical polishing liquid, wherein the polishing method is to carry out ultrasonic treatment on the chemical mechanical polishing liquid in the polishing process.
The beneficial effects of the invention are as follows:
according to the invention, the formula and the composition of the polishing solution are optimized, the Fenton reagent is added in the polishing solution, and the removal efficiency of the polishing solution is improved by utilizing the oxidizing property of the Fenton reagent; in order to exert the removal effect of the corrosive reagent, the pH value of the polishing solution is fixed between 8 and 12, the hard brittle material in the range has high removal rate and good surface quality, but as the Fenton reagent is easy to generate a precipitate under the pH condition, the chelating agent and the ferrous ions in the Fenton reagent are added into the polishing solution to generate a chelate, so that the failure of the Fenton reagent is avoided;
according to the invention, the polishing method is optimized, the ultrasonic effect is adopted on the polishing solution, the cavitation phenomenon of the polishing solution is promoted, the oxidative free radicals are continuously generated, and the promotion effect is realized on stably maintaining the high removal efficiency of the polishing solution. Meanwhile, in order to avoid consumption of other components in the polishing solution by oxidation free radicals generated in a large quantity instantaneously, hydrogen peroxide is added in a continuous dropwise manner in polishing, so that decomposition of the hydrogen peroxide and other components in the polishing solution under an ultrasonic condition is reduced, the performance of the polishing solution is prevented from being reduced, and the removal efficiency of the polishing solution is maintained stable;
the polishing solution can be recycled, and the polishing method can maintain the high efficiency and the stable removal rate of the removal process in the recycling of the polishing solution.
Detailed Description
It should be noted that, without conflict, the embodiments and features of the embodiments in the present application may be combined with each other, and the present invention will be further described in detail with reference to specific embodiments.
The chemical mechanical polishing solution provided by the embodiment of the invention comprises the following components in percentage by weight:
silica particles, 20-50wt%;
1-10wt% of alkaline corrosive agent;
fenton reagent, 1-10wt%;
complexing agent, 0.1-1wt%;
0.01-1wt% of a dispersant;
the Fenton reagent comprises ferrous sulfate and hydrogen peroxide.
The alkaline corrosive agent comprises one or two of sodium hydroxide and potassium hydroxide.
The ratio of the ferrous sulfate to the hydrogen peroxide is 1:1-1:3.
By adopting the technical scheme, the polishing solution composition is optimized, and the oxidation requirement of the Fenton reagent is met by improving the content of hydrogen peroxide; on the other hand, the free radical generated by decomposing hydrogen peroxide under the ultrasonic condition further improves the oxidation efficiency.
The complexing agent comprises one or more of ethylenediamine tetraacetic acid, hexametaphosphate and hydroxyethylidene diphosphonic acid.
By adopting the technical scheme, the complexing agent added by the invention is complexed with ferrous ions in the Fenton reagent, so that the generation of ferric hydroxide precipitate by ferrous ions under alkaline conditions is avoided, and the oxidizing property of the Fenton reagent is reduced. Under the ultrasonic condition, ferrous ions are separated from the complexing agent and form Fenton reagent with hydrogen peroxide, so that oxidation is realized.
The dispersing agent comprises one or more of chitosan, polyacrylamide and sodium alginate.
By adopting the technical scheme, the added dispersing agent forms a network structure in the polishing solution, so that the agglomeration of silicon dioxide particles under the ultrasonic condition is prevented, and the defects of fluctuation of removal rate and surface scratch caused by particle agglomeration in the polishing process are avoided.
The pH value of the chemical mechanical polishing liquid is between 8 and 12.
By adopting the technical scheme, the pH value of the polishing solution is kept in alkalescent and alkaline conditions, and the chemical corrosion effect of the alkaline corrosive is exerted. The complexing agent added in the invention can avoid the problem that Fenton reagent is effective due to generation of precipitate.
As an embodiment, the polishing liquid of the present invention is applied to polishing under ultrasonic-assisted conditions, i.e., the polishing liquid of the present invention is subjected to ultrasonic treatment during polishing. The hydrogen peroxide in the Fenton reagent is slowly dripped into the polishing solution in the polishing process. As one embodiment, the polishing solution is recycled during the polishing process.
By adopting the technical scheme, the ultrasonic treatment mode of the invention promotes the cavitation phenomenon of the polishing solution, continuously and stably generates oxidative free radicals in the polishing solution, promotes the decomposition and conversion of hydrogen peroxide into the oxidative free radicals, keeps the content of the oxidative free radicals in the polishing solution stable, and promotes the improvement of polishing efficiency.
By adopting the technical scheme, the reaction rate of the Fenton reagent is controlled by slowly dripping hydrogen peroxide, and the reaction degree of the Fenton reagent and other reagents in the polishing solution under the ultrasonic condition is reduced. Meanwhile, the generation of a large amount of oxidative free radicals by instantaneous decomposition under the ultrasonic condition after the hydrogen peroxide is added at one time is avoided. The oxidation free radicals can react with chemical reagents in the polishing solution, a large amount of surplus free radicals can consume active ingredients in the polishing solution, and hydrogen peroxide is slowly added dropwise, so that the defects are overcome.
The polishing method of the chemical mechanical polishing solution comprises the following steps:
step 1: sequentially adding the silicon dioxide particles and alkaline corrosive into a first container under stirring, and uniformly stirring to obtain a component A; sequentially adding ferrous sulfate, complexing agent and dispersing agent into the second container under the stirring condition, and uniformly stirring to obtain a component B;
step 2: slowly adding the component B into the component A, and uniformly stirring for standby to obtain uniformly-stirred polishing solution;
step 3: placing the uniformly stirred polishing solution into an ultrasonic container for ultrasonic treatment, and simultaneously slowly dripping hydrogen peroxide into the prepared polishing solution and using the solution for polishing experiments.
The polishing solution is recycled in the polishing process.
The polishing solution prepared without hydrogen peroxide in Fenton reagent is placed in an ultrasonic container, and an ultrasonic device is turned on to carry out ultrasonic treatment on the polishing solution. And slowly dripping hydrogen peroxide in the Fenton reagent into the polishing solution in the polishing process. The complexing agent is used for avoiding the generation of precipitation of iron ions under the alkaline condition, so that the oxidizing property of the Fenton reagent is reduced; meanwhile, the reaction rate of the Fenton reagent is controlled by slowly dripping hydrogen peroxide, the reaction degree of the Fenton reagent and other reagents in the polishing solution under the ultrasonic condition is reduced, and the effectiveness of the polishing solution and the polishing method is improved.
Example 1
Silica sol particles and alkaline corrosive (sodium hydroxide) are sequentially added into a container I under the stirring condition and uniformly stirred to be used as a component A, and ferrous sulfate, complexing agent (ethylenediamine tetraacetic acid) and dispersing agent (chitosan) are sequentially added into a container II under the stirring condition and uniformly stirred to be used as a component B. Slowly adding the component B into the component A and uniformly stirring for later use. Wherein the content of the silicon dioxide particles is 30wt%, the content of sodium hydroxide is 5wt%, the content of ferrous sulfate is 1wt%, the content of ethylenediamine tetraacetic acid is 0.1wt%, and the content of chitosan is 0.01wt%. Placing the uniformly stirred polishing solution into an ultrasonic container for ultrasonic treatment, and simultaneously slowly dropwise adding hydrogen peroxide into the prepared polishing solution and polishing a silicon carbide material, wherein the proportion of ferrous sulfate to hydrogen peroxide is 1:1. the removal rate for polishing for 1 hour is shown in table 1.
Example two
Silica sol particles and alkaline corrosive (potassium hydroxide) are sequentially added into a first container under the stirring condition and uniformly stirred to form a component A, and ferrous sulfate, complexing agent (sodium hexametaphosphate) and dispersing agent (polyacrylamide) are sequentially added into a second container under the stirring condition and uniformly stirred to form a component B. Slowly adding the component B into the component A and uniformly stirring for later use. Wherein the content of the silicon dioxide particles is 20wt%, the content of sodium hydroxide is 1wt%, the content of ferrous sulfate is 5wt%, the content of sodium hexametaphosphate is 1wt%, and the content of polyacrylamide is 0.5wt%. Placing the uniformly stirred polishing solution into an ultrasonic container for ultrasonic treatment, and simultaneously slowly dropwise adding hydrogen peroxide into the prepared polishing solution and polishing a silicon carbide material, wherein the proportion of ferrous sulfate to hydrogen peroxide is 1:1. the removal rate for polishing for 1 hour is shown in table 1.
Example III
Silica sol particles and alkaline corrosive (sodium hydroxide) are sequentially added into a container I under the stirring condition and uniformly stirred to be used as a component A, and ferrous sulfate, complexing agent (hydroxyethylidene diphosphonic acid) and dispersing agent (sodium alginate) are sequentially added into a container II under the stirring condition and uniformly stirred to be used as a component B. Slowly adding the component B into the component A and uniformly stirring for later use. Wherein the content of the silicon dioxide particles is 50wt%, the content of sodium hydroxide is 10wt%, the content of ferrous sulfate is 10wt%, the content of hydroxyethylidene diphosphonic acid is 0.5wt%, and the content of sodium alginate is 1wt%. Placing the uniformly stirred polishing solution into an ultrasonic container for ultrasonic treatment, and simultaneously slowly dropwise adding hydrogen peroxide into the prepared polishing solution and polishing a silicon carbide material, wherein the proportion of ferrous sulfate to hydrogen peroxide is 1:2. the removal rate for polishing for 1 hour is shown in table 1.
Comparative example one
Silica sol particles and alkaline corrosive (sodium hydroxide) are sequentially added into a first container under the stirring condition and uniformly stirred to form a component A, and ferrous sulfate and dispersing agent (sodium alginate) are sequentially added into a second container under the stirring condition and uniformly stirred to form a component B. Slowly adding the component B into the component A and uniformly stirring for later use. Wherein the content of the silicon dioxide particles is 50wt%, the content of the sodium hydroxide is 10wt%, the content of the ferrous sulfate is 10wt%, and the content of the sodium alginate is 1wt%. Placing the uniformly stirred polishing solution into an ultrasonic container for ultrasonic treatment, and simultaneously slowly dropwise adding hydrogen peroxide into the prepared polishing solution and polishing a silicon carbide material, wherein the proportion of ferrous sulfate to hydrogen peroxide is 1:2. the removal rate for polishing for 1 hour is shown in table 1.
Comparative example two
Silica sol particles and alkaline corrosive (sodium hydroxide) are sequentially added into a container I under the stirring condition and uniformly stirred to be used as a component A, fenton reagent (the proportion of ferrous sulfate to hydrogen peroxide is 1:2), complexing agent (hydroxyethylidene diphosphonic acid) and dispersing agent (sodium alginate) are sequentially added into the container II under the stirring condition and uniformly stirred to be used as a component B. Slowly adding the component B into the component A and uniformly stirring for later use. Wherein the content of the silicon dioxide particles is 50wt%, the content of sodium hydroxide is 10wt%, the content of ferrous sulfate is 10wt%, the content of hydroxyethylidene diphosphonic acid is 0.5wt%, and the content of sodium alginate is 1wt%. The uniformly stirred polishing solution was placed in an ultrasonic container for ultrasonic treatment and used for polishing silicon carbide materials, and the removal rate of polishing for 1 hour is shown in table 1.
Comparative example three
Silica sol particles and alkaline corrosive (sodium hydroxide) are sequentially added into a first container under the stirring condition and uniformly stirred to form a component A, and ferrous sulfate and dispersing agent (sodium alginate) are sequentially added into a second container under the stirring condition and uniformly stirred to form a component B. Slowly adding the component B into the component A and uniformly stirring for later use. Wherein the content of the silicon dioxide particles is 50wt%, the content of the sodium hydroxide is 10wt%, the content of the ferrous sulfate is 10wt%, and the content of the sodium alginate is 1wt%. Meanwhile, hydrogen peroxide is slowly dripped into the prepared polishing solution and is used for polishing the silicon carbide material, and the proportion of ferrous sulfate to hydrogen peroxide is 1:2. the removal rate for polishing for 1 hour is shown in table 1.
The polishing results of each example and comparative example are shown in Table 1:
TABLE 1
| Removal rate (nm/h) of 0-30min | Removal rate (nm/h) of 30-60min | |
| Example 1 | 120 | 120 |
| Example two | 123 | 123 |
| Example III | 125 | 125 |
| Comparative example one | 70 | 70 |
| Comparative example two | 130 | 50 |
| Comparative example three | 75 | 75 |
As can be seen from the first to third embodiments, the silicon carbide material removal rate is 120-125 nm/h, and the removal rate is stable within 1 hour by using the polishing solution and the polishing method; comparative example one the removal rate was reduced to 70 nm/h as part of the Fenton reagent lost the oxidizing property due to no complexing agent added; the removal rate of the second first half hour of the comparative example reaches 130 nm/h, because the oxydol is added at one time, so that the oxidation free radical in the polishing solution is suddenly increased, the removal efficiency is increased, however, because a large amount of free radicals react with the components of the polishing solution, the removal rate of the second half hour is sharply reduced to 50 nm/h; in the third comparative example, no ultrasonic auxiliary effect is adopted, free radicals generated by cavitation effect are not contained in the polishing solution, and the removal rate is reduced to 75 nm/h. Thus, the advantages of the polishing solution and the polishing method can be seen.
The invention can be applied to hard brittle materials such as silicon, gallium nitride and the like to show the same advantages.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the spirit and scope of the invention as defined by the appended claims and their equivalents.
Claims (5)
1. A polishing method of a chemical mechanical polishing liquid, which is characterized in that the polishing method is to carry out ultrasonic treatment on the chemical mechanical polishing liquid in the polishing process;
the polishing solution comprises the following components in percentage by weight:
silica particles, 20-50wt%;
1-10wt% of alkaline corrosive agent;
fenton reagent, 1-10wt%;
complexing agent, 0.1-1wt%;
0.01-1wt% of a dispersant;
the Fenton reagent comprises ferrous sulfate and hydrogen peroxide;
the complexing agent comprises one or more of ethylenediamine tetraacetic acid, hexametaphosphate and hydroxyethylidene diphosphonic acid; the ratio of the ferrous sulfate to the hydrogen peroxide is in the range of 1:1 to 1:3; the pH value range of the polishing solution is 8-12;
and slowly dripping hydrogen peroxide in the Fenton reagent into the polishing solution in the polishing process.
2. The method of polishing a chemical mechanical polishing slurry according to claim 1, comprising:
step 1: sequentially adding the silicon dioxide particles with specific gravity as set forth in claim 1 and an alkaline corrosive into a first container under stirring, and uniformly stirring to obtain a component A; sequentially adding ferrous sulfate with specific gravity as defined in claim 1, a complexing agent and a dispersing agent into a second container under stirring, and uniformly stirring to obtain a component B;
step 2: slowly adding the component B into the component A, and uniformly stirring for standby to obtain uniformly-stirred polishing solution;
step 3: placing the uniformly stirred polishing solution in an ultrasonic container for ultrasonic treatment and polishing, and simultaneously slowly dropwise adding the hydrogen peroxide with specific gravity as defined in claim 1 into the polishing solution in the polishing process.
3. The method of claim 1, wherein the polishing solution is recycled during polishing.
4. The method for polishing a chemical mechanical polishing liquid according to claim 1, wherein the alkaline etchant is one or both of sodium hydroxide and potassium hydroxide.
5. The method of polishing a chemical mechanical polishing liquid according to claim 1, wherein the dispersant comprises one or more of chitosan, polyacrylamide, and sodium alginate.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101180379A (en) * | 2005-03-25 | 2008-05-14 | 杜邦纳米材料气体产品有限公司 | Dihydroxy enol compounds used in chemical mechanical polishing compositions having metal ion oxidizers |
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| JP3075352B2 (en) * | 1998-04-15 | 2000-08-14 | 日本電気株式会社 | Method and apparatus for supplying chemical mechanical polishing liquid |
| JP6148932B2 (en) * | 2013-08-20 | 2017-06-14 | 花王株式会社 | Polishing liquid composition for magnetic disk substrate |
| CN104745094B (en) * | 2013-12-26 | 2018-09-14 | 安集微电子（上海）有限公司 | A kind of chemical mechanical polishing liquid |
| US9481811B2 (en) * | 2015-02-20 | 2016-11-01 | Cabot Microelectronics Corporation | Composition and method for polishing memory hard disks exhibiting reduced edge roll-off |
| CN108581817B (en) * | 2018-04-02 | 2020-11-27 | 浙江工业大学 | Method and device for Fenton-assisted three-phase flow hydrodynamic cavitation polishing of SiC optical curved surface |
| CN110370100B (en) * | 2019-05-30 | 2020-11-03 | 浙江工业大学 | Method for preparing hemispherical concave die array by Fenton auxiliary composite rod micro-ultrasonic sphere |
| CN110181388B (en) * | 2019-06-03 | 2020-09-11 | 浙江工业大学 | Cavitation and Fenton reaction assisted SiC plane low-pressure homogenizing polishing method and device |
| CN115011256A (en) * | 2022-07-01 | 2022-09-06 | 盐城工学院 | Chemical mechanical polishing solution for gallium nitride soft and hard mixed abrasive combined with photocatalysis and Fenton reaction and polishing method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101180379A (en) * | 2005-03-25 | 2008-05-14 | 杜邦纳米材料气体产品有限公司 | Dihydroxy enol compounds used in chemical mechanical polishing compositions having metal ion oxidizers |
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