CN114806414B - Silicon polishing composition, preparation method and application thereof - Google Patents
Silicon polishing composition, preparation method and application thereof Download PDFInfo
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- CN114806414B CN114806414B CN202210480119.8A CN202210480119A CN114806414B CN 114806414 B CN114806414 B CN 114806414B CN 202210480119 A CN202210480119 A CN 202210480119A CN 114806414 B CN114806414 B CN 114806414B
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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
- B24B29/00—Machines or devices for polishing surfaces on work by means of tools made of soft or flexible material with or without the application of solid or liquid polishing agents
- B24B29/02—Machines or devices for polishing surfaces on work by means of tools made of soft or flexible material with or without the application of solid or liquid polishing agents designed for particular workpieces
Abstract
The invention provides a silicon polishing composition, a preparation method and application thereof. The piperazine substance and the furan ring-containing water-soluble organic weak acid are added into the silicon polishing composition as the stability auxiliary agent, so that the abrasive aggregation can be effectively inhibited, the storage time and the service life of the polishing solution are prolonged, and the silicon polishing composition has obvious advantages compared with the prior art.
Description
Technical Field
The invention relates to the technical field of chemical mechanical polishing, in particular to a silicon polishing composition, a preparation method and application thereof.
Background
Silicon is the most widely used semiconductor material at present, and plays an irreplaceable role in realizing global informatization of human beings. High purity monocrystalline silicon is mainly used as a substrate material in integrated circuit fabrication, and on the surface thereof, hundreds of millions of transistors including a source electrode, a gate electrode, and a drain electrode are formed through processes such as photolithography, ion implantation, deposition, and the like, thereby forming a "base stone" of the entire chip. With the advent of VLSI, ULSI, SLSI level integrated circuits, the chip integration level has increased and feature sizes have decreased, and thus higher demands have been placed on the substrate wafer.
The preparation method of the monocrystalline silicon substrate comprises two methods of smelting purification and epitaxial growth, wherein the smelting purification uses quartz sand as a raw material, and the quartz sand is processed into a silicon wafer through processes of purifying, pulling, slicing and the like. Polishing is an indispensable process, and by polishing, a surface damage layer generated during a silicon wafer dicing process can be effectively removed, improving surface quality, and Chemical Mechanical Polishing (CMP) technology is considered to be the most effective method for global planarization of a wafer at present. Chemical mechanical polishing techniques rely on chemical action, mechanical action, and a combination of both actions in the polishing process to polish the surface. In the silicon wafer polishing process, the silicon wafer reacts with chemical additives in the polishing solution to form a soft layer on the surface, and the soft layer is peeled off and removed under the mechanical action of the abrasive and the polishing pad, so that the polishing solution has an important influence on the polishing quality of the surface of the silicon wafer.
Because the Mohs hardness of silicon dioxide and silicon is 7, and the silicon dioxide also has the advantages of fine granularity, thinner damaged layer on the surface of the polished wafer, small oxidation induced stacking fault (OSF) and the like, the nano-scale silicon dioxide colloid becomes a main abrasive of the silicon wafer polishing liquid at present, and components such as a speed accelerator, a pH regulator, a surfactant, a humectant and the like are also added into the polishing liquid. However, due to nano SiO 2 The particle size is small, the specific surface area is large, the surface energy is high, the conductivity of the polishing solution is large when the polishing solution is concentrated in a high-power way (15-40), the nanometer silicon oxide particles in the system are under high ionic strength, the surface double electric layer is compressed, the zeta potential is reduced, the particles have a tendency of mutually attracting and agglomerating to reduce the surface energy, and the polishing solution can deteriorate and lose efficacy.
Korean patent application KR1020050067846a proposes adding anionic surfactants such as sodium dodecyl sulfate and sodium dodecyl ether sulfate to a silicon polishing liquid, enhancing negative charges on surfaces of silica sol particles by physical adsorption, increasing inter-particle repulsive force, and achieving an improvement in storage stability of the polishing liquid. However, the adsorption of the anionic surfactant also increases the repulsive force between the silica sol particles and the silicon wafer, and the surfactant also obviously weakens the sliding friction force between the abrasive and the substrate, reduces the mechanical action in the polishing process, and leads to the reduction of the polishing rate. In addition, sodium ions are introduced into the substances, so that metal ions on the surface of the polished silicon wafer are easy to pollute.
Chinese patent applications CN201811627080.8 and CN201110002321.1 respectively propose that silane coupling agents such as 3-aminopropyl triethoxysilane and methyltrimethoxysilane are added into a silicon polishing solution, and organic matters with sulfonic groups are grafted on the surfaces of silica sol particles to improve the storage stability of the polishing solution and reduce the silica sol particles on the polishing surfaceResidual, however due to nano SiO 2 The grafting coating of the surface molecular layer weakens the adsorption and carrying effects of the surface molecular layer on reaction products such as silicate ions and the like, and can also have obvious adverse effects on the polishing rate. The method for preparing the high-stability silica sol is proposed in the U.S. Pat. No. 3,970A 1 and Canadian patent CA2936498C, which are favorable for preparing the high-stability polishing solution, but the method has higher cost and low practical application value in the field of silicon wafer polishing solution.
In the aspect of the research of polishing solution components, chinese patent application CN 111378384A proposes to polish a silicon wafer by adopting 4-10% of piperazine and monoethanolamine to perform a synergistic effect, while patent CN104046246B selects piperazine derivatives as corrosion inhibitors for polishing metal tungsten, and the main mechanisms of the piperazine derivatives are alkalinity of piperazine substances and adsorptivity of the piperazine substances to the surface of a polished material. Also patent CN104099026B mentions that piperazine or piperazine derivatives and guanidine carbonate are used as a rate accelerator, both exert a synergistic effect to enhance the polishing rate of silicon wafers, and piperazine derivatives, such as piperazine hydrochloride, may also have the effect of preventing precipitation of the composition. However, the patent only mentions that the concentrated composition is capable of remaining free from precipitation for two weeks at 21 ℃, and the polishing composition is often not used for a short period of time after preparation during actual production and use, and the storage time may be several months or even one year, so that not only is it required that the composition is free from precipitation during storage, but also that an increase in average particle size due to aggregation of the abrasive is avoided to prevent variations in uniformity of polishing rate. Thus, even though piperazine-based materials are added as stabilizers for polishing compositions in the prior art, the stability of the polishing compositions is far from the level of application by the addition of only such materials.
Therefore, there remains a need for a new silicon polishing composition that reduces the tendency of silica sol abrasive agglomeration through chemical formulation control and improves the storage stability and cyclical polishing performance of the polishing slurry to overcome the above-described deficiencies of the prior art.
Disclosure of Invention
In order to solve the technical problems, the invention provides a silicon polishing composition, which can effectively inhibit abrasive agglomeration and prolong the storage time and recycling performance of polishing solution by adding piperazine substances and furan ring-containing water-soluble organic weak acid as stabilizers.
It is another object of the present invention to provide a method of preparing such a silicon polishing composition.
It is a further object of the present invention to provide the use of such a silicon polishing composition in the chemical mechanical polishing of silicon wafers.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a silicon polishing composition comprises nano silicon dioxide colloid, piperazine substance, water-soluble organic weak acid containing furan ring, speed accelerator, pH regulator, surfactant, optional humectant and antibacterial agent, and deionized water.
In a preferred embodiment, the silicon polishing composition comprises the following components in percentage by mass: 2.5 to 40 weight percent of nano silicon dioxide colloid, 0.2 to 3.5 weight percent of piperazine substance, 0.01 to 1.4 weight percent of water-soluble organic weak acid containing furan ring, 1 to 15 weight percent of speed accelerator, 0.1 to 4 weight percent of pH regulator, 0.005 to 1.5 weight percent of surfactant, 0 to 2.5 weight percent of humectant, 0 to 1.0 weight percent of bacteriostat and the balance of deionized water.
In a more preferred embodiment, the silicon polishing composition comprises the following components in percentage by mass: 5 to 25 weight percent of nano silicon dioxide colloid, 0.5 to 2.5 weight percent of piperazine substance, 0.075 to 0.75 weight percent of water-soluble organic weak acid containing furan ring, 3 to 10 weight percent of speed accelerator, 1.0 to 2.5 weight percent of acid pH regulator, 0.01 to 0.5 weight percent of surfactant, 0.1 to 1.0 weight percent of humectant, 0.05 to 0.1 weight percent of bacteriostat, and the balance of deionized water.
In a specific embodiment, the mass ratio of the furan ring-containing water-soluble organic weak acid to the piperazine-based substance is 0.05-0.4.
In a specific embodiment, the nanosilica colloid has an average particle size of 25 to 100nm and a raw material concentration of 30 to 50wt%.
In a specific embodiment, the piperazine is selected from at least one of piperazine, 1-methylpiperazine, 2-methylpiperazine, 1-formylpiperazine, 2-oxopiperazine, 2-ethoxypiperazine, 1, 4-dimethylpiperazine, 2, 6-dimethylpiperazine, 1-ethylpiperazine, N-aminoethylpiperazine, N- (2-hydroxyethyl) piperazine, 1-acetylpiperazine, N-isopropylpiperazine, 1-allylpiperazine, N-t-butylpiperazine, 1- (3-methoxypropyl) piperazine, 1- (2-dimethylaminoethyl) piperazine, 1- (3-aminopropyl) -4-methylpiperazine, 1- (2-pyrimidinyl) piperazine, 1- (2-furoyl) piperazine, 1- (2-tetrahydrofurfuryl) piperazine, 1- (2-pyridyl) piperazine, 1- (3-pyridyl) piperazine, 1- (4-pyridyl) piperazine, preferably any of piperazine, 1-methylpiperazine, 1-ethylpiperazine, 1-allyl, 1- (2-pyrimidinyl) piperazine, 1- (2-acyl) piperazine, or 1- (4-pyridyl) piperazine.
In a specific embodiment, the furan ring-containing water-soluble organic weak acid is selected from at least any one of 2-furancarboxylic acid, 3-furancarboxylic acid, 2-tetrahydrofurancarboxylic acid, 3-methyl-2-furancarboxylic acid, 2, 5-furandicarboxylic acid, 5-hydroxymethyl-2-furancarboxylic acid, 2-furanacetic acid, 2- (furan-2-yl) -2-oxyacetic acid, 2- (5-oxotetrahydrofuran-2-yl) acetic acid, 2- (tetrahydrofuran-2-yl) acetic acid, (R) -2- (tetrahydrofuran-3-yl) acetic acid, (S) -2- (tetrahydrofuran-3-yl) acetic acid, 2-furanmethylene acetic acid, 2- (tetrahydrofuranmethoxy) acetic acid, preferably any one of 2-furancarboxylic acid, 3-furancarboxylic acid, 2-tetrahydrofurancarboxylic acid, 2-furanacetic acid, 2, 5-furandicarboxylic acid, 2- (tetrahydrofuranmethoxy) acetic acid.
In a specific embodiment, the rate accelerator is a basic compound selected from at least one of potassium hydroxide, ethylenediamine, hydroxyethyl ethylenediamine, tetrahydroxypropyl ethylenediamine, tetramethyl ammonium hydroxide, tetraethyl ammonium hydroxide, tetrapropyl ammonium hydroxide, tetrabutyl ammonium hydroxide, diethyl dimethyl ammonium hydroxide, methyl triethyl ammonium hydroxide, tetramethyl guanidine, potassium carbonate, preferably any one of potassium hydroxide, ethylenediamine, tetramethyl ammonium hydroxide, tetraethyl ammonium hydroxide, diethyl dimethyl ammonium hydroxide, tetramethyl guanidine, potassium carbonate.
In a specific embodiment, the pH adjuster is selected from at least any one of citric acid, tartaric acid, malic acid, oxalic acid, malonic acid, potassium bicarbonate, imidazole, preferably any one of citric acid, oxalic acid, potassium bicarbonate, imidazole; preferably, the pH of the silicon polishing composition is adjusted to 10 to 12.5.
In a specific embodiment, the surfactant is at least one selected from fatty alcohol polyoxyethylene ether, laureth, isomerous alcohol polyoxyethylene ether and alkylphenol polyoxyethylene, and preferably is fatty alcohol polyoxyethylene ether or isomerous alcohol polyoxyethylene ether.
In a specific embodiment, the humectant is selected from at least any one of propylene glycol, butylene glycol, hexylene glycol, glycerol, aminocyclopentanol.
In a specific embodiment, the bacteriostatic agent is selected from at least any one of 2-methyl-4-isothiazolin-3-one, 2-methyl-5-chloro-4-isothiazolin-3-one, 2-n-octyl-4-isothiazolin-3-one.
In another aspect, the method of preparing a silicon polishing composition as described above comprises the steps of:
1) Fully mixing and dispersing a rate accelerator, a pH regulator, a surfactant, an optional humectant and a bacteriostatic agent, and then dripping the mixture into a nano silicon dioxide colloid for uniform mixing;
2) Fully mixing and dispersing piperazine substances and furan ring-containing water-soluble organic weak acid, and then adding the mixture into the nano silicon dioxide colloid containing the auxiliary agent in the step 1) for mixing and dispersing to form the silicon polishing composition.
In yet another aspect, the use of the foregoing silicon polishing composition in the chemical mechanical polishing of silicon wafers.
Compared with the prior art, the invention has the following beneficial effects:
the silicon polishing composition disclosed by the invention takes the nano silicon dioxide colloid as a basic abrasive, has the advantages of high polishing speed, clean polishing surface and difficulty in scratching the surface of a silicon substrate, and in addition, piperazine substances and furan ring-containing water-soluble organic weak acid are added into the polishing composition as stability aids, and the stability of the polishing composition can be improved, the storage time and the recycling performance of the polishing composition can be prolonged, the cost is reduced, and compared with the prior art, the silicon polishing composition has remarkable advantages.
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 silicon polishing composition takes nano silicon dioxide colloid as a main polishing component, piperazine substances and furan ring-containing water-soluble organic weak acid are added as a stability auxiliary agent, namely, the piperazine substances and the furan ring-containing water-soluble organic weak acid are added as auxiliary agents on the basis of the existing silicon mechanical polishing solution taking the nano silicon dioxide colloid as an abrasive material to obtain the silicon polishing composition.
The piperazine substance is structurally characterized in that groups such as methyl, formyl, acetyl, pyrimidinyl, pyridyl and the like are respectively connected to a piperazine ring, piperazine derivatives containing halogen and benzene rings are not included, one or two carboxyl groups are mainly connected to a furan ring on the structure of a furan ring-containing water-soluble organic weak acid, and after the water-soluble organic weak acid containing the furan ring and the piperazine substance are mixed according to the mass ratio of 0.05-0.4, the solution is alkaline.
The nanometer silicon dioxide colloid particles mainly depend on mutual electrostatic repulsion in a dispersion system to avoid agglomeration and maintain stability, the electrostatic repulsion is mainly determined by the thickness of a surface double electric layer, and the higher the ionic strength of the system is, the thinner the double electric layer thickness is compressed. In general, the determination of the total ionic strength of the system is more complex, but according to Russell in 1976, it was proposed that the relationship between conductivity and ionic strength: μ=1.6x10 -5 (specific conductance) where μ represents conductivity and specific conductance represents conductivity, i.e., both are proportional, conductivity can be measured indirectly by a conductivity meterThe ionic strength of the system is described. The high-concentration silicon wafer polishing composition which is prepared by taking nano silicon dioxide colloid particles as main components has higher conductivity (generally more than 10 mS/cm), higher ionic strength, compressed double electric layers of the nano silicon dioxide colloid particles, weakened electrostatic repulsive force and easy agglomeration or sedimentation.
Piperazine substances have low solubility in water and are alkaline after hydrolysis, but have weak hydrolysis capability, and piperazine rings cannot crack, so that the piperazine substances mainly exist in the form of organic molecules in an aqueous solution system. The solubility of the water-soluble organic weak acid containing furan ring in water is smaller, the pKa value is generally larger, the ionization degree in water is weaker, and the furan ring is not broken, so that the substance mainly exists in the form of organic molecules in aqueous solution. In the high-concentration silicon wafer polishing composition, the two low-conductivity substances are added at the same time according to a proportion, the two substances have the function of promoting dissolution mutually, the pH value of a system is basically unchanged after dissolution, the viscosity is increased, and cyclic organic molecules generated by dissolution of the two substances also have the effect of preventing and buffering the movement of ions in the system, namely the substances with different acid and alkali properties of the two substances play a synergistic effect, so that the conductivity of the system is reduced, the ionic strength is weakened, the tendency of agglomeration of silica sol particles is weakened, and the stability is improved.
Wherein the particle size of the nano silica colloid is 25-100nm, including but not limited to 25nm, 30nm, 35nm, 40nm, 45nm, 50nm, 55nm, 60nm, 65nm, 70nm, 75nm, 80nm, 85nm, 90nm, 95nm and 100nm, and the raw material concentration (solid content) of the silica sol is 30-50wt%, including but not limited to 30wt%, 35wt%, 40wt%, 45wt% and 50wt%.
The piperazine is, for example, at least one selected from the group consisting of piperazine, 1-methylpiperazine, 2-methylpiperazine, 1-formylpiperazine, 2-oxopiperazine, 2-ethoxypiperazine, 1, 4-dimethylpiperazine, 2, 6-dimethylpiperazine, 1-ethylpiperazine, N-aminoethylpiperazine, N- (2-hydroxyethyl) piperazine, 1-acetylpiperazine, N-isopropylpiperazine, 1-allylpiperazine, N-t-butylpiperazine, 1- (3-methoxypropyl) piperazine, 1- (2-dimethylaminoethyl) piperazine, 1- (3-aminopropyl) -4-methylpiperazine, 1- (2-pyrimidinyl) piperazine, 1- (2-furoyl) piperazine, 1- (2-tetrahydrofurfuryl) piperazine, 1- (2-pyridinyl) piperazine, 1- (3-pyridinyl) piperazine, and 1- (4-pyridinyl) piperazine, and any one, two or more combinations of the above-mentioned piperazine substances, and preferably 1-methylpiperazine, 1-ethylpiperazine, 1-allyl, 1- (2-pyrimidinyl) piperazine, 1- (2-pyridinyl) piperazine, and 1- (2-pyridinyl) piperazine.
The above-mentioned furan ring-containing water-soluble organic weak acid is, for example, any one or more selected from the group consisting of 2-furoic acid, 3-furoic acid, 2-tetrahydrofuranoic acid, 3-tetrahydrofurancarboxylic acid, 3-methyl-2-furoic acid, 2, 5-furandicarboxylic acid, 5-hydroxymethyl-2-furoic acid, 2- (furan-2-yl) -2-oxyacetic acid, 2- (5-oxotetrahydrofuran-2-yl) acetic acid, 2- (tetrahydrofuran-2-yl) acetic acid, (R) -2- (tetrahydrofuran-3-yl) acetic acid, (S) -2- (tetrahydrofuran-3-yl) acetic acid, 2-furanmethylene acetic acid, and 2- (tetrahydrofuranmethoxy) acetic acid, and any one or more combinations of any two or more thereof, preferably 2-furoic acid, 3-furoic acid, 2-tetrahydrofurancarboxylic acid, 2-furoic acid, 2, 5-furandicarboxylic acid, and 2- (tetrahydrofuranmethoxy) acetic acid.
The mass ratio of the furan ring-containing water-soluble organic weak acid to the piperazine is 0.05 to 0.4, and for example, the mass ratio is 0.05, 0.1, 0.15, 0.2, 0.25, 0.3, 0.35, 0.4, preferably 0.15 to 0.3.
Besides the three main components of the nano silica colloid, namely piperazine substances and furan ring-containing water-soluble organic weak acid, the polishing composition is not limited to any other additive components added in the polishing composition, and can be applied to various conventional silicon chemical mechanical polishing liquid systems, and one or more of alkaline compounds, pH regulators, surfactants, optional moisturizers and/or bacteriostats can be selected by a technician to be added into the polishing composition according to the requirements of improving the silicon removal rate and improving the polishing surface quality.
Wherein the basic compound acts as a primary rate accelerator to ionize or hydrolyze in the dispersion such that OH of the polishing composition - The concentration is kept at a certain level during the recycling process so as to be beneficial to the continuous formation of the soft layer on the silicon surface. The rate accelerator is selected from at least any one of potassium hydroxide, ethylenediamine, hydroxyethyl ethylenediamine, tetrahydroxypropyl ethylenediamine, tetramethyl ammonium hydroxide, tetraethyl ammonium hydroxide, tetrapropyl ammonium hydroxide, tetrabutyl ammonium hydroxide, diethyl dimethyl ammonium hydroxide, methyl triethyl ammonium hydroxide, tetramethyl guanidine, and potassium carbonate, for example, any one of the above rate accelerators, any two or more combinations, and preferably any one of potassium hydroxide, ethylenediamine, tetramethyl ammonium hydroxide, tetraethyl ammonium hydroxide, diethyl dimethyl ammonium hydroxide, tetramethyl guanidine, and potassium carbonate.
The pH adjuster is, for example, at least one selected from the group consisting of citric acid, tartaric acid, malic acid, oxalic acid, malonic acid, potassium bicarbonate and imidazole, and is, for example, any one, a combination of any two or more of the above pH adjusters, preferably any one of citric acid, oxalic acid, potassium bicarbonate and imidazole. The pH regulator is used for regulating the pH value of the concentrated solution, so that the concentrated solution is prevented from being too strong in alkalinity to cause the dissolution of nano silicon oxide particles, and anions generated by ionization or hydrolysis of the concentrated solution have complexation effect on metal ions in the composition.
The surfactant is, for example, at least one selected from the group consisting of fatty alcohol polyoxyethylene ether, laureth, isomeric alcohol polyoxyethylene ether, and alkylphenol polyoxyethylene ether, for example, nonylphenol polyoxyethylene ether, and the like, and, for example, any one, a combination of any two or more of the above surfactants, preferably fatty alcohol polyoxyethylene ether and isomeric alcohol polyoxyethylene ether. The surfactant is used for reducing the surface tension of the composition, reducing the contact angle between the composition and the surface of the silicon wafer, and enhancing the spreadability of the composition on the surface of the silicon wafer, so that the surface roughness of the silicon wafer after polishing is reduced.
The humectant is, for example, at least one selected from propylene glycol, butylene glycol, hexylene glycol, glycerol, and aminocyclopentanol, for example, any one, a combination of any two or more of the above humectants, and preferably propylene glycol and aminocyclopentanol. The humectant is used for inhibiting the volatilization of moisture of the composition, reducing the moisture loss of the composition in the storage and cyclic polishing processes, enhancing the stability of nano silicon dioxide particles and being beneficial to enhancing the consistency of polishing rate.
The bacteriostatic agent is, for example, at least one selected from the group consisting of 2-methyl-4-isothiazolin-3-one, 2-methyl-5-chloro-4-isothiazolin-3-one and 2-n-octyl-4-isothiazolin-3-one, and for example, any one, a combination of any two or more of the above bacteriostatic agents, preferably 2-methyl-4-isothiazolin-3-one and 2-methyl-5-chloro-4-isothiazolin-3-one. The bacteriostatic agent is used for inhibiting the propagation of bacteria and fungi in the polishing solution and preventing the aging failure of the polishing solution caused by the metabolites of microorganisms.
In a specific embodiment, the composition is prepared from the following components in parts by weight:
wherein the mass ratio of the furan ring-containing water-soluble organic weak acid to the piperazine-based substance is 0.05-0.4, and the final pH of the silicon polishing composition is 10-12.5, including, for example, but not limited to, 10, 10.5, 11, 11.5, 12, 12.5, preferably 10.5-12.
The preparation method of the silicon polishing composition comprises the steps of fully mixing the speed accelerator, the pH regulator, the surfactant, the humectant and the bacteriostat firstly, and then fully mixing and dispersing the mixture with the nano silicon dioxide colloid to form a composition intermediate product; then, the piperazine substance and the water-soluble organic weak acid containing furan ring are mixed and dispersed, and then added into the composition intermediate product, and the silicon polishing composition is formed after full stirring and dispersion, wherein the dispersing means in the process comprise any one or more of mechanical stirring, ultrasonic dispersion and magnetic stirring.
The invention is further illustrated, but not limited, by the following more specific examples.
In the following examples, the polishing machine used in the polishing test of silicon wafers was a Speedfam 36B type single-sided polishing machine; the polishing pad used was a Suba800 type, the polishing rotation speed was 45rpm, the polishing pressure was 160-180 kgf, the flow was 1.5L/min, the polishing time was 10min, and the polishing temperature was controlled at 30-33 ℃. The polishing solution is filtered and then is conveyed to a polishing disk by a peristaltic pump, a trimmer is used for trimming and maintaining the polishing pad after each polishing, and pre-polishing is carried out before each polishing.
Polishing composition stability test: the average particle size of the polishing composition was measured using a Malvern Zetasizer type particle sizer.
Removal rate test: the mass of the silicon wafer before and after polishing was measured by a precision balance to obtain a mass difference Deltam, and the removal rate MRR (μm/min) was calculated from the density and surface area of the silicon wafer and the polishing time.
Unless otherwise specified, the raw materials and reagents used in the examples and comparative examples of the present invention were commercially available.
Example 1
(1) Composition intermediate preparation
20g of potassium hydroxide, 2g of oxalic acid, 0.1g of fatty alcohol polyoxyethylene ether, 1g of propylene glycol, 0.025g of 2-methyl-4-isothiazolin-3-one and 0.075g of 2-methyl-5-chloro-4-isothiazolin-3-one are dissolved in 200g of deionized water, uniformly stirred, and then the solution is added into 166.7g of 30wt% nano silicon dioxide colloid (average particle size 25 nm) while stirring, and the solution is dispersed for 15min by ultrasonic waves for later use.
(2) Formulation of polishing composition
Dissolving 4g of piperazine and 0.2g of 2-furancarboxylic acid in 100g of deionized water, stirring uniformly, adding the solution into the composition intermediate treated in the step (1) while stirring, continuously adding deionized water until the total mass of the dispersion is 2kg, magnetically stirring for 30min, packaging, and keeping the pH value of the dispersion at 10.
Example 2
(1) Composition intermediate preparation
60g of ethylenediamine, 10g of citric acid, 0.2g of fatty alcohol polyoxyethylene ether, 2g of propylene glycol, 0.25g of 2-methyl-4-isothiazolin-3-one and 0.75g of 2-methyl-5-chloro-4-isothiazolin-3-one are dissolved in 200g of deionized water and uniformly stirred, and then the solution is added into 250g of 40wt% nano silicon dioxide colloid (average particle size 40 nm) while stirring, and is dispersed for 15min by ultrasound for later use.
(2) Formulation of polishing composition
10g of 1-methylpiperazine and 1.5g of 2-tetrahydrofuranic acid are dissolved in 150g of deionized water, the mixture is stirred uniformly, the solution is added into the composition intermediate treated in the step (1) while being stirred, deionized water is continuously added until the total mass of the dispersion is 2kg, the dispersion is magnetically stirred for 30min and then packaged, and the pH value of the dispersion is 10.5.
Example 3
(1) Composition intermediate preparation
100g of tetramethylammonium hydroxide, 20g of citric acid, 2g of isomeric alcohol polyoxyethylene ether, 8g of propylene glycol, 0.3g of 2-methyl-4-isothiazolin-3-one and 0.9g of 2-methyl-5-chloro-4-isothiazolin-3-one are dissolved in 300g of deionized water and stirred uniformly, and then 750g of 40wt% nano silicon dioxide colloid (average particle size 40 nm) is added into the solution while stirring, and the solution is dispersed for 15min by ultrasound for later use.
(2) Formulation of polishing composition
30g of 1-ethylpiperazine and 6g of 2-furoic acid are dissolved in 200g of deionized water, the mixture is stirred uniformly, the solution is added into the composition intermediate product treated in the step (1) while being stirred, deionized water is continuously added until the total mass of the dispersion is 2kg, the dispersion is magnetically stirred for 30min and then packaged, and the pH value of the dispersion is 11.3.
Example 4
(1) Composition intermediate preparation
100g of diethyl dimethyl ammonium hydroxide, 50g of potassium hydroxide, 24g of oxalic acid, 5g of isomeric alcohol polyoxyethylene ether, 12g of aminocyclopentanol, 0.4g of 2-methyl-4-isothiazolin-3-one and 1.2g of 2-methyl-5-chloro-4-isothiazolin-3-one are dissolved in 300g of deionized water, uniformly stirred, and then the solution is added into 1000g of 40wt% nano silicon dioxide colloid (average particle size 70 nm) while stirring, and is dispersed for 15min by ultrasonic waves for later use.
(2) Formulation of polishing composition
40g of 1-allyl piperazine and 10g of 3-furancarboxylic acid are dissolved in 250g of deionized water, the mixture is stirred uniformly, the solution is added into the composition intermediate treated in the step (1) while being stirred, deionized water is continuously added until the total mass of the dispersion is 2kg, the dispersion is magnetically stirred for 30min and then packaged, and the pH value of the dispersion is 11.5.
Example 5
(1) Composition intermediate preparation
100g of tetramethylammonium hydroxide, 50g of tetramethylguanidine, 40g of imidazole, 8g of fatty alcohol polyoxyethylene ether, 20g of aminocyclopentanol, 0.5g of 2-methyl-4-isothiazolin-3-one and 1.5g of 2-methyl-5-chloro-4-isothiazolin-3-one are dissolved in 300g of deionized water, uniformly stirred, and then the solution is added into 1000g of 50wt% nano silicon dioxide colloid (average particle size 50 nm) while stirring, and is dispersed for 15min by ultrasonic waves for later use.
(2) Formulation of polishing composition
50g of 1- (2-pyrimidinyl) piperazine and 15g of 2, 5-furandicarboxylic acid are dissolved in 250g of deionized water, the mixture is stirred uniformly, the solution is added into the composition intermediate treated in the step (1) while being stirred, deionized water is continuously added until the total mass of the dispersion is 2kg, the dispersion is magnetically stirred for 30min and then packaged, and the pH value of the dispersion is 11.5.
Example 6
(1) Composition intermediate preparation
100g of potassium hydroxide, 100g of potassium carbonate, 50g of imidazole, 10g of fatty alcohol polyoxyethylene ether, 40g of aminocyclopentanol, 2.5g of 2-methyl-4-isothiazolin-3-one and 7.5g of 2-methyl-5-chloro-4-isothiazolin-3-one are dissolved in 500g of deionized water, uniformly stirred, and then the solution is added into 750g of 40wt% nano silicon dioxide colloid (average particle size 70 nm) while stirring, and is subjected to ultrasonic dispersion for 15min for later use.
(2) Formulation of polishing composition
60g of 1- (2-furoyl) piperazine and 21g of 2- (tetrahydrofuranmethoxy) acetic acid are dissolved in 300g of deionized water, the solution is stirred uniformly, the solution is added into the composition intermediate product treated in the step (1) while being stirred, deionized water is continuously added until the total mass of the dispersion is 2kg, the dispersion is magnetically stirred for 30min and then packaged, and the pH value of the dispersion is 12.0.
Example 7
(1) Composition intermediate preparation
200g of tetramethylammonium hydroxide, 100g of potassium carbonate, 80g of imidazole, 30g of fatty alcohol polyoxyethylene ether, 50g of aminocyclopentanol, 5g of 2-methyl-4-isothiazolin-3-one and 15g of 2-methyl-5-chloro-4-isothiazolin-3-one are dissolved in 700g of deionized water, uniformly stirred, and then the solution is added into 400g of 50wt% nano silicon dioxide colloid (average particle size 50 nm) while stirring, and is subjected to ultrasonic dispersion for 15min for later use.
(2) Formulation of polishing composition
70g of 1- (4-pyridyl) piperazine and 28g of 3-furancarboxylic acid are dissolved in 300g of deionized water, the mixture is stirred uniformly, the solution is added into the composition intermediate treated in the step (1) while being stirred, deionized water is continuously added until the total mass of the dispersion is 2kg, the dispersion is magnetically stirred for 30min and then packaged, and the pH value of the dispersion is 12.5.
Example 8
(1) Composition intermediate preparation
60g of potassium carbonate, 12g of citric acid, 20g of fatty alcohol polyoxyethylene ether, 12g of propylene glycol, 0.5g of 2-methyl-4-isothiazolin-3-one and 1.5g of 2-methyl-5-chloro-4-isothiazolin-3-one are dissolved in 200g of deionized water, uniformly stirred, and then the solution is added into 160 g of 50wt% nano silicon dioxide colloid (average particle size 50 nm) while stirring, and is subjected to ultrasonic dispersion for 15min for later use.
(2) Formulation of polishing composition
10g of 1-methylpiperazine and 1.5g of 2-tetrahydrofuranic acid are dissolved in 80g of deionized water, the solution is stirred uniformly, the solution is added into the composition intermediate treated in the step (1) while being stirred, deionized water is continuously added until the total mass of the dispersion is 2kg, the dispersion is magnetically stirred for 30min and then packaged, and the pH value of the dispersion is 11.0.
Example 9
(1) Composition intermediate preparation
50g of potassium hydroxide, 50g of potassium carbonate, 50g of potassium bicarbonate, 10g of isomeric alcohol polyoxyethylene ether, 0.25g of 2-methyl-4-isothiazolin-3-ketone and 0.75g of 2-methyl-5-chloro-4-isothiazolin-3-ketone are dissolved in 400g of deionized water and stirred uniformly, and then the solution is added into 1200g of 50wt% nano silicon dioxide colloid (average particle size 50 nm) while stirring, and dispersed for 15min by ultrasonic for later use.
(2) Formulation of polishing composition
30g of 1- (2-furoyl) piperazine and 6g of 2-furoic acid are dissolved in 150g of deionized water, the mixture is stirred uniformly, the solution is added into the composition intermediate treated in the step (1) while being stirred, deionized water is continuously added until the total mass of the dispersion is 2kg, the dispersion is magnetically stirred for 30min and then packaged, and the pH value of the dispersion is 11.5.
Example 10
(1) Composition intermediate preparation
200g of tetraethylammonium hydroxide, 50g of potassium carbonate, 64g of citric acid, 6g of isomeric alcohol polyoxyethylene ether and 8g of propylene glycol are dissolved in 600g of deionized water, stirred uniformly, and then the solution is added into 750g of 40wt% nano silicon dioxide colloid (average particle size 100 nm) while stirring, and dispersed for 15min by ultrasonic for later use.
(2) Formulation of polishing composition
40g of 1- (4-pyridyl) piperazine and 6g of 2- (tetrahydrofuranmethoxy) acetic acid are dissolved in 200g of deionized water, the solution is stirred uniformly, the solution is added into the composition intermediate product treated in the step (1) while being stirred, deionized water is continuously added until the total mass of the dispersion is 2kg, the dispersion is magnetically stirred for 30min and then packaged, and the pH value of the dispersion is 11.5.
Comparative example 1
In comparison with example 3, step (2) is as follows, the other process conditions being exactly the same.
And (3) directly adding deionized water into the composition processed in the step (1) until the total mass of the dispersion liquid is 2kg, magnetically stirring for 30min, and packaging.
Comparative example 2
In comparison with example 5, step (2) is as follows, the other process conditions being exactly the same.
And (3) directly adding deionized water into the composition processed in the step (1) until the total mass of the dispersion liquid is 2kg, magnetically stirring for 30min, and packaging.
Comparative example 3
In comparison with example 5, step (2) is as follows, the other process conditions being exactly the same.
50g of 1- (2-pyrimidinyl) piperazine is dissolved in 250g of deionized water, stirred uniformly, then the solution is added into the composition intermediate product treated in the step (1) while being stirred, deionized water is continuously added until the total mass of the dispersion is 2kg, and the mixture is magnetically stirred for 30min and then packaged.
Comparative example 4
In comparison with example 7, step (2) is as follows, the other process conditions being exactly the same.
70g of 1- (4-pyridyl) piperazine is dissolved in 250g of deionized water, stirred uniformly, then the solution is added into the composition intermediate product treated in the step (1) while being stirred, deionized water is continuously added until the total mass of the dispersion is 2kg, and the mixture is magnetically stirred for 30min and then packaged.
Comparative example 5
In comparison with example 5, step (2) is as follows, the other process conditions being exactly the same.
15g of 2, 5-furandicarboxylic acid is dissolved in 250g of deionized water, stirred uniformly, then the solution is added into the composition intermediate product treated in the step (1) while being stirred, deionized water is continuously added until the total mass of the dispersion is 2kg, and the mixture is magnetically stirred for 30min and then packaged.
Comparative example 6
In comparison with example 6, step (2) is as follows, the other process conditions being exactly the same.
21g of 2- (tetrahydrofuranylmethoxy) acetic acid is dissolved in 250g of deionized water, stirred uniformly, then the solution is added into the composition intermediate product treated in the step (1) while being stirred, deionized water is continuously added until the total mass of the dispersion is 2kg, and the mixture is magnetically stirred for 30min and then packaged.
Comparative example 7
In comparison with example 6, steps (1) and (2) were combined as follows.
100g of potassium hydroxide, 100g of potassium carbonate, 50g of imidazole, 10g of fatty alcohol polyoxyethylene ether, 40g of aminocyclopentanol, 2.5g of 2-methyl-4-isothiazolin-3-one, 7.5g of 2-methyl-5-chloro-4-isothiazolin-3-one, 60g of 1- (2-furoyl) piperazine and 21g of 2- (tetrahydrofurfuryl methoxy) acetic acid are dissolved in 800g of deionized water, uniformly stirred, then 750g of 40wt% nano silicon dioxide colloid (average particle size 70 nm) is added while stirring the solution, deionized water is continuously added until the total mass of the dispersion is 2kg, and the mixture is magnetically stirred for 30min and then packaged.
100g of each of the polishing compositions of examples and comparative examples was placed in a 40℃oven for stability testing; polishing tests were performed after each of the example and comparative polishing compositions were diluted with deionized water at a volume ratio of 1:20. The results of the placement stability test and the polishing test are shown in tables 1 and 2, respectively.
TABLE 1 shelf stability test results
Table 2 polishing test results
Comparing comparative example 1 with example 3 in table 1 above, comparative example 2 with example 5, it can be seen that the composition of the examples showed significantly less variation in average particle size after 20 days and 70 days at 40 c, and had greater stability, while the composition of the comparative example was unstable under the same conditions. Comparing comparative example 3 with example 5 in table 1 above, and comparative example 4 with example 7, it was found that the average particle size showed a significant tendency to rise after the comparative example composition was left to stand at 40 ℃ for 20 days with a small rise in particle size for 70 days after the piperazine-based material was added alone. Comparing comparative example 5 with example 5 in Table 1 above, comparative example 6 with example 6, it was found that the particle size change trend of the comparative example composition was similar to that of comparative examples 3 and 4 after the addition of the furan ring-containing water-soluble organic weak acid alone. Thus, it was revealed that the long-term stability of the polishing composition could be improved by adding the piperazine-based substance and the furan ring-containing water-soluble organic weak acid simultaneously in proportion to the highly concentrated polishing composition. Analysis shows that the two auxiliary agents have low solubility and opposite acid-base properties, and can be dissolved more fully when added simultaneously, so that a synergistic effect is exerted, the content of organic annular molecules in a system is increased, the viscosity is increased, the movement of ions is blocked or delayed, the conductivity is reduced (the ionic strength is weakened), the thickness of a diffusion double electric layer of nano silica sol particles is increased, the agglomeration trend among the particles is weakened, and the effects of improving the stability of the composition and prolonging the storage time are achieved. From the difference between comparative example 7 and example 6, it can be seen that the initial average particle size of the composition is smaller by the preparation process of example, i.e., the preparation process of example can reduce agglomeration of nano silica sol particles during addition of the auxiliary agent, and reduce generation of large particles of the composition.
Comparing comparative example 1 with example 3 in table 2 above, comparative example 2 with example 5, it can be found that the compositions of examples have smaller variation in the cyclic polishing rate and better consistency. The two stability aids can weaken agglomeration of nano silica sol in the polishing process, reduce fluctuation of the cyclic polishing rate and prolong the service life of the composition. Comparing comparative example 3 with example 5, comparative example 4 with example 7, comparative example 5 with example 5, and comparative example 6 with example 6 in Table 2 above, it was found that neither piperazine-based material nor furan ring-containing water-soluble organic weak acid alone significantly stabilizes the cyclic polishing rate consistently, again indicating a significant synergy of the two stability aids. From the difference between comparative example 7 and example 6, it can be found that the preparation process of example can further reduce agglomeration of nano silica sol particles in the system, and the variation of the cyclic polishing rate can be made relatively smaller.
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 teaching 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 (19)
1. A silicon polishing composition is characterized by comprising the following components in percentage by mass: 2.5-40 wt% of nano silicon dioxide colloid, 0.2-3.5 wt% of piperazine substance, 0.01-1.4 wt% of furan ring-containing water-soluble organic weak acid, 1-15 wt% of rate accelerator, 0.1-4 wt% of pH regulator, 0.005-1.5 wt% of surfactant, 0-2.5 wt% of humectant, 0-1.0 wt% of bacteriostat and the balance of deionized water;
the piperazine substance is piperazine derivative which does not contain halogen and benzene ring on piperazine ring;
the mass ratio of the furan ring-containing water-soluble organic weak acid to the piperazine substance is 0.05-0.4.
2. The silicon polishing composition as recited in claim 1 wherein the mass percentages of the components are: 5-25 wt% of nano silicon dioxide colloid, 0.5-2.5 wt% of piperazine substance, 0.075-0.75 wt% of furan ring-containing water-soluble organic weak acid, 3-10 wt% of rate accelerator, 1.0-2.5 wt% of acid pH regulator, 0.01-0.5 wt% of surfactant, 0.1-1.0 wt% of humectant, 0.05-0.1 wt% of bacteriostat, and the balance of deionized water.
3. The silicon polishing composition according to claim 1 or 2, wherein the average particle diameter of the nano-silica colloid is 25 to 100nm and the raw material concentration is 30 to 50wt%.
4. The silicon polishing composition according to claim 1 or 2, wherein the piperazine-based substance is at least one selected from the group consisting of piperazine, 1-methylpiperazine, 2-methylpiperazine, 1-formylpiperazine, 2-oxopiperazine, 2-ethoxypiperazine, 1, 4-dimethylpiperazine, 2, 6-dimethylpiperazine, 1-ethylpiperazine, N-aminoethylpiperazine, N- (2-hydroxyethyl) piperazine, 1-acetylpiperazine, N-isopropylpiperazine, 1-allylpiperazine, N-t-butylpiperazine, 1- (3-methoxypropyl) piperazine, 1- (2-dimethylaminoethyl) piperazine, 1- (3-aminopropyl) -4-methylpiperazine, 1- (2-pyrimidinyl) piperazine, 1- (2-furoyl) piperazine, 1- (2-tetrahydrofurfuryl) piperazine, 1- (2-pyridyl) piperazine, 1- (3-pyridyl) piperazine, and 1- (4-pyridyl) piperazine.
5. The silicon polishing composition according to claim 4, wherein the piperazine-based substance is any one selected from piperazine, 1-methylpiperazine, 1-ethylpiperazine, 1-allylpiperazine, 1- (2-pyrimidinyl) piperazine, 1- (2-furoyl) piperazine, and 1- (4-pyridyl) piperazine.
6. The silicon polishing composition according to claim 1 or 2, wherein the furan ring-containing water-soluble organic weak acid is selected from at least any one of 2-furancarboxylic acid, 3-furancarboxylic acid, 2-tetrahydrofurancarboxylic acid, 3-methyl-2-furancarboxylic acid, 2, 5-furandicarboxylic acid, 5-hydroxymethyl-2-furancarboxylic acid, 2-furanacetic acid, 2- (furan-2-yl) -2-oxyacetic acid, 2- (5-oxotetrahydrofuran-2-yl) acetic acid, 2- (tetrahydrofuran-2-yl) acetic acid, (R) -2- (tetrahydrofuran-3-yl) acetic acid, (S) -2- (tetrahydrofuran-3-yl) acetic acid, 2-furanmethylene acetic acid, 2- (tetrahydrofuranmethoxy) acetic acid.
7. The silicon polishing composition according to claim 6, wherein the furan ring-containing water-soluble organic weak acid is selected from any one of 2-furancarboxylic acid, 3-furancarboxylic acid, 2-tetrahydrofurancarboxylic acid, 2-furanacetic acid, 2, 5-furandicarboxylic acid, 2- (tetrahydrofuranmethoxy) acetic acid.
8. The silicon polishing composition according to claim 1 or 2, wherein the rate accelerator is an alkaline compound.
9. The silicon polishing composition of claim 8, wherein the rate accelerator is selected from at least one of potassium hydroxide, ethylenediamine, hydroxyethylethylenediamine, tetrahydroxypropylethylenediamine, tetramethylammonium hydroxide, tetraethylammonium hydroxide, tetrapropylammonium hydroxide, tetrabutylammonium hydroxide, diethyldimethylammonium hydroxide, methyltriethylammonium hydroxide, tetramethylguanidine, potassium carbonate.
10. The silicon polishing composition of claim 9, wherein the rate accelerator is selected from any one of potassium hydroxide, ethylenediamine, tetramethylammonium hydroxide, tetraethylammonium hydroxide, diethyldimethylammonium hydroxide, tetramethylguanidine, and potassium carbonate.
11. The silicon polishing composition according to claim 1 or 2, wherein the pH adjustor is at least one selected from the group consisting of citric acid, tartaric acid, malic acid, oxalic acid, malonic acid, potassium bicarbonate, and imidazole.
12. The silicon polishing composition of claim 11, wherein the pH adjustor is selected from any one of citric acid, oxalic acid, potassium bicarbonate, and imidazole.
13. The silicon polishing composition of claim 12, wherein the pH adjustor adjusts the pH of the silicon polishing composition to 10 to 12.5.
14. The silicon polishing composition according to claim 1 or 2, wherein the surfactant is at least one selected from the group consisting of fatty alcohol polyoxyethylene ether, laureth, isomeric alcohol polyoxyethylene ethers, alkylphenol polyoxyethylene ethers.
15. The silicon polishing composition of claim 14, wherein the surfactant is a fatty alcohol-polyoxyethylene ether or an isomeric alcohol-polyoxyethylene ether.
16. The silicon polishing composition according to claim 1 or 2, wherein the humectant is at least any one selected from propylene glycol, butylene glycol, hexylene glycol, glycerol, and aminocyclopentanol.
17. The silicon polishing composition according to claim 1 or 2, wherein the bacteriostatic agent is selected from at least any one of 2-methyl-4-isothiazolin-3-one, 2-methyl-5-chloro-4-isothiazolin-3-one, 2-n-octyl-4-isothiazolin-3-one.
18. A method of preparing a silicon polishing composition as recited in any one of claims 1 to 17, comprising the steps of:
1) Fully mixing and dispersing a rate accelerator, a pH regulator, a surfactant, an optional humectant and a bacteriostatic agent, and then dripping the mixture into a nano silicon dioxide colloid for uniform mixing;
2) Fully mixing and dispersing piperazine substances and furan ring-containing water-soluble organic weak acid, and then adding the mixture into the nano silicon dioxide colloid containing the auxiliary agent in the step 1) for mixing and dispersing to form the silicon polishing composition.
19. Use of the silicon polishing composition of any one of claims 1-17 in chemical mechanical polishing of a silicon wafer.
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