CN115093794A - Polysilicon polishing composition and application thereof - Google Patents
Polysilicon polishing composition and application thereof Download PDFInfo
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- CN115093794A CN115093794A CN202210690202.8A CN202210690202A CN115093794A CN 115093794 A CN115093794 A CN 115093794A CN 202210690202 A CN202210690202 A CN 202210690202A CN 115093794 A CN115093794 A CN 115093794A
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- homopiperazine
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
- H01L21/3205—Deposition of non-insulating-, e.g. conductive- or resistive-, layers on insulating layers; After-treatment of these layers
- H01L21/321—After treatment
- H01L21/32115—Planarisation
- H01L21/3212—Planarisation by chemical mechanical polishing [CMP]
Abstract
The invention discloses a polysilicon polishing composition and application thereof, wherein the polysilicon polishing composition takes nano silicon dioxide colloid as a main polishing component and is added with high piperazine substances and keto acid substances as auxiliaries. The polishing composition disclosed by the invention is simultaneously added with the high piperazine substances and the keto acid substances which are respectively used as the rate accelerator and the selective inhibitor, so that the polishing composition is green and low in toxicity, high in removal rate of polycrystalline silicon materials, high in selectivity to silicon oxide and silicon nitride, and few in polishing defects, and 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 polysilicon polishing composition and application thereof.
Background
The development of integrated circuits greatly promotes the advancing speed of human society to informatization and intellectualization, and the development and application of some key materials play an important role in the process, and polycrystalline silicon is one of the key materials. Polycrystalline silicon is one of simple substances, crystal planes of crystal grains in the polycrystalline silicon have different orientations, and the conductivity of the polycrystalline silicon is obviously weaker than that of monocrystalline silicon, but the conductivity of the polycrystalline silicon can be greatly influenced by trace doping. In the process of preparing the MOSFET, compared with aluminum, polysilicon has lower work function and corresponding lower threshold voltage, so that a circuit can be operated at lower power supply voltage.
The traditional preparation process of the polysilicon gate comprises three main steps of deposition, photoetching and etching, but with the continuous reduction of technical nodes, the surface and the side wall of the polysilicon gate prepared by adopting the process can not meet the requirements of the subsequent process. Therefore, when the IC process is developed to be less than 28nm, a new process is required for preparing the polysilicon gate, and the specific steps include: 1) in thermally oxidized SiO 2 Or vapor deposited Si 3 N 4 Etching the upper part to form a groove; 2) vapor depositing a polysilicon layer; 3) removing redundant polysilicon by CMP; 4) removal of SiO by means of etching solutions 2 Or Si 3 N 4 The dielectric layer can form a polysilicon gate with a smooth and flat surface and a steep side wall, so that the introduction of the CMP technology plays an important role in the process. In the process, CMP (chemical mechanical polishing) is used for polishing the surface of the polycrystalline silicon by using polishing solution containing abrasive and polyurethane polishing pad under the chemical action, the mechanical action and the combination of the two actions, wherein in the polishing process, chemical substances react with surface polycrystalline silicon to form a soft layer, and the soft layer is stripped and removed by the mechanical action of the abrasive and the polishing pad, so that the polishing solution plays an important role in the CMP process.
Because the Mohs hardness of the silicon oxide is close to that of the polysilicon, and the silicon oxide also has the advantages of fine granularity, small surface damage after polishing, easy cleaning and the like, the silicon sol is mainly used as the abrasive of the polysilicon polishing solution in the industry at present. In addition, in order to ensure a certain polysilicon removal rate, the uniformity of a polished surface and the selectivity to a dielectric material, the polysilicon polishing solution is also added with components such as a rate accelerator, a selectivity inhibitor, a surfactant, a rate inhibitor, a pH regulator and the like. However, the main rate accelerator added to the polysilicon polishing solution in the current market is organic ammonium or aliphatic organic amine with high toxicity and strong corrosivity, so that the method has greater safety risk to production and transportation related personnel; meanwhile, related components such as a rate inhibitor, a surfactant and the like are not sufficiently researched, selectivity among polishing materials is not enough, uniformity of a polished surface is poor, defects such as discing, Erosis and the like easily occur in large quantities, and the performance of a device is easily influenced.
Korean laid-open patent nos. KR100643628B1, KR100660767B1, KR 101094662B 1, and KR101178716B1 all propose that adding quaternary ammonium bases, such as tetramethylammonium hydroxide, tetraethylammonium hydroxide, tetrapropylammonium hydroxide, and tetrabutylammonium hydroxide, to a polysilicon polishing composition as a rate accelerator to polish a polysilicon material can achieve a higher polysilicon removal rate while maintaining a relatively low silicon oxide and silicon nitride removal rate, but such materials are severely corroded statically and control of polishing defects (e.g., Dishing) is not ideal. In addition, quaternary ammonium base compounds have high toxicity, high corrosivity and high safety risk to production personnel, and the waste liquid treatment after polishing is high in cost, so that the quaternary ammonium base compounds are gradually not suitable for the development trend of green and environment protection in the current industry.
The patent publication CN103080256B adopts cerium oxide abrasive and is added with anionic phosphate dispersant, triazole, piperazine and other organic amines, so that high removal rate of silicon oxide and silicon nitride is realized, while the removal rate of polysilicon is only tens of angstroms per minute, and the reverse selectivity is obvious. Still other patents mention the addition of adjuvants to the composition system to modify the isoelectric points of silica and silicon nitride by adsorption, thereby adjusting the selectivity between silica and silicon nitride, such as U.S. Pat. No. 20080116171A1 and Korean patent KR1020090035063A, which mention the addition of amino acids to the compositionSuch as to suppress the removal rate of silicon oxide, korean laid-open patent KR100851235B1 mentions that the removal rate of silicon nitride is suppressed by using a cerium oxide abrasive and adding an anionic or nonionic surfactant. Most of these compositions are neutral or acidic, with the OH groups in the system - The concentration of (2) is low, the polarization effect on Si-Si bonds is weak, and the removal rate of the polysilicon is obviously inhibited, so that the application of the polysilicon is limited.
Further, korean laid-open patent KR20100014849A proposes the addition of an aliphatic ammonium salt type cationic surfactant, such as octyltrimethylammonium bromide, decyltrimethylammonium bromide, and lauryltrimethylammonium chloride, to a polysilicon composition for the purpose of simultaneously suppressing the removal rate of silicon oxide and silicon nitride and improving the polishing selectivity, but these assistants also introduce harmful halogens into the polishing composition, easily cause corrosion damage to polishing equipment, and also easily adversely affect the quality of the polished surface.
Therefore, there is a need to improve the components of the polishing composition from the chemical formulation point of view to achieve the objectives of high polysilicon removal rate, high polishing selectivity, and low polishing defects on the basis of green and low toxicity, and to overcome the drawbacks of the prior art described above.
Disclosure of Invention
In order to solve the technical problems, the invention provides a polysilicon polishing composition, wherein a high piperazine substance and a keto acid substance are added into a nano silicon dioxide colloid to be respectively used as a rate accelerator and a selectivity inhibitor, so that the removal rate of polysilicon can be effectively increased, the removal rate of silicon oxide and silicon nitride can be inhibited, and the high selectivity of the composition on polishing of polysilicon, silicon oxide and silicon nitride can be realized.
It is another object of the present invention to provide the use of such a polysilicon polishing composition for chemical mechanical polishing of polysilicon.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the polysilicon polishing composition takes nano silicon dioxide colloid as an abrasive, and also comprises a high piperazine substance as a rate accelerator and a keto acid substance as a selective inhibitor.
In a preferred embodiment, the polysilicon polishing composition comprises nano silica colloid, homopiperazine substances, keto acid substances, surfactants, a pH regulator, a humectant, a bacteriostatic agent and deionized water.
In a preferred embodiment, the polysilicon polishing composition comprises the following components: 5-30 wt% of nano silica colloid, 0.5-8 wt% of homopiperazine substance, 0.05-2 wt% of keto acid substance, 0.05-2 wt% of surfactant, 0.05-3 wt% of pH regulator, 0.01-2 wt% of humectant, 0.005-1.0 wt% of bacteriostatic agent, and the balance of deionized water.
In a more preferred embodiment, the polysilicon polishing composition comprises the following components: 10-25 wt% of nano silica colloid, 2-6 wt% of homopiperazine substance, 0.1-1 wt% of ketonic acid substance, 0.1-1 wt% of surfactant, 0.5-1.5 wt% of pH regulator, 0.1-1.0 wt% of humectant, 0.05-0.1 wt% of bacteriostatic agent and the balance of deionized water.
In a specific embodiment, the nano silica colloid has an average particle size of 30 to 90nm and a concentration of 20 to 40 wt%.
In a specific embodiment, the homopiperazine is selected from homopiperazine, 1-Boc-homopiperazine, 1-methylpiperazine, 1-ethylpiperazine, 1-formylhomopiperazine, 1-acetylhomopiperazine, 1, 7-dimethyl-1, 4-homopiperazine, 1- (2-methoxyethyl) homopiperazine, 1- (2-aminoethyl) -4-methylpiperazine, 1-isobutyl-1, 4-homopiperazine, 1-pyrazin-2-yl-1, 4-homopiperazine, 1- (2-pyrimidinyl) homopiperazine, 1- (2-pyridyl) -homopiperazine, 1- (3-methyl-2-pyridyl) homopiperazine, 1-Boc-homopiperazine, 1-methylpiperazine, 1-ethylpiperazine, 1-formylhomopiperazine, 1-4-homopiperazine, 1-methylethyl-homopiperazine, 1- (2-pyridyl) homopiperazine, and mixtures thereof, 1- (6-methyl-2-piperidinyl) homopiperazine, 1-pyridin-2-ylmethyl-1, 4-homopiperazine, 1-benzylhomopiperazine, 1- (2-pyridin-4-ylethyl) -1, 4-homopiperazine, 1- (2-methylbenzyl) homopiperazine, 1- (3-methylbenzyl) homopiperazine, 1- (4-methylbenzyl) homopiperazine, 1-Boc-5-methyl-1, 4-homopiperazine, 1-Boc-3-oxopropiperazine, 1-Boc-4- (2-hydroxyethyl) homopiperazine, 2-Boc-4- (2-pyridinyl) homopiperazine, 1-cyclobutyl-4- (piperidine-4-carbonyl) -1, at least any one of 4-homopiperazine; preferably at least one of homopiperazine, 1-methylpiperazine, 1- (2-methoxyethyl) homopiperazine, 1-pyrazin-2-yl-1, 4-homopiperazine, 1- (2-pyrimidinyl) homopiperazine, and 1-benzylhomopiperazine.
In a particular embodiment, the ketonic acid species is selected from the group consisting of tetronic acid, 2-ketobutyric acid, 2-hydroxy-butanoic acid ketone, 2-imidazolinone-4-carboxylic acid, croconic acid, 2-ketoglutaric acid, 2-pentanoic acid, (R) -3-ketocyclopentanecarboxylic acid, 4-cyclohexanone carboxylic acid, 4-ketopimelic acid, at least one of 2-indolone-4-carboxylic acid, kuronic acid, 6-methylchromone-2-carboxylic acid, nalidixic acid, 9-fluorenone-1-carboxylic acid, 9-fluorenone-2-carboxylic acid, ketorolac, 2, 7-dimethyl-9-fluorenone-4-carboxylic acid, 3-methylflavone-8-carboxylic acid, and 4-diethylaminoketonic acid; preferably at least one of tetronic acid, 2-pentanoic acid, 4-cyclohexanone carboxylic acid, 2-indolone-4-carboxylic acid, ketorolac and 4-diethylaminoketo acid.
In a specific embodiment, the surfactant is selected from at least any one of fatty alcohol polyoxyethylene ether, lauryl alcohol polyoxyethylene ether, isomeric alcohol polyoxyethylene ether, nonylphenol polyoxyethylene ether, alkylphenol polyoxyethylene ether, polyoxyethylene alkylamine, and polyoxyethylene alkylolamide.
In a specific embodiment, the pH regulator is selected from at least any one of tetrazole, imidazole, 1-methylimidazole, 2-methylimidazole, 4-methylimidazole, pyrazole, 1-methylpyrazole, 3-methylpyrazole and 4-methylpyrazole; preferably, the pH of the silicon polishing composition is adjusted to 10 to 12.5.
In a particular embodiment, the humectant is selected from at least any one of propylene glycol, butylene glycol, hexylene glycol, glycerin, sorbitol, 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, and 2-n-octyl-4-isothiazolin-3-one.
In another aspect, the foregoing polysilicon polishing composition is used in chemical mechanical polishing of polysilicon.
Compared with the prior art, the invention has the following beneficial effects:
the nano silicon dioxide colloid is used as a basic abrasive, so that the polishing composition has the advantages of high polishing rate, clean polishing surface and difficulty in generating concave defects (such as discing) on the surface of polycrystalline silicon, and in addition, the high piperazine substance and the keto acid substance are added into the polishing composition and are respectively used as a rate accelerator and a selectivity inhibitor, so that the removal rate of the polycrystalline silicon material and the polishing selectivity on a dielectric material are improved, and meanwhile, the polishing composition has the characteristics of greenness and low toxicity, and has remarkable advantages compared with the prior art.
Detailed Description
The following examples will further illustrate the method provided by the present invention in order to better understand the technical solution of the present invention, but the present invention is not limited to the listed examples, and also includes any other known modifications within the scope of the claims of the present invention.
The invention relates to a polysilicon polishing composition, which takes nano silicon dioxide colloid as a main polishing component, and is added with high piperazine substances and ketonic acid substances which are respectively used as a rate accelerator and a selectivity inhibitor, namely, the polysilicon polishing composition is obtained by adding the high piperazine substances and the ketonic acid substances as auxiliary agents on the basis of the existing polysilicon chemical mechanical polishing solution taking the nano silicon dioxide colloid as an abrasive.
Wherein the homopiperazine substance is heterocyclic organic weak base with short-chain alkyl, acyl, pyrimidyl, pyridyl, piperidyl and other groups connected to the homopiperazine ring, the ketoacid substance is organic weak acid containing carbonyl and carboxyl simultaneously, the high piperazine species and the keto acid species are each present in the polishing composition at a mass ratio of 0.5 to 8 wt.% (including, but not limited to, 0.8 wt.%, 1.0 wt.%, 1.2 wt.%, 1.5 wt.%, 2.0 wt.%, 2.5 wt.%, 3.0 wt.%, 3.5 wt.%, 4.0 wt.%, 4.5 wt.%, 5.0 wt.%, 5.5 wt.%, 6.0 wt.%, 6.5 wt.%, 7.0 wt.%, 7.5 wt.%), 0.05 to 2 wt.% (including, but not limited to, 0.1 wt.%, 0.12 wt.%, 0.15 wt.%, 0.2 wt.%, 0.3 wt.%, 0.4 wt.%, 0.5 wt.%, 0.6 wt.%, 0.7 wt.%, 0.8 wt.%, 0.9 wt.%, 1.0 wt.%, 1.2 wt.%, 1.4 wt.%, 1.6 wt.%, 1.8 wt.%).1.8 wt.%).5 wt.%.
Silica sol abrasives mainly exert a mechanical grinding action in a composition, but since a deposited polycrystalline silicon film layer has a hardness close to that of a silica abrasive, the removal rate of direct polishing with silica sol is low, and defects are easily generated, so that it is necessary to add a rate accelerator to soften the surface layer of polycrystalline silicon. The compound as the rate accelerator can be ionized or hydrolyzed to generate a large amount of OH in the system - In addition, the polishing composition of IC grade also requires that the rate accelerator does not contain various harmful metal ions, so the rate accelerator of the general polysilicon polishing composition is mainly organic alkali. The quaternary ammonium base compound and the aliphatic organic amine which are usually used have high corrosivity and strong toxicity, and have high static corrosion rate on the surface of polycrystalline silicon, so that defects are easily caused; in addition, these materials also have a high ionic strength in the concentrated system, and tend to cause agglomeration of the silica sol abrasive.
The rate accelerator adopted by the invention is a high piperazine substance, belongs to heterocyclic organic amine, has high density of lone pair electron cloud on N, is difficult to break N-H bond, and has certain proton absorption capacity after being dissolved in water, so that OH in a system can be absorbed - The whole ring structure is stable and positively charged, and is very easy to be contacted with SiO on the surface of the polysilicon soft layer 3 2- The formation of micelles, which act as rate promoters, both increase the polishing rate and contribute to the production of a high quality polished surface. The high piperazine substance belongs to organic weak base, and has small ionic strength, so that the addition amount of the high piperazine substance in the composition can be relatively higher, and the high piperazine substance does not cause agglomeration of silica sol particles under the concentration condition. In addition, compared with piperazine which is heterocyclic organic amine, the distance between two N in the homopiperazine substance ring is farther, the electron-withdrawing induction effect between the two N is lower, the alkalinity is relatively stronger, and therefore the polishing efficiency is higher.
It is highly desirable that the dielectric material be stable to prevent significant Dishing, Erosion, etc. defects during polysilicon polishing, so that selective inhibitors in the chemical adjuvant system are desirableIt is also important. The keto acid substance as the selective inhibitor of the present invention belongs to a carbonyl group-containing weak organic acid, in which a carbonyl group and a carboxyl group are present simultaneously in the molecule, and the carbonyl group enhances the electron-withdrawing ability of the whole group after ionization in an aqueous phase system, so that the keto acid is more likely to be closely adsorbed to silicon oxide or silicon nitride in the form of a C — O — Si bond than a general weak organic acid, and the adsorption thereof on the surface of a polycrystalline silicon is not significant. During polishing, keto acid is in SiO 2 、Si 3 N 4 The surface is adsorbed to form a film, so that the mechanical friction action of the two materials is inhibited, but the influence on the polysilicon material is small, so that the selectivity of the polysilicon to silicon oxide and silicon nitride materials in the polishing process is enhanced, and the polishing defect is favorably reduced.
Wherein the nano silica colloid has a particle size of 30-90nm, such as but not limited to 30nm, 35nm, 40nm, 45nm, 50nm, 55nm, 60nm, 65nm, 70nm, 75nm, 80nm, 85nm, 90nm, and the silica sol has a concentration of 20-40 wt%, such as but not limited to 20 wt%, 25 wt%, 30 wt%, 35 wt%, 40 wt%.
Examples of the homopiperazine include homopiperazine, 1-Boc-homopiperazine, 1-methylpiperazine, 1-ethylpiperazine, 1-formylhomopiperazine, 1-acetylhomopiperazine, 1, 7-dimethyl-1, 4-homopiperazine, 1- (2-methoxyethyl) homopiperazine, 1- (2-aminoethyl) -4-methylpiperazine, 1-isobutyl-1, 4-homopiperazine, 1-pyrazin-2-yl-1, 4-homopiperazine, 1- (2-pyrimidinyl) homopiperazine, 1- (2-pyridyl) -homopiperazine, 1- (3-methyl-2-pyridyl) homopiperazine, 1- (6-methyl-2-piperidyl) homopiperazine, and, At least any one of 1-pyridin-2-ylmethyl-1, 4-homopiperazine, 1-benzylhomopiperazine, 1- (2-pyridin-4-ylethyl) -1, 4-homopiperazine, 1- (2-methylbenzyl) homopiperazine, 1- (3-methylbenzyl) homopiperazine, 1- (4-methylbenzyl) homopiperazine, 1-Boc-5-methyl-1, 4-homopiperazine, 1-Boc-3-oxohomopiperazine, 1-Boc-4- (2-hydroxyethyl) homopiperazine, 2-Boc-4- (2-pyridyl) homopiperazine, 1-cyclobutyl-4- (piperidine-4-carbonyl) -1, 4-homopiperazine, for example, any one, any two or more of the above homopiperazines are preferably homopiperazine, 1-methylpiperazine, 1- (2-methoxyethyl) homopiperazine, 1-pyrazin-2-yl-1, 4-homopiperazine, 1- (2-pyrimidinyl) homopiperazine, or 1-benzylhomopiperazine.
Examples of the keto acid-like substance include any one, any two or more of tetronic acid, 2-ketobutyric acid, 2-hydroxy-butanoic acid, 2-imidazolidinone-4-carboxylic acid, croconic acid, 2-ketoglutaric acid, 2-pentanoic acid, (R) -3-ketocyclopentanoic acid, 4-cyclohexanone carboxylic acid, 4-ketopimelic acid, 2-indolone-4-carboxylic acid, picric acid, 6-methylchromone-2-carboxylic acid, nalidixic acid, 9-fluorenone-1-carboxylic acid, 9-fluorenone-2-carboxylic acid, ketorolac, 2, 7-dimethyl-9-fluorenone-4-carboxylic acid, 3-methylflavone-8-carboxylic acid, and 4-diethylaminoketonic acid, preferred are tetronic acid, 2-pentanonic acid, 4-cyclohexanone carboxylic acid, 2-indolone-4-carboxylic acid, ketorolac and 4-diethylaminoketo acid.
In addition to the above-mentioned nano silica colloid as an abrasive, and the addition of three main components, namely, a high piperazine substance and a keto acid substance, the present invention does not limit any other additive component added to the polishing composition, and can be applied to various conventional polysilicon chemical mechanical polishing liquid systems, and one or more of a surfactant, a pH adjustor, a humectant and a bacteriostatic agent can be optionally selected by a skilled person to be added to the polishing composition according to the requirements for improving the quality of the polishing surface and the stability of the composition.
The surfactant is at least one selected from fatty alcohol polyoxyethylene ether, lauryl alcohol polyoxyethylene ether, isomeric alcohol polyoxyethylene ether, nonylphenol polyoxyethylene ether, alkylphenol polyoxyethylene ether, polyoxyethylene alkylamine and polyoxyethylene alkylolamide, for example, any one, any two or more of the above rate accelerators are preferably selected, and fatty alcohol polyoxyethylene ether, polyoxyethylene alkylamine and polyoxyethylene alkylolamide are preferably selected. The surfactant is used for reducing the surface tension of the composition, reducing the contact angle between the composition and the surface of the polycrystalline silicon material and enhancing the spreading performance of the composition on the surface of the polycrystalline silicon material, so that the surface roughness of the polished polycrystalline silicon material is reduced, the uniformity of the polished wafer surface is improved, and the polished surface quality is improved.
The pH adjuster is, for example, at least one selected from the group consisting of tetrazole, imidazole, 1-methylimidazole, 2-methylimidazole, 4-methylimidazole, pyrazole, 1-methylpyrazole, 3-methylpyrazole and 4-methylpyrazole, and, for example, any one, any two or more of the pH adjusters are combined, and tetrazole and imidazole are preferable. The pH regulator is used for regulating the pH value of the concentrated solution, preventing the concentrated solution from being too strong in alkalinity to cause the dissolution of nano silicon oxide particles, and simultaneously, anions generated by ionization or hydrolysis of the concentrated solution have a complexing effect on metal ions in the composition.
The humectant is, for example, at least one selected from propylene glycol, butylene glycol, hexylene glycol, glycerin, sorbitol, and aminocyclopentanol, and is, for example, any one, any two or more of the above humectants, preferably glycerin and aminocyclopentanol. The humectant is used to inhibit water loss of the composition during storage, to enhance the stability of the silica sol particles, and to extend the shelf life of the composition.
The bacteriostatic agent is at least one selected from 2-methyl-4-isothiazolin-3-one, 2-methyl-5-chloro-4-isothiazolin-3-one and 2-n-octyl-4-isothiazolin-3-one, such as any one, any two or more of the above bacteriostatic agents, and is preferably 2-n-octyl-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 metabolites of microorganisms.
In a specific embodiment, the composition is prepared from the following components in proportion:
wherein the polysilicon polishing composition has a pH of 10 to 12.5, including but not limited to 10, 10.5, 11, 11.5, 12, 12.5, preferably 11 to 12.
The method of preparing the polysilicon polishing composition of the present invention may be, for example, mixing the components according to the methods known in the art, and specifically, for example, a method of preparing a polysilicon polishing composition, comprising the step of mixing a homopiperazine-based substance and a keto acid-based substance with a nano silica colloid and other auxiliary agents.
In a preferred embodiment, the homopiperazine substance, the keto-acid substance, the surfactant, the pH regulator, the humectant and the bacteriostatic agent are fully mixed and dispersed to form the chemical auxiliary agent of the composition.
Then, adding the chemical auxiliary agent into the nano silicon dioxide colloid, and fully stirring and dispersing to form the polysilicon polishing composition of the invention, wherein the dispersing means in the process comprises 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 polysilicon wafer polishing test was a Speedfam 36B single-side polishing machine; the polishing pad is IC1010 type, the polishing material is 200mm wafer, the polishing speed is 65rpm, the polishing pressure is 2.0psi, the flow is 1.2L/min, the polishing time is 1min, and the polishing temperature is controlled to be 30-32 ℃. The polishing solution is filtered and then is conveyed to a polishing disc by a peristaltic pump, a dresser is used for dressing and maintaining the polishing pad after each polishing, and pre-polishing is carried out before each polishing.
And (3) removing rate testing: respectively measuring the thickness of the polished polysilicon film, the thickness of the silicon oxide film and the thickness of the silicon nitride film by using a film thickness meter, and respectively calculating the removal rates of the polysilicon film, the silicon oxide film and the silicon nitride film (MRR) ((MRR)) according to the polishing time
)。
And (4) selectively comparing, namely calculating the ratio of the removal rate of the polysilicon to the removal rate of the silicon oxide in the same time, calculating the ratio of the removal rate of the polysilicon to the removal rate of the silicon nitride in the same time, and comparing.
Unless otherwise specified, the raw materials and reagents used in the examples of the present invention and comparative examples were all commercially available.
Example 1
Dissolving 10g of homopiperazine, 1g of tetronic acid, 1g of fatty alcohol-polyoxyethylene ether, 1g of tetrazole, 0.2g of glycerol and 0.1g of 2-n-octyl-4-isothiazoline-3-ketone in 400g of deionized water, uniformly stirring, adding the solution into 500g of 20 wt% nano silica colloid (with the average particle size of 30nm) while stirring, continuously adding deionized water until the total mass of the dispersion liquid is 2kg, magnetically stirring for 30min, and packaging, wherein the pH value of the dispersion liquid is 10.
Example 2
Dissolving 20g of 1-methylpiperazine, 2g of 2-pentanoic acid, 2g of polyoxyethylene alkylamine, 10g of tetrazole, 2g of glycerol and 1g of 2-n-octyl-4-isothiazoline-3-ketone in 400g of deionized water, uniformly stirring, adding the solution into 1000g of 20 wt% nano silica colloid (with the average particle size of 30nm) while stirring, continuously adding the deionized water until the total mass of the dispersion liquid is 2kg, magnetically stirring for 30min, and packaging, wherein the pH value of the dispersion liquid is 10.5.
Example 3
40g of 1- (2-methoxyethyl) homopiperazine, 6g of 4-cyclohexanecarboxylic acid, 8g of polyoxyethylene alkylolamide, 12g of tetrazole, 6g of aminocyclopentanol and 1.6g of 2-n-octyl-4-isothiazoline-3-ketone are dissolved in 400g of deionized water, the mixture is stirred uniformly, then 1200g of 30 wt% nano silica colloid (with the average particle size of 50nm) is added to the solution while stirring, the deionized water is continuously added until the total mass of the dispersion is 2kg, the mixture is stirred magnetically for 30min, and the mixture is packaged, wherein the pH value of the dispersion is 11.0.
Example 4
Dissolving 80g of 1-pyrazin-2-yl-1, 4-homopiperazine, 10g of 2-indolone-4-carboxylic acid, 12g of polyoxyethylene alkylamine, 22g of imidazole, 10g of aminocyclopentanol and 2g of 2-n-octyl-4-isothiazolin-3-ketone in 400g of deionized water, uniformly stirring, adding the solution to 1000g of 40 wt% nano silica colloid (average particle size is 70nm) while stirring, continuously adding deionized water until the total mass of the dispersion is 2kg, magnetically stirring for 30min, and packaging, wherein the pH value of the dispersion is 11.3.
Example 5
100g of 1- (2-pyrimidinyl) homopiperazine, 16g of ketorolac, 16g of polyoxyethylene alkylolamide, 30g of imidazole, 16g of aminocyclopentanol and 7g of 2-n-octyl-4-isothiazoline-3-ketone are dissolved in 400g of deionized water, the mixture is stirred uniformly, then the solution is added to 1250g of 40 wt% nano silica colloid (the average particle size is 70nm) while stirring, the deionized water is continuously added until the total mass of the dispersion liquid is 2kg, the mixture is stirred magnetically for 30min and packaged, and the pH value of the dispersion liquid is 11.5.
Example 6
Dissolving 120g of 1-benzyl homopiperazine, 20g of 4-diethylamino keto acid, 20g of polyoxyethylene alkylolamide, 50g of imidazole, 20g of aminocyclopentanol and 2g of 2-n-octyl-4-isothiazoline-3-ketone in 400g of deionized water, uniformly stirring, adding the solution to 1000g of 40 wt% nano silica colloid (average particle size is 70nm) while stirring, continuously adding deionized water until the total mass of the dispersion is 2kg, magnetically stirring for 30min, and packaging, wherein the pH value of the dispersion is 11.5.
Example 7
160g of homopiperazine, 30g of 2-pentanoic acid, 28g of polyoxyethylene alkylamine, 60g of imidazole, 30g of aminocyclopentanol and 20g of 2-n-octyl-4-isothiazolin-3-ketone are dissolved in 400g of deionized water and stirred uniformly, then the solution is added to 1000g of 40 wt% nano silica colloid (with the average particle size of 50nm) while stirring, the deionized water is continuously added until the total mass of the dispersion is 2kg, the mixture is magnetically stirred for 30min and packaged, and the pH value of the dispersion is 12.0.
Example 8
Dissolving 80g of 1-methyl homopiperazine, 40g of tetronic acid, 40g of fatty alcohol-polyoxyethylene ether, 20g of tetrazole, 40g of glycerol and 1.2g of 2-n-octyl-4-isothiazoline-3-ketone in 400g of deionized water, stirring uniformly, adding the solution to 1000g of 30 wt% nano silica colloid (the average particle size is 50nm) while stirring, continuing to add deionized water until the total mass of the dispersion liquid is 2kg, stirring for 30min by magnetic force, and packaging, wherein the pH value of the dispersion liquid is 11.6.
Example 9
Dissolving 40g of 1- (2-pyrimidinyl) homopiperazine, 10g of ketorolac, 10g of polyoxyethylene alkylamine, 4g of tetrazole, 10g of glycerol and 10g of 2-n-octyl-4-isothiazoline-3-ketone in 400g of deionized water, uniformly stirring, adding the solution into 1500g of 40 wt% nano silica colloid (the average particle size is 90nm) while stirring, continuously adding the deionized water until the total mass of the dispersion liquid is 2kg, magnetically stirring for 30min, and packaging, wherein the pH value of the dispersion liquid is 11.2.
Example 10
100g of 1-methylpiperazine, 10g of 4-diethylamino keto acid, 6g of fatty alcohol-polyoxyethylene ether, 40g of imidazole, 16g of glycerol and 2g of 2-n-octyl-4-isothiazoline-3-ketone are dissolved in 400g of deionized water, the mixture is uniformly stirred, then 1200g of 30 wt% nano silica colloid (with the average particle size of 50nm) is added to the solution while stirring, the deionized water is continuously added until the total mass of the dispersion liquid is 2kg, the mixture is magnetically stirred for 30min, and the mixture is packaged, wherein the pH value of the dispersion liquid is 12.5.
Comparative example 1
The amount of piperazine added to the adjuvant was 10g without adding high piperazine, and the procedure was otherwise the same as in example 1.
Comparative example 2
The auxiliary agent was prepared in the same manner as in example 6 except that 1-benzylhomopiperazine was not added and 120g of ethylenediamine was added.
Comparative example 3
The auxiliary agent was added with 80g of tetraethylammonium hydroxide in the absence of 1-pyrazin-2-yl-1, 4-homopiperazine, and the rest was the same as in example 4.
Comparative example 4
The amount of oxalic acid added to the adjuvant was 6g, except that the amount was the same as in example 3.
Comparative example 5
The adjuvant was added without ketorolac and 16g malonic acid, the rest being the same as in example 5.
Comparative example 6
The adjuvant was not ketorolac and the procedure was as in example 5.
The polishing compositions of the examples and comparative examples were diluted at a volume ratio of 1:10 and tested for polishing, the results of which are shown in Table 1 below:
TABLE 1 polishing test results
Comparing table 1, comparative example 1 and example 1 above, it can be seen that when the rate accelerator is also a heterocyclic organic amine, the removal rate of polysilicon is significantly higher in example 1 in which piperazine of the same quality is added than in comparative example 1, while the removal rates of silicon oxide and silicon nitride are not significantly different in comparative example and example, but dishing defects in comparative example are greater than in example, which indicates that piperazine has a higher polishing rate and better polished surface quality as the rate accelerator of the composition.
Comparing comparative example 2 with example 6, and comparative example 3 with example 4, it can be seen that the removal rates of the polysilicon in comparative example 2 and comparative example 3 are not higher than those in examples 6 and 4 under the same conditions, while the removal rates of the silicon oxide and silicon nitride in comparative example are slightly higher than those in examples, and the dishing corrosion generated by polishing is higher than that in examples, so that the polishing selectivity of the comparative example is lower than that in examples, and the polishing quality is inferior to that in examples. This indicates that the homopiperazine substance used in the examples has a better removal effect on polysilicon and can avoid polishing defects than the aliphatic organic amine or organic ammonium used in the comparative examples, and the reason for this is probably that the chemical action exerted by the homopiperazine substance in the polishing process is more coordinated with the mechanical action exerted by the abrasive, and the problems such as malignant corrosion or over-polishing are less likely to occur.
Comparing comparative example 4 with example 3 and comparative example 5 with example 5 in table 1 above, it can be seen that the removal rates of comparative examples 3 and 4 for silicon oxide and silicon nitride are significantly higher than those of examples 3 and 5 under the same conditions, while the removal rates of comparative examples and examples for polysilicon materials are close, so that the selectivity of comparative examples is significantly lower than that of examples, and dishing defects generated by polishing are significantly higher than those of examples. This indicates that the ketonic acid-type substance added to the composition as a selective inhibitor can exert an effect of inhibiting the removal rate of silicon oxide and silicon nitride more than general weak organic acids (e.g., oxalic acid and malonic acid). The reason may be that the keto acid-like substance contains a carbonyl group in its molecule and is adsorbed on the surface of silicon oxide or silicon nitride more strongly than a general weak organic acid. Comparing comparative example 6 and example 5, the effect of the keto acid-type substance on the improvement of polishing selectivity and the reduction of polishing defects is also demonstrated again.
While the present invention has been described in detail with reference to the preferred embodiments, it should be understood that the above description should not be taken as limiting the invention. It will be appreciated by those skilled in the art that modifications and adaptations to the invention may be made in light of the teachings of the present disclosure. Such modifications or adaptations are intended to be within the scope of the present invention as defined in the claims.
Claims (10)
1. The polysilicon polishing composition takes nano silicon dioxide colloid as an abrasive, and is characterized by further comprising high piperazine substances as a rate accelerator and keto acid substances as a selective inhibitor.
2. The polysilicon polishing composition according to claim 1, comprising nano silica colloid, homopiperazine-based material, keto acid-based material, surfactant, pH adjuster, humectant, bacteriostatic agent, and deionized water; preferably, the content of each component is as follows: 5-30 wt% of nano silica colloid, 0.5-8 wt% of homopiperazine substance, 0.05-2 wt% of keto acid substance, 0.05-2 wt% of surfactant, 0.05-3 wt% of pH regulator, 0.01-2 wt% of humectant, 0.005-1.0 wt% of bacteriostatic agent and the balance of deionized water; more preferably, the content of each component is as follows: 10-25 wt% of nano silica colloid, 2-6 wt% of homopiperazine substance, 0.1-1 wt% of ketonic acid substance, 0.1-1 wt% of surfactant, 0.5-1.5 wt% of pH regulator, 0.1-1 wt% of humectant, 0.05-0.1 wt% of bacteriostatic agent and the balance of deionized water.
3. The polysilicon polishing composition according to claim 1 or 2, wherein the nano silica colloid has an average particle diameter of 30 to 90nm and a mass concentration of 20 to 40 wt%.
4. The polysilicon polishing composition according to claim 1 or 2, wherein the homopiperazine-based substance is selected from homopiperazine, 1-methylpiperazine, 1-ethylpiperazine, 1-Boc-homopiperazine, 1-formylhomopiperazine, 1-acetylhomopiperazine, 1, 7-dimethyl-1, 4-homopiperazine, 1- (2-methoxyethyl) homopiperazine, 1- (2-aminoethyl) -4-methylpiperazine, 1-isobutyl-1, 4-homopiperazine, 1-pyrazin-2-yl-1, 4-homopiperazine, 1- (2-pyrimidinyl) homopiperazine, 1- (2-pyridyl) -homopiperazine, 1- (3-methyl-2-pyridyl) homopiperazine, 1-ethylpiperazine, 1-4-dimethylpiperazine, and 1, 4-dimethylpiperazine, 1- (6-methyl-2-piperidinyl) homopiperazine, 1-pyridin-2-ylmethyl-1, 4-homopiperazine, 1-benzylhomopiperazine, 1- (2-pyridin-4-ylethyl) -1, 4-homopiperazine, 1- (2-methylbenzyl) homopiperazine, 1- (3-methylbenzyl) homopiperazine, 1- (4-methylbenzyl) homopiperazine, 1-Boc-5-methyl-1, 4-homopiperazine, 1-Boc-3-oxohomopiperazine, 1-Boc-4- (2-hydroxyethyl) homopiperazine, 2-Boc-4- (2-pyridinyl) homopiperazine, 1-cyclobutyl-4- (piperidine-4-carbonyl) -1, at least any one of 4-homopiperazine; preferably at least any one of homopiperazine, 1-methyl homopiperazine, 1- (2-methoxyethyl) homopiperazine, 1-pyrazin-2-yl-1, 4-homopiperazine, 1- (2-pyrimidinyl) homopiperazine, and 1-benzyl homopiperazine.
5. The polysilicon polishing composition according to claim 1 or 2, wherein the ketonic acid is selected from the group consisting of tetronic acid, 2-ketobutyric acid, 2-hydroxy-butanoic acid ketone, 2-imidazolidinone-4-carboxylic acid, croconic acid, 2-ketoglutaric acid, 2-pentanoic acid, (R) -3-ketocyclopentanecarboxylic acid, 4-cyclohexanone carboxylic acid, 4-ketopimelic acid, 2-indolone-4-carboxylic acid, ketopicric acid, 6-methylchromone-2-carboxylic acid, nalidixic acid, 9-fluorenone-1-carboxylic acid, 9-fluorenone-2-carboxylic acid, ketorolac, 2, 7-dimethyl-9-fluorenone-4-carboxylic acid, 3-methylflavone-8-carboxylic acid, and mixtures thereof, At least one of 4-diethylaminoketoacid; preferably at least one of tetronic acid, 2-pentanoic acid, 4-cyclohexanone carboxylic acid, 2-indolone-4-carboxylic acid, ketorolac and 4-diethylaminoketo acid.
6. The polysilicon polishing composition as set forth in claim 2, wherein the surfactant is nonionic and is selected from at least any one of fatty alcohol polyoxyethylene ether, lauryl alcohol polyoxyethylene ether, isoalcohol polyoxyethylene ether, nonylphenol polyoxyethylene ether, alkylphenol polyoxyethylene ether, polyoxyethylene alkylamine, and polyoxyethylene alkylolamide.
7. The polysilicon polishing composition according to claim 2, wherein the pH adjusting agent is at least any one selected from the group consisting of tetrazole, imidazole, 1-methylimidazole, 2-methylimidazole, 4-methylimidazole, pyrazole, 1-methylpyrazole, 3-methylpyrazole, and 4-methylpyrazole; preferably, the pH of the polysilicon polishing composition is adjusted to 10 to 12.5.
8. The polysilicon polishing composition according to claim 2, wherein the humectant is selected from at least any one of propylene glycol, butylene glycol, hexylene glycol, glycerin, sorbitol, aminocyclopentanol.
9. The polysilicon polishing composition according to claim 2, wherein the bacteriostatic agent is at least any 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.
10. Use of the polysilicon polishing composition of any one of claims 1-9 in polysilicon chemical mechanical polishing.
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