CN113637413A - Silicon polishing composition, preparation method and application thereof - Google Patents
Silicon polishing composition, preparation method and application thereof Download PDFInfo
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- CN113637413A CN113637413A CN202111024184.1A CN202111024184A CN113637413A CN 113637413 A CN113637413 A CN 113637413A CN 202111024184 A CN202111024184 A CN 202111024184A CN 113637413 A CN113637413 A CN 113637413A
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- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
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Abstract
The invention provides a silicon polishing composition, a preparation method and application thereof. The polishing composition disclosed by the invention is simultaneously added with amino alcohol substances and water-soluble vitamins as auxiliaries, so that the abrasive agglomeration can be effectively inhibited, the service life of the polishing solution is prolonged, and the storage time of the polishing solution is prolonged.
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
High-purity monocrystalline silicon is the main substrate material for IC manufacturing at present, and as the integration degree of ICs is increased, the characteristic size of the monocrystalline silicon is reduced, so that higher requirements are made on the surface quality of large-size silicon wafers. Polishing can remove a surface damage layer generated in the silicon wafer cutting process and improve the surface quality of the silicon wafer, and a Chemical Mechanical Polishing (CMP) technology is considered to be the most effective method for global planarization of the wafer at present.
CMP is to polish the surface of a silicon wafer by using a polishing solution containing an abrasive and a polishing pad to generate chemical action, mechanical action and combination of the two actions, wherein the surface of the silicon wafer reacts with a chemical substance to form a soft layer in the polishing process, 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 dioxide and the silicon is 7, and the silicon dioxide also has fine granularity, the damaged layer on the surface of the polished wafer is thin, and the oxidation induced stacking fault (OSF) is basically less than 100/cm2The polishing solution has the advantages of meeting the requirements of LSI and VLSI integrated circuits, so that the polishing solution mainly takes nano silica colloid as abrasive particles and is combined with alkaline compounds as a rate accelerator, an acidic pH regulator, a surfactant and the like in the precision processing of the surface of monocrystalline silicon in the current market. However, due to the nano SiO2Small particle size, large specific surface area and high surface energy, and has the tendency of mutually attracting and agglomerating to reduce the surface energy, so that the nano SiO is concentrated under the condition of high concentration (15-40)2The agglomeration is easy to occur between the two, so that the performance of the polishing solution is reduced.
Korean patent publication KR1020050067846A proposes that anionic surfactants such as sodium dodecyl sulfate and sodium dodecyl ether sulfate are added to a silicon polishing solution to enhance the negative charges on the surface of silica sol particles, thereby achieving improved storage stability of the polishing solution and also reducing scratches on the polished surface. However, the anionic surfactant enhances the negative charge on the surface of the silica sol particles, so that the repulsive force between the silica sol particles and the silicon wafer is increased, and meanwhile, the surfactant also weakens the sliding friction force between the abrasive and the substrate, reduces the mechanical action in the polishing process, and both of the surfactants can cause the reduction of the polishing rate. In addition, sodium ions are also introduced into the substances, so that metal ions on the surface of the polished silicon wafer are easily polluted.
Chinese patent applications CN201110002321.1 and CN201811627080.8 propose to add silane coupling agents such as methyltrimethoxysilane and 3-aminopropyltriethoxysilane to silicon polishing solution, and to improve the storage stability of the polishing solution by grafting the surface of silica sol particles, while reducing the residue of silica sol particles on the polished surface, but because of the nano SiO2The graft coating of the surface molecular layer weakens the adsorption and carrying effects on reaction products such as silicate ions and the like, and has obvious adverse effect on the polishing rate. Therefore, there is a need to improve the components of the polishing solution from the viewpoint of chemical formulation to improve the storage stability and polishing performance of the polishing solution, and to overcome the above-mentioned drawbacks of the prior art.
Disclosure of Invention
In order to solve the technical problems, the invention provides a silicon polishing composition, and amino alcohol substances and water-soluble vitamins are added into nano silicon dioxide colloid as an auxiliary agent, so that abrasive agglomeration can be effectively inhibited, and the service life and the storage time of a polishing solution are prolonged.
It is another object of the present invention to provide a method for 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 for the chemical mechanical polishing of silicon wafers.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a silicon polishing composition takes nano silicon dioxide colloid as an abrasive, wherein the silicon polishing composition also comprises amino alcohol substances and water-soluble vitamins.
In a preferred embodiment, the silicon polishing composition comprises nano silicon dioxide colloid, amino alcohol substances, water-soluble vitamins, a rate accelerator, an acidic pH regulator, a surfactant, a bacteriostatic agent and the balance of deionized water; preferably, the mass ratio of the water-soluble vitamin to the amino alcohol substance is 0.05-0.9.
In a preferred embodiment, the silicon polishing composition comprises the following components: 1.5-40 wt% of nano silicon dioxide colloid, 0.5-5 wt% of amino alcohol substance, 0.02-4.5 wt% of water-soluble vitamin, 1-15 wt% of rate accelerator, 0.25-4 wt% of acidic pH regulator, 0.01-3 wt% of surfactant, 0.05-3 wt% of bacteriostatic agent and the balance of deionized water; wherein the mass ratio of the water-soluble vitamins to the amino alcohol substances is 0.05-0.9.
In a preferred embodiment, the silicon polishing composition comprises the following components: 5-30 wt% of nano silicon dioxide colloid, 1-4.0 wt% of amino alcohol substance, 0.15-3 wt% of water-soluble vitamin, 3-10 wt% of rate accelerator, 0.5-3.5 wt% of acidic pH regulator, 0.1-1.5 wt% of surfactant, 0.1-1.5 wt% of bacteriostatic agent and the balance of deionized water; wherein the mass ratio of the water-soluble vitamins to the amino alcohol substances is 0.05-0.9.
In a specific embodiment, the nano silica colloid has an average particle size of 30 to 80nm and a concentration of 30 to 50 wt%.
In a particular embodiment, the aminoalcohol species is selected from the group consisting of monoethanolamine, diethanolamine, triethanolamine, 3-amino-1-propanol, 1-amino-2-propanol, 2-amino-2-methyl-1-propanol, 2-dimethylamino-2-methyl-1-propanol, 2-amino-1, 3-propanediol, 2-amino-2-methyl-1, 3-propanediol, 2-amino-2- (hydroxymethyl) -1, 3-propanediol, 2-amino-2-ethyl-1, 3-propanediol, 2-amino-1-butanol, (R) -3-aminobutanol, (S) -3-aminobutanol, methanol, ethanol, 2-amino-2-amino-2-amino-2-amino-2-amino-2-amino-2-amino-2-3-2-1-amino-2-1, 2-amino-2-3-1-3-1-3-1-3-2-3-1-2-3-2-3-1-3-1-3-1-3-1, 2-3-1, 2-1-3-1, 4-amino-1-butanol, 2-amino-1-pentanol, 3-amino-1-pentanol, 4-amino-1-pentanol, 5-amino-1-pentanol, (2S) -2-amino-1, 5-pentanediol.
In a specific embodiment, the water-soluble vitamin is selected from at least any one of L-ascorbic acid, L-dehydroascorbic acid, L-isoascorbic acid, L-isodehydroascorbic acid, D-ascorbic acid, D-dehydroascorbic acid, vitamin B2, vitamin B5, vitamin B6.
In a specific embodiment, the rate accelerator is a basic compound selected from at least any one of potassium hydroxide, hydroxyethylethylenediamine, tetrahydroxypropylethylenediamine, ammonium hydroxide, tetramethylammonium hydroxide, tetraethylammonium hydroxide, tetrapropylammonium hydroxide, tetrabutylammonium hydroxide, (2-hydroxyethyl) trimethylammonium hydroxide, diethyldimethylammonium hydroxide, methyltriethylammonium hydroxide, benzyltrimethylammonium hydroxide, benzyltriethylammonium hydroxide, guanidine hydrochloride, guanidine carbonate, metformin, tetramethylguanidine, pyridazine, piperazine, pyrimidine, pyridine, triazole.
In a specific embodiment, the acidic pH adjusting agent is selected from at least any one of nitric acid, phosphoric acid, formic acid, acetic acid, citric acid, tartaric acid, lactic acid, malic acid, oxalic acid, malonic acid, succinic acid, glutaric acid; preferably, the pH of the silicon polishing composition is adjusted to 10 to 12.5.
In a specific embodiment, the surfactant is selected from at least any one of fatty alcohol polyoxyethylene ether, lauryl alcohol polyoxyethylene ether, fatty acid methyl ester ethoxylate, fatty acid polyoxyethylene ester, alkylphenol polyoxyethylene, nonylphenol polyoxyethylene ether, polyoxyethylene alkylamine, polyoxyethylene alkylolamide, N-bis-hydroxyethyl alkylamide, isomeric alcohol polyoxyethylene ether, alkylpolyglucoside, and tween.
In a specific embodiment, the bacteriostatic agent is selected from at least any one of polyhexamethylene guanidine hydrochloride, 2-methyl-4-isothiazolin-3-one, 2-methyl-5-chloro-4-isothiazolin-3-one, 2-n-octyl-4-isothiazolin-3-one, and fluorine-containing diphenylacryloyl morpholine.
On the other hand, the preparation method of the silicon polishing composition comprises the step of mixing the amino alcohol substance, the water-soluble vitamin and the nano silicon dioxide colloid in deionized water.
In a preferred embodiment, the amino alcohol substance and the water-soluble vitamin are thoroughly mixed and dispersed, and then mixed with the nano-silica colloid.
In a more preferable embodiment, after the amino alcohol substances, the water-soluble vitamins and the nano silicon dioxide colloid are mixed, the mixture is placed at a constant temperature of 20-25 ℃ for 24 hours, then the rate accelerator and the acidic pH regulator are mixed and added, and then the surfactant and the bacteriostatic agent are sequentially added to form the silicon polishing composition.
In yet another aspect, the use of the foregoing silicon polishing composition for chemical mechanical polishing of silicon wafers.
Compared with the prior art, the invention has the following beneficial effects:
in addition, amino alcohol substances and water-soluble vitamins are added into the polishing composition as an auxiliary agent to generate a synergistic effect, so that the stability of the polishing composition can be improved, the cycle service life and the storage time of the polishing composition can be prolonged, the cost is saved, and the polishing composition 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 silicon polishing composition takes nano silicon dioxide colloid as a main polishing component, and amino alcohol substances and water-soluble vitamins are added as auxiliary agents, namely, the silicon polishing composition is obtained by adding the amino alcohol substances and the water-soluble vitamins as the auxiliary agents on the basis of the existing silicon chemical mechanical polishing solution taking the nano silicon dioxide colloid as an abrasive.
The amino alcohol substance used in the method contains amino and one or more alcoholic hydroxyl groups, the water-soluble vitamin contains an acidic group and an alcoholic hydroxyl group, after the water-soluble vitamin and the amino alcohol substance are mixed according to the mass ratio of 0.05-0.9, the solution is alkaline, the pH value is 10-11, the structure of the water-soluble vitamin is destroyed, the alcoholic hydroxyl groups are retained and uniformly distributed in the solution, and at the moment, the solution contains a large number of alcoholic hydroxyl groups generated by the co-release of the amino alcohol substance and the water-soluble vitamin. When the solution is added into the nano-silica sol, the nano-SiO2The particles are in a dispersed system of polyhydroxy polyamine, under the alkaline environment, silicon hydroxyl (Si-OH) on the surfaces of the particles can form hydrogen bonds with alcoholic hydroxyl (R-OH) in the dispersion liquid,nano SiO2The condensation reactions between the silicon hydroxyl groups (Si-OH) of the particles are significantly reduced. By strengthening nano SiO2The interaction between the particles and the dispersion medium weakens the interaction between the nanoparticles, thereby reducing their tendency to agglomerate. Nano SiO in dispersion system2The particles are used as a dispersed phase and a dispersed medium, and the stability of the particles is obviously improved through a similar solvation mechanism, so that large particles generated by abrasive agglomeration in a cyclic polishing process can be effectively reduced, the polishing quality is improved, and meanwhile, the long-term storage of the polishing composition is facilitated. In addition, the amino alcohol substance also has the function of absorbing CO2And the like, also facilitates long-term storage of the polishing composition.
Wherein the nano silica colloid has a particle size of 30-80nm, such as but not limited to 30nm, 35nm, 40nm, 45nm, 50nm, 55nm, 60nm, 65nm, 70nm, 75nm, 80nm, and the silica sol has a concentration of 30-50 wt%, such as but not limited to 30 wt%, 35 wt%, 40 wt%, 45 wt%, 50 wt%.
Examples of the aminoalcohol are monoethanolamine, diethanolamine, triethanolamine, 3-amino-1-propanol, 1-amino-2-propanol, 2-amino-2-methyl-1-propanol, 2-dimethylamino-2-methyl-1-propanol, 2-amino-1, 3-propanediol, 2-amino-2-methyl-1, 3-propanediol, 2-amino-2- (hydroxymethyl) -1, 3-propanediol, 2-amino-2-ethyl-1, 3-propanediol, 2-amino-1-butanol, (R) -3-aminobutanol, (S) -3-aminobutanol, water-soluble salts of these amino alcohols, and salts thereof, At least one of 4-amino-1-butanol, 2-amino-1-pentanol, 3-amino-1-pentanol, 4-amino-1-pentanol, 5-amino-1-pentanol, (2S) -2-amino-1, 5-pentanediol, for example, any one, any two or more of the above amino alcohol substances, preferably monoethanolamine, triethanolamine, 1-amino-2-propanol, 2-amino-2-methyl-1-propanol, 2-amino-1, 3-propanediol, 2-amino-2-ethyl-1, 3-propanediol, 2-amino-1-butanol, 4-amino-1-butanol, 2-amino-1-pentanol, 2-amino-1, 5-pentanediol, and the like, 3-amino-1-pentanol or (2S) -2-amino-1, 5-pentanediol.
The water-soluble vitamin is, for example, at least one selected from the group consisting of L-ascorbic acid, L-dehydroascorbic acid, L-isoascorbic acid, L-isodehydroascorbic acid, D-ascorbic acid, D-dehydroascorbic acid, vitamin B2, vitamin B5 and vitamin B6, for example, any one, any two combinations or more of the above water-soluble vitamins, and preferably L-ascorbic acid, L-dehydroascorbic acid, D-ascorbic acid, D-dehydroascorbic acid or vitamin B2.
The mass ratio of the water-soluble vitamin and the amino alcohol substance is 0.05-0.9, such as but not limited to 0.05, 0.1, 0.15, 0.3, 0.45, 0.5, 0.6, 0.75, 0.8 and 0.9, preferably 0.3-0.75.
In addition to the above-mentioned nano silica colloid as abrasive, and three main components of amino alcohol substance and water-soluble vitamin are added, said invention does not limit any other additive component added in the polishing composition, and can be applicable to conventional various silicon chemical-mechanical polishing liquor systems, and also can arbitrarily select one or several of alkaline compound, acidic pH regulating agent, surfactant, bacteriostatic agent and wetting agent to add into the polishing composition according to the requirements for raising silicon removal rate and improving polished surface quality.
Wherein the basic compound acts as a primary rate accelerator and ionizes or hydrolyzes in the dispersion to render the OH of the polishing composition-The concentration is maintained at a level during recycling to facilitate the continued formation of a soft layer on the silicon surface. The rate accelerator is selected from at least any one of potassium hydroxide, hydroxyethylethylenediamine, tetrahydroxypropylethylenediamine, ammonium hydroxide, tetramethylammonium hydroxide, tetraethylammonium hydroxide, tetrapropylammonium hydroxide, tetrabutylammonium hydroxide, (2-hydroxyethyl) trimethylammonium hydroxide, diethyldimethylammonium hydroxide, methyltriethylammonium hydroxide, benzyltrimethylammonium hydroxide, benzyltriethylammonium hydroxide, guanidine hydrochloride, guanidine carbonate, metformin, tetramethylguanidine, pyridazine, piperazine, pyrimidine, pyridine, and triazole, for example, any one, any two combinations or more of the above rate accelerators, preferably potassium hydroxide, hydroxyethylethylenediamine, tetramethylammonium hydroxide, tetraethylammonium hydroxide, diethyldimethylammonium hydroxide, tetramethylguanidine, pyridazine, piperazine, pyrimidine, and triazole.
The acidic pH adjuster is, for example, at least one selected from nitric acid, phosphoric acid, formic acid, acetic acid, citric acid, tartaric acid, lactic acid, malic acid, oxalic acid, malonic acid, succinic acid, and glutaric acid, and is, for example, any one, any two combinations, or more of the above acidic pH adjusters, preferably phosphoric acid, citric acid, tartaric acid, oxalic acid, malonic acid, and succinic acid. The acidic pH regulator is used for regulating the pH value of the concentrated solution and preventing the concentrated solution from being too strong in alkalinity to cause nano SiO2The particles dissolve and the anions produced by their ionization have a complexing effect on the metal ions in the composition.
The surfactant is, for example, at least one selected from the group consisting of fatty alcohol polyoxyethylene ether, lauryl alcohol polyoxyethylene ether, fatty acid methyl ester ethoxylate, fatty acid polyoxyethylene ester, alkylphenol polyoxyethylene ether, nonylphenol polyoxyethylene ether, polyoxyethylene alkylamine, polyoxyethylene alkylolamide, N-hydroxyethyl alkylamide, isomeric alcohol polyoxyethylene ether, alkylpolyglucoside, and tween. The surfactant is used for reducing the surface tension of the composition, reducing the contact angle between the composition and the surface of a silicon wafer and enhancing the spreading performance of the composition on the surface of the silicon wafer.
The bacteriostatic agent is at least one selected from polyhexamethylene guanidine hydrochloride, 2-methyl-4-isothiazolin-3-one, 2-methyl-5-chloro-4-isothiazolin-3-one, 2-n-octyl-4-isothiazolin-3-one and fluorine-containing diphenylacryloyl morpholine, and is preferably any one, any two or more of the above bacteriostatic agents, preferably 2-n-octyl-4-isothiazolin-3-one, 2-methyl-4-isothiazolin-3-one and 2-methyl-5-chloro-4-isothiazolin-3-one. The bacteriostatic agent is used for inhibiting the reproduction 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 mass ratio of the water-soluble vitamin to the amino alcohol is 0.05-0.9, and the pH of the final silicon polishing composition is 10-12.5, such as but not limited to 10, 10.5, 11, 11.5, 12, 12.5, preferably 10.5-12.
The method for producing the silicon polishing composition of the present invention may be, for example, a method for producing a silicon polishing composition by mixing the components as is well known in the art, and specifically, for example, a method for producing a silicon polishing composition comprising a step of mixing a solution containing an aminoalcohol-based substance and a water-soluble vitamin with a nano silica colloid.
In a preferred embodiment, the amino alcohol substance and the water-soluble vitamin are fully mixed, then are mixed with the nano silicon dioxide colloid to form a dispersion, and then are kept stand at a constant temperature of 20-25 ℃ for 24 hours. The dispersing means in this process includes, but is not limited to, any one or more of mechanical stirring, ultrasonic dispersing, and magnetic stirring.
Then, after the amino alcohol substance, the water-soluble vitamin and the nano silicon dioxide colloid are mixed to form a dispersion liquid, the mixed liquid of the alkaline compound and the acidic pH regulator is continuously added, then the surfactant and the bacteriostatic agent are sequentially added, and the silicon polishing composition is formed after stirring and dispersing.
The invention is further illustrated, but not limited, by the following more specific examples.
In the following examples, the polishing machine used in the silicon wafer polishing test was a Speedfam 36B single-side polishing machine; the polishing pad is of Suba800 type, the polishing rotation speed is 40rpm, the polishing pressure is 160-180 kgf, the flow rate is 1.5L/min, the polishing time is 20min, and the polishing temperature is controlled to be 35-37 ℃. 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: the mass of the silicon wafer before and after polishing was measured by a precision balance to obtain a mass difference Δ m, and the removal rate MRR (μm/min) was calculated from the density and surface area of the silicon wafer and the polishing time.
Silicon wafer surface quality test: the root mean square surface roughness rms (nm) of the silicon wafers after polishing was tested using a Bruker-type atomic force microscope.
Particle size test of polishing composition: 1) the polishing composition was tested for average particle size using a Malvern Zetasizer type particle sizer; 2) the polishing composition was tested for large particle count (>0.50 μm) using an AccuSizer model 780 particle counter.
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
(1) Pretreatment of nano-silica colloid
10g of monoethanolamine and 0.5g L-ascorbic acid are dissolved in 200g of deionized water, the mixture is uniformly stirred, then the solution is added into 100g of 30 wt% nano silica colloid (with the average particle size of 30nm) while being stirred, ultrasonic dispersion is carried out for 20min, and then the mixture is placed for 24h at the constant temperature of 20-25 ℃ for standby.
(2) Formulation of polishing compositions
Dissolving 10g of hydroxyethyl ethylenediamine, 10g of piperazine and 5.5g of phosphoric acid in 400g of deionized water, and uniformly stirring; respectively adding 0.2g of fatty alcohol-polyoxyethylene ether and 1g of 2-n-octyl-4-isothiazoline-3-ketone into the mixture, and uniformly stirring the mixture; and (2) adding the solution into the nano silicon dioxide colloid treated in the step (1) while stirring, continuously adding deionized water until the total mass of the dispersion liquid is 2kg, and packaging after magnetic stirring for 30min, wherein the pH value of the dispersion liquid is 10.
Example 2
(1) Pretreatment of nano-silica colloid
Dissolving 20g of triethanolamine and 3g L-dehydroascorbic acid in 200g of deionized water, uniformly stirring, adding the solution into 250g of 40 wt% nano silica colloid (average particle size of 40nm) while stirring, performing ultrasonic dispersion for 20min, and standing at constant temperature of 20-25 ℃ for 24h for later use.
(2) Formulation of polishing compositions
Dissolving 30g of tetramethylammonium hydroxide, 30g of pyridazine and 25g of tartaric acid in 400g of deionized water, and uniformly stirring; respectively adding 2g of lauryl alcohol polyoxyethylene ether, 0.5g of 2-methyl-4-isothiazoline-3-ketone and 1.5g of 2-methyl-5-chloro-4-isothiazoline-3-ketone into the mixture, and uniformly stirring the mixture; and (2) adding the solution into the nano silicon dioxide colloid treated in the step (1) while stirring, continuously adding deionized water until the total mass of the dispersion liquid is 2kg, and packaging after magnetic stirring for 30min, wherein the pH value of the dispersion liquid is 10.5.
Example 3
(1) Pretreatment of nano-silica colloid
Dissolving 55g of 1-amino-2-propanol and 16.5g D-ascorbic acid in 200g of deionized water, uniformly stirring, adding the solution into 600g of 50 wt% nano silica colloid (with the average particle size of 60nm) while stirring, performing ultrasonic dispersion for 20min, and standing at a constant temperature of 20-25 ℃ for 24h for later use.
(2) Formulation of polishing compositions
60g of tetraethylammonium hydroxide, 40g of pyrimidine and 38g of citric acid are dissolved in 400g of deionized water and stirred uniformly; respectively adding 10g of isomeric alcohol polyoxyethylene and 10g of 2-n-octyl-4-isothiazoline-3-ketone into the mixture, and uniformly stirring the mixture; and (2) adding the solution into the nano silicon dioxide colloid treated in the step (1) while stirring, continuously adding deionized water until the total mass of the dispersion liquid is 2kg, and packaging after magnetic stirring for 30min, wherein the pH value of the dispersion liquid is 11.
Example 4
(1) Pretreatment of nano-silica colloid
Dissolving 70g of 2-amino-2-methyl-1-propanol and 35g of vitamin B2 in 200g of deionized water, uniformly stirring, adding the solution into 1000g of 40 wt% nano silicon dioxide colloid (with the average particle size of 80nm) while stirring, performing ultrasonic dispersion for 20min, and standing at a constant temperature of 20-25 ℃ for 24h for later use.
(2) Formulation of polishing compositions
Dissolving 100g of diethyl dimethyl ammonium hydroxide, 50g of piperazine and 53g of anhydrous oxalic acid in 400g of deionized water, and uniformly stirring; respectively adding 17g of isomeric alcohol polyoxyethylene, 7.5g of 2-methyl-4-isothiazoline-3-ketone and 22.5g of 2-methyl-5-chloro-4-isothiazoline-3-ketone into the mixture, and uniformly stirring the mixture; and (2) adding the solution into the nano silicon dioxide colloid treated in the step (1) while stirring, continuously adding deionized water until the total mass of the dispersion liquid is 2kg, and packaging after magnetic stirring for 30min, wherein the pH value of the dispersion liquid is 11.5.
Example 5
(1) Pretreatment of nano-silica colloid
Dissolving 80g of 2-amino-1, 3-propylene glycol and 60g D-dehydroascorbic acid in 200g of deionized water, uniformly stirring, adding the solution into 1200g of 50 wt% nano silicon dioxide colloid (with the average particle size of 60nm) while stirring, performing ultrasonic dispersion for 20min, and standing at a constant temperature of 20-25 ℃ for 24h for later use.
(2) Formulation of polishing compositions
Dissolving 80g of tetramethylammonium hydroxide, 20g of triazole and 18g of phosphoric acid in 200g of deionized water, and uniformly stirring; respectively adding 30g of polyoxyethylene lauryl ether and 40g of 2-n-octyl-4-isothiazoline-3-ketone into the mixture, and uniformly stirring the mixture; and (2) adding the solution into the nano silicon dioxide colloid treated in the step (1) while stirring, continuously adding deionized water until the total mass of the dispersion liquid is 2kg, and packaging after magnetic stirring for 30min, wherein the pH value of the dispersion liquid is 11.5.
Example 6
(1) Pretreatment of nano-silica colloid
Dissolving 100g of 2-amino-2-ethyl-1, 3-propylene glycol and 90g of L-ascorbic acid in 200g of deionized water, uniformly stirring, adding the solution into 900g of 40 wt% nano silica colloid (with the average particle size of 80nm) while stirring, performing ultrasonic dispersion for 20min, and standing at a constant temperature of 20-25 ℃ for 24h for later use.
(2) Formulation of polishing compositions
Dissolving 150g of potassium hydroxide, 50g of tetramethylguanidine and 70g of malonic acid in 300g of deionized water, and uniformly stirring; then 60g of Tween, 15g of 2-methyl-4-isothiazolin-3-one and 45g of 2-methyl-5-chloro-4-isothiazolin-3-one are respectively added into the mixture and stirred uniformly; and (2) adding the solution into the nano silicon dioxide colloid treated in the step (1) while stirring, continuously adding deionized water until the total mass of the dispersion liquid is 2kg, and packaging after magnetic stirring for 30min, wherein the pH value of the dispersion liquid is 12.
Example 7
(1) Pretreatment of nano-silica colloid
Dissolving 55g of 2-amino-1-butanol and 22g of vitamin B2 in 200g of deionized water, uniformly stirring, adding the solution into 800g of 30 wt% nano silicon dioxide colloid (with the average particle size of 30nm) while stirring, performing ultrasonic dispersion for 20min, and standing at the constant temperature of 20-25 ℃ for 24h for later use.
(2) Formulation of polishing compositions
Dissolving 250g of tetramethylammonium hydroxide, 50g of triazole and 80g of succinic acid in 400g of deionized water, and uniformly stirring; respectively adding 35g of fatty alcohol-polyoxyethylene ether, 2.5g of 2-methyl-4-isothiazoline-3-ketone and 7.5g of 2-methyl-5-chloro-4-isothiazoline-3-ketone into the mixture, and uniformly stirring the mixture; and (2) adding the solution into the nano silicon dioxide colloid treated in the step (1) while stirring, continuously adding deionized water until the total mass of the dispersion liquid is 2kg, and packaging after magnetic stirring for 30min, wherein the pH value of the dispersion liquid is 12.5.
Example 8
(1) Pretreatment of nano-silica colloid
Dissolving 20g of 4-amino-1-butanol and 3g L-dehydroascorbic acid in 200g of deionized water, uniformly stirring, adding the solution into 1600g of 50 wt% nano silica colloid (with the average particle size of 60nm) while stirring, performing ultrasonic dispersion for 20min, and standing at a constant temperature of 20-25 ℃ for 24h for later use.
(2) Formulation of polishing compositions
Dissolving 30g of tetramethylammonium hydroxide, 10g of triazole and 10g of citric acid in 100g of deionized water, and uniformly stirring; respectively adding 10g of fatty alcohol-polyoxyethylene ether, 2.5g of 2-methyl-4-isothiazoline-3-ketone and 7.5g of 2-methyl-5-chloro-4-isothiazoline-3-ketone into the mixture, and uniformly stirring the mixture; and (2) adding the solution into the nano silicon dioxide colloid treated in the step (1) while stirring, continuously adding deionized water until the total mass of the dispersion liquid is 2kg, and packaging after magnetic stirring for 30min, wherein the pH value of the dispersion liquid is 11.5.
Example 9
(1) Pretreatment of nano-silica colloid
Dissolving 70g of 3-amino-1-pentanol and 21g of L-ascorbic acid in 200g of deionized water, uniformly stirring, adding the solution into 750g of 40 wt% nano silica colloid (with the average particle size of 40nm) while stirring, performing ultrasonic dispersion for 20min, and standing at the constant temperature of 20-25 ℃ for 24h for later use.
(2) Formulation of polishing compositions
Dissolving 100g of potassium hydroxide, 50g of pyridazine and 50g of citric acid in 400g of deionized water, and uniformly stirring; respectively adding 17g of isomeric alcohol polyoxyethylene ether and 15g of 2-n-octyl-4-isothiazoline-3-ketone into the mixture, and uniformly stirring the mixture; and (2) adding the solution into the nano silicon dioxide colloid treated in the step (1) while stirring, continuously adding deionized water until the total mass of the dispersion liquid is 2kg, and packaging after magnetic stirring for 30min, wherein the pH value of the dispersion liquid is 11.5.
Example 10
(1) Pretreatment of nano-silica colloid
Dissolving 80g of (2S) -2-amino-1, 5-pentanediol and 40g of L-ascorbic acid in 200g of deionized water, uniformly stirring, adding the solution into 1000g of 50 wt% nano silicon dioxide colloid (with the average particle size of 60nm) while stirring, performing ultrasonic dispersion for 20min, and standing at the constant temperature of 20-25 ℃ for 24h for later use;
(2) formulation of polishing compositions
Dissolving 150g of tetraethylammonium hydroxide, 50g of piperazine and 65g of oxalic acid in 400g of deionized water, and uniformly stirring; respectively adding 17g of polyoxyethylene lauryl ether and 15g of 2-n-octyl-4-isothiazoline-3-ketone into the mixture, and uniformly stirring the mixture; and (2) adding the solution into the nano silicon dioxide colloid treated in the step (1) while stirring, continuously adding deionized water until the total mass of the dispersion liquid is 2kg, and packaging after magnetic stirring for 30min, wherein the pH value of the dispersion liquid is 11.5.
Comparative example 1
Compared with example 3, step (1) is as follows, and other process conditions are exactly the same.
(1) Pretreatment of nano-silica colloid
Adding 200g of deionized water into 600g of 50 wt% nano silicon dioxide colloid (with the average particle size of 60nm), carrying out ultrasonic dispersion for 20min, and then standing at a constant temperature of 20-25 ℃ for 24h for later use.
Comparative example 2
Compared with example 5, step (1) is as follows, and other process conditions are exactly the same.
(1) Pretreatment of nano-silica colloid
200g of deionized water is added into 1200g of 50 wt% nano silicon dioxide colloid (with the average particle size of 60nm), ultrasonic dispersion is carried out for 20min, and then the mixture is placed at a constant temperature of 20-25 ℃ for 24h for later use.
Comparative example 3
Compared with example 5, step (1) is as follows, and other process conditions are exactly the same.
(1) Pretreatment of nano-silica colloid
Dissolving 80g of 2-amino-1, 3-propylene glycol in 200g of deionized water, uniformly stirring, adding the solution into 1200g of 50 wt% nano silica colloid (with the average particle size of 60nm) while stirring, performing ultrasonic dispersion for 20min, and standing at a constant temperature of 20-25 ℃ for 24h for later use.
Comparative example 4
Compared with example 5, step (1) is as follows, and other process conditions are exactly the same.
(1) Pretreatment of nano-silica colloid
Dissolving 60g D-dehydroascorbic acid in 200g of deionized water, uniformly stirring, adding the solution into 1200g of 50 wt% nano silicon dioxide colloid (with the average particle size of 60nm) while stirring, performing ultrasonic dispersion for 20min, and standing at a constant temperature of 20-25 ℃ for 24h for later use.
Comparative example 5
Compared with the embodiment 7, the raw materials are the same, the preparation process (silica sol pretreatment) is different, and the step (1) is as follows:
(1) pretreatment of nano-silica colloid
Dissolving 55g of 2-amino-1-butanol and 22g of vitamin B2 in 200g of deionized water, stirring uniformly, adding the solution into 800g of 30 wt% nano silicon dioxide colloid (with the average particle size of 30nm) while stirring, and performing ultrasonic dispersion for 20min for later use.
Comparative example 6
Compared with the example 9, the raw materials are the same, the preparation process is different, and the method specifically comprises the following steps:
(1) pretreatment of nano-silica colloid
Adding 200g of deionized water into 750g of 40 wt% nano silicon dioxide colloid (with the average particle size of 40nm), carrying out ultrasonic dispersion for 20min, and then standing at a constant temperature of 20-25 ℃ for 24h for later use.
(2) Formulation of polishing compositions
70g of 3-amino-1-pentanol, 21g of L-ascorbic acid, 100g of potassium hydroxide, 50g of pyridazine and 50g of citric acid; dissolving in 400g of deionized water, and uniformly stirring; respectively adding 17g of isomeric alcohol polyoxyethylene ether and 15g of 2-n-octyl-4-isothiazoline-3-ketone into the mixture, and uniformly stirring the mixture; and (2) adding the solution into the nano silicon dioxide colloid treated in the step (1) while stirring, continuously adding deionized water until the total mass of the dispersion liquid is 2kg, and packaging after magnetic stirring for 30min, wherein the pH value of the dispersion liquid is 11.5.
Each of the example and comparative example polishing compositions was diluted at a volume ratio of 1:20 and then subjected to a polishing test; each of the example and comparative polishing compositions was placed in an oven at 40 ℃ at 200g for stability testing. The polishing test results and the standing stability test results are shown in tables 1 and 2, respectively:
TABLE 1 results of polishing tests
Table 2 standing stability test results
Comparing comparative example 1 with example 3, and comparative example 2 with example 5 in table 1 above, it can be seen that the average particle size of the compositions of examples 3 and 5 is significantly lower, the removal rate variation is smaller, and the root mean square surface roughness of the polished wafer is relatively smaller, which indicates that alcoholic hydroxyl groups generated by amino alcohol substances and water-soluble vitamins in the dispersion system can effectively inhibit the agglomeration of silica sol particles during the cyclic polishing process, and has a positive effect on prolonging the service life and improving the polishing performance of the polishing composition.
Comparing comparative example 5 with example 7 and comparative example 6 with example 9, it can be found that the average particle size, the removal rate and the root mean square surface roughness are improved to some extent after the polishing of examples 7 and 9 is carried out for 15 times, which shows that the pretreatment process of the nano silica colloid has a certain influence on the polishing performance of the composition, presumably because the alcoholic hydroxyl group can be sufficiently released and is more favorable for generating solvation effect with the silicon hydroxyl group on the surface of the silica sol particle when the silica sol is treated by the two substances and is left for a certain time.
Comparing comparative example 1 with example 3, and comparative example 2 with example 5 in table 2 above, it can be seen that the compositions of examples 3 and 5 have significantly smaller average particle size change after being placed at a constant temperature of 40 ℃ for 70 days, and the large particle count (>0.5 μm) in the LPC test is significantly lower, which reflects that alcoholic hydroxyl groups generated by amino alcohol substances and water-soluble vitamins can inhibit agglomeration and sedimentation of silica sol particles for a long time, and has a positive effect on improving the storage property of the polishing composition. Comparing comparative example 5 with example 7, and comparative example 6 with example 9, it is found that the change range of the average particle size is smaller after the samples 7 and 9 are placed at a constant temperature of 40 ℃ for 70 days, and the large particle number (>0.5 μm) of the LPC test is lower, and the combination of comparative example 1 and comparative example 2 shows that the nano-silica pretreatment process adopted in the samples 1-10 can effectively reduce the agglomeration of silica sol particles in the storage process.
Compared with the comparative example 2, the average grain diameter of the compositions after the cyclic polishing of the comparative examples 3 and 4 is slightly reduced, the root mean square surface roughness of the polished wafer is slightly reduced, and the change range of the average grain diameter is relatively smaller after the wafer is placed at a constant temperature of 40 ℃ for 70 days, but compared with the example 5, the difference is still obvious. This shows that a single alcamines substance can play a certain role in improving the stability of the composition, but the effect is limited, and the long-term stable placement and other performances of the composition are not enough; in comparison, the effect of the single water-soluble vitamin is less obvious, and the alcohol amine substance and the water-soluble vitamin are added simultaneously, so that the performance of the composition can be obviously improved through the synergistic effect of the alcohol amine substance and the water-soluble vitamin.
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 or adaptations to the invention may be made in light of the teachings of the present specification. Such modifications or adaptations are intended to be within the scope of the present invention as defined in the claims.
Claims (11)
1. A silicon polishing composition takes nano silicon dioxide colloid as an abrasive, and is characterized by also comprising amino alcohol substances and water-soluble vitamins.
2. The silicon polishing composition as set forth in claim 1, comprising a nano silica colloid, an aminoalcohol substance, a water-soluble vitamin, a rate accelerator, an acidic pH adjuster, a surfactant, a bacteriostatic agent, and the balance being deionized water; preferably, the mass ratio of the water-soluble vitamin to the amino alcohol substance is 0.05-0.9; more preferably, the content of each component is as follows: 1.5-40 wt% of nano silicon dioxide colloid, 0.5-5 wt% of amino alcohol substance, 0.02-4.5 wt% of water-soluble vitamin, 1-15 wt% of rate accelerator, 0.25-4 wt% of acidic pH regulator, 0.01-3 wt% of surfactant, 0.05-3 wt% of bacteriostatic agent and the balance of deionized water; further preferably, the content of each component is as follows: 5-30 wt% of nano silicon dioxide colloid, 1-4.0 wt% of amino alcohol substance, 0.15-3 wt% of water-soluble vitamin, 3-10 wt% of rate accelerator, 0.5-3.5 wt% of acidic pH regulator, 0.1-1.5 wt% of surfactant, 0.1-1.5 wt% of bacteriostatic agent and the balance of deionized water.
3. The silicon polishing composition according to claim 1 or 2, wherein the nano silica colloid has an average particle diameter of 30 to 80nm and a concentration of 30 to 50 wt%.
4. The silicon polishing composition according to claim 1 or 2, wherein the aminoalcohol compound is selected from the group consisting of monoethanolamine, diethanolamine, triethanolamine, 3-amino-1-propanol, 1-amino-2-propanol, 2-amino-2-methyl-1-propanol, 2-dimethylamino-2-methyl-1-propanol, 2-amino-1, 3-propanediol, 2-amino-2-methyl-1, 3-propanediol, 2-amino-2- (hydroxymethyl) -1, 3-propanediol, 2-amino-2-ethyl-1, 3-propanediol, 2-amino-1-butanol, (R) -3-aminobutanol, diethanolamine, triethanolamine, and mixtures thereof, (S) -3-aminobutanol, 4-amino-1-butanol, 2-amino-1-pentanol, 3-amino-1-pentanol, 4-amino-1-pentanol, 5-amino-1-pentanol, and (2S) -2-amino-1, 5-pentanediol.
5. The silicon polishing composition according to claim 1 or 2, wherein the water-soluble vitamin is at least any one selected from the group consisting of L-ascorbic acid, L-dehydroascorbic acid, L-isoascorbic acid, L-isodehydroascorbic acid, D-ascorbic acid, D-dehydroascorbic acid, vitamin B2, vitamin B5, and vitamin B6.
6. The silicon polishing composition according to claim 2, wherein the rate accelerator is a basic compound selected from at least any one of potassium hydroxide, hydroxyethylethylenediamine, tetrahydroxypropylethylenediamine, ammonium hydroxide, tetramethylammonium hydroxide, tetraethylammonium hydroxide, tetrapropylammonium hydroxide, tetrabutylammonium hydroxide, (2-hydroxyethyl) trimethylammonium hydroxide, diethyldimethylammonium hydroxide, methyltriethylammonium hydroxide, benzyltrimethylammonium hydroxide, benzyltriethylammonium hydroxide, guanidine hydrochloride, guanidine carbonate, metformin, tetramethylguanidine, pyridazine, piperazine, pyrimidine, pyridine, and triazole.
7. The silicon polishing composition according to claim 2, wherein the acidic pH adjusting agent is selected from at least any one of nitric acid, phosphoric acid, formic acid, acetic acid, citric acid, tartaric acid, lactic acid, malic acid, oxalic acid, malonic acid, succinic acid, glutaric acid; preferably, the pH of the silicon polishing composition is adjusted to 10 to 12.5.
8. The silicon polishing composition according to claim 2, wherein the surfactant is selected from at least any one of fatty alcohol polyoxyethylene ether, lauryl alcohol polyoxyethylene ether, fatty acid methyl ester ethoxylate, fatty acid polyoxyethylene ester, alkylphenol polyoxyethylene ether, nonylphenol polyoxyethylene ether, polyoxyethylene alkylamine, polyoxyethylene alkylolamide, N-bis-hydroxyethyl alkylamide, isoalcohol polyoxyethylene ether, alkylpolyglucoside, and tween.
9. The silicon polishing composition according to claim 2, wherein the bacteriostatic agent is at least any one selected from polyhexamethyleneguanidine hydrochloride, 2-methyl-4-isothiazolin-3-one, 2-methyl-5-chloro-4-isothiazolin-3-one, 2-n-octyl-4-isothiazolin-3-one, and fluorine-containing diphenylacryloylmorpholine.
10. The method of producing a silicon polishing composition according to any one of claims 1 to 9, comprising the steps of mixing an aminoalcohol substance, a water-soluble vitamin and a nano silica colloid in deionized water; preferably, the amino alcohol substance and the water-soluble vitamin are fully mixed and dispersed firstly, and then are mixed with the nano silicon dioxide colloid; more preferably, the amino alcohol substance, the water-soluble vitamin and the nano silicon dioxide colloid are mixed and then placed at a constant temperature of 20-25 ℃ for 24 hours, then the rate accelerator and the acidic pH regulator are mixed and added, and then the surfactant and the bacteriostatic agent are sequentially added to form the silicon polishing composition.
11. Use of a silicon polishing composition according to any one of claims 1 to 9 for chemical mechanical polishing of silicon wafers.
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| CN115093794A (en) * | 2022-06-17 | 2022-09-23 | 万华化学集团电子材料有限公司 | Polysilicon polishing composition and application thereof |
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