CN102775915A - Silicon wafer fine polishing combined solution capable of inhibiting particle deposition and preparation method thereof - Google Patents
Silicon wafer fine polishing combined solution capable of inhibiting particle deposition and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a silicon wafer fine polishing combined solution capable of inhibiting particle deposition and a preparation method thereof, belonging to the field of CMP (chemical mechanical polishing). The silicon wafer fine polishing combined solution capable of inhibiting particle deposition is prepared by using silicon dioxide/water-soluble polymer composite abrasive particles, hydroxyl-containing and/or amino-containing surface protecting agent, alkali compound, surfactant and deionized water. The pH (potential of hydrogen) of the silicon wafer fine polishing combined solution is 8-12. Compared with the prior art, the deposition of particles is effectively inhibited, and the precision and the quality of polished silicon wafer surfaces are improved. The silicon wafer fine polishing combined solution provided by the invention has the advantages that the used raw materials are easy to obtain, the silicon wafer fine polishing combined solution is pollution free, the requirements on environmental protection are satisfied and the large-scale industrial production is easy to realize.
Description
Technical field
The present invention relates to chemically machinery polished (CMP) field, particularly a kind of silicon wafer finishing polish combination liquid that suppresses particle deposition.
Background technology
Silicon wafer is the main substrate of unicircuit (IC), along with improving constantly of unicircuit integrated level, constantly the reducing of characteristic dimension, to the working accuracy of silicon wafer and surface quality require increasingly high.At present; Utilize chemically machinery polished (CMP) technology that silicon wafer surface is carried out planarization; Become ic manufacturing technology and got into deep-submicron one of requisite process step of Age of Technology later on; A collection of related patent U.S. Patent No. technology is disclosed both at home and abroad in succession, like EP0371147B1, US5352277, CN101671528A, CN102061131A.
Traditional CMP system is made up of following three parts: the silicon wafer clamping device of rotation, worktable, polishing fluid (slurry) supply system of carrying polishing pad.During polishing; The silicon wafer of rotation imposes on the polishing pad that rotates with worktable with certain pressure; Polishing fluid flows between silicon wafer and polishing pad, and produces chemical reaction at silicon wafer surface, and the chemical reactant that silicon wafer surface forms is removed by the mechanical friction effect of abrasive material.In the alternation procedure of chemical membrane and mechanical striping, remove layer of material as thin as a wafer through the chemistry and the acting in conjunction of machinery from silicon wafer surface, finally realize ultra-precision surface processing.
Usually; In industry in order to realize the polishing working accuracy of silicon wafer; Reach the technical indicator of unicircuit silicon wafer requirement, need carry out two step chemically machinery polisheds (CMP) (rough polishing and finishing polish), when silicon wafer surface is carried out step chemical mechanical polishing; Per step polishes employed polishing fluid and corresponding polishing technological conditions is all different, and the working accuracy that each step institute of pairing silicon wafer will reach is difference also.In the rough polishing step, remove silicon wafer cutting and the surface damage layer under residual of being shaped, be processed into minute surface, at last through silicon wafer is carried out finishing polish, thereby reduce surfaceness and other free tiny flaws to the full extent.
In actual production, the final finishing polish of silicon wafer is the decisive step of surface quality, in the finishing polish process, be prone to produce defectives such as polishing mist and cut, and one of reason that produces these defectives is exactly the particulate deposition.The generation that the particulate deposition causes polishing mist and cut causes the integrity that graphic defects, epitaxy defect, influence are connected up, and is the biggest obstacle of high yield; Particularly when the silicon wafer bonding; Introduce microgap, also cause dislocation simultaneously, influence bond strength and surface quality.Therefore, effectively controlling particle deposition is one of important indicator of check silicon wafer precise polishing solution.At present; Can submicron and nano particle that major part remain in silicon wafer surface be removed through cleaning preferably, but still have some " stubbornness " particles that in polishing process, form (being generally particle or cluster of grains) to remove through cleaning thoroughly less than 500nm.Therefore, if in polishing process, just particle residue is controlled, pass through follow-up cleaning process again, the particle that is deposited on silicon wafer surface just is hopeful thorough removal.The enough sizes with deposited particles of silicon wafer finishing polish combination fluid power of the present invention are controlled in the 100nm, and realize that simultaneously surface quality is high, and surfaceness is low.
Summary of the invention
The present invention has overcome the difficult problem of silicon wafer precise polishing solution particle deposition in polishing process in the prior art, and it is high to have proposed a kind of polished silicon wafer surface precision, the silicon wafer finishing polish combination liquid that particle residue is few.
In order to realize above-mentioned target, the present invention has adopted colloid silica/water-soluble polymers Compostie abrasive particles, the surface protectant of hydroxyl and/or amido, and these components have effectively suppressed the particulate deposition, have improved the precision and the quality of polishing back silicon wafer surface.
Liquid is made up in a kind of silicon wafer finishing polish that suppresses particle deposition of the present invention, comprises surface protectant, basic cpd, tensio-active agent and the deionized water of colloid silica/water-soluble polymers Compostie abrasive particles, hydroxyl and/or amido; The pH value of this finishing polish combination liquid is 8～12.
The set of dispense ratio of finishing polish combination liquid of the present invention is:
Both ratios of described colloid silica/water-soluble polymers Compostie abrasive particles are 12～400:1.
The median size of described colloid silica is 18～80nm.
The water-soluble polymers of described colloid silica/water-soluble polymers Compostie abrasive particles is one or more in the hydroxypropylcellulose of Natvosol or lipid modification of guar gum, XG 550, sodium-alginate, CMS, FM, CMC 99.5, sulfonic acid TKK 021, Tylose CH 50, methylcellulose gum, carboxyethyl methylphosphinate Mierocrystalline cellulose, Vltra tears, hydroxy butyl methyl cellulose, Natvosol, lipid modification.
The surface protectant of described said hydroxyl and/or amido is one or more in Z 150PH, Z 150PH and polystyrene block copolymer, polyoxyethylene glycol, polyoxyethylene, polyoxyethylene and ethylene oxide-propylene oxide block copolymer, ROHM, methylamine, dimethyl amine, Trimethylamine, ethylamine, DIETHANOL AMINE, triethylamine, Yi Bingchunan, tetraethyl-amine, diethyl triamine, triethyl tetramine, AEEA, hexamethylene-diamine, NSC 446, Triethylenetetramine (TETA), thanomin, diethylolamine, the trolamine.
Described basic cpd is one or more in Pottasium Hydroxide, sodium hydroxide, volatile salt, bicarbonate of ammonia, saleratus, salt of wormwood, sodium hydrogencarbonate, yellow soda ash, ammoniacal liquor, aminopropanol, TMAH, tetraethyl ammonium hydroxide, TPAOH, TBAH, trimethyl hydroxyethylammoniumhydroxide hydroxide, dimethyl-dihydroxy ethyl volatile caustic, Piperazine anhydrous or the Uricida.
Described tensio-active agent is one or more in nonionogenic tenside, AS or the cats product.
Described nonionogenic tenside is one or more in YSR 3286, T 46155 (9) lauryl alcohol, AEO, polyoxyethylene nonylphenol, polyoxyethylene octylphenol ether, the polyoxyethylene polyoxypropylene segmented copolymer; AS is X 2073, sodium laurylsulfonate, one or more in terminal olefin sodium sulfonate, succinate sodium 2-ethylhexyl, Fatty Alcohol(C12-C14 and C12-C18) (10) T 46155, the polyoxyethylenated alcohol sodium sulfate; Cats product is one or more in tetradecyl dimethyl benzyl ammonium chloride, DTAC, guar hydroxypropyl trimonium chloride, bromination dodecyl trimethyl ammonium, the bromination dodecyl dimethyl hexadecyldimethyl benzyl ammonium.
Described colloid silica/water-soluble polymers Compostie abrasive particles 5.1005wt%, wherein, colloid silica 5wt%, water-soluble polymers are guar gum 0.005wt% and Natvosol 0.1wt%; Surface protectant is triethylamine 0.04wt%, and tensio-active agent is AEO 0.004wt%, and alkalify is combined into thing ammoniacal liquor 1.0wt%, and surplus is a deionized water.
A kind of preparation method who suppresses the silicon wafer finishing polish combination liquid of particle deposition is characterized in that this method may further comprise the steps:
Take by weighing colloid silica and water-soluble polymers in proportion, by the physical blending mode both are mixed, and at the uniform velocity stir, prepare colloid silica/water-soluble polymers Compostie abrasive particles with whisking appliance;
Colloid silica/water-soluble polymers Compostie abrasive particles is scattered in the deionized water, and fully stirs with whisking appliance;
The surface protectant that adds hydroxyl and/or amido makes itself and Compostie abrasive particles thorough mixing in whisking appliance;
Add tensio-active agent and basic cpd successively, and liquid pH regulator to 8～12 are made up in finishing polish;
Using the aperture is that the following filter core of 0.5 μ m filters finishing polish combination liquid, removes the large granular impurity in the finishing polish combination liquid.
The present invention compared with prior art has following advantage:
1) colloid silica/water-soluble polymers Compostie abrasive particles in the finishing polish combination liquid of the present invention; Make water-soluble polymers be wrapped in the surface of titanium dioxide colloid silica uniformly; Improved the sticking power of titanium dioxide colloid silica; Form the inorganic nucleocapsid structure of a kind of organic parcel, effectively suppress particle deposition, reduce residual in silicon wafer surface and the polishing pad;
2) finishing polish combination liquid of the present invention is through adding the surface protectant of hydroxyl and/or amido; Reduced the firmness of silicon wafer surface particle deposition; Make the particle that remains in silicon wafer surface more be prone to polished liquid and take away, help polishing the cleaning of back silicon wafer and polishing pad;
3) liquid is raw materials used is easy to get in finishing polish of the present invention combination, and is pollution-free, compliance with environmental protection requirements and carry out large-scale industrial production easily.
Description of drawings
Fig. 1 uses general silica colloidal sol in the prior art, do not add the surface protectant of water-soluble polymers and hydroxyl and/or amido, the AFM of silicon wafer (AFM) photo (comparative example 5) after the finishing polish.
Fig. 2 has added the surface protectant of hydroxyl and/or amido for having adopted colloid silica/water-soluble polymers Compostie abrasive particles in the finishing polish of the present invention combination liquid, but each components do match AFM photo (embodiment 2) of silicon wafer after finishing polish when relatively poor.
Fig. 3 has added the surface protectant of hydroxyl and/or amido for having adopted colloid silica/water-soluble polymers Compostie abrasive particles in the finishing polish of the present invention combination liquid, and each components do match AFM photo (embodiment 6) of silicon wafer after finishing polish when better.
Embodiment
Through specific embodiment the present invention is done further elaboration below, the scope that in no case should be construed as limiting the invention certainly.
Liquid is made up in a kind of silicon wafer finishing polish that suppresses particle deposition of the present invention, comprises surface protectant, basic cpd, tensio-active agent and the deionized water of colloid silica/water-soluble polymers Compostie abrasive particles, hydroxyl and/or amido; The pH value of this finishing polish combination liquid is 8～12.Wherein, The weight percent content of colloid silica/water-soluble polymers Compostie abrasive particles is 2～13wt%; The weight percent content of the surface protectant of hydroxyl and/or amido is 0.002～0.5wt%; The weight percent content of basic cpd is 0.5～4wt%, and the weight percent content of tensio-active agent is 0.002～0.5wt%, and surplus is a deionized water.Colloid silica/water-soluble polymers Compostie abrasive particles does, adopts the mode of physical blending that colloid silica and water-soluble polymers are mixed together by a certain percentage, and colloid silica is that median size is 18～80nm.
Wherein, the ratio of colloid silica and water-soluble polymers is 12～400:1.
Described water-soluble polymers is one or more in the hydroxypropylcellulose of Natvosol or lipid modification of guar gum, XG 550, sodium-alginate, CMS, FM, CMC 99.5, sulfonic acid TKK 021, Tylose CH 50, methylcellulose gum, carboxyethyl methylphosphinate Mierocrystalline cellulose, Vltra tears, hydroxy butyl methyl cellulose, Natvosol, lipid modification.
The surface protectant of described hydroxyl and/or amido is one or more in Z 150PH, Z 150PH and polystyrene block copolymer, polyoxyethylene glycol, polyoxyethylene, polyoxyethylene and ethylene oxide-propylene oxide block copolymer, ROHM, methylamine, dimethyl amine, Trimethylamine, ethylamine, DIETHANOL AMINE, triethylamine, Yi Bingchunan, tetraethyl-amine, diethyl triamine, triethyl tetramine, AEEA, hexamethylene-diamine, NSC 446, Triethylenetetramine (TETA), thanomin, diethylolamine, the trolamine.
Described basic cpd is one or more in Pottasium Hydroxide, sodium hydroxide, volatile salt, bicarbonate of ammonia, saleratus, salt of wormwood, sodium hydrogencarbonate, yellow soda ash, ammoniacal liquor, aminopropanol, TMAH, tetraethyl ammonium hydroxide, TPAOH, TBAH, trimethyl hydroxyethylammoniumhydroxide hydroxide, dimethyl-dihydroxy ethyl volatile caustic, Piperazine anhydrous or the Uricida.Basic cpd plays the corrosive effect to silicon wafer surface, and kind that can be through regulating basic cpd and content are regulated finishing polish and removed speed, and the final pH of polishing fluid is controlled at 8～12.
Described tensio-active agent is one or more in nonionogenic tenside, AS or the cats product.
Wherein, nonionogenic tenside is one or more in YSR 3286, T 46155 (9) lauryl alcohol, AEO, polyoxyethylene nonylphenol, polyoxyethylene octylphenol ether, the polyoxyethylene polyoxypropylene segmented copolymer; AS is X 2073, sodium laurylsulfonate, one or more in terminal olefin sodium sulfonate, succinate sodium 2-ethylhexyl, Fatty Alcohol(C12-C14 and C12-C18) (10) T 46155, the polyoxyethylenated alcohol sodium sulfate; Cats product is one or more in tetradecyl dimethyl benzyl ammonium chloride, DTAC, guar hydroxypropyl trimonium chloride, bromination dodecyl trimethyl ammonium, the bromination dodecyl dimethyl hexadecyldimethyl benzyl ammonium.
A kind of preparation method who suppresses the silicon wafer finishing polish combination liquid of particle deposition of the present invention may further comprise the steps:
Take by weighing colloid silica and water-soluble polymers in above-mentioned ratio, by the physical blending mode both are mixed, and at the uniform velocity stir with whisking appliance, preparing degree is colloid silica/water-soluble polymers Compostie abrasive particles of 2～13wt%;
Colloid silica/water-soluble polymers Compostie abrasive particles is scattered in the deionized water, and fully stirs with whisking appliance;
Adding weight percent content is the hydroxyl of 0.002～0.5wt% and/or the surface protectant of amido, in whisking appliance, makes itself and Compostie abrasive particles thorough mixing;
Adding tensio-active agent and the weight percent content that weight percent content is 0.002～0.5wt% successively is the basic cpd of 0.5～4wt%, and liquid pH regulator to 8～12 are made up in finishing polish;
Using the aperture is that the following filter core of 0.5 μ m filters finishing polish combination liquid, removes the large granular impurity in the finishing polish combination liquid.
According to silicon wafer surface roughness after polishing and surface deposition situation, can finishing polish combination liquid of the present invention dilution be used the back more than 10,20,30,40 even 40 times.
Test example
Polishing after configuration combination liquid is used for polishing experiments, and the polishing experiments parameter is following:
Polishing machine: the CP-4 type chemically machinery polished experimental machine that U.S. CE TR-BRUKER company produces, be furnished with 1 rubbing head, can throw 1 silicon wafer;
Polish pressure: 0.4PSI;
Polishing rotary speed: 40 commentaries on classics/min;
Polished silicon single-chip specification: P type < 100 >, diameter 100mm, resistivity: 0.1～100 Ω cm;
Polishing time: 30min;
Polishing pad: Politex type polyurethane foamed solidification polishing pad;
Polishing fluid flow: 80ml/min;
Polish temperature: 25 ° of C
The silicon wafer surface quality examination of polishing back:
Use AFM (AFM) to detect the surfaceness of polishing back silicon wafer.The AFM that experiment is adopted is that U.S. Brooker company produces, and model is DIMENSION ICON., the probe radius is 10nm, and its vertical resolution is 0.01nm, and sweep rate is 1.5Hz, sweep limit 10 * 10 μ m
2Adhere to the influence of impurity for what avoid that silicon wafer surface exists, before experiment, silicon wafer is carried out ultrasonic cleaning respectively in acetone, absolute ethyl alcohol, deionized water experimental result.
According to the AFM detection case polished section surface particles deposition conditions is divided into ☆ (the surface particles size is in the 100nm), zero (the surface particles size is in the 250nm), ◎ (the surface particles size is in 450nm), ◎ ◎ (the surface particles size is not controlled), visible by the foregoing description; Each component concentration is in the best polishing combination liquid under polishing technological conditions according to the invention: contain colloid silica/water-soluble polymers Compostie abrasive particles 5.1005wt% and (wherein contain colloid silica 5wt%; Contain water-soluble polymers guar gum 0.005wt%, Natvosol 0.1wt%); Contain surface protectant triethylamine 0.04wt%; Contain tensio-active agent AEO 0.004wt%; Contain basic cpd ammoniacal liquor 1.0wt%; Silicon wafer surface roughness after the polishing of polishing combination liquid is low to moderate 0.05nm, and the surface does not have particle residue basically.
The foregoing description proves absolutely that the CMP that polishing combination liquid of the present invention is a kind of excellent property uses polishing material, is suitable for the silicon wafer finishing polish.
The above only is a preferred implementation of the present invention; Should be noted that those skilled in the art for the present technique field; Under the prerequisite that does not break away from know-why of the present invention, can also make corresponding adjustment and improvement, these adjustment and improvement also should be regarded as protection scope of the present invention.
The roughness and the surface particles deposition conditions of the silicon wafer surface after following table is polished for the component of polishing combination liquid among each embodiment and content and by it.
Claims (10)
1. liquid is made up in the silicon wafer finishing polish that can suppress particle deposition; It is characterized in that this finishing polish combination liquid comprises surface protectant, basic cpd, tensio-active agent and the deionized water of colloid silica/water-soluble polymers Compostie abrasive particles, hydroxyl and/or amido; The pH value of this finishing polish combination liquid is 8～12.
2. finishing polish combination liquid according to claim 1 is characterized in that, the set of dispense ratio of this finishing polish combination liquid is:
Described colloid silica/both ratios of water-soluble polymers Compostie abrasive particles are 12～400: 1.
3. finishing polish combination liquid according to claim 1 and 2, it is characterized in that: the median size of described silicon-dioxide is 18～80nm.
4. finishing polish according to claim 1 and 2 combination liquid is characterized in that: the water-soluble polymers of described colloid silica/water-soluble polymers Compostie abrasive particles is one or more in the hydroxypropylcellulose of Natvosol or lipid modification of guar gum, XG 550, sodium-alginate, CMS, FM, CMC 99.5, sulfonic acid TKK 021, Tylose CH 50, methylcellulose gum, carboxyethyl methylphosphinate Mierocrystalline cellulose, Vltra tears, hydroxy butyl methyl cellulose, Natvosol, lipid modification.
5. finishing polish combination liquid according to claim 1 and 2; It is characterized in that: the surface protectant of described said hydroxyl and/or amido is one or more in Z 150PH, Z 150PH and polystyrene block copolymer, polyoxyethylene glycol, polyoxyethylene, polyoxyethylene and ethylene oxide-propylene oxide block copolymer, ROHM, methylamine, dimethyl amine, Trimethylamine, ethylamine, DIETHANOL AMINE, triethylamine, Yi Bingchunan, tetraethyl-amine, diethyl triamine, triethyl tetramine, AEEA, hexamethylene-diamine, NSC 446, Triethylenetetramine (TETA), thanomin, diethylolamine, the trolamine.
6. finishing polish combination liquid according to claim 1 and 2; It is characterized in that: described basic cpd is one or more in Pottasium Hydroxide, sodium hydroxide, volatile salt, bicarbonate of ammonia, saleratus, salt of wormwood, sodium hydrogencarbonate, yellow soda ash, ammoniacal liquor, aminopropanol, TMAH, tetraethyl ammonium hydroxide, TPAOH, TBAH, trimethyl hydroxyethylammoniumhydroxide hydroxide, dimethyl-dihydroxy ethyl volatile caustic, Piperazine anhydrous or the Uricida.
7. finishing polish combination liquid according to claim 1 and 2, it is characterized in that: described tensio-active agent is one or more in nonionogenic tenside, AS or the cats product.
8. finishing polish combination liquid according to claim 8, it is characterized in that: described nonionogenic tenside is one or more in YSR 3286, T 46155 (9) lauryl alcohol, AEO, polyoxyethylene nonylphenol, polyoxyethylene octylphenol ether, the polyoxyethylene polyoxypropylene segmented copolymer; AS is X 2073, sodium laurylsulfonate, one or more in terminal olefin sodium sulfonate, succinate sodium 2-ethylhexyl, Fatty Alcohol(C12-C14 and C12-C18) (10) T 46155, the polyoxyethylenated alcohol sodium sulfate; Cats product is one or more in tetradecyl dimethyl benzyl ammonium chloride, DTAC, guar hydroxypropyl trimonium chloride, bromination dodecyl trimethyl ammonium, the bromination dodecyl dimethyl hexadecyldimethyl benzyl ammonium.
9. according to the described combination liquid of claim 1-2; It is characterized in that: described colloid silica/water-soluble polymers Compostie abrasive particles 5.1005wt%; Wherein, colloid silica 5wt%, water-soluble polymers are guar gum 0.005wt% and Natvosol 0.1wt%; Surface protectant is triethylamine 0.04wt%, and tensio-active agent is AEO 0.004wt%, and alkalify is combined into thing ammoniacal liquor 1.0wt%, deionized water surplus.
10. the preparation method of the silicon wafer finishing polish combination liquid that can suppress particle deposition is characterized in that this method may further comprise the steps:
Take by weighing colloid silica and water-soluble polymers in proportion, by the physical blending mode both are mixed, and at the uniform velocity stir, prepare colloid silica/water-soluble polymers Compostie abrasive particles with whisking appliance;
Colloid silica/water-soluble polymers Compostie abrasive particles is scattered in the deionized water, and fully stirs with whisking appliance;
The surface protectant that adds hydroxyl and/or amido makes itself and Compostie abrasive particles thorough mixing in whisking appliance;
Add tensio-active agent and basic cpd successively, and liquid pH regulator to 8～12 are made up in finishing polish;
Using the aperture is that the following filter core of 0.5 μ m filters finishing polish combination liquid, removes the large granular impurity in the finishing polish combination liquid.
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