CN102775915B - 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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- CN102775915B CN102775915B CN201210209794.3A CN201210209794A CN102775915B CN 102775915 B CN102775915 B CN 102775915B CN 201210209794 A CN201210209794 A CN 201210209794A CN 102775915 B CN102775915 B CN 102775915B
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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, and constantly the reducing of characteristic dimension, the working accuracy to silicon wafer and the requirement of surface quality are more and more higher.At present, utilize chemically machinery polished (CMP) technology to carry out planarization to silicon wafer surface, become ic manufacturing technology and entered deep-submicron one of requisite processing step of Age of Technology later, a collection of Patents technology is disclosed both at home and abroad in succession, as EP0371147B1, US5352277, CN101671528A, CN102061131A.
Traditional CMP system is comprised 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 certain pressure on the polishing pad rotating with worktable, 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, by chemistry and mechanical acting in conjunction, from silicon wafer surface, remove layer of material as thin as a wafer, finally realize ultra-precision surface processing.
Conventionally, in industry in order to realize the polishing precision 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 to step chemical mechanical polishing, the polishing fluid that every step polishing is used and corresponding polishing technological conditions are all different, and it is also different that corresponding silicon wafer respectively walks the working accuracy that will reach.In rough polishing step, the surface damage layer of removing silicon wafer cutting and being shaped under residual, is processed into minute surface, finally by silicon wafer is carried out to finishing polish, thereby reduces to the full extent surfaceness and other free tiny flaws.
In actual production, the final finishing polish of silicon wafer is the decisive step of surface quality, easily produces the defects such as polishing mist and cut, and produce the deposition that one of reason of these defects is exactly particle in finishing polish process.The deposition of particle causes the generation of polishing mist and cut, causes the integrity of graphic defects, epitaxy defect, impact wiring, is the biggest obstacle of high rate of finished products, particularly when silicon wafer bonding, introduce microgap, also cause dislocation, affect bond strength and surface quality simultaneously.Therefore, effectively controlling particle deposition is one of important indicator of check silicon wafer precise polishing solution.At present; submicron and the nano particle that by good cleaning, major part can be remained in to silicon wafer surface are removed, but still have some " stubbornness " particles that form in polishing process (being generally the particle or the cluster of grains that are less than 500nm) to remove by cleaning thoroughly.Therefore, if just particle residue is controlled, then pass through follow-up cleaning process in polishing process, the particle that is deposited on silicon wafer surface is just hopeful thorough removal.Silicon wafer finishing polish combination liquid of the present invention can be controlled at the size of deposited particles in 100nm, and to realize surface quality high simultaneously, and surfaceness is low.
Summary of the invention
The present invention has overcome a difficult problem for silicon wafer precise polishing solution particle deposition in polishing process in prior art, has proposed a kind of polished silicon wafer surface precision high, 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 deposition of particle, have improved precision and the quality of silicon wafer surface after polishing.
Liquid is combined 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 component proportion 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 Natvosol of guar gum, xanthan gum, sodium alginate, carboxymethyl starch, cellulose acetate, carboxymethyl cellulose, sulfonic acid ethyl cellulose, carboxymethyl hydroxyethyl cellulose, methylcellulose gum, carboxyethyl methylphosphinate Mierocrystalline cellulose, Vltra tears, hydroxy butyl methyl cellulose, Natvosol, lipid modification or the hydroxypropylcellulose of lipid modification.
Described described hydroxyl and/or the surface protectant of amido are, polyvinyl alcohol, polyvinyl alcohol and polystyrene block copolymer, polyoxyethylene glycol, polyoxyethylene, polyoxyethylene and ethylene oxide-propylene oxide block copolymer, polyacrylic acid, methylamine, dimethyl amine, Trimethylamine, ethylamine, diethylamide, triethylamine, α-amino isopropyl alcohol, tetraethyl-amine, diethyl triamine, trientine, hydroxyethylethylene diamine, hexamethylene-diamine, diethylenetriamine, Triethylenetetramine (TETA), thanomin, diethanolamine, one or more in trolamine.
Described basic cpd is, one or more in potassium hydroxide, sodium hydroxide, volatile salt, bicarbonate of ammonia, saleratus, salt of wormwood, sodium bicarbonate, sodium carbonate, ammoniacal liquor, aminopropanol, Tetramethylammonium hydroxide, tetraethyl ammonium hydroxide, TPAOH, TBAH, trimethyl hydroxyethylammoniumhydroxide hydroxide, dimethyl dihydroxy ethyl ammonium hydroxide, Piperazine anhydrous or Uricida.
Described tensio-active agent is one or more in nonionogenic tenside, anion surfactant or cats product.
Described nonionogenic tenside is one or more in polydimethylsiloxane, polyoxyethylene (9) lauryl alcohol, fatty alcohol-polyoxyethylene ether, polyoxyethylene nonylphenol ether, polyoxyethylene octylphenol ether, polyoxyethylene polyoxypropylene segmented copolymer; Anion surfactant is Sodium dodecylbenzene sulfonate, sodium laurylsulfonate, one or more in alpha-olefin sodium sulfonate, succinate sodium 2-ethylhexyl, fatty alcohol (10) polyoxyethylene, polyoxyethylenated alcohol sodium sulfate; Cats product is one or more in tetradecyl dimethyl benzyl ammonium chloride, Dodecyl trimethyl ammonium chloride, guar hydroxypropyl trimonium chloride, bromination dodecyl trimethyl ammonium, bromination dodecyl dimethyl hexadecyldimethyl benzyl ammonium.
Described colloid silica/water-soluble polymers Compostie abrasive particles 5.1005wt%, wherein, colloid silica 5wt%, water-soluble polymers is guar gum 0.005wt% and Natvosol 0.1wt%; Surface protectant is triethylamine 0.04wt%, and tensio-active agent is fatty alcohol-polyoxyethylene ether 0.004wt%, and alkalify is combined into thing ammoniacal liquor 1.0wt%, and surplus is deionized water.
A preparation method who suppresses the silicon wafer finishing polish combination liquid of particle deposition, is characterized in that, the method comprises the following steps:
Take in proportion colloid silica and water-soluble polymers, by physical blending mode, both are mixed, and at the uniform velocity stir with agitator, prepare colloid silica/water-soluble polymers Compostie abrasive particles;
Colloid silica/water-soluble polymers Compostie abrasive particles is scattered in deionized water, and fully stirs with agitator;
Add the surface protectant of hydroxyl and/or amido, in agitator, make it fully mix with Compostie abrasive particles;
Add successively tensio-active agent and basic cpd, and finishing polish is combined to liquid pH regulator to 8~12;
With aperture, be that filter core below 0.5 μ m filters finishing polish combination liquid, remove the large granular impurity in finishing polish combination liquid.
The present invention compared with prior art has the following advantages:
1) colloid silica/water-soluble polymers Compostie abrasive particles in finishing polish combination liquid of the present invention, make water-soluble polymers be wrapped in uniformly the surface of titanium dioxide colloid silica, improved the sticking power of titanium dioxide colloid silica, form the inorganic nucleocapsid structure of a kind of organic-capping, effectively suppress particle deposition, reduce residual in silicon wafer surface and polishing pad;
2) finishing polish combination liquid of the present invention is by adding the surface protectant of hydroxyl and/or amido, reduced the firmness of silicon wafer surface particle deposition, the easier polished liquid of particle that remains in silicon wafer surface is taken away, be conducive to the cleaning of silicon wafer and polishing pad after polishing;
3) liquid is raw materials used is easy to get in finishing polish of the present invention combination, pollution-free, meets environmental requirement and easily carries out large-scale industrial production.
Accompanying drawing explanation
Fig. 1 is used general silica colloidal sol in prior art, do not add the surface protectant of water-soluble polymers and hydroxyl and/or amido, the atomic force microscope of silicon wafer (AFM) photo (comparative example 5) after finishing polish.
Fig. 2 has adopted colloid silica/water-soluble polymers Compostie abrasive particles in finishing polish of the present invention combination liquid, has added the surface protectant of hydroxyl and/or amido, but each components do match AFM photo (embodiment 2) of silicon wafer after finishing polish when poor.
Fig. 3 has adopted colloid silica/water-soluble polymers Compostie abrasive particles in finishing polish of the present invention combination liquid, has added the surface protectant of hydroxyl and/or amido, and each components do match AFM photo (embodiment 6) of silicon wafer after finishing polish when better.
Embodiment
Below by specific embodiment, the invention will be further elaborated, certainly in no case should be construed as limiting the scope of the invention.
Liquid is combined 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%; the weight percent content of tensio-active agent is 0.002~0.5wt%, and surplus is deionized water.Colloid silica/water-soluble polymers Compostie abrasive particles is, 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 Natvosol of guar gum, xanthan gum, sodium alginate, carboxymethyl starch, cellulose acetate, carboxymethyl cellulose, sulfonic acid ethyl cellulose, carboxymethyl hydroxyethyl cellulose, methylcellulose gum, carboxyethyl methylphosphinate Mierocrystalline cellulose, Vltra tears, hydroxy butyl methyl cellulose, Natvosol, lipid modification or the hydroxypropylcellulose of lipid modification.
Described hydroxyl and/or the surface protectant of amido be, one or more in polyvinyl alcohol, polyvinyl alcohol and polystyrene block copolymer, polyoxyethylene glycol, polyoxyethylene, polyoxyethylene and ethylene oxide-propylene oxide block copolymer, polyacrylic acid, methylamine, dimethyl amine, Trimethylamine, ethylamine, diethylamide, triethylamine, α-amino isopropyl alcohol, tetraethyl-amine, diethyl triamine, trientine, hydroxyethylethylene diamine, hexamethylene-diamine, diethylenetriamine, Triethylenetetramine (TETA), thanomin, diethanolamine, trolamine.
Described basic cpd is, one or more in potassium hydroxide, sodium hydroxide, volatile salt, bicarbonate of ammonia, saleratus, salt of wormwood, sodium bicarbonate, sodium carbonate, ammoniacal liquor, aminopropanol, Tetramethylammonium hydroxide, tetraethyl ammonium hydroxide, TPAOH, TBAH, trimethyl hydroxyethylammoniumhydroxide hydroxide, dimethyl dihydroxy ethyl ammonium hydroxide, Piperazine anhydrous or Uricida.Basic cpd plays the effect of corrosion to silicon wafer surface, can, by regulating the contamination of basic cpd to regulate finishing polish to remove speed, the final pH of polishing fluid be controlled to 8~12.
Described tensio-active agent is one or more in nonionogenic tenside, anion surfactant or cats product.
Wherein, nonionogenic tenside is one or more in polydimethylsiloxane, polyoxyethylene (9) lauryl alcohol, fatty alcohol-polyoxyethylene ether, polyoxyethylene nonylphenol ether, polyoxyethylene octylphenol ether, polyoxyethylene polyoxypropylene segmented copolymer; Anion surfactant is Sodium dodecylbenzene sulfonate, sodium laurylsulfonate, one or more in alpha-olefin sodium sulfonate, succinate sodium 2-ethylhexyl, fatty alcohol (10) polyoxyethylene, polyoxyethylenated alcohol sodium sulfate; Cats product is one or more in tetradecyl dimethyl benzyl ammonium chloride, Dodecyl trimethyl ammonium chloride, guar hydroxypropyl trimonium chloride, bromination dodecyl trimethyl ammonium, bromination dodecyl dimethyl hexadecyldimethyl benzyl ammonium.
The preparation method of a kind of silicon wafer finishing polish combination liquid that suppresses particle deposition of the present invention, comprises the following steps:
In above-mentioned ratio, take colloid silica and water-soluble polymers, by physical blending mode, both are mixed, and at the uniform velocity stir with agitator, 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 deionized water, and fully stirs with agitator;
Adding weight percent content is the hydroxyl of 0.002~0.5wt% and/or the surface protectant of amido, makes it fully mix with Compostie abrasive particles in agitator;
Adding successively weight percent content is the tensio-active agent of 0.002~0.5wt% and the basic cpd that weight percent content is 0.5~4wt%, and finishing polish is combined to liquid pH regulator to 8~12;
With aperture, be that filter core below 0.5 μ m filters finishing polish combination liquid, remove the large granular impurity in finishing polish combination liquid.
According to silicon wafer surface roughness and the surface deposition situation of carrying out after polishing, can be by even 40 times of above rear uses of finishing polish combination liquid of the present invention dilution 10,20,30,40.
Experimental example
By the polishing combination liquid after configuration, for polishing experiments, polishing experiments parameter is as follows:
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 turn/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
Silicon wafer surface quality examination after polishing:
The surfaceness of silicon wafer after use atomic force microscope (AFM) detection polishing.The AFM that experiment adopts is that U.S. Brooker company produces, and model is DIMENSION ICON., probe radius is 10nm, and its vertical resolution is 0.01nm, and sweep rate is 1.5Hz, sweep limit 10 × 10 μ m
2.For what avoid that silicon wafer surface exists, adhere to the impact of impurity on experimental result, before experiment, silicon wafer is carried out respectively to ultrasonic cleaning in acetone, dehydrated alcohol, deionized water.
According to AFM detection case, polished section surface particles deposition conditions is divided into ☆ (surface particles size is in 100nm), zero (surface particles size is in 250nm), ◎ (surface particles size is in 450nm), ◎ ◎ (surface particles size is not controlled), as seen from the above-described embodiment, in best polishing combination liquid under polishing technological conditions of the present invention, each component concentration is: containing colloid silica/water-soluble polymers Compostie abrasive particles 5.1005wt%(, wherein contain colloid silica 5wt%, containing water-soluble polymer guar 0.005wt%, Natvosol 0.1wt%), containing surface protectant triethylamine 0.04wt%, containing tensio-active agent fatty alcohol-polyoxyethylene ether 0.004wt%, containing basic cpd ammoniacal liquor 1.0wt%, silicon wafer surface roughness after the polishing of polishing combination liquid is low to moderate 0.05nm, surface is substantially without particle residue.
Above-described embodiment absolutely proves that polishing combination liquid of the present invention is a kind of CMP polishing material of excellent property, is suitable for silicon wafer finishing polish.
The above is only the preferred embodiment of the present invention; it should be noted that the those skilled in the art for the art; not departing under the prerequisite of the technology of the present invention principle, can also make corresponding adjustment and improvement, these adjustment and improvement also should be considered as protection scope of the present invention.
Following table is the component of polishing combination liquid in each embodiment and content and carries out roughness and the surface particles deposition conditions of the silicon wafer surface after polishing by it.
Claims (3)
1. one kind can be suppressed the silicon wafer finishing polish combination liquid of 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, and the pH value of this finishing polish combination liquid is 8~12; Described colloid silica/water-soluble polymers Compostie abrasive particles 5.105wt%, wherein, colloid silica 5wt%, water-soluble polymers is guar gum 0.005wt% and Natvosol 0.1wt%; Surface protectant is triethylamine 0.04wt%, and tensio-active agent is fatty alcohol-polyoxyethylene ether 0.004wt%, and alkalify is combined into thing ammoniacal liquor 1.0wt%, deionized water surplus.
2. combination liquid according to claim 1, is characterized in that, the median size of described silicon-dioxide is 18~80nm.
3. the preparation method that can suppress the silicon wafer finishing polish combination liquid of particle deposition, is characterized in that, the method comprises the following steps:
Take in proportion colloid silica and water-soluble polymers, by physical blending mode, both are mixed, and at the uniform velocity stir with agitator, prepare colloid silica/water-soluble polymers Compostie abrasive particles;
Colloid silica/water-soluble polymers Compostie abrasive particles is scattered in deionized water, and fully stirs with agitator;
Add the surface protectant of hydroxyl and/or amido, in agitator, make it fully mix with Compostie abrasive particles;
Add successively tensio-active agent and basic cpd, and finishing polish is combined to liquid pH regulator to 8~12;
With aperture, be that filter core below 0.5 μ m filters finishing polish combination liquid, remove the large granular impurity in finishing polish combination liquid.
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US7037351B2 (en) * | 2003-07-09 | 2006-05-02 | Dynea Chemicals Oy | Non-polymeric organic particles for chemical mechanical planarization |
JP2007300070A (en) * | 2006-04-05 | 2007-11-15 | Nippon Chem Ind Co Ltd | Etchant composition for polishing semiconductor wafer, manufacturing method of polishing composition using same, and polishing method |
CN102061131B (en) * | 2010-11-22 | 2013-06-19 | 上海新安纳电子科技有限公司 | Polishing liquid for reducing microscratch of surfaces of silicon wafers and preparation and use method thereof |
CN102093819B (en) * | 2011-01-06 | 2013-05-22 | 清华大学 | Polishing composition for fine polishing of silicon wafer |
CN102516873B (en) * | 2011-10-24 | 2014-06-04 | 清华大学 | Silicon wafer polishing composition and preparation method thereof |
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