CN104559797A - Silicon wafer fine polishing combination and preparation method thereof - Google Patents
Silicon wafer fine polishing combination and preparation method thereof Download PDFInfo
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- CN104559797A CN104559797A CN201410811996.4A CN201410811996A CN104559797A CN 104559797 A CN104559797 A CN 104559797A CN 201410811996 A CN201410811996 A CN 201410811996A CN 104559797 A CN104559797 A CN 104559797A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
Abstract
The invention relates to a silicon wafer fine polishing combination and a preparation method thereof and belongs to the technical field of chemical-mechanical polishing (CMP). The combination comprises an acidic silica sol, a diol compound, a thiourea compound, an alkaline compound, salt, a surfactant and deionized water. According to the silicon wafer fine polishing combination provided by the invention, while the surface defect after rough polishing can be overcome, the stress generated in the rough polishing process is reduced, and the surface precision is improved; meanwhile, the polishing rate is close to that of silicon wafer rough polishing liquid.
Description
Technical field
The invention belongs to chemically machinery polished (CMP) technical field, particularly a kind of silicon wafer fine polishing composition.
Background technology
Semiconductor materials based on silicon materials has been the most important basic function material of electronics and information industry, occupies very consequence in national economy and war industry.Have more than 95% to be make with silicon materials in global semiconducter device, wherein the unicircuit of 85% is also fabricated from a silicon.At present, IC technology has entered the nanoelectronic epoch that live width is less than 0.1 μm, and require more and more high to the suface processing quality of silicon single-crystal polishing plate, traditional polishing fluid can not meet polishing silicon single crystal sheet requirement.In order to ensure silicon polished angularity, the surface working accuracy that locally planeness, surfaceness etc. are higher, the polishing fluid and glossing that make new advances must be developed.Obtaining the higher silicon wafer of surface processing accuracy is the important step manufacturing unicircuit, is directly connected to the qualification rate of unicircuit.
Simple chemical rightenning, polishing speed is comparatively slow, surface accuracy is higher, it is low to damage, integrity good, but it can not revise surperficial surface precision, and polishing consistence is also poor; Simple mechanical polishing consistence is good, and surface finish is high, and polishing speed is higher, but damage layer depth, surface accuracy is lower; Chemically machinery polished both can obtain comparatively perfectly surface, and can obtain higher polishing speed again, be the unique method that can realize global planarizartion.Traditional CMP system is made up of following three parts: the silicon chip clamping device of rotation, worktable, polishing fluid (slurry) supply system of carrying polishing pad.During polishing, the workpiece rotated imposes on the polishing pad that rotates with worktable with certain pressure, polishing fluid flows between workpiece and polishing pad, and produces chemical reaction at workpiece surface, and the chemical reactant that workpiece surface is formed is removed by the mechanical friction effect of abrasive material.In the alternation procedure of chemical membrane and mechanical striping, remove very thin layer of material by chemistry and the acting in conjunction of machinery from workpiece surface, finally realize ultra-precision surface processing.Therefore, high-level efficiency, high-quality polishing be realized, chemical action process and good the mating of mechanical effect process implementation must be made.
At present, silicon wafer diameter develops into more than 200mm, higher to the requirement of silicon wafer surface quality, in order to ensure the polishing precision of silicon wafer, reach the technical indicator of integrated circuits silicon wafers requirement, need to carry out three step chemically machinery polisheds (CMP) (rough polishing, fine polishing, finishing polish) to silicon chip.
Because the polishing accuracy requirement of each step of polishing is different, also different to the requirement of polishing fluid, then need development three kinds of polishing fluids to carry out polishing targetedly to its each step, to meet each step polishing requirement, (difference has: the chemical composition of polishing fluid, polishing wear particle size and distribution, polishing wear particle concentration and polishing fluid pH value etc.; The material of polishing cloth, porosity, hole size, surface groove structures and hardness etc.; Polish pressure, temperature, rotating speed, polishing fluid flow etc.), it is also different that corresponding silicon chip respectively walks the working accuracy that will reach: first carry out rough polishing to silicon chip, object removes the surperficial affected layer stayed by front road manufacturing procedure, and meet the requirements of geometrical dimension working accuracy, general requirement polishing speed reaches more than 1 micron, and roughness is at about 1nm; Then carry out fine polishing, guarantee that silicon chip surface is eliminated and remove at a high speed due to rough polishing the stress caused and to go forward side by side a step-down low surface roughness, speed is at 0.5 microns, and roughness is at about 0.7nm; Finally carry out " mist elimination " finishing polish, guarantee that silicon chip surface has high surface nanotopology characteristic.
Similar with other silicon wafer polishing liquids, silicon wafer fine polishing liquid forms primarily of three parts: abrasive material, chemical constitution and water; In order to realize removing in silicon wafer fine polishing process the target of the defects such as stress that rough polishing introduces and burn into remain, have employed various ways both at home and abroad attempts, and achieves certain progress.
Abrasive material aspect, the abrasive material as polishing fluid is mostly oxide particle or organic granular, such as silicon-dioxide, aluminum oxide, cerium oxide, granules of polystyrene etc., and wherein silicon-dioxide uses the widest silicon wafer polishing liquid abrasive material at present.Silica particle surface is rich in oh group, has stronger activity, can react under certain condition with some chemical substances.Utilize this character of silicon dioxide granule, the transformation of chemical property can be carried out silica particle surface.
In integrated circuit wiring polishing, patent US6646348 discloses the component of a kind of silane coupling agent as polishing fluid, form oligopolymer after the hydrolysis of this silane coupling agent to mix mutually with the abrasive material in polishing fluid and other chemical reagent, the polishing speed of lower TEOS and Ta can be obtained, and obtain good glazed surface.Patent US6656241 discloses a kind of silica aggregate of dichlorodimethylsilane modification, and be applied to Cu polishing fluid, silica aggregate can be dispersed in polishing fluid well through modification, and the polishing speed of Cu and Ta and Selection radio are subject to the impact of modification.Patent EP0371147B1 discloses the silicon wafer polishing composition of the silane coupler modified silicon sol of a kind of trialkyl, plays the effect of stabilized colloidal silica in polishing process, decreases the scuffing in polishing process; These process are all only centered around stability, the degree of scatter of improving polish abrasive, utilize the abrasive hardness after silylating reagent to obtain appropriateness to reduce, polishing microcell inorganic abradant " firmly impacting " to workpiece surface is replaced " Elastic Contact ", silanization layer serves shock absorption, for improving polishing defect.
More than improve and all certain effect is achieved to defects controlling, but for being applicable to reduce the silicon single crystal fine polishing polishing fluid of stress that silicon wafer surface rough polishing causes and defect, while having lower surfaceness, higher surface accuracy, less corrosion default, the requirement in higher polishing speed also to be had also to there is certain limitation.
Summary of the invention
Instant invention overcomes the problem that silicon wafer surface defect control only focused on by traditional silicon wafer fine polishing polishing fluid in polishing process, disclose a kind of silicon wafer fine polishing composition, while can not only eliminating rough polishing rear surface defect, reduce the stress produced in rough polishing process, improve surface accuracy; Polishing speed is close to the polishing speed of silicon wafer rough polishing solution simultaneously.Different from general silicon wafer fine polishing liquid, polishing composition of the present invention can realize the polishing speed of general silicon wafer rough polishing liquid, and can realize higher polishing precision, polishing precision can reach below 0.3nm, and general rough polishing precision is at 0.6 ~ 0.9nm simultaneously.
A kind of silicon wafer fine polishing composition of the present invention, it is characterized in that, described composition comprises following component and content:
The acid silicon dioxide sol of 10 % by weight to 50 % by weight;
One or more diol compounds of 0.01 % by weight to 1 % by weight;
A kind of thiourea of 0.1 % by weight to 1 % by weight;
One or more basic cpds of 0.5 % by weight to 5 % by weight;
A kind of salt of 0.01 % by weight to 3 % by weight;
A kind of tensio-active agent of 0.001 % by weight to 0.05 % by weight;
Deionized water surplus.
The pH value of described composition is 9 to 12.
Described acid silicon dioxide sol is the acidic silicasol that 10 ~ 100nm, pH are less than 6.
Described diol compound is one or more in ethylene glycol (EG), propylene glycol (PG), butyleneglycol (BG), hexylene glycol (HG), Diethylene Glycol (DEG), triethylene glycol (TEG), polyoxyethylene glycol (PEG), polypropylene glycol (PPG).
Described thiourea is the one in thiocarbamide (TU), methylthiourea (MTU), dimethyl thiourea (DMTU), tetramethyl thiourea (TMTU), ethyl thiourea (ETU), diethyl thiourea (DETU), n-propyl thiocarbamide (PTU), di-isopropyl thiourea (DPTU), thiosinamine (ATU), phenylthiourea (PHTU), tolylthiourea (TTU) and chloro-phenyl-thiocarbamide (CPTU).
Described basic cpd is potassium hydroxide (KOH), sodium hydroxide (NaOH), Tetramethylammonium hydroxide (TMAH), ammonia (NH3), methylamine (MA), dimethyl amine (DMA), Trimethylamine (TMA), ethylamine (EA), diethylamide (DEA), triethylamine (TEA), α-amino isopropyl alcohol (MIPA), aminopropanol (AP), tetraethyl-amine (TEAH), thanomin (MEA), diethyl triamine (DTA), trientine (TTA), hydroxyethylethylene diamine (AEEA), hexamethylene-diamine (HDA), diethylenetriamine (DETA), Triethylenetetramine (TETA) (TETA), Piperazine anhydrous (PIZ), one or more in Uricida (PHA).
Described salt is precipitation membranous type inhibiter, is carbonic acid, phosphoric acid, is specially the ammonium of carbonic acid and acid thereof, potassium, sodium salt; One in the ammonium of phosphoric acid and acid thereof, potassium, sodium salt.
Described tensio-active agent is the one in nonionogenic tenside, anion surfactant or cats product.
Described nonionogenic tenside is polydimethylsiloxane (PDMS), fatty alcohol-polyoxyethylene ether (AEO), polyoxyethylene polyoxypropylene segmented copolymer (EO-PO); Anion surfactant is Sodium dodecylbenzene sulfonate (SDBS), sodium laurylsulfonate (K-12), alpha-olefin sodium sulfonate (AOS), succinate sodium 2-ethylhexyl (AOT), polyoxyethylenated alcohol sodium sulfate (AES); Cats product is the one in myristyl benzyl dimethyl ammonium chloride, Dodecyl trimethyl ammonium chloride (TDBAC), guar hydroxypropyl trimonium chloride (C-162), bromination dodecyl trimethyl ammonium (DTAB), bromination dodecyl dimethyl hexadecyldimethyl benzyl ammonium (DDBA).
The preparation method of a kind of silicon wafer fine polishing composition of the present invention, it is characterized in that, the method comprises the following steps:
1) take each component in described ratio, with agitator, acid silicon dioxide sol is scattered in deionized water;
2) thiourea is added again after under agitation, adding diol compound;
3) add tensio-active agent again, and add the mixture of basic cpd and salt, and polishing composition pH value is adjusted to 9 ~ 12;
4) with the filter core that aperture is 0.5 μm, polishing composition is filtered, to remove the large granular impurity in polishing composition, namely obtain finished product.Each component of the present invention forms the chemistry that effectively improves in polishing process and mechanical effect, improve polishing after also maintain high removal speed while the precision of silicon wafer and surface quality.In the present invention, acidic silicasol pH used specifically controls at 3-5, and with diol compound process acidic silicasol, improves polishing particles density of surface hydroxyl, promotes granule surface activity; The thiourea then added will act on the high polishing particles surface of surfactivity, and silicon chip surface while improving the mechanical effect of polishing particles and after protecting polishing, eliminates the stress produced in rough polishing process.
Basic cpd in forming with polishing fluid matches, basic cpd etching silicon layer, forms soft layer, and the particle of surface containing thiourea can form adsorption film on soft layer, plays the effect of protection silicon chip surface; Recycling precipitation membranous type inhibiter, to the further increase provide protection of silicon chip surface, can be avoided the corrosion that the damage because particle effects on surface causes and chemical action cause, and keep higher removal speed.
In addition, for improving the surface accuracy of silicon wafer after polishing further, also in polishing fluid composition, adding appropriate tensio-active agent in the present invention, improving the wetting ability on polishing fluid surface further, make the silicon wafer surface quality after polishing better.
Accompanying drawing explanation
Fig. 1 is the atomic force microscope figure of silicon chip after the employing embodiment of the present invention 2 polishing composition.
Fig. 2 is the atomic force microscope figure of the silicon chip after adopting the embodiment of the present invention 6 polishing composition.
Fig. 3 is the atomic force microscope figure of the silicon chip after adopting comparative example 2 polishing composition.
Fig. 4 is the atomic force microscope figure of the silicon chip after adopting comparative example 3 polishing composition.
Embodiment
Below by embodiment and comparative example, the invention will be further elaborated, certainly in no case should be construed as limiting the scope of the invention, and as without special mark, each component addition is all mass percent.
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; under the prerequisite not departing from the technology of the present invention principle, can also make corresponding adjustment and improve, these adjustment and improvement also should be considered as protection scope of the present invention.
Polishing composition after configuration is used for polishing experiments, and polishing experiments parameter is as follows:
Polishing machine: single side polishing machine, is furnished with 4 rubbing heads, and each rubbing head can throw 4 silicon chips;
Polish pressure: 32kPa;
Polishing rotary speed: 90 turns/min;
Rubbing head rotating speed: 100 turns/min;
Polished silicon single-chip specification: P type <100>, diameter 100mm, resistivity: 0.1 ~ 100. Ω cm;
Polishing time: 20min;
Polishing pad: polyurethane foam solidification polishing pad, Rodel company SUB 600 type polishing pad;
Polishing fluid flow: 230ml/min;
Polish temperature: 20 DEG C
Silicon chip surface quality examination after polishing:
Silicon wafer, on the impact of detected result, is carried out ultrasonic cleaning by attachment impurity before detection respectively that exist for avoiding silicon wafer surface in acetone, dehydrated alcohol, deionized water.
The surfaceness of silicon wafer after use AFM detection polishing.Testing the AFM adopted is Bruker DIMENSION ICON, and probe radius is 10nm, and its vertical resolution is 0.01nm, and sweep rate is 1.5Hz, sweep limit 50 × 50 μm 2.
High strength is used to converge light source (tengsten lamp), from light source 100mm place converging beam spot diameter 20 ~ 40mm, the defect (road plan) on the whole polished section surface of visualize, is divided into very well (◎ ◎), good (◎), better (zero), poor (☆), poor (☆ ☆) according to detection case by polished section surface imperfection degree.
Polishing mean rate: polish removal rate is obtained by the change calculations of silicon chip center portion thickness before and after polishing, be the mean value of four silicon chip center thickness differences, its available thickness tester records, polishing speed is the ratio of polishing clearance and polishing time, and polishing mean rate is the mean value of polishing speed within the polishing pad time in work-ing life.
As can be seen from the polishing experiments result of table 1 embodiment and comparative example, compared with conventional polishing compositions, the polishing composition in the present invention, while keeping high polishing clearance, silicon wafer surface precision is higher and surface imperfection is less.
As seen from the above-described embodiment, in the best polishing composition under polishing technological conditions of the present invention, each component concentration is: pH is that the acid silicon dioxide sol of 3, median size 30nm is containing 40%; Diol compound PG0.2%; Thiourea TU is containing 0.1%; Basic cpd DETA2%, KOH1%; Saleratus 0.3%, during containing tensio-active agent EO-PO 0.05%, the silicon chip surface roughness after polishing composition polishing is low causes 0.173nm, removes rate 0.89 μm/min.
Above-described embodiment absolutely proves that polishing composition of the present invention is a kind of CMP polishing material of excellent property, is particularly suitable for silicon wafer fine polishing.
The preparation of table 1 embodiment and comparative example and test experiments result
Claims (10)
1. a silicon wafer fine polishing composition, is characterized in that, described composition comprises following component and content:
The acid silicon dioxide sol of 10 % by weight to 50 % by weight;
One or more diol compounds of 0.01 % by weight to 1 % by weight;
A kind of thiourea of 0.1 % by weight to 1 % by weight;
One or more basic cpds of 0.5 % by weight to 5 % by weight;
A kind of salt of 0.01 % by weight to 3 % by weight;
A kind of tensio-active agent of 0.001 % by weight to 0.05 % by weight;
Deionized water surplus.
2. composition according to claim 1, is characterized in that, the pH value of described composition is 9 to 12.
3. composition according to claim 1 and 2, is characterized in that, described acid silicon dioxide sol is the acidic silicasol that 10 ~ 100nm, pH are less than 6.
4. composition according to claim 1 and 2, it is characterized in that, described diol compound is one or more in ethylene glycol (EG), propylene glycol (PG), butyleneglycol (BG), hexylene glycol (HG), Diethylene Glycol (DEG), triethylene glycol (TEG), polyoxyethylene glycol (PEG), polypropylene glycol (PPG).
5. composition according to claim 1 and 2, it is characterized in that, described thiourea is the one in thiocarbamide (TU), methylthiourea (MTU), dimethyl thiourea (DMTU), tetramethyl thiourea (TMTU), ethyl thiourea (ETU), diethyl thiourea (DETU), n-propyl thiocarbamide (PTU), di-isopropyl thiourea (DPTU), thiosinamine (ATU), phenylthiourea (PHTU), tolylthiourea (TTU) and chloro-phenyl-thiocarbamide (CPTU).
6. composition according to claim 1 and 2, it is characterized in that, described basic cpd is potassium hydroxide (KOH), sodium hydroxide (NaOH), Tetramethylammonium hydroxide (TMAH), ammonia (NH3), methylamine (MA), dimethyl amine (DMA), Trimethylamine (TMA), ethylamine (EA), diethylamide (DEA), triethylamine (TEA), α-amino isopropyl alcohol (MIPA), aminopropanol (AP), tetraethyl-amine (TEAH), thanomin (MEA), diethyl triamine (DTA), trientine (TTA), hydroxyethylethylene diamine (AEEA), hexamethylene-diamine (HDA), diethylenetriamine (DETA), Triethylenetetramine (TETA) (TETA), Piperazine anhydrous (PIZ), one or more in Uricida (PHA).
7. composition according to claim 1 and 2, is characterized in that, described salt is precipitation membranous type inhibiter, is carbonic acid, phosphoric acid, is specially the ammonium of carbonic acid and acid thereof, potassium, sodium salt; One in the ammonium of phosphoric acid and acid thereof, potassium, sodium salt.
8. composition according to claim 1 and 2, is characterized in that, described tensio-active agent is the one in nonionogenic tenside, anion surfactant or cats product.
9. composition according to claim 8, it is characterized in that, described nonionogenic tenside is polydimethylsiloxane (PDMS), fatty alcohol-polyoxyethylene ether (AEO), polyoxyethylene polyoxypropylene segmented copolymer (EO-PO); Anion surfactant is Sodium dodecylbenzene sulfonate (SDBS), sodium laurylsulfonate (K-12), alpha-olefin sodium sulfonate (AOS), succinate sodium 2-ethylhexyl (AOT), polyoxyethylenated alcohol sodium sulfate (AES); Cats product is the one in myristyl benzyl dimethyl ammonium chloride, Dodecyl trimethyl ammonium chloride (TDBAC), guar hydroxypropyl trimonium chloride (C-162), bromination dodecyl trimethyl ammonium (DTAB), bromination dodecyl dimethyl hexadecyldimethyl benzyl ammonium (DDBA).
10. the preparation method of composition according to any one of claim 1-9, it is characterized in that, the method comprises the following steps:
1) take each component in described ratio, with agitator, acid silicon dioxide sol is scattered in deionized water;
2) thiourea is added again after under agitation, adding diol compound;
3) add tensio-active agent again, and add the mixture of basic cpd and salt, and polishing composition pH value is adjusted to 9 ~ 12;
4) with the filter core that aperture is 0.5 μm, polishing composition is filtered, to remove the large granular impurity in polishing composition, namely obtain finished product.
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| CN201410811996.4A CN104559797B (en) | 2014-12-22 | 2014-12-22 | Silicon wafer fine polishing combination and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105710760A (en) * | 2016-04-22 | 2016-06-29 | 衡阳市宏达威环保科技有限公司 | Aluminium alloy alkaline grinding fluid |
| WO2018120808A1 (en) * | 2016-12-28 | 2018-07-05 | 安集微电子科技（上海）股份有限公司 | Chem-mechanical polishing liquid for barrier layer |
| CN109554119A (en) * | 2018-11-02 | 2019-04-02 | 山东天岳先进材料科技有限公司 | A kind of stability-enhanced silicon carbide chemical mechanical polishing liquid of pH and its application |
| CN111098237A (en) * | 2019-12-24 | 2020-05-05 | 常州万博金属构件厂 | Preparation method of non-adhesive polished wafer |
| WO2020087721A1 (en) * | 2018-11-02 | 2020-05-07 | 山东天岳先进材料科技有限公司 | Chemical-mechanical polishing solution for silicon carbide having increased ph stability, preparation method therefor, and use thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102585706A (en) * | 2012-01-09 | 2012-07-18 | 清华大学 | Acidic chemical and mechanical polishing composition |
| CN103911617A (en) * | 2014-03-13 | 2014-07-09 | 深圳市宇泰隆科技有限公司 | A silicon oxide polishing solution and a preparation method thereof |
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2014
- 2014-12-22 CN CN201410811996.4A patent/CN104559797B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102585706A (en) * | 2012-01-09 | 2012-07-18 | 清华大学 | Acidic chemical and mechanical polishing composition |
| CN103911617A (en) * | 2014-03-13 | 2014-07-09 | 深圳市宇泰隆科技有限公司 | A silicon oxide polishing solution and a preparation method thereof |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105710760A (en) * | 2016-04-22 | 2016-06-29 | 衡阳市宏达威环保科技有限公司 | Aluminium alloy alkaline grinding fluid |
| WO2018120808A1 (en) * | 2016-12-28 | 2018-07-05 | 安集微电子科技（上海）股份有限公司 | Chem-mechanical polishing liquid for barrier layer |
| CN109554119A (en) * | 2018-11-02 | 2019-04-02 | 山东天岳先进材料科技有限公司 | A kind of stability-enhanced silicon carbide chemical mechanical polishing liquid of pH and its application |
| WO2020087721A1 (en) * | 2018-11-02 | 2020-05-07 | 山东天岳先进材料科技有限公司 | Chemical-mechanical polishing solution for silicon carbide having increased ph stability, preparation method therefor, and use thereof |
| CN111098237A (en) * | 2019-12-24 | 2020-05-05 | 常州万博金属构件厂 | Preparation method of non-adhesive polished wafer |
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