US20090053981A1 - Method of recycling abrasive slurry - Google Patents

Method of recycling abrasive slurry Download PDF

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Publication number
US20090053981A1
US20090053981A1 US12/192,351 US19235108A US2009053981A1 US 20090053981 A1 US20090053981 A1 US 20090053981A1 US 19235108 A US19235108 A US 19235108A US 2009053981 A1 US2009053981 A1 US 2009053981A1
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Prior art keywords
slurry
used slurry
recycling
dispersant
experiment
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US12/192,351
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English (en)
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Kazuaki Kozasa
Isamu Gotou
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Sumco Techxiv Corp
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Sumco Techxiv Corp
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Assigned to SUMCO TECHXIV CORPORATION reassignment SUMCO TECHXIV CORPORATION ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: GOTOU, ISAMU, KOZASA, KAZUAKI
Publication of US20090053981A1 publication Critical patent/US20090053981A1/en
Abandoned legal-status Critical Current

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B24—GRINDING; POLISHING
    • B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B57/00—Devices for feeding, applying, grading or recovering grinding, polishing or lapping agents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B24—GRINDING; POLISHING
    • B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B37/00—Lapping machines or devices; Accessories
    • B24B37/005—Control means for lapping machines or devices
    • B24B37/0056—Control means for lapping machines or devices taking regard of the pH-value of lapping agents

Definitions

  • the present invention relates to a method of recycling an abrasive slurry for recycling a used slurry having been used in polishing semiconductor wafer(s).
  • Polishing of semiconductor wafer(s) is generally classified into two major categories of rough polishing and finish polishing according to surface roughness to be made on the semiconductor wafer(s).
  • the semiconductor wafer(s) is usually polished with an ammonia-base colloidal silica slurry having been added with a water-soluble polymer such as ethylcellulose.
  • the colloidal silica slurry having been used in finish polishing has conventionally been discarded because the slurry may contain metal contamination originating from components of a polishing apparatus, a giant silica solid formed by aggregation of silica in the slurry, and the like.
  • a Document 1 JP-A-2002-170793 proposes a method of reproducing a slurry, according to which coarse particles in a CMP (chemical mechanical polishing) slurry are filtrated by a filter and the filtrated slurry is condensed by such a method as centrifugation.
  • CMP chemical mechanical polishing
  • JP-A-2004-63858 proposes a method of retrieving a slurry, according to which aggregated abrasive grains contained in a used slurry are crushed by ultrasound, a temperature of the slurry is adjusted and the aggregated abrasive grains are separated from non-aggregated abrasive grains.
  • a pH value of the colloidal silica slurry may be varied by the time when the slurry is retrieved, so that the retrieved slurry may not be directly recycled.
  • the water-soluble polymer contained in the slurry tends to be aggregated to form a gel.
  • gel-like aggregation can easily clog the filter.
  • finish polishing which is the last process in manufacturing processes of semiconductor wafer(s)
  • greater cautions are required to be paid to metal contamination.
  • An object of the invention is to provide a method of recycling an abrasive slurry, by which a used slurry having been used in polishing semiconductor wafer(s), particularly a slurry having been used in finish polishing, can be recycled, so that considerable reduction in slurry usage can contribute to reduction in manufacturing cost of the semiconductor wafer(s).
  • a method of recycling an abrasive slurry according to an aspect of the invention is for recycling a slurry containing colloidal silica, the slurry being a used slurry having been used in polishing semiconductor wafer(s), the method including:
  • the dispersant may be any one of (1) salt, (2) polarizable molecule and (3) pH stabilizer.
  • the gelled portion of the slurry and the aggregated silica are dispersed by the irradiation of ultrasound, and foreign substance(s) contained therein is removed by the filter.
  • foreign substance(s) can be efficiently removed by the filter while an amount of silica contained in the slurry can be prevented from being reduced due to a capture of gelled and aggregated silica by the filter.
  • the used slurry can be favorably recycled.
  • a pH value of the used slurry is measured and the pH value is adjusted by adding an alkali solution before the dispersant is added to the used slurry.
  • An example of the alkali solution for adjusting the pH value is ammonia water.
  • the slurry and silica can be further prevented from being aggregated.
  • viscosity of the used slurry is preferably measured and adjusted with a supplement of a water-soluble polymer before the dispersant is added to the used slurry.
  • water-soluble polymer for adjusting the viscosity examples include ethylcellulose and ethylene glycol.
  • the viscosity of the used slurry can be suitably adjusted. In this manner, an abrasive slurry suitable for recycling can be obtained.
  • a temperature of the used slurry is preferably measured and adjusted with a use of a heat exchanger before the dispersant is added to the used slurry.
  • gelled substance(s) contained in the used slurry can be dispersed therein at the optimal temperature condition.
  • metal ion contained in the used slurry is preferably removed after the ultrasound is irradiated to the used slurry.
  • An exemplary method of removing the metal ion is to add a chelate agent to the used slurry.
  • the chelate agent may be an organic-base agent formed of aminocarboxylate.
  • examples of the chelate agent are EDTA (ethylenediaminetetraacetic acid), DTPA (diethylenetriaminepentaacetic acid) and NTA (nitrilotriacetic acid).
  • the metal ion having been mixed into the slurry during polishing can be removed.
  • semiconductor wafer is polished with the used slurry, it is possible to prevent the semiconductor wafer(s) from being contaminated by metal ion.
  • FIG. 1 schematically shows an arrangement of a recycling apparatus according to an exemplary embodiment of the invention.
  • FIG. 2 is a flow chart showing steps of a recycling method according to the exemplary embodiment.
  • FIG. 3 is a graph showing differences in dispersion effects between dispersants.
  • FIG. 1 shows a recycling apparatus 1 for recycling an abrasive slurry according to the exemplary embodiment of the invention.
  • the recycling apparatus 1 collects a slurry having been used in a finish-polishing machine 2 , adjusts a pH value, a relative density and viscosity of the collected abrasive slurry and then removes foreign metal substance(s) therefrom so as to reproduce a slurry, thereby recycling the used slurry as an abrasive slurry to be used again in the finish-polishing machine 2 .
  • the recycling apparatus 1 includes a multiple-stage cascade tank 3 , a heat exchanger 4 , a storage tank 5 and a foreign-substance filtrating filter 6 .
  • the multi-stage cascade tank 3 serves as a precipitator that removes giant silica solids contained in the collected slurry by sedimentation separation.
  • the inside of the tank 3 is partitioned into plural processing tanks by plural shuttering boards 31 each of which has a different height.
  • the plural shuttering boards 31 are arranged such that the plural shuttering boards 31 as a whole reduces its height as extending to a lateral lace 32 (i.e., where an outlet is provided) from a side to which the collected slurry is supplied. Then, when the used slurry is supplied in a first processing tank and subsequently overflows therein, an amount of the overflowing slurry flows into a processing tank contiguous to the first processing tank. This operation is sequentially repeated, and then the used slurry is finally ejected from the outlet.
  • a lateral lace 32 i.e., where an outlet is provided
  • giant silica solids which have a higher specific gravity than the used slurry, are settled out while supernatant fluid of the used slurry, which has the lower specific gravity than the giant silica solids, flows into a processing tank contiguous thereto. With this operation being repeated, giant silica solids are separated and removed by sedimentation from the used slurry.
  • the heat exchanger 4 which is connected to a rear portion of the multiple-stage cascade tank 3 via a piping, is for adjusting a temperature of the used slurry by cooling the used slurry ejected from the multiple-stage cascade tank 3 .
  • the heat exchanger 4 is so arranged that a channel for the used slurry ejected from the outlet provided on a lower portion of the multiple-stage cascade tank 3 and a channel for circulation of cooling water are partitioned by a highly thermally-conductive material, thereby exchanging heat between the used slurry and the cooling water for temperature adjustment of the used slurry.
  • the heat exchanger 4 may be selected from various heat exchangers, as long as the heat exchanger can exchange heat between liquid and liquid, examples of which are a plate-type heat exchanger, a double pipe-type heat exchanger, and a multitubular cylinder-type heat exchanger.
  • the storage tank 5 which is connected to a rear portion of the heat exchanger 4 via a piping, stores the used slurry having experienced temperature adjustment by the heat exchanger 4 and adjusts conditions of the used slurry.
  • the storage tank 5 is provided with a thermometer 51 , a viscometer 52 , a hydrometer 53 and a pH meter 54 respectively for measuring temperature, viscosity, relative density and pH values of the used slurry stored in the storage tank 5 .
  • a bottom of the storage tank 5 is additionally provided with a ultrasonic oscillator.
  • the ultrasonic oscillator irradiates ultrasound to the used slurry in the storage tank 5 so as to disperse gelled portions and aggregated silica in the used slurry.
  • the ultrasound to be irradiated to the used slurry is preferably kHz-frequency ultrasound because MHz-frequency ultrasound may not be able to disperse aggregated silica due to influence of the water-soluble polymer agent.
  • the foreign-substance filtrating filter 6 which is connected to a rear portion of the storage tank 5 via a piping, filters the used slurry to capture foreign substances such as giant silica solids present in the used slurry.
  • the foreign-substance filtrating filter 6 includes filters such as a depth filter and a membrane filter disposed in the channel in which the used slurry flows.
  • step S 1 After the used slurry is collected from the finish-polishing machine 2 (step S 1 ), the collected used slurry is supplied to the multiple-stage cascade tank 3 of the recycling apparatus 1 , and the supplied used slurry experiences sedimentation separation in each of the processing tanks thereof, so that giant silica solids are removed by sedimentation (step S 2 ).
  • a temperature of the used slurry from which giant silica solids have been removed is adjusted to a suitable temperature by circulating cooling water in the heat exchanger 4 (step S 3 ), and the used slurry having experienced temperature adjustment is subsequently supplied to the storage tank 5 .
  • the temperature of the used slurry is adjusted to be in a range of approximately 20 to 30 degrees C. based on the measurement of the thermometer 51 in the storage tank 5 .
  • Relative density, viscosity and a pH value of the used slurry supplied to the storage tank 5 are sequentially adjusted.
  • Relative density of the used slurry is adjusted by supplementing a stock solution of colloidal silica slurry to the storage tank 5 based on the measurement of the hydrometer 53 (step S 4 ). Relative density of the used slurry is adjusted within a range of 1.010 to 1.020.
  • Viscosity of the used slurry is adjusted by supplementing a water-soluble polymer such as ethylcellulose to the storage tank 5 based on the measurement of the viscometer 52 (step S 5 ). Viscosity of the used slurry is adjusted within a range of 0.004 to 0.01 Pa ⁇ s (values obtained by converting 4 to 10 cP).
  • a pH value of the used slurry is adjusted by supplementing ammonia water to the storage tank 5 based on the measurement of the pH meter 54 (step S 6 ).
  • a targeted pH value is roughly in a range of pH 10 to pH 11.
  • An excessively low value of pH may reduce a polishing rate while an excessively high value of pH may dissolve silica.
  • one of salt, polarizable molecule and pH stabilizer is added thereto as a dispersant so as to prevent aggregation of the used slurry (step S 7 ).
  • ultrasound is irradiated to the used slurry with the ultrasonic oscillator driven, so that gelled portions of the slurry and aggregated silica are dispersed (step S 8 ).
  • the dispersant are KCl, NH 4 HCO 3 (examples of salt).
  • step S 9 the used slurry having been irradiated with ultrasound is filtrated by the foreign-substance filtrating filter 6 , so that foreign substances are removed. Then, a reproduced abrasive slurry is collected through a branch piping to be supplied to the finish-polishing machine 2 for use again.
  • a slurry was obtained by diluting a stock solution of colloidal silica slurry with water 20 times.
  • a semiconductor wafer having a diameter of 150 mm was polished using the slurry according to each of the experiment examples 1 to 5. Then, the quality of a surface of the polished semiconductor wafer was evaluated for each.
  • the semiconductor wafer was polished under the following conditions: PolitexTM was used as an abrasive pad; a table rotation number was 50 rpm; a head rotation number was 70 rpm; pressure of 80 g/cm 2 was applied; and the wafer was polished for 30 minutes.
  • the polishing rate corresponds to a value after the wafer having a diameter of 150 mm was polished for 30 minutes.
  • Microroughness for short wavelengths is represented by an index number that is calculated in relation to a value indicated by a particle counter (SP1 manufactured by KLA-Tencor Corporation) after 30 minutes of polishing in the experiment example 4 (the value is set as 100).
  • microroughness for long wavelengths is represented by an index number that is calculated in relation to a value obtained by averaging rms values of three points in the vicinity of the wafer center after 30 minutes of polishing in the experiment example 4 (the value is set as 100).
  • the number of defects is obtained by counting the number of defects on a polished surface of a single wafer after 30 minutes of polishing.
  • the slurry irradiated with ultrasound as a whole exhibited enhanced polishing rates.
  • the slurry according to the experiment example 3 which was added with a dispersant made of KCl water, exhibited a greatly-enhanced polishing rate.
  • the water-soluble polymer is considered to have had such a low dispersivity as to be partially aggregated on the to-be-polished surface at the time of polishing, and to have served like a protective film thereon. It is presumed that, as the consequence, the polishing rate of the slurry according to the experiment example 4 was low.
  • any one of the experiment examples 1 to 3 exhibited a level of haze that is approximate to that of the experiment example 4, in which the slurry was prepared by diluting the stock solution with water.
  • the experiment example 5 in which the slurry experienced neither ultrasound irradiation nor filtering, exhibited a greatly-reduced value of haze.
  • any one of the experiment examples 1 to 3 is also observed to have exhibited a level of roughness that is approximate to that of the experiment example 4.
  • the experiment example 5 likewise exhibited an increased value of roughness.
  • any one of the experiment examples 1 to 3 is also observed to have exhibited the number of defects that is approximate to that of the experiment example 4.
  • defects in the experiment example 5 were greatly increased.
  • a polishing level i.e., polishing rate, microroughness and the number of defects
  • a polishing level exerted by directly applying the collected used slurry to polishing for recycling is not comparable to a polishing level exerted by a slurry prepared by diluting the stock solution as in the experiment example 4.
  • ultrasound irradiation on the used slurry and addition of a dispersant to the used slurry can so greatly improve the values of the polishing level exerted by the slurry as to make the used slurry applicable as a reproduced slurry.
  • the slurry according to each of the experiment examples 1 to 5 was filtrated by foreign-substance filtrating filters 6 each of which had a different filter size so as to verify to what degree of fineness in filter the slurry could pass through the filter.
  • the results are shown in Table 2.
  • Example 1 Example 2
  • Example 3 Example 4
  • Example 5 Filter Size: 20 ⁇ m A
  • Table 2 “A” means that the slurry could pass through the filter; “B” means that the slurry could partially pass through the filter; and “C” means that the slurry could not pass through the filter.
  • the slurry according to the experiment example 1 (i.e., slurry irradiated with ultrasound) could pass through a filter having a filter size of 20 ⁇ m.
  • the slurry clogged filters respectively having finer filter sizes of 10 ⁇ m and 5 ⁇ m and could not pass through the filters.
  • the slurry according to the experiment example 2 (slurry added with ammonia water and irradiated with ultrasound) and the slurry according to the experiment example 3 (slurry added with KCl water and irradiated with ultrasound) could pass through even a filter having a filter size of 5 ⁇ m. It has been found that silica solids (dried silica) of 1 to 10 ⁇ m order can be captured by filters.
  • a filter having a filter size of 20 ⁇ m was used for the slurry according to the experiment example 1; a filter having a filter size of 10 ⁇ m was used for the slurry according to the experiment example 2; and a filter having a filter size of 5 ⁇ m was used for the slurry according to the experiment example 3.
  • Example 1 Example 2
  • Example 3 Example 4
  • Example 5 Number of 80 to 100 10 to 20 1 to 10 1000 to 6000 to Remaining Dried Silica 2000 8000 (After 300 minutes)
  • Dispersive effect brought about by ultrasound irradiation and addition of a dispersant was checked by measuring an average particle diameter of fine silica particles in the slurry and zeta potential of the slurry. The above checking was conducted on the slurries according to the experiment examples 1, 3 to 5. In addition, in order to see a difference between dispersants, the following experiment example 6 was prepared.
  • the zeta potential represents electrification of a surface of silica. The larger a value of the zeta potential becomes, the more favorable the dispersion is.
  • Example 1 Example 3
  • Example 4 Example 5
  • Example 6 Average Particle Diameter 137.5 77.2 134.5 129.2 148.3 (nm)
  • the slurry according to the experiment example 5 As compared with the slurry according to the experiment example 4 (slurry prepared by diluting the stock solution), the slurry according to the experiment example 5 (used slurry with no treatment) exhibited a greatly reduced value of the zeta potential and deteriorated slurry dispersivity. In contrast, the slurry according to the experiment example 1 (slurry irradiated with ultrasound) has been found to have restored a value of the zeta potential up to a zeta potential level of the slurry according to the experiment example 4. From the above, slurry dispersivity thereof has been found considerably enhanced.
  • the slurry according to the experiment example 6 (slurry added with methanol and irradiated with ultrasound) has been found to have exhibited slightly better dispersivity than the slurry according to the experiment example 1.
  • the slurry according to the experiment example 3 (slurry added with KCl water and irradiated with ultrasound) exhibited much more increased value of the zeta potential than the slurries according the other experiment examples. From the above, it has been found that dispersivity can be considerably enhanced by adding the slurry with KCl water as a dispersant. In addition, the slurry reproduced by the method of the experiment example 3 exhibited a smaller value of the average particle diameter than the slurries according to the other experiment examples. In this respect as well, it has been found that the slurry according to the experiment example 3 is favorably applicable to polishing.
US12/192,351 2007-08-23 2008-08-15 Method of recycling abrasive slurry Abandoned US20090053981A1 (en)

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US20090298393A1 (en) * 2008-05-30 2009-12-03 Sumco Techxiv Corporation Slurry supplying apparatus and method of polishing semiconductor wafer utilizing same
US20110177623A1 (en) * 2010-01-15 2011-07-21 Confluense Llc Active Tribology Management of CMP Polishing Material
US20110180512A1 (en) * 2010-01-28 2011-07-28 Environmental Process Solutions, Inc. Accurately Monitored CMP Recycling
US8696404B2 (en) 2011-12-21 2014-04-15 WD Media, LLC Systems for recycling slurry materials during polishing processes
US20140242884A1 (en) * 2010-07-26 2014-08-28 Shin-Etsu Chemical Co., Ltd. Synethetic quartz glass subtrate polishing slurry and manufacture of synethetic quartz glass substrate using the same
CN105313015A (zh) * 2014-07-29 2016-02-10 盛美半导体设备（上海）有限公司 抛光液过滤装置
US20160376468A1 (en) * 2015-06-23 2016-12-29 Konica Minolta, Inc. Method For Preparing Recycled Abrasive Slurry
CN107004594A (zh) * 2014-12-15 2017-08-01 信越半导体株式会社 硅晶圆的研磨方法
CN110746889A (zh) * 2019-09-03 2020-02-04 福建晶安光电有限公司 一种半导体晶圆加工过程中抛光液循环利用的方法
US20200298371A1 (en) * 2014-09-30 2020-09-24 Taiwan Semiconductor Manufacturing Co., Ltd. Slurry dispersion system with real time control

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JP2011011307A (ja) 2009-07-03 2011-01-20 Sumco Corp ウェーハ研磨用スラリーのリサイクル方法およびそのリサイクル装置
CN102725374B (zh) * 2010-01-29 2016-04-27 福吉米株式会社 半导体晶片的再生方法和研磨用组合物
JP5760403B2 (ja) * 2010-11-24 2015-08-12 株式会社Sumco 薬液リサイクル方法および該方法に用いる装置
CN103931005A (zh) * 2011-09-14 2014-07-16 玛太克司马特股份有限公司 Led制造方法、led制造设备和led
JP6174625B2 (ja) * 2015-05-22 2017-08-02 株式会社フジミインコーポレーテッド 研磨方法及び組成調整剤
JP7395105B2 (ja) 2018-03-28 2023-12-11 株式会社山本金属製作所 冷却液良否管理システム及び冷却液良否検出ユニット

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US20090298393A1 (en) * 2008-05-30 2009-12-03 Sumco Techxiv Corporation Slurry supplying apparatus and method of polishing semiconductor wafer utilizing same
US8303373B2 (en) * 2008-05-30 2012-11-06 Sumco Techxiv Corporation Slurry supplying apparatus and method of polishing semiconductor wafer utilizing same
US20110177623A1 (en) * 2010-01-15 2011-07-21 Confluense Llc Active Tribology Management of CMP Polishing Material
US20110180512A1 (en) * 2010-01-28 2011-07-28 Environmental Process Solutions, Inc. Accurately Monitored CMP Recycling
US8557134B2 (en) 2010-01-28 2013-10-15 Environmental Process Solutions, Inc. Accurately monitored CMP recycling
US9050851B2 (en) 2010-01-28 2015-06-09 Environmental Process Solutions, Inc. Accurately monitored CMP recycling
US20140242884A1 (en) * 2010-07-26 2014-08-28 Shin-Etsu Chemical Co., Ltd. Synethetic quartz glass subtrate polishing slurry and manufacture of synethetic quartz glass substrate using the same
US8696404B2 (en) 2011-12-21 2014-04-15 WD Media, LLC Systems for recycling slurry materials during polishing processes
CN105313015A (zh) * 2014-07-29 2016-02-10 盛美半导体设备（上海）有限公司 抛光液过滤装置
US20200298371A1 (en) * 2014-09-30 2020-09-24 Taiwan Semiconductor Manufacturing Co., Ltd. Slurry dispersion system with real time control
CN107004594A (zh) * 2014-12-15 2017-08-01 信越半导体株式会社 硅晶圆的研磨方法
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US20170345662A1 (en) * 2014-12-15 2017-11-30 Shin-Etsu Handotai Co., Ltd. Method for polishing silicon wafer
US10460947B2 (en) * 2014-12-15 2019-10-29 Shin-Etsu Handotai Co., Ltd. Method for polishing silicon wafer
KR102346305B1 (ko) * 2014-12-15 2022-01-03 신에쯔 한도타이 가부시키가이샤 실리콘 웨이퍼의 연마방법
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US20160376468A1 (en) * 2015-06-23 2016-12-29 Konica Minolta, Inc. Method For Preparing Recycled Abrasive Slurry
US10266725B2 (en) * 2015-06-23 2019-04-23 Konica Minolta, Inc. Method for preparing recycled abrasive slurry
CN110746889A (zh) * 2019-09-03 2020-02-04 福建晶安光电有限公司 一种半导体晶圆加工过程中抛光液循环利用的方法

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