WO2019131885A1 - Suspension épaisse pour polissage - Google Patents

Suspension épaisse pour polissage Download PDF

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Publication number
WO2019131885A1
WO2019131885A1 PCT/JP2018/048163 JP2018048163W WO2019131885A1 WO 2019131885 A1 WO2019131885 A1 WO 2019131885A1 JP 2018048163 W JP2018048163 W JP 2018048163W WO 2019131885 A1 WO2019131885 A1 WO 2019131885A1
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WO
WIPO (PCT)
Prior art keywords
polishing
polishing slurry
ammonium cation
abrasive grains
mass
Prior art date
Application number
PCT/JP2018/048163
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English (en)
Japanese (ja)
Inventor
木村　浩
Original Assignee
ニッタ・ハース株式会社
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by ニッタ・ハース株式会社 filed Critical ニッタ・ハース株式会社
Priority to KR1020207018100A priority Critical patent/KR20200100660A/ko
Priority to JP2019562169A priority patent/JPWO2019131885A1/ja
Publication of WO2019131885A1 publication Critical patent/WO2019131885A1/fr

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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
    • B24B37/00—Lapping machines or devices; Accessories
    • 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
    • B24B37/04—Lapping machines or devices; Accessories designed for working plane surfaces
    • B24B37/042—Lapping machines or devices; Accessories designed for working plane surfaces operating processes therefor
    • B24B37/044—Lapping machines or devices; Accessories designed for working plane surfaces operating processes therefor characterised by the composition of the lapping agent
    • 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
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00—Materials not provided for elsewhere
    • C09K3/14—Anti-slip materials; Abrasives
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00—Materials not provided for elsewhere
    • C09K3/14—Anti-slip materials; Abrasives
    • C09K3/1409—Abrasive particles per se
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00—Materials not provided for elsewhere
    • C09K3/14—Anti-slip materials; Abrasives
    • C09K3/1454—Abrasive powders, suspensions and pastes for polishing
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
    • H01L21/304—Mechanical treatment, e.g. grinding, polishing, cutting

Definitions

  • the present invention relates to a polishing slurry.
  • Patent Document 1 As a polishing slurry for polishing an interlayer insulating film which is an object to be polished, a polishing slurry containing silica abrasive grains has been used (for example, Patent Document 1).
  • the abrasive grains are large, the polishing object tends to be easily scratched. On the other hand, when the abrasive grains are small, the polishing rate tends to be low. Therefore, the abrasive grains are required to have an appropriate size.
  • the polishing slurry is subjected to a dynamic load (pressure, shear force, etc.) during transportation, polishing, etc., and the abrasive grains in the polishing slurry aggregate.
  • a dynamic load pressure, shear force, etc.
  • this invention makes it a subject to provide the slurry for grinding
  • the polishing slurry according to the present invention is used to polish an interlayer insulating film, Silica abrasive grains, And an organic ammonium cation having a molecular weight of 155 or less.
  • FIG. 16 is a graph showing the number of defects when the polishing slurry of Example 5 and Comparative Example 3 is used.
  • the polishing slurry according to the present embodiment is used to polish an interlayer insulating film.
  • the interlayer insulating film include a silicon oxide film, a silicon nitride film, and a low-k film.
  • the silicon oxide film include a film containing SiO 2 formed by plasma CVD using tetraethoxysilane (TEOS).
  • TEOS tetraethoxysilane
  • the Low-k film means a film having a dielectric constant lower than that of a silicon oxide film (SiO 2 film).
  • the polishing slurry according to the present embodiment contains silica abrasive grains and an organic ammonium cation having a molecular weight of 155 or less.
  • the polishing slurry according to the present embodiment further contains an alkali and water.
  • the polishing slurry according to the present embodiment may be used for polishing after being diluted with water or the like, or may be used for polishing without being diluted.
  • the pH of the polishing slurry according to this embodiment is preferably 8 to 12, and more preferably 10 to 12.
  • the polishing slurry according to the present embodiment has a preferable pH by containing the alkali.
  • the polishing slurry according to this embodiment is preferably 1.0 to 25% by mass, more preferably 5.0 to 20% by mass, and further preferably 1.0 to 25% by mass, when it is used as it is without being diluted.
  • the content is 9.0 to 14% by mass.
  • the polishing slurry according to the present embodiment is preferably a silica abrasive when it is used after being diluted (for example, when components other than water are diluted to a half concentration).
  • the content is 40% by mass, more preferably 10 to 30% by mass, and still more preferably 20 to 26% by mass.
  • the slurry for polishing according to the present embodiment preferably contains 0.1 to 1.0 parts by mass, more preferably 0.1 to 0. parts by mass of the organic ammonium cation with respect to 100 parts by mass of the silica abrasive grains. It contains 25 parts by mass.
  • the content of the organic ammonium cation in an amount of 0.1 parts by mass or more with respect to 100 parts by mass of the silica abrasive grains further suppresses the change in the size of the abrasive grains.
  • the polishing slurry according to the present embodiment has an advantage that the polishing rate can be increased by containing the organic ammonium cation in an amount of 1.0 parts by mass or less with respect to 100 parts by mass of the silica abrasive grains.
  • the molecular weight of the organic ammonium cation is preferably 135 or less, more preferably 35 to 95, still more preferably 70 to 90, and still more preferably 75 to 90.
  • the organic ammonium cation is represented by the following formula (1).
  • R 1 is H or a monovalent organic group
  • R 2 is H or a monovalent organic group
  • R 3 is H or a monovalent organic group
  • R 4 is H or a monovalent organic group.
  • R 1 , R 2 , R 3 and R 4 all become H is excluded.
  • As said monovalent organic group an alkyl group, an allyl group, an aromatic alkyl group etc. are mentioned, for example.
  • R 1 is preferably a monovalent organic group having 3 or less carbon atoms, or H.
  • R 2 is preferably a monovalent organic group having 3 or less carbon atoms, or H.
  • R 3 is preferably a monovalent organic group having 3 or less carbon atoms, or H.
  • R 4 is preferably a monovalent organic group having 3 or less carbon atoms, or H.
  • R 1 is a monovalent organic group having 3 or less carbon atoms or H
  • R 2 is a monovalent organic group having 3 or less carbon atoms or H
  • R 4 is preferably a monovalent organic group having 3 or less carbon atoms, or H.
  • Examples of the organic ammonium cation include primary ammonium cation, secondary ammonium cation, tertiary ammonium cation, and quaternary ammonium cation.
  • As the organic ammonium cation a quaternary ammonium cation is preferable.
  • Examples of primary ammonium cations include ethylene diamine and spermine. The spermine is also a secondary ammonium cation.
  • Examples of the secondary ammonium cation piperazine, piperidine and the like can be mentioned.
  • Examples of the quaternary ammonium cation include tetramethyl ammonium cation, ethyl trimethyl ammonium cation and tetraethyl ammonium cation.
  • the organic ammonium cation is included in the polishing slurry according to the present embodiment by mixing the organic ammonium salt and another material for the polishing slurry.
  • the organic ammonium salt include organic ammonium hydroxide, organic halogen halide, organic ammonium nitrate and the like.
  • the silica abrasive grains are contained in the polishing slurry according to the present embodiment as primary particles or as secondary particles in which a plurality of primary particles are aggregated.
  • Examples of the silica abrasive include fumed silica abrasive and colloidal silica abrasive, and fumed silica abrasive is preferable.
  • alkali examples include inorganic alkali agents which are inorganic substances.
  • inorganic alkaline agent potassium hydroxide, sodium hydroxide, ammonia and the like can be mentioned.
  • the polishing slurry according to the present embodiment is configured as described above, and thus has the following advantages.
  • the polishing slurry according to the present embodiment contains silica abrasive grains and an organic ammonium cation having a molecular weight of 155 or less.
  • a polishing slurry is one in which the change in size of the abrasive grains is suppressed.
  • Such a polishing slurry is one in which the change in the size of the abrasive grains is suppressed because the organic ammonium cation is adsorbed to the SiO 2 - group present on the surface of the silica abrasive grains, whereby the three dimensional silica abrasive grains are obtained. It is considered that this causes a failure, and as a result, the silica abrasive grains are less likely to aggregate.
  • polishing slurry according to the present invention is not limited to the above embodiment. Further, the polishing slurry according to the present invention is not limited by the above-described effects. Furthermore, the polishing slurry according to the present invention can be variously modified without departing from the scope of the present invention.
  • the dynamic stability is evaluated by continuously giving shaking (dynamic load) to the polishing slurry of Examples and Comparative Examples with a shaker for 10 days to confirm the growth of the abrasive grains of the polishing slurry. went.
  • the conditions of shaking are shown below.
  • the growth rate of the abrasive grain was calculated
  • the median diameter of the abrasive grains of the following formula was determined by a laser diffraction / scattering particle size distribution measuring device (LA-920) manufactured by Horiba, Ltd. The results are shown in Table 1 below and in FIGS.
  • the polishing slurry of the example is the polishing slurry of Comparative Example 1 using no organic ammonium cation, and the polishing slurry of Comparative Example 2 having a large molecular weight of organic ammonium cation.
  • the growth rate of abrasive grains was smaller than that of the slurry.
  • polishing rate A polishing slurry was prepared containing a salt of ethyltrimethylammonium cation and hydroxide, 20.0% by mass of fumed silica, potassium hydroxide as an alkali, and water (pH: 11.0, as described above). Salt concentration: 200 ppm, 800 ppm, 2000 ppm). Then, immediately before polishing, the polishing slurry is diluted twice with water and the diluted polishing slurry is used to polish a blanket wafer having a SiO 2 film formed by plasma CVD using tetraethoxysilane (TEOS). And the polishing rate was determined. The polishing conditions are shown below.
  • Polishing machine EPO222D (made by Ebara Corp.) Polishing pressure: 35MPa Plate rotation speed: 60 min -1 Carrier rotation speed: 40 min -1 Slurry flow rate: 150 mL / min Polishing time: 60 min The polishing rate was determined by dividing the thickness reduced by polishing by the polishing time. The thickness was measured by Nano spec AFT 5100 manufactured by Nano-metrics. The results are shown in FIG.
  • Example 5 A polishing slurry of Example 5 containing 500 ppm of a salt of ethyltrimethylammonium cation and hydroxide, 12.5% by mass of fumed silica, potassium hydroxide as an alkali, and water was produced (pH: 11.0).
  • a polishing slurry of Comparative Example 3 was produced in the same manner as the polishing slurry except that the salt was not used.
  • a blanket wafer having a SiO 2 film formed by plasma CVD using tetraethoxysilane (TEOS) was polished (wafer area: 706.5 cm 2 , number of wafers: 20). The polishing conditions are shown below.
  • Polishing machine FREX (made by Ebara Corp.) Head: G2 Polishing pressure CAP / RAP / OAP / EAR / RRP / PCP [hPa]: 285/280/250/240/350/140 Head / platen rotation speed [min -1 ]: 60/61 Slurry flow rate: 200 mL / min Polishing time: 60 min. Then, the number of defects on the wafer (pieces / wafer) was measured. The number of defects was measured using a wafer surface inspection apparatus (model name: LS6600) manufactured by Hitachi High-Technologies Corporation. The results are shown in Table 2 below and FIG.
  • the polishing slurry of Example 5 had a smaller number of defects than the polishing slurry of Comparative Example 3 in which the organic ammonium cation was not used.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Manufacturing & Machinery (AREA)
  • Computer Hardware Design (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Power Engineering (AREA)
  • General Physics & Mathematics (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Mechanical Treatment Of Semiconductor (AREA)
  • Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)

Abstract

L'invention concerne une suspension épaisse destinée au polissage, qui est utilisée pour le polissage d'un film isolant intercalaire, et qui contient des grains abrasifs de silice et des cations d'ammonium organiques qui ont un poids moléculaire inférieur ou égal à 155.
PCT/JP2018/048163 2017-12-27 2018-12-27 Suspension épaisse pour polissage WO2019131885A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
KR1020207018100A KR20200100660A (ko) 2017-12-27 2018-12-27 연마용 슬러리
JP2019562169A JPWO2019131885A1 (ja) 2017-12-27 2018-12-27 研磨用スラリー

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JP2017252453 2017-12-27
JP2017-252453 2017-12-27

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WO2019131885A1 true WO2019131885A1 (fr) 2019-07-04

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5139571A (en) * 1991-04-24 1992-08-18 Motorola, Inc. Non-contaminating wafer polishing slurry
JP2009081200A (ja) * 2007-09-25 2009-04-16 Fujifilm Corp 研磨液
WO2015005433A1 (fr) * 2013-07-11 2015-01-15 株式会社フジミインコーポレーテッド Composition de polissage et son procédé de production

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP4214093B2 (ja) 2004-08-24 2009-01-28 花王株式会社 研磨液組成物
JP2006278522A (ja) * 2005-03-28 2006-10-12 Seimi Chem Co Ltd 半導体集積回路装置用研磨剤、研磨方法および半導体集積回路装置の製造方法
JP2007273641A (ja) * 2006-03-30 2007-10-18 Fujifilm Corp 研磨方法
JP5285866B2 (ja) * 2007-03-26 2013-09-11 富士フイルム株式会社 研磨液
JP2010073999A (ja) * 2008-09-19 2010-04-02 Fujifilm Corp 化学的機械的研磨液
JP5843036B1 (ja) * 2015-06-23 2016-01-13 コニカミノルタ株式会社 再生研磨材スラリーの調製方法

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5139571A (en) * 1991-04-24 1992-08-18 Motorola, Inc. Non-contaminating wafer polishing slurry
JP2009081200A (ja) * 2007-09-25 2009-04-16 Fujifilm Corp 研磨液
WO2015005433A1 (fr) * 2013-07-11 2015-01-15 株式会社フジミインコーポレーテッド Composition de polissage et son procédé de production

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KR20200100660A (ko) 2020-08-26
TW201930542A (zh) 2019-08-01
JPWO2019131885A1 (ja) 2021-01-14

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