CN110072966B - Polishing composition - Google Patents

Polishing composition Download PDF

Info

Publication number
CN110072966B
CN110072966B CN201780077276.1A CN201780077276A CN110072966B CN 110072966 B CN110072966 B CN 110072966B CN 201780077276 A CN201780077276 A CN 201780077276A CN 110072966 B CN110072966 B CN 110072966B
Authority
CN
China
Prior art keywords
abrasive grains
silica abrasive
rsp
polishing
polishing composition
Prior art date
Legal status (The legal status 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 status listed.)
Active
Application number
CN201780077276.1A
Other languages
Chinese (zh)
Other versions
CN110072966A (en
Inventor
江泽俊二
大藤健
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Nida Dupont Co Ltd
Original Assignee
Nida Dupont Co Ltd
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 Nida Dupont Co Ltd filed Critical Nida Dupont Co Ltd
Publication of CN110072966A publication Critical patent/CN110072966A/en
Application granted granted Critical
Publication of CN110072966B publication Critical patent/CN110072966B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B24GRINDING; POLISHING
    • B24BMACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B37/00Lapping machines or devices; Accessories
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09GPOLISHING COMPOSITIONS; SKI WAXES
    • C09G1/00Polishing compositions
    • C09G1/02Polishing compositions containing abrasives or grinding agents
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00Materials not provided for elsewhere
    • C09K3/14Anti-slip materials; Abrasives
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04Manufacture 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
    • H01L21/18Manufacture 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
    • H01L21/30Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/302Treatment 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
    • H01L21/304Mechanical treatment, e.g. grinding, polishing, cutting
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02ATECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A90/00Technologies having an indirect contribution to adaptation to climate change
    • Y02A90/30Assessment of water resources

Landscapes

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

Abstract

The invention provides a polishing composition capable of obtaining a high polishing rate. The polishing composition comprises: silicon dioxide abrasive grains, a pH regulator and water. The affinity AV of the silica abrasive grains with water is 0.51 or more, and the affinity AV is represented by the following formula (1). AV ═ Rsp/TSA (1) in formula (1), Rsp is represented by the following formula (2), and TSA is the total surface area of the silica abrasive grains. In formula (2), Rsp ═ Rav/Rb) -1(2), Rav is the reciprocal of the NMR relaxation time observed in a state where the silica abrasive grains are dispersed. Rb is the reciprocal of the NMR relaxation time observed in a state where the silica abrasive grains are not dispersed.

Description

Polishing composition
Technical Field
The present invention relates to a polishing composition.
Background
Sapphire is a material that is very hard, has a mohs hardness of 9, and is chemically stable, and therefore, it is difficult to polish with high efficiency. Therefore, the sapphire substrate is polished for a long time.
Jp 2015-196704 a discloses a polishing composition for polishing a sapphire substrate. In the polishing composition, the BET specific surface area of silica was 30m2A specific surface area of 10m or more in terms of NMR2(ii) at least g so as to be able to maintain the polishing rate at a high level for a long period of time.
Disclosure of Invention
As described above, a high polishing rate is desired for shortening the polishing time, but a high polishing rate cannot be obtained with conventional polishing compositions.
The invention aims to provide a polishing composition which can obtain a high polishing rate.
The polishing composition according to one embodiment of the present invention includes silica abrasive grains, a pH adjuster, and water. The affinity AV of the silica abrasive grains with water is 0.51 or more, and the affinity AV is represented by the following formula (1).
AV=Rsp/TSA (1)
In formula (1), Rsp is represented by formula (2) below, and TSA is the total surface area of the silica abrasive grains.
Rsp=(Rav/Rb)-1 (2)
In formula (2), Rav is the reciprocal of the NMR relaxation time observed in a state where the silica abrasive grains are dispersed. Rb is the reciprocal of the NMR relaxation time observed in a state where the silica abrasive grains are not dispersed.
According to the present invention, a high polishing rate can be obtained.
Drawings
FIG. 1 is a graph showing the relationship between Rsp and the total surface area of silica abrasive grains in examples 1 to 4 and comparative examples 1 to 3.
Detailed Description
The present inventors have made various studies to solve the above problems. As a result, the following findings were obtained.
The abrasive grains having high affinity with the solvent are easily wetted and have good dispersibility. On the other hand, abrasive grains having low affinity with a solvent are not easily wetted, and aggregation of abrasive grains is easily caused. When the abrasive grains having good dispersibility are used, aggregation of the abrasive grains during polishing is suppressed, the abrasive grains can efficiently function, and the polishing rate can be increased. It is considered that when the dispersibility is good, the contact point with the object to be polished and the number of times of contact increase, and thus the polishing rate increases. It is considered that the abrasive grains having high hydrophilicity are inhibited from aggregating by inhibiting the contact between the abrasive grains due to water molecules covering the surface, while the abrasive grains having low hydrophilicity are likely to aggregate because the contact between the abrasive grains cannot be completely prevented.
The present invention has been completed based on these findings. Hereinafter, a polishing composition according to an embodiment of the present invention will be described in detail.
The polishing composition according to one embodiment of the present invention includes silica abrasive grains, a pH adjuster, and water. The affinity AV of the silica abrasive grains with water is 0.51 or more, and the affinity AV is represented by the following formula (1).
AV=Rsp/TSA (1)
In formula (1), Rsp is represented by formula (2) below, and TSA is the total surface area of the silica abrasive grains.
Rsp=(Rav/Rb)-1 (2)
In formula (2), Rav is the reciprocal of the NMR relaxation time observed in a state where the silica abrasive grains are dispersed. Rb is the reciprocal of the NMR relaxation time observed in a state where the silica abrasive grains are not dispersed.
The silica abrasive may be any silica abrasive commonly used in the art, and for example, colloidal silica, fumed silica, or the like may be used.
The content of the silica abrasive grains is 0.5 to 60 mass% of the entire polishing composition. The upper limit of the content of the silica particles is preferably 50 mass%, and more preferably 40 mass%. The lower limit of the content of the silica particles is preferably 1% by mass, and more preferably 5% by mass.
The polishing composition of the present embodiment further includes a pH adjuster. Examples of the compound for adjusting the polishing composition to the alkaline side include: and basic compounds such as potassium hydroxide, sodium hydroxide, potassium bicarbonate, potassium carbonate, sodium bicarbonate, and sodium carbonate. Examples of the compound for adjusting the polishing composition to the acidic side include: acidic compounds such as hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, and the like. The polishing composition of the present embodiment preferably has a pH of 8.5 to 11.0.
In the polishing composition of the present embodiment, in addition to the above, a compounding agent generally known in the field of polishing compositions can be optionally compounded.
The polishing composition of the present embodiment is produced by appropriately mixing silica abrasive grains, a pH adjuster, and other blending materials and adding water. Alternatively, the polishing composition of the present embodiment can be prepared by sequentially mixing silica abrasive grains, a pH adjuster, and other blending materials into water. As a method for mixing these components, a method commonly used in the technical field of polishing compositions, such as a homogenizer and ultrasonic waves, can be used.
The polishing composition described above is diluted with water to an appropriate concentration, and then used for polishing a sapphire substrate.
Examples
The present invention will be described more specifically with reference to examples. The present invention is not limited to these examples.
Polishing compositions of examples 1 to 4 and comparative examples 1 to 3 shown in Table 1 were prepared.
[ Table 1]
Content (%) Particle size (nm) Median particle diameter (nm) Affinity of the amino acid sequence pH Grinding speed (μm/hr)
Example 1 19 82 62 0.51 10 4.3
Example 2 19 84 75 0.75 10 4.1
Example 3 19 127 48 0.59 10 4.2
Example 4 19 127 87 0.53 10 4.0
Comparative example 1 19 93 88 0.31 10 1.7
Comparative example 2 19 112 104 0.46 10 1.6
Comparative example 3 19 138 124 0.39 10 1.1
[ method of measuring particle diameter ]
The average particle diameter of the silica abrasive grains was measured by a dynamic light scattering method using a particle diameter measurement system "ELS-Z2" manufactured by Otsuka Denshi K.K.
[ method for measuring median diameter ]
Median particle diameter (D) of the silica abrasive grains50) The particle size distribution was measured by a frequency difference centrifugal sedimentation method using a "disk centrifugal high-resolution particle size distribution measuring apparatus (DC24000 UHR)" manufactured by CPS Instruments in the united states, and the particle size distribution was converted into a cumulative distribution, and the cumulative particle size at which the cumulative particle size distribution was 50% was obtained.
[ method for measuring affinity ]
The interfacial properties between the silica abrasive grains (hereinafter also simply referred to as "particles") and the dispersion medium were evaluated by pulse NMR described below.
The dispersion medium molecules in contact with or adsorbed to the particle surfaces respond differently to changes in the magnetic field than the dispersion medium molecules in the bulk of the dispersion medium (the dispersion medium molecules in a free state that are not in contact with the particle surfaces). In general, the movement of liquid molecules adsorbed to the particle surface is restricted, and liquid molecules in the body fluid can move freely. As a result, the NMR relaxation time of the liquid molecules adsorbed on the particle surface becomes shorter than that of the liquid molecules in the body fluid. The NMR relaxation time observed in the liquid in which the particles are dispersed is an average value of 2 relaxation times reflecting the liquid volume concentration on the particle surface and the liquid volume concentration in a free state.
The relaxation time constant Rav observed in the liquid in which the particles are dispersed is expressed by the following equation.
Rav=PsRs+PbRb
Pb: volume concentration of body fluid
Ps: volume concentration of liquid over surface area of particle
Rs: relaxation time constant of liquid molecules of the absorption layer absorbed to the particle surface
Rb: relaxation time constant of liquid molecules in body fluid
The relationship between the specific surface area S and the relaxation time constant Rav is expressed by the following equation.
Rav=ΨPSLρP(Rs-Rb)+Rb
Ψ P: volume concentration of particles
L: thickness of liquid-absorbing layer absorbed to particle surface
ρ P: density of particles
Assuming that Rav is the inverse of the relaxation time observed in the liquid in which the particles are dispersed (NMR relaxation time constant), Rb is the inverse of the relaxation time observed in the liquid before the particles are dispersed (NMR relaxation time constant), Rsp — 1 is calculated. Rsp is an index of affinity between the dispersion medium and the particle surface, and if the total surface area of the particles is the same, the larger Rsp indicates the higher affinity between the dispersion medium and the particle surface.
In the present embodiment, the value obtained by dividing Rsp by the total surface area of the particles is defined as "affinity" between the particles and the dispersion medium in the polishing composition.
Rav and Rb are obtained by measuring the relaxation times (specifically, NMR relaxation time after dispersing silica abrasive grains and NMR relaxation time before dispersing silica abrasive grains) using a pulse NMR apparatus Acorn area manufactured by Xigo nanols, inc. The measurement condition is set to magneticField: 0.3T, measurement frequency: 13MHz, assay nuclei:1h NHR, determination method: CPMG pulse sequence method, sample amount: 1ml, temperature: at 25 ℃.
The total surface area TSA of the particles is determined by the following equation.
TSA=S×V×ΨP×ρP
S: specific surface area of the particles
V: NMR tube volume of radio wave-irradiated portion
Ψ P: volume concentration of particles
ρ P: density of particles
The particle specific surface area S is determined by the following equation.
S=6/(n×ρP)
n: density of particles
The particle volume concentration Ψ P was determined according to the following equation.
ΨP=(λ/100)/[(1-(λ/100))×ρP]×κ
λ: weight% concentration of particles
Kappa: density of blank sample (dispersion medium)
Then, the polishing compositions of examples 1 to 4 and comparative examples 1 to 3 were used to polish the c-plane of a sapphire substrate having a diameter of 4 inches. The grinding apparatus used was a single-side grinder manufactured by Strasbaugh. The polishing pad used was a urethane polishing pad. The polishing composition was diluted so that the content of the diluted silica abrasive grains became 19 wt%, and was supplied at a supply rate of 300 mL/min. The rotation speed of the stage was set to 140rpm, the rotation speed of the polishing head was set to 130rpm, and the polishing load was set to 500gf/cm2Then, the polishing was carried out for 15 minutes.
[ method for measuring polishing Rate ]
The amount of change in the mass of the sapphire wafer before and after polishing was measured, and the amount of change in the thickness of the sapphire wafer was calculated, and the amount of change in the thickness per unit time was used as the polishing rate.
[ evaluation of Experimental results ]
Since a larger Rsp indicates a higher affinity when the specific surface area S of the particle is the same, the higher the slope of the graph shown in fig. 1, the higher the affinity. The affinities of examples 1 to 4 were higher than those of comparative examples 1 to 3. As shown in Table 1, the polishing rates of examples 1 to 4 having high affinity were about 2 to 4 times higher than those of comparative examples 1 to 3 having low affinity.
The embodiments of the present invention have been described above. The above embodiments are merely illustrative for implementing the present invention. Therefore, the present invention is not limited to the above embodiments, and the above embodiments may be modified as appropriate without departing from the scope of the invention.

Claims (1)

1. A polishing composition comprising: silicon dioxide abrasive grains, a pH regulator and water;
the silica abrasive has an affinity AV of 0.51 or more with the water, the affinity AV being represented by the following formula (1):
AV=Rsp/TSA (1)
in formula (1), Rsp is represented by formula (2) below, TSA is the total surface area of the silica abrasive grains;
Rsp=(Rav/Rb)-1 (2)
in formula (2), Rav is the reciprocal of the NMR relaxation time observed in a state where the silica abrasive grains are dispersed, and Rb is the reciprocal of the NMR relaxation time observed in a state where the silica abrasive grains are not dispersed.
CN201780077276.1A 2016-12-22 2017-12-11 Polishing composition Active CN110072966B (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
JP2016-249265 2016-12-22
JP2016249265 2016-12-22
PCT/JP2017/044431 WO2018116890A1 (en) 2016-12-22 2017-12-11 Polishing composition

Publications (2)

Publication Number Publication Date
CN110072966A CN110072966A (en) 2019-07-30
CN110072966B true CN110072966B (en) 2021-06-15

Family

ID=62626458

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201780077276.1A Active CN110072966B (en) 2016-12-22 2017-12-11 Polishing composition

Country Status (4)

Country Link
JP (1) JP7061966B2 (en)
CN (1) CN110072966B (en)
TW (1) TWI739974B (en)
WO (1) WO2018116890A1 (en)

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3876264B1 (en) * 2018-11-01 2024-09-11 Nissan Chemical Corporation Polishing composition using polishing particles that have high water affinity
US20220228031A1 (en) * 2019-06-27 2022-07-21 Nissan Chemical Corporation Polishing composition using polishing particles containing basic substance and having high water affinity
CN110514687B (en) * 2019-09-19 2022-11-29 上海景瑞阳实业有限公司 Method and system for testing quality guarantee period of silver powder dispersion system
WO2023037930A1 (en) * 2021-09-07 2023-03-16 日本化学工業株式会社 Negative thermal expansion material, method for producing same, and paste
DE112021008471T5 (en) * 2021-12-23 2024-09-05 Fuso Chemical Co., Ltd. Colloidal silicon dioxide and manufacturing process therefor

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105027267A (en) * 2013-02-20 2015-11-04 福吉米株式会社 Polishing composition
CN105038698A (en) * 2014-04-15 2015-11-11 福吉米株式会社 Polishing composition
JP2016141765A (en) * 2015-02-04 2016-08-08 ニッタ・ハース株式会社 Polishing composition
CN106133107A (en) * 2014-03-31 2016-11-16 霓达哈斯股份有限公司 Composition for polishing and Ginding process

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP6589622B2 (en) 2015-12-22 2019-10-16 日立化成株式会社 Polishing liquid, polishing method, semiconductor substrate and electronic device

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105027267A (en) * 2013-02-20 2015-11-04 福吉米株式会社 Polishing composition
CN106133107A (en) * 2014-03-31 2016-11-16 霓达哈斯股份有限公司 Composition for polishing and Ginding process
CN105038698A (en) * 2014-04-15 2015-11-11 福吉米株式会社 Polishing composition
JP2016141765A (en) * 2015-02-04 2016-08-08 ニッタ・ハース株式会社 Polishing composition

Also Published As

Publication number Publication date
TWI739974B (en) 2021-09-21
JPWO2018116890A1 (en) 2019-10-24
WO2018116890A1 (en) 2018-06-28
CN110072966A (en) 2019-07-30
JP7061966B2 (en) 2022-05-02
TW201831624A (en) 2018-09-01

Similar Documents

Publication Publication Date Title
CN110072966B (en) Polishing composition
TWI242589B (en) Dispersion for chemical mechanical polishing
WO2019181013A1 (en) Polishing liquid, polishing liquid set, and polishing method
JP6375623B2 (en) Abrasive, abrasive set, and substrate polishing method
WO2015152151A1 (en) Polishing composition and polishing method
TWI804660B (en) Slurry, manufacturing method of polishing liquid, and polishing method
JP5856256B2 (en) Polishing composition for nickel-phosphorus storage disk
KR20130114635A (en) Polishing agent and polishing method
WO2018179787A1 (en) Polishing liquid, polishing liquid set, and polishing method
JP2019522896A (en) Slurry composition for chemical-mechanical polishing
US9469787B2 (en) Nickel phosphorous CMP compositions and methods
WO2018179064A1 (en) Slurry and polishing method
JP6960328B2 (en) Polishing composition
JP2014216369A (en) Abrasive and polishing method
JP6191433B2 (en) Abrasive and polishing method
JP7163387B2 (en) Compositions and methods for polishing memory hard disks exhibiting reduced surface scratches
WO2018179062A1 (en) Polishing liquid, polishing liquid set, additive liquid, and polishing method
JP2014216368A (en) Polishing agent and polishing method
JP2018104547A (en) Slurry for polishing
JP5554052B2 (en) Polishing composition and polishing method
JP2006344786A (en) Polishing material for polysilicon and polishing method thereof
JP2022527089A (en) Additives to improve particle dispersion in CMP slurries
JP2015120846A (en) Polishing agent and polishing method

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
CB02 Change of applicant information

Address after: Osaka Japan

Applicant after: Nida DuPont Co., Ltd

Address before: Osaka Japan

Applicant before: NITTA HAAS Inc.

CB02 Change of applicant information
GR01 Patent grant
GR01 Patent grant