JP7061966B2 - Polishing composition - Google Patents
Polishing composition Download PDFInfo
- Publication number
- JP7061966B2 JP7061966B2 JP2018557686A JP2018557686A JP7061966B2 JP 7061966 B2 JP7061966 B2 JP 7061966B2 JP 2018557686 A JP2018557686 A JP 2018557686A JP 2018557686 A JP2018557686 A JP 2018557686A JP 7061966 B2 JP7061966 B2 JP 7061966B2
- Authority
- JP
- Japan
- Prior art keywords
- abrasive grains
- polishing
- silica abrasive
- polishing composition
- rsp
- 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
Links
- 238000005498 polishing Methods 0.000 title claims description 47
- 239000000203 mixture Substances 0.000 title claims description 26
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 58
- 239000006061 abrasive grain Substances 0.000 claims description 35
- 239000000377 silicon dioxide Substances 0.000 claims description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 239000002245 particle Substances 0.000 description 36
- 239000007788 liquid Substances 0.000 description 18
- 239000002612 dispersion medium Substances 0.000 description 9
- 229910052594 sapphire Inorganic materials 0.000 description 7
- 239000010980 sapphire Substances 0.000 description 7
- 238000009826 distribution Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 238000000691 measurement method Methods 0.000 description 5
- 239000003002 pH adjusting agent Substances 0.000 description 5
- 239000000758 substrate Substances 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000004220 aggregation Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 238000013329 compounding Methods 0.000 description 3
- 230000001186 cumulative effect Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000000685 Carr-Purcell-Meiboom-Gill pulse sequence Methods 0.000 description 1
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 150000007514 bases Chemical class 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000008119 colloidal silica Substances 0.000 description 1
- 238000002296 dynamic light scattering Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 229910021485 fumed silica Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000011736 potassium bicarbonate Substances 0.000 description 1
- 229910000028 potassium bicarbonate Inorganic materials 0.000 description 1
- 235000015497 potassium bicarbonate Nutrition 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- 235000011181 potassium carbonates Nutrition 0.000 description 1
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 description 1
- 229940086066 potassium hydrogencarbonate Drugs 0.000 description 1
- 235000011118 potassium hydroxide Nutrition 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 235000017550 sodium carbonate Nutrition 0.000 description 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Images
Classifications
-
- 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
-
- 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
-
- 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
-
- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A90/00—Technologies having an indirect contribution to adaptation to climate change
- Y02A90/30—Assessment 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)
Description
本発明は、研磨用組成物に関する。 The present invention relates to a polishing composition.
サファイアは、モース硬度9と非常に硬く、化学的な安定性が高いため、高効率で研磨するのが難しい材料である。そのため、サファイア基板の製造では長時間の研磨が行われている。 Sapphire is a material that is extremely hard with a Mohs hardness of 9 and has high chemical stability, making it difficult to polish with high efficiency. Therefore, in the production of the sapphire substrate, polishing is performed for a long time.
特開2015-196704号公報は、サファイア基板の研磨に用いられる研磨用組成物を開示する。この研磨用組成物は、研磨速度を比較的高くかつ長時間維持できるように、シリカのBET比表面積が30m2/g以上であり、かつ、NMR比表面積が10m2/g以上である。Japanese Unexamined Patent Publication No. 2015-196704 discloses a polishing composition used for polishing a sapphire substrate. In this polishing composition, the BET specific surface area of silica is 30 m 2 / g or more and the NMR specific surface area is 10 m 2 / g or more so that the polishing rate can be maintained relatively high and for a long time.
上述した通り、研磨時間を短縮するために高い研磨速度が望まれているが、従来の研磨組成物では高い研磨速度を得ることはできない。 As described above, a high polishing rate is desired in order to shorten the polishing time, but a high polishing rate cannot be obtained with a conventional polishing composition.
本発明の目的は、高い研磨速度を得ることができる研磨用組成物を提供することである。 An object of the present invention is to provide a polishing composition capable of obtaining a high polishing rate.
本発明の一実施形態による研磨用組成物は、シリカ砥粒と、pH調整剤と、水とを含む。シリカ砥粒と水との親和性AVは0.51以上であり、親和性AVは次の式(1)で表される。 The polishing composition according to one embodiment of the present invention contains silica abrasive grains, a pH adjuster, and water. The affinity AV between the silica abrasive grains and water is 0.51 or more, and the affinity AV is represented by the following formula (1).
AV=Rsp/TSA (1)
式(1)中、Rspは次の式(2)で表され、TSAはシリカ砥粒の総表面積である。AV = Rsp / TSA (1)
In the formula (1), Rsp is represented by the following formula (2), and TSA is the total surface area of the silica abrasive grains.
Rsp=(Rav/Rb)-1 (2)
式(2)中、Ravはシリカ砥粒を分散させた状態で観測されるNMR緩和時間の逆数である。Rbはシリカ砥粒を分散させていない状態で観測されるNMR緩和時間の逆数である。Rsp = (Rav / Rb) -1 (2)
In equation (2), Rav is the reciprocal of the NMR relaxation time observed with the silica abrasive grains dispersed. Rb is the reciprocal of the NMR relaxation time observed in the state where the silica abrasive grains are not dispersed.
本発明によれば、高い研磨速度を得ることができる。 According to the present invention, a high polishing rate can be obtained.
本発明者らは、上記の課題を解決するため、種々の検討を行った。その結果、以下の知見を得た。 The present inventors have conducted various studies in order to solve the above-mentioned problems. As a result, the following findings were obtained.
溶媒との親和性が高い砥粒はぬれやすく、分散性が良好である。一方、溶媒との親和性が低い砥粒はぬれにくく、砥粒の凝集が起こりやすい。分散性の良好な砥粒を用いれば、研磨時における砥粒の凝集を抑制し、砥粒が効率的に働くことにより研磨速度を高くできる。分散性が良好であれば、研磨対象物との接触点及び接触回数が増え、これにより研磨速度が高くなると考えられる。親水性が高い砥粒では表面を覆っている水分子によって砥粒間の接触を妨げることで凝集を抑制できるが、親水性が低い砥粒では砥粒間の接触を防ぎきれないために凝集が起こりやすいと考えられる。 Abrasive grains having a high affinity with a solvent are easy to get wet and have good dispersibility. On the other hand, abrasive grains having a low affinity with a solvent are less likely to get wet, and the abrasive grains tend to aggregate. If the abrasive grains having good dispersibility are used, the aggregation of the abrasive grains during polishing can be suppressed, and the abrasive grains work efficiently, so that the polishing speed can be increased. If the dispersibility is good, the contact points with the object to be polished and the number of contacts are increased, which is considered to increase the polishing speed. Aggregation can be suppressed by hindering contact between abrasive grains with water molecules covering the surface in highly hydrophilic abrasive grains, but aggregation cannot be completely prevented in abrasive grains with low hydrophilicity. It is thought that it is likely to occur.
本発明は、これらの知見に基づいて完成された。以下、本発明の一実施形態による研磨用組成物を詳述する。 The present invention has been completed based on these findings. Hereinafter, the polishing composition according to one embodiment of the present invention will be described in detail.
本発明の一実施形態による研磨用組成物は、シリカ砥粒と、pH調整剤と、水とを含む。シリカ砥粒と水との親和性AVは0.51以上であり、親和性AVは次の式(1)で表される。 The polishing composition according to one embodiment of the present invention contains silica abrasive grains, a pH adjuster, and water. The affinity AV between the silica abrasive grains and water is 0.51 or more, and the affinity AV is represented by the following formula (1).
AV=Rsp/TSA (1)
式(1)中、Rspは次の式(2)で表され、TSAはシリカ砥粒の総表面積である。AV = Rsp / TSA (1)
In the formula (1), Rsp is represented by the following formula (2), and TSA is the total surface area of the silica abrasive grains.
Rsp=(Rav/Rb)-1 (2)
式(2)中、Ravはシリカ砥粒を分散させた状態で観測されるNMR緩和時間の逆数である。Rbはシリカ砥粒を分散させていない状態で観測されるNMR緩和時間の逆数である。Rsp = (Rav / Rb) -1 (2)
In equation (2), Rav is the reciprocal of the NMR relaxation time observed with the silica abrasive grains dispersed. Rb is the reciprocal of the NMR relaxation time observed in the state where the silica abrasive grains are not dispersed.
シリカ砥粒は、この分野で常用されるものを使用でき、例えば、コロイダルシリカ、ヒュームドシリカ等を用いることができる。 As the silica abrasive grains, those commonly used in this field can be used, and for example, colloidal silica, fumed silica and the like can be used.
シリカ砥粒の含有量は、研磨用組成物全体の0.5~60質量%である。シリカ粒子の含有量の上限は、好ましくは50質量%であり、さらに好ましくは40質量%である。シリカ粒子の含有量の下限は、好ましくは1質量%であり、さらに好ましくは5質量%である。 The content of silica abrasive grains is 0.5 to 60% by mass of the entire polishing composition. The upper limit of the content of the silica particles is preferably 50% by mass, more preferably 40% by mass. The lower limit of the content of the silica particles is preferably 1% by mass, more preferably 5% by mass.
本実施形態による研磨用組成物はさらに、pH調整剤を含む。研磨用組成物を塩基性側に調整するための化合物としては、例えば水酸化カリウム、水酸化ナトリウム、炭酸水素カリウム、炭酸カリウム、炭酸水素ナトリウム、炭酸ナトリウム等の塩基性化合物が挙げられる。研磨用組成物を酸性側に調整するための化合物としては、例えば塩酸、硫酸、硝酸、リン酸等の酸性化合物が挙げられる。本実施形態による研磨用組成物のpHは、好ましくは8.5~11.0である。 The polishing composition according to this embodiment further contains a pH adjuster. Examples of the compound for adjusting the polishing composition to the basic side include basic compounds such as potassium hydroxide, sodium hydroxide, potassium hydrogencarbonate, potassium carbonate, sodium hydrogencarbonate, 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, and phosphoric acid. The pH of the polishing composition according to this embodiment is preferably 8.5 to 11.0.
本実施形態による研磨用組成物は、上記の他、研磨用組成物の分野で一般に知られた配合剤を任意に配合することができる。 In addition to the above, the polishing composition according to the present embodiment may optionally contain a compounding agent generally known in the field of polishing composition.
本実施形態による研磨用組成物は、シリカ砥粒、pH調整剤、その他の配合材料を適宜混合して水を加えることによって作製される。本実施形態による研磨用組成物は、あるいは、シリカ砥粒、pH調整剤、その他の配合材料を、順次、水に混合することによって作製される。これらの成分を混合する手段としては、ホモジナイザー、超音波等、研磨用組成物の技術分野において常用される手段が用いられる。 The polishing composition according to the present embodiment is prepared by appropriately mixing silica abrasive grains, a pH adjuster, and other compounding materials and adding water. The polishing composition according to the present embodiment is also produced by sequentially mixing silica abrasive grains, a pH adjuster, and other compounding materials with water. As a means for mixing these components, means commonly used in the technical field of polishing compositions such as homogenizers and ultrasonic waves are used.
以上で説明した研磨用組成物は、適当な濃度となるように水で希釈した後、サファイア基板の研磨に用いられる。 The polishing composition described above is diluted with water to an appropriate concentration and then used for polishing the sapphire substrate.
以下、実施例によって本発明をより具体的に説明する。本発明はこれらの実施例に限定されない。 Hereinafter, the present invention will be described in more detail by way of examples. The present invention is not limited to these examples.
表1に示す実施例1~4及び比較例1~3の研磨用組成物を作製した。 The polishing compositions of Examples 1 to 4 and Comparative Examples 1 to 3 shown in Table 1 were prepared.
[粒子径の測定方法]
シリカ砥粒の平均粒子径は、大塚電子株式会社製の粒径測定システム「ELS-Z2」を用い、動的光散乱法によって測定した。[Measurement method of particle size]
The average particle size of the silica abrasive grains was measured by a dynamic light scattering method using a particle size measuring system "ELS-Z2" manufactured by Otsuka Electronics Co., Ltd.
[メジアン径の測定方法]
シリカ砥粒のメジアン径(D50)は、米国CPS Instruments社製「ディスク遠心式高分解能粒度分布測定装置(DC24000UHR)」を用い、頻度別遠心沈降法によって粒度分布を測定し、その粒度分布を累積分布に変換し、その累積分布における累積が50%となる粒子径を求めた。[Measurement method of median diameter]
For the median diameter ( D50 ) of the silica abrasive grains, the particle size distribution was measured by the frequency-based centrifugal sedimentation method using a "disc centrifugal high-resolution particle size distribution measuring device (DC24000UHR)" manufactured by CPS Instruments, Inc. of the United States, and the particle size distribution was determined. It was converted into a cumulative distribution, and the particle size at which the cumulative distribution in the cumulative distribution was 50% was determined.
[親和性の測定方法]
以下に説明するパルスNMRによって、シリカ砥粒(以下、単に「粒子」ともいう。)と分散媒との界面特性を評価した。[Affinity measurement method]
The interface characteristics between the silica abrasive grains (hereinafter, also simply referred to as “particles”) and the dispersion medium were evaluated by pulse NMR described below.
粒子表面に接触又は吸着している分散媒分子と分散媒バルク中の分散媒分子(粒子表面と接触していない自由な状態の分散媒分子)とでは、磁場の変化に対する応答が異なる。一般に、粒子表面に吸着している液体分子の運動は制限を受けるが、バルク液中の液体分子は自由に動くことができる。その結果、粒子表面に吸着している液体分子のNMR緩和時間は、バルク液中の液体分子のNMR緩和時間よりも短くなる。粒子を分散させた液体で観測されるNMR緩和時間は、粒子表面上の液体体積濃度と自由状態の液体体積濃度とを反映した2つの緩和時間の平均値となる。 The response to changes in the magnetic field differs between the dispersion medium molecules that are in contact with or adsorbed on the particle surface and the dispersion medium molecules in the dispersion medium bulk (dispersion medium molecules that are not in contact with the particle surface in a free state). Generally, the movement of liquid molecules adsorbed on the particle surface is restricted, but the liquid molecules in the bulk liquid can move freely. As a result, the NMR relaxation time of the liquid molecules adsorbed on the particle surface is shorter than the NMR relaxation time of the liquid molecules in the bulk liquid. The NMR relaxation time observed in the liquid in which the particles are dispersed is the average value of the two relaxation times reflecting the liquid volume concentration on the particle surface and the liquid volume concentration in the free state.
なお、粒子を分散させた液体で観測される緩和時定数Ravは、次の式で表される。 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:バルク液の体積濃度
Ps:粒子表面積上の液体の体積濃度
Rs:粒子表面への吸収層液体分子の緩和時定数
Rb:バルク液中の液体分子の緩和時定数
また、比表面積Sと緩和時定数Ravとの関係は次の式で表される。Rav = PsRs + PbRb
Pb: Volume concentration of bulk liquid Ps: Volume concentration of liquid on particle surface area Rs: Relaxation time constant of absorption layer liquid molecule on particle surface Rb: Relaxation time constant of liquid molecule in bulk liquid Also, specific surface area S and relaxation The relationship with the time constant Rav is expressed by the following equation.
Rav=ΨPSLρP(Rs-Rb)+Rb
ΨP:粒子体積濃度
L:粒子表面への液体吸収層の厚さ
ρP:粒子密度
粒子を分散させた液体で観測される緩和時間の逆数(NMR緩和時定数)をRav、粒子を分散させる前の液体で観測される緩和時間の逆数(NMR緩和時定数)をRbとし、Rsp=(Rav/Rb)-1を計算する。Rspは、分散媒と粒子表面との親和性の指標であり、粒子の総表面積が同一であれば、Rspが大きいほど分散媒と粒子表面との親和性が高いことを意味する。Rav = ΨPSLρP (Rs-Rb) + Rb
ΨP: Particle volume concentration L: Thickness of liquid absorption layer to the particle surface ρP: Particle density The inverse number of relaxation time (NMR relaxation time constant) observed in the liquid in which the particles are dispersed is Rav, before the particles are dispersed. Let Rb be the inverse of the relaxation time observed in the liquid (NMR relaxation time constant), and calculate Rsp = (Rav / Rb) -1. Rsp is an index of the affinity between the dispersion medium and the particle surface, and if the total surface area of the particles is the same, it means that the larger the Rsp, the higher the affinity between the dispersion medium and the particle surface.
本実施形態では、Rspを粒子の総表面積で除した値を、その研磨用組成物における粒子と分散媒との「親和性」と定義する。 In this embodiment, the value obtained by dividing Rsp by the total surface area of the particles is defined as the "affinity" between the particles and the dispersion medium in the polishing composition.
Rav、Rbは、Xigo nanotools社製のパルスNMR装置Acorn areaを用いて緩和時間(具体的には、シリカ砥粒を分散させた後のNMR緩和時間、及びシリカ砥粒を分散させる前のNMR緩和時間)を測定し、その逆数を求めた。測定条件は、磁場:0.3T、測定周波数:13MHz、測定核:1H NHR、測定方法:CPMG パルスシークエンス法、サンプル量:1ml、温度:25℃とした。For Rav and Rb, a relaxation time (specifically, an NMR relaxation time after dispersing silica abrasive grains and an NMR relaxation before dispersing silica abrasive grains) were performed using a pulse NMR apparatus Acorn area manufactured by Xigo nanotools. Time) was measured and the reciprocal of it was calculated. The measurement conditions were magnetic field: 0.3 T, measurement frequency: 13 MHz, measurement nucleus: 1 H NHR, measurement method: CPMG pulse sequence method, sample volume: 1 ml, temperature: 25 ° C.
粒子の総表面積TSAは、次の式から求めた。 The total surface area TSA of the particles was calculated from the following formula.
TSA=S×V×ΨP×ρP
S:粒子比表面積
V:ラジオ波が照射される部分のNMRチューブ体積
ΨP:粒子体積濃度
ρP:粒子密度
粒子比表面積Sは、次の式から求めた。TSA = S x V x ΨP x ρP
S: Particle specific surface area V: NMR tube volume of the portion irradiated with radio waves ΨP: Particle volume concentration ρP: Particle density The particle specific surface area S was calculated from the following equation.
S=6/(n×ρP)
n:粒子密度
粒子体積濃度ΨPは、次の式から求めた。S = 6 / (n × ρP)
n: Particle density The particle volume concentration ΨP was calculated from the following equation.
ΨP=(λ/100)/[(1-(λ/100))×ρP]×κ
λ:粒子の重量%濃度
κ:ブランク(分散媒)の密度
次に、作製した実施例1~4及び比較例1~3の研磨用組成物を使用して、直径4インチのサファイア基板のc面を研磨した。研磨装置は、Strasbaugh社製の片面研磨機を使用した。研磨パッドは、ウレタンの研磨パッドを使用した。希釈後のシリカ砥粒の含有量が19重量%となるように研磨用組成物を希釈して、300mL/分の供給速度で供給した。定盤の回転速度は140rpm、ヘッドの回転速度は130rpm、研磨荷重は500gf/cm2として、15分間の研磨を行った。ΨP = (λ / 100) / [(1- (λ / 100)) × ρP] × κ
λ: Weight% concentration of particles κ: Density of blank (dispersion medium) Next, using the polishing compositions of Examples 1 to 4 and Comparative Examples 1 to 3 prepared, c of a sapphire substrate having a diameter of 4 inches. The surface was polished. The polishing device used was a single-sided polishing machine manufactured by Strasbaugh. As the polishing pad, a urethane polishing pad was used. The polishing composition was diluted so that the content of the diluted silica abrasive grains was 19% by weight, and the mixture was supplied at a supply rate of 300 mL / min. The surface plate rotation speed was 140 rpm, the head rotation speed was 130 rpm, and the polishing load was 500 gf / cm2, and polishing was performed for 15 minutes.
[研磨速度の測定方法]
研磨前後でのサファイアウェーハの質量変化量を測定し、サファイアウェーハの厚み変化量を算出し、単位時間当たりの厚み変化量を研磨速度とした。[Measurement method of polishing speed]
The amount of change in mass of the sapphire wafer before and after polishing was measured, the amount of change in thickness of the sapphire wafer was calculated, and the amount of change in thickness per unit time was taken as the polishing rate.
[実験結果の評価]
粒子比表面積Sが同じときにはRspが大きいほど親和性が高いことを示すことから、図1に示したグラフの傾きが大きいほど親和性は高い。実施例1~4の親和性は比較例1~3の親和性よりも高い。前述した表1に記載した通り、親和性の高い実施例1~4は、親和性の低い比較例1~3と比べ、約2~4倍も高い研磨速度を得ることができた。[Evaluation of experimental results]
When the particle specific surface area S is the same, the larger the Rsp, the higher the affinity. Therefore, the larger the slope of the graph shown in FIG. 1, the higher the affinity. The affinity of Examples 1 to 4 is higher than that of Comparative Examples 1 to 3. As described in Table 1 described above, Examples 1 to 4 having a high affinity could obtain a polishing rate about 2 to 4 times higher than those of Comparative Examples 1 to 3 having a low affinity.
以上、本発明の実施の形態を説明した。上述した実施の形態は本発明を実施するための例示に過ぎない。よって、本発明は上述した実施の形態に限定されることなく、その趣旨を逸脱しない範囲内で上述した実施の形態を適宜変形して実施することが可能である。 The embodiment of the present invention has been described above. The embodiments described above are merely examples for carrying out the present invention. Therefore, the present invention is not limited to the above-described embodiment, and the above-described embodiment can be appropriately modified and implemented within a range that does not deviate from the gist thereof.
Claims (1)
pH調整剤と、
水とを含み、
pHが8.5~11.0であり、
前記シリカ砥粒と前記水との親和性AVは0.51以上であり、前記親和性AVは次の式(1)で表される、研磨用組成物。
AV=Rsp/TSA (1)
式(1)中、Rspは次の式(2)で表され、TSAは前記シリカ砥粒の総表面積である。
Rsp=(Rav/Rb)-1 (2)
式(2)中、Ravは前記シリカ砥粒を分散させた状態で観測されるNMR緩和時間の逆数であり、Rbは前記シリカ砥粒を分散させていない状態で観測されるNMR緩和時間の逆数である。 With silica abrasive grains,
With a pH regulator,
Including water
The pH is 8.5 to 11.0 and
The affinity AV between the silica abrasive grains and the water is 0.51 or more, and the affinity AV is represented by the following formula (1), a polishing composition.
AV = Rsp / TSA (1)
In the formula (1), Rsp is represented by the following formula (2), and TSA is the total surface area of the silica abrasive grains.
Rsp = (Rav / Rb) -1 (2)
In the formula (2), Rav is the reciprocal of the NMR relaxation time observed in the state where the silica abrasive grains are dispersed, and Rb is the reciprocal of the NMR relaxation time observed in the state where the silica abrasive grains are not dispersed. Is.
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2016249265 | 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 |
---|---|
JPWO2018116890A1 JPWO2018116890A1 (en) | 2019-10-24 |
JP7061966B2 true JP7061966B2 (en) | 2022-05-02 |
Family
ID=62626458
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP2018557686A Active JP7061966B2 (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)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
MY193758A (en) * | 2018-11-01 | 2022-10-27 | Nissan Chemical Corp | Polishing composition using polishing particles having high hyrophilic property |
KR20220024083A (en) | 2019-06-27 | 2022-03-03 | 닛산 가가쿠 가부시키가이샤 | Polishing composition using abrasive particles with high water affinity containing a basic substance |
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 |
WO2023119549A1 (en) * | 2021-12-23 | 2023-06-29 | 扶桑化学工業株式会社 | Colloidal silica and production method therefor |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2015196704A (en) | 2014-03-31 | 2015-11-09 | ニッタ・ハース株式会社 | Polishing composition and polishing method |
JP2016141765A (en) | 2015-02-04 | 2016-08-08 | ニッタ・ハース株式会社 | Polishing composition |
JP2017117894A (en) | 2015-12-22 | 2017-06-29 | 日立化成株式会社 | Polishing liquid, polishing method, semiconductor substrate and electronic apparatus |
Family Cites Families (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP6436517B2 (en) * | 2013-02-20 | 2018-12-12 | 株式会社フジミインコーポレーテッド | Polishing composition |
JP2015203081A (en) * | 2014-04-15 | 2015-11-16 | 株式会社フジミインコーポレーテッド | polishing composition |
-
2017
- 2017-12-11 WO PCT/JP2017/044431 patent/WO2018116890A1/en active Application Filing
- 2017-12-11 CN CN201780077276.1A patent/CN110072966B/en active Active
- 2017-12-11 JP JP2018557686A patent/JP7061966B2/en active Active
- 2017-12-22 TW TW106145227A patent/TWI739974B/en active
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2015196704A (en) | 2014-03-31 | 2015-11-09 | ニッタ・ハース株式会社 | Polishing composition and polishing method |
JP2016141765A (en) | 2015-02-04 | 2016-08-08 | ニッタ・ハース株式会社 | Polishing composition |
JP2017117894A (en) | 2015-12-22 | 2017-06-29 | 日立化成株式会社 | Polishing liquid, polishing method, semiconductor substrate and electronic apparatus |
Also Published As
Publication number | Publication date |
---|---|
WO2018116890A1 (en) | 2018-06-28 |
TWI739974B (en) | 2021-09-21 |
CN110072966B (en) | 2021-06-15 |
JPWO2018116890A1 (en) | 2019-10-24 |
TW201831624A (en) | 2018-09-01 |
CN110072966A (en) | 2019-07-30 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
JP7061966B2 (en) | Polishing composition | |
TWI242589B (en) | Dispersion for chemical mechanical polishing | |
JP6375623B2 (en) | Abrasive, abrasive set, and substrate polishing method | |
TWI804660B (en) | Slurry, manufacturing method of polishing liquid, and polishing method | |
WO2019181013A1 (en) | Polishing liquid, polishing liquid set, and polishing method | |
WO2018012174A1 (en) | Polishing composition, method for producing polishing composition, and polishing method | |
JP6506913B2 (en) | Polishing composition and polishing method | |
TW201213472A (en) | Polishing agent and polishing method | |
TW201811944A (en) | Chemical mechanical polishing slurry composition | |
JP6827318B2 (en) | Cerium oxide abrasive grains | |
US9469787B2 (en) | Nickel phosphorous CMP compositions and methods | |
JP2009260236A (en) | Abrasive powder, polishing method of substrate employing the same as well as solution and slurry employed for the polishing method | |
JP6436018B2 (en) | Polishing slurry for oxide single crystal substrate and method for producing the same | |
JP6960328B2 (en) | Polishing composition | |
JP7163387B2 (en) | Compositions and methods for polishing memory hard disks exhibiting reduced surface scratches | |
JP2019099590A (en) | Polishing liquid composition | |
JP4955253B2 (en) | Polishing composition for polishing device wafer edge, method for producing the same, and polishing method | |
JP6985904B2 (en) | Abrasive liquid composition | |
JP5554052B2 (en) | Polishing composition and polishing method | |
TWI819067B (en) | Polishing composition and polishing system | |
WO2019180887A1 (en) | Polishing liquid, polishing liquid set, and polishing method | |
JP2011054906A (en) | Storage method and storage container for slurry | |
JP2006344786A (en) | Polishing material for polysilicon and polishing method thereof | |
WO2016072371A1 (en) | Polishing composition | |
JP2015120846A (en) | Polishing agent and polishing method |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
A621 | Written request for application examination |
Free format text: JAPANESE INTERMEDIATE CODE: A621 Effective date: 20200807 |
|
A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20210921 |
|
A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20211110 |
|
TRDD | Decision of grant or rejection written | ||
A01 | Written decision to grant a patent or to grant a registration (utility model) |
Free format text: JAPANESE INTERMEDIATE CODE: A01 Effective date: 20220329 |
|
A61 | First payment of annual fees (during grant procedure) |
Free format text: JAPANESE INTERMEDIATE CODE: A61 Effective date: 20220419 |
|
R150 | Certificate of patent or registration of utility model |
Ref document number: 7061966 Country of ref document: JP Free format text: JAPANESE INTERMEDIATE CODE: R150 |