WO2016072371A1 - Composition de polissage - Google Patents

Composition de polissage Download PDF

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Publication number
WO2016072371A1
WO2016072371A1 PCT/JP2015/080844 JP2015080844W WO2016072371A1 WO 2016072371 A1 WO2016072371 A1 WO 2016072371A1 JP 2015080844 W JP2015080844 W JP 2015080844W WO 2016072371 A1 WO2016072371 A1 WO 2016072371A1
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WO
WIPO (PCT)
Prior art keywords
polishing
orp
polishing composition
polished
oxidation
Prior art date
Application number
PCT/JP2015/080844
Other languages
English (en)
Japanese (ja)
Inventor
修平 ▲高▼橋
正利 戸松
Original Assignee
株式会社フジミインコーポレーテッド
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
Priority claimed from JP2015130440A external-priority patent/JP6656829B2/ja
Application filed by 株式会社フジミインコーポレーテッド filed Critical 株式会社フジミインコーポレーテッド
Priority to EP20209757.2A priority Critical patent/EP3800229B1/fr
Priority to EP15858037.3A priority patent/EP3216839B1/fr
Priority to KR1020177014192A priority patent/KR20170080616A/ko
Priority to US15/524,989 priority patent/US11015098B2/en
Priority to CN201580060437.7A priority patent/CN107109191B/zh
Publication of WO2016072371A1 publication Critical patent/WO2016072371A1/fr

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Classifications

    • 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
    • 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
    • B24B1/00—Processes of grinding or polishing; Use of auxiliary equipment in connection with such processes
    • 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
    • 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
    • C09K3/1454—Abrasive powders, suspensions and pastes for polishing
    • C09K3/1463—Aqueous liquid suspensions
    • 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
    • H01L21/02002—Preparing wafers
    • H01L21/02005—Preparing bulk and homogeneous wafers
    • H01L21/02008—Multistep processes
    • H01L21/0201—Specific process step
    • H01L21/02024—Mirror 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L29/00—Semiconductor devices specially adapted for rectifying, amplifying, oscillating or switching and having potential barriers; Capacitors or resistors having potential barriers, e.g. a PN-junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
    • H01L29/02—Semiconductor bodies ; Multistep manufacturing processes therefor
    • H01L29/12—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed
    • H01L29/16—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed including, apart from doping materials or other impurities, only elements of Group IV of the Periodic Table
    • H01L29/1608—Silicon carbide

Definitions

  • the present invention relates to a polishing composition. Specifically, the present invention relates to a polishing composition used for polishing a high hardness material such as a silicon carbide single crystal.
  • a polishing composition used for polishing a high hardness material such as a silicon carbide single crystal.
  • the polishing rate (amount for removing the surface of the object to be polished per unit time) by devising the components (abrasive grains, oxidizing agent, etc.) of the slurry (polishing composition) used for polishing. Improvement of surface smoothness has been proposed. However, even such a technique is insufficient to satisfy a practical required level regarding the polishing rate, and there is still room for improvement.
  • a polishing composition for polishing a material to be polished having a Vickers hardness of 1500 Hv or more is provided.
  • the relationship between the oxidation-reduction potential ORP x [mV] of the polishing composition and the oxidation-reduction potential ORP y [mV] of the material to be polished satisfies the following formula (1).
  • the polishing rate can be greatly improved by using a polishing composition having a redox potential higher by 100 mV or more than the material to be polished.
  • the polishing composition contains abrasive grains and a polishing aid.
  • content W [wt%] of the abrasive grains in the polishing composition and content C [wt%] of the polishing aid satisfies the following formula (2). W / C ⁇ 1.5 (2) According to said polishing composition, the polishing rate improvement effect can be exhibited more suitably.
  • the polishing composition contains abrasive grains.
  • the abrasive grain content W [wt%] in the polishing composition, the oxidation-reduction potential ORP x [mV] of the polishing composition, and the oxidation-reduction potential ORP y [mV] of the material to be polished Satisfies the following formula (3). (ORP x -ORP y ) ⁇ W ⁇ 1000 (3) According to said polishing composition, the polishing rate improvement effect can be exhibited more suitably.
  • the abrasive grain content W is 4 wt% to 10 wt%. When it is within the range of the content of such abrasive grains, a higher polishing rate can be realized.
  • the technique disclosed herein is preferably carried out in such a manner that the oxidation-reduction potential ORP x of the polishing composition is in the range of 750 mV to 1500 mV, and the oxidation-reduction potential ORP y of the material to be polished is in the range of 500 mV to 700 mV. Can be done. When ORP x and ORP y are within the above ranges, the polishing rate improvement effect can be more suitably exhibited.
  • the pH is in the range of 8-11.
  • the application effect of the present invention can be suitably exhibited.
  • a method for producing a polished article is provided.
  • the manufacturing method is to supply any polishing composition disclosed herein to a polishing object composed of a material to be polished having a Vickers hardness of 1500 Hv or more, and polish the polishing object. Including. According to this manufacturing method, it is possible to efficiently provide a polished object having a polished high hardness material surface.
  • the polishing composition disclosed herein is used for polishing a material to be polished (high hardness material) having a Vickers hardness of 1500 Hv or more.
  • the Vickers hardness of the material to be polished is preferably 1800 Hv or higher (for example, 2000 Hv or higher, typically 2200 Hv or higher).
  • the upper limit of Vickers hardness is not particularly limited, but may be about 7000 Hv or less (for example, 5000 Hv or less, typically 3000 Hv or less).
  • the Vickers hardness can be measured based on JIS R 1610: 2003.
  • An international standard corresponding to the JIS standard is ISO 14705: 2000.
  • Examples of the material having a Vickers hardness of 1500 Hv or more include diamond, sapphire (aluminum oxide), silicon carbide, boron carbide, tungsten carbide, silicon nitride, and titanium nitride.
  • the polishing method disclosed herein can be preferably applied to a single crystal surface of the above material that is mechanically and chemically stable. Especially, it is preferable that the grinding
  • the polishing composition disclosed herein is particularly preferably applied to a silicon carbide single crystal surface.
  • the oxidation-reduction potential ORP y with respect to the standard hydrogen electrode of the material to be polished is not particularly limited as long as the relationship of the formula (1) described later is satisfied with the oxidation-reduction potential ORP x of the polishing composition. Absent.
  • the technique disclosed herein can be preferably applied to a material to be polished whose ORP y is about 500 mV to 700 mV (for example, about 600 mV to 700 mV).
  • the oxidation-reduction potential ORP y of the material to be polished is determined by dispersing the powder of the material in water to form a slurry, which is then polished with a pH adjuster (for example, potassium hydroxide (KOH)).
  • KOH potassium hydroxide
  • the oxidation-reduction potential of the polishing composition and the oxidation-reduction potential of the material to be polished referred to in this specification indicate values of the oxidation-reduction potential with respect to the standard hydrogen electrode measured at a liquid temperature of 25 ° C.
  • the oxidation-reduction potential ORP x of the polishing composition is 100 mV higher than the oxidation-reduction potential ORP y [mV] of the material to be polished (material constituting the surface of the object to be polished). More expensive. That is, the relationship between ORP x [mV] and ORP y [mV] satisfies the following formula (1).
  • ORP x only needs to be 100 mV or more higher than ORP y , and is preferably 200 mV or more (for example, 300 mV or more) higher from the viewpoint of polishing efficiency. Further, the value obtained by subtracting ORP y from ORP x (ORP x -ORP y ) is preferably 1000 mV or less, more preferably 800 mV or less, and further preferably from the viewpoint of easily obtaining a higher quality surface. Is 500 mV or less. For example, by setting the value of ORP x -ORP y to 100 mV or more and 500 mV or less, both the polishing efficiency and the surface smoothness after polishing can be realized at a higher level.
  • ORP x is not particularly limited as long as it satisfies the relationship of the above formula (1) with ORP y , but is preferably 750 mV or more, more preferably 800 mV or more (for example, 900 mV or more) from the viewpoint of polishing efficiency and the like. ).
  • the upper limit of ORP x is not particularly limited, but is preferably 1500 mV or less, more preferably 1200 mV or less, and still more preferably 1000 mV or less from the viewpoint of easily obtaining a higher quality surface.
  • ORP x is, for example, the type of abrasive grains and / or polishing aids (for example, an auxiliary agent that exhibits an action of oxidizing and altering the surface of a polishing object in polishing) contained in the polishing composition, or abrasive grains and polishing aids. It can adjust by changing the ratio of the content of. That is, by appropriately selecting the types of abrasive grains and polishing aids and the ratio of the content of abrasive grains and polishing aids, ORP x can be adjusted to the appropriate relationship and range disclosed herein. it can. In addition, as a method of adjusting the ORP x to the appropriate relationship and the above range, a method such as changing the pH of the composition can be employed. The method for controlling the ORP x can be used alone or in combination.
  • the polishing composition disclosed herein typically comprises abrasive grains.
  • the material and properties of the abrasive grains are not particularly limited as long as the polishing composition satisfies the relationship of the above formula (1) with respect to the oxidation-reduction potential with the material to be polished.
  • the abrasive grains can be any of inorganic particles, organic particles, and organic-inorganic composite particles.
  • oxide particles such as silica particles, alumina particles, cerium oxide particles, chromium oxide particles, zirconium oxide particles, manganese dioxide particles, and iron oxide particles are preferable because a good surface can be efficiently formed.
  • oxide particles such as silica particles, alumina particles, cerium oxide particles, chromium oxide particles, zirconium oxide particles, manganese dioxide particles, and iron oxide particles are preferable because a good surface can be efficiently formed.
  • alumina particles, zirconium oxide particles, chromium oxide particles, and iron oxide particles are more preferable, and alumina particles are particularly preferable.
  • composition of the abrasive grains “substantially consisting of X” or “substantially consisting of X” means that the proportion of X in the abrasive grains (the purity of X) is the weight. It is 90% or more on the basis (preferably 95% or more, more preferably 97% or more, further preferably 98% or more, for example 99% or more).
  • the ratio of the alumina particles in the entire abrasive grains contained in the polishing composition is high.
  • the proportion of alumina particles in the whole abrasive grains contained in the polishing composition is preferably 70% by weight or more, more preferably 90% by weight or more, and further preferably 95% by weight or more (eg, 95 to 100% by weight). It is.
  • the polishing composition disclosed herein does not substantially contain diamond particles as abrasive grains.
  • Diamond particles can be a limiting factor for improving smoothness due to their high hardness.
  • diamond particles are generally expensive, they cannot be said to be an advantageous material in terms of cost performance. From a practical aspect, it is desirable that the degree of dependence on high-priced materials such as diamond particles is low.
  • the Vickers hardness of the abrasive grains is preferably 800 Hv or more, more preferably 1200 Hv or more, and further preferably 1500 Hv or more from the viewpoint of polishing efficiency and the like.
  • the upper limit of the Vickers hardness of the abrasive grains is not particularly limited, but is preferably 3000 Hv or less, more preferably 2000 Hv or less, and even more preferably 1700 Hv or less from the viewpoint of achieving both polishing efficiency and surface smoothness after polishing.
  • the value measured based on said JISR1610: 2003 is employ
  • the Vickers hardness of the abrasive grains is preferably equal to or lower than the Vickers hardness of the material constituting the surface of the object to be polished (the material to be polished). Since the hardness of the abrasive grains is limited in the relative relationship with the hardness of the material to be polished, deterioration of smoothness tends to be suppressed.
  • the Vickers hardness of the abrasive grains is more preferably 300 Hv or more (for example, 500 Hv or more) lower than the Vickers hardness of the material to be polished.
  • the difference between the Vickers hardness of the abrasive grains and the Vickers hardness of the material to be polished is preferably within 1000 Hv (for example, within 800 Hv) from the viewpoint of improving flatness.
  • the average secondary particle diameter of the abrasive grains is usually 20 nm or more, and is preferably 100 nm or more, more preferably 200 nm or more (for example, 400 nm or more) from the viewpoint of polishing efficiency and the like. Higher polishing rates can be achieved with abrasive grains having the above average secondary particle size.
  • the upper limit of the average secondary particle diameter of the abrasive grains is suitably about 5000 nm or less from the viewpoint of sufficiently securing the number per unit weight.
  • the average secondary particle diameter is preferably 3000 nm or less, more preferably 2000 nm or less (for example, 800 nm or less) from the viewpoint of achieving both higher polishing efficiency and surface smoothness after polishing.
  • the average secondary particle diameter of the abrasive grains is less than 500 nm, for example, by a dynamic light scattering method using a model “UPA-UT151” manufactured by Nikkiso Co., Ltd. Mv) can be measured. Moreover, about 500 nm or more particle
  • the content W of the abrasive grains in the polishing composition is not particularly limited as long as the polishing composition satisfies the relationship of the formula (1) with respect to the oxidation-reduction potential with the material to be polished. It is appropriate that the amount is not less than 2%, preferably not less than 2% by weight, more preferably more than 3% by weight, still more preferably not less than 4% by weight, particularly preferably not less than 5% by weight.
  • ORP x is effectively increased, and as a result, ORP x -ORP y is increased, and the polishing rate can be improved efficiently.
  • the content W of the abrasive grains in the polishing composition is usually 50% by weight or less from the viewpoint of achieving both a high level of polishing efficiency and surface smoothness after polishing, and from the viewpoint of obtaining good dispersibility. Is preferably 20% by weight or less, more preferably 10% by weight or less, and still more preferably 8% by weight or less.
  • the polishing composition disclosed herein preferably contains a polishing aid.
  • the polishing aid is a component that enhances the effect of polishing, and typically a water-soluble one is used.
  • the polishing aid is not particularly limited, but exhibits an action of modifying the surface of the object to be polished (typically oxidative deterioration) in polishing, thereby causing weakening of the surface of the object to be polished. It is thought that it contributes to polishing with abrasive grains.
  • polishing aids include peroxides such as hydrogen peroxide; nitric acid, nitrates such as iron nitrate, silver nitrate, aluminum nitrate, and nitrates such as cerium ammonium nitrate as complexes thereof; peroxomonosulfuric acid, peroxodisulfuric acid Persulfuric acid such as persulfate such as ammonium persulfate and potassium persulfate; chloric acid and salts thereof, perchloric acid and perchloric salts such as potassium perchlorate; bromic acid and salts thereof Bromine compounds such as certain potassium bromate; iodine compounds such as iodic acid, its salt ammonium iodate, periodic acid, its salt sodium periodate, potassium periodate, etc
  • permanganic acid or a salt thereof chromic acid or a salt thereof, iron acid or a salt thereof is preferable, and sodium permanganate or potassium permanganate is particularly preferable.
  • polishing aids ORP x is effectively increased, and the polishing rate can be improved efficiently.
  • the polishing composition contains a composite metal oxide as a polishing aid.
  • the composite metal oxide include nitrate metal salts, iron acids, permanganic acids, chromic acids, vanadic acids, ruthenium acids, molybdic acids, rhenic acids, and tungstic acids.
  • iron acids, permanganic acids, and chromic acids are more preferable, and permanganic acids are more preferable.
  • the composite metal oxide includes a monovalent or divalent metal element (excluding transition metal elements) and a fourth periodic transition metal element in the periodic table.
  • CMO is used.
  • ORP x is effectively increased.
  • ORP x -ORP y is increased, so that the polishing rate can be improved efficiently.
  • the monovalent or divalent metal element include Na, K, Mg, and Ca. Of these, Na and K are more preferable.
  • the fourth periodic transition metal element in the periodic table include Fe, Mn, Cr, V, and Ti. Among these, Fe, Mn, and Cr are more preferable, and Mn is more preferable.
  • the polishing composition disclosed herein contains a composite metal oxide (preferably a composite metal oxide CMO) as a polishing aid, it may or may not contain a polishing aid other than the composite metal oxide. Also good.
  • the technique disclosed herein can also be preferably implemented in an embodiment that does not substantially contain a polishing aid (for example, hydrogen peroxide) other than a composite metal oxide (preferably a composite metal oxide CMO) as a polishing aid.
  • the content C of the polishing aid in the polishing composition is not particularly limited as long as the polishing composition satisfies the relationship of the above formula (1) with respect to the oxidation-reduction potential with the material to be polished. It is appropriate to set it to 1 weight% or more. From the viewpoint of polishing efficiency and the like, the content C is preferably 0.5% by weight or more, and more preferably 1% by weight or more. On the other hand, when the content C of the polishing aid is too large, the effect of improving the polishing rate tends to become slow, and the stability of the composition may be lowered. From the viewpoint of the stability of the polishing composition, the content C of the polishing aid is usually suitably 10% by weight or less, preferably 3% by weight or less, and preferably 2% by weight or less. More preferably.
  • the polishing composition disclosed herein is a chelating agent, a thickener, a dispersant, a pH adjuster, a surfactant, an organic acid, an organic acid salt, an inorganic acid, an inorganic material, as long as the effects of the present invention are not impaired.
  • Known additives that can be used in polishing compositions typically high-hardness material polishing compositions such as silicon carbide substrate polishing compositions
  • acid salts, rust inhibitors, antiseptics, and fungicides May be further contained as necessary.
  • the content of the additive may be set as appropriate according to the purpose of the addition, and does not characterize the present invention, so a detailed description is omitted.
  • the solvent used in the polishing composition is not particularly limited as long as it can disperse the abrasive grains.
  • ion exchange water deionized water
  • pure water pure water
  • ultrapure water distilled water and the like
  • the polishing composition disclosed herein may further contain an organic solvent (lower alcohol, lower ketone, etc.) that can be uniformly mixed with water, if necessary.
  • 90% by volume or more of the solvent contained in the polishing composition is preferably water, and more preferably 95% by volume or more (typically 99 to 100% by volume) is water.
  • the relationship between the abrasive grain content W [wt%] and the polishing aid content C [wt%] in the polishing composition is expressed by the following formula: Satisfy (2).
  • the W / C is preferably 2 or more, more preferably 3 or more, still more preferably 4 or more, and particularly preferably 5 or more.
  • a polishing rate improvement effect can be more suitably exhibited as it is the ratio (W / C) of the content of the abrasive grains and the polishing aid.
  • the upper limit of W / C is not particularly limited, but is preferably 20 or less, more preferably 15 or less, still more preferably 10 or less, and particularly preferably 8 or less, from the viewpoint of the stability of the polishing composition.
  • the relationship between the content W [wt%] of the abrasive grains in the polishing composition, the ORP x [mV] of the polishing composition, and the ORP y [mV] of the material to be polished is The following formula (3) is satisfied.
  • the abrasives are satisfied so as to satisfy the relationship of ⁇ ⁇ 1000 while satisfying the relationship of the formula (1).
  • the polishing rate improvement effect can be more suitably exhibited.
  • those satisfying ⁇ ⁇ 1200 are preferable, those satisfying ⁇ ⁇ 1500 are more preferable, and those satisfying ⁇ ⁇ 1800 are particularly preferable.
  • the upper limit of ⁇ is not particularly limited.
  • those satisfying ⁇ ⁇ 4000 are usually suitable, those satisfying ⁇ ⁇ 3500 are preferable, and those satisfying ⁇ ⁇ 2500 are more preferable.
  • a polishing composition that satisfies 1200 ⁇ ⁇ ⁇ 2000 is preferable from the viewpoint of achieving both high polishing efficiency and surface smoothness.
  • the pH of the polishing composition is not particularly limited as long as the polishing composition satisfies the relationship of the above formula (1) with respect to the oxidation-reduction potential with the material to be polished. Usually, it is appropriate that the polishing composition has a pH of about 2 to 12. When the pH of the polishing composition is within the above range, a practical polishing rate is easily achieved.
  • the pH of the polishing composition is preferably 6 to 10, more preferably 8 to 11, particularly preferably 8.5 to 9.5, from the viewpoint of better exerting the application effect of the technology disclosed herein. .
  • each component contained in the polishing composition may be mixed using a well-known mixing device such as a blade-type stirrer, an ultrasonic disperser, or a homomixer.
  • a well-known mixing device such as a blade-type stirrer, an ultrasonic disperser, or a homomixer.
  • the aspect which mixes these components is not specifically limited, For example, all the components may be mixed at once and may be mixed in the order set suitably.
  • the polishing composition disclosed herein can be used for polishing a polishing object, for example, in an embodiment including the following operations. That is, a polishing liquid (slurry) containing any of the polishing compositions disclosed herein is prepared. Preparing the polishing liquid may include preparing a polishing liquid by adding operations such as concentration adjustment (for example, dilution) and pH adjustment to the polishing composition. Or you may use the said polishing composition as polishing liquid as it is. Further, in the case of a multi-drug type polishing composition, to prepare the polishing liquid, mixing those agents, diluting one or more agents before the mixing, and after the mixing Diluting the mixture, etc. can be included.
  • the polishing liquid is supplied to the surface of the high-hardness material that is the object to be polished, and is polished by a conventional method.
  • a polishing object is set in a general polishing apparatus, and the polishing liquid is supplied to a high hardness surface (polishing object surface) of the polishing object through a polishing pad of the polishing apparatus.
  • the polishing pad is pressed against the high-hardness surface of the object to be polished, and both are relatively moved (for example, rotated). The polishing of the object to be polished is completed through the polishing step.
  • a polishing method for polishing a material to be polished having a Vickers hardness of 1500 Hv or more and a method for producing a polished article using the polishing method.
  • the above polishing method is characterized by including a step of polishing an object to be polished using the polishing composition disclosed herein.
  • a polishing method according to a preferred embodiment includes a step of performing preliminary polishing (preliminary polishing step) and a step of performing final polishing (finishing polishing step).
  • the preliminary polishing step is a step of performing preliminary polishing on a polishing object made of a material having at least a surface (surface to be polished) having a Vickers hardness of 1500 Hv or more.
  • the preliminary polishing process is a polishing process that is arranged immediately before the finishing polishing process.
  • the preliminary polishing process may be a single-stage polishing process or a multi-stage polishing process of two or more stages.
  • the finish polishing step referred to here is a step of performing finish polishing on the polishing target that has been subjected to preliminary polishing, and is the last of the polishing steps performed using a polishing slurry containing abrasive grains ( That is, it means a polishing step arranged on the most downstream side.
  • the polishing composition disclosed herein may be used in the preliminary polishing step, may be used in the final polishing step, or preliminary polishing. It may be used in both the process and the finish polishing process.
  • the polishing step using the polishing composition is a preliminary polishing step.
  • a required polishing rate is larger than that in the finishing polishing process. Therefore, the polishing composition disclosed herein is suitable as a polishing composition (preliminary polishing composition) used in a preliminary polishing step on the surface of a high hardness material.
  • the polishing composition disclosed herein can be preferably applied to the preliminary (upstream) preliminary polishing. Especially, it can be preferably used in the first preliminary polishing step (typically the primary polishing step) that has passed through the lapping step described later.
  • the preliminary polishing step includes two or more stages of polishing steps
  • two or more of the polishing steps may be performed using any of the polishing compositions disclosed herein.
  • the polishing composition used in each of the two or more stages of polishing steps described above has an oxidation-reduction potential with respect to the standard hydrogen electrode of the polishing composition used for the downstream preliminary polishing used for the upstream preliminary polishing. It is preferable to select the polishing composition to be lower than the oxidation-reduction potential with respect to the standard hydrogen electrode. According to such a combination of polishing compositions, a polishing surface with higher smoothness tends to be realized in a short time in the preliminary polishing of a high hardness material.
  • the polishing composition (finishing polishing composition) used for the preliminary polishing composition and the finishing polishing step is finished.
  • the difference (ORP FIN ⁇ ORP y ) between the oxidation-reduction potential ORP FIN [mV] and ORP y [mV] of the polishing composition is equal to the oxidation-reduction potential ORP PRE [mV] and ORP y [mV] of the preliminary polishing composition.
  • the polishing method disclosed herein is a preliminary polishing composition having an oxidation-reduction potential ORP PRE [mV], and a preliminary polishing composition in which ORP PRE- ORP y is 100 mV or more is used as a preliminary polishing target. Polishing the polishing object using a polishing step and a finishing polishing composition having an oxidation-reduction potential ORP FIN [mV], wherein ORP FIN -ORP y is less than 100 mV And the step of performing can be preferably carried out in an embodiment including in this order. According to such a combination of the preliminary polishing composition and the finish polishing composition, a polished surface with higher smoothness tends to be realized in a shorter time in polishing a high-hardness material.
  • an ORP FIN- ORP y of 50 mV or less can be preferably used.
  • ORP FIN -ORP y is preferably ⁇ 500 mV or more, more preferably ⁇ 200 mV or more, from the viewpoint of polishing efficiency and the like.
  • the oxidation-reduction potential ORP FIN of the finish polishing composition can be, for example, 300 mV to 750 mV (preferably 400 mV to 700 mV).
  • Pre-polishing and finish polishing can be applied to both polishing using a single-side polishing apparatus and polishing using a double-side polishing apparatus.
  • a polishing object is affixed to a ceramic plate with wax, or a polishing object is held using a holder called a carrier, and a polishing pad is pressed against one side of the polishing object while supplying a polishing composition. Then, one side of the object to be polished is polished by relatively moving both of them (for example, rotational movement).
  • a polishing object is held by using a holder called a carrier, and a polishing pad is pressed against the opposite surface of the polishing object while supplying a polishing composition from above, and these are rotated in a relative direction.
  • a polishing pad is pressed against the opposite surface of the polishing object while supplying a polishing composition from above, and these are rotated in a relative direction.
  • the polishing pad used in each polishing step disclosed herein is not particularly limited.
  • any of a non-woven fabric type, a suede type, a rigid foamed polyurethane type, a product containing abrasive grains, a product containing no abrasive grains, and the like may be used.
  • the polishing object polished by the method disclosed herein is typically cleaned after polishing. This washing can be performed using an appropriate washing solution.
  • the cleaning liquid to be used is not particularly limited, and a known and commonly used cleaning liquid can be appropriately selected and used.
  • the polishing method disclosed herein may include any other process in addition to the preliminary polishing process and the finishing polishing process.
  • An example of such a process is a lapping process performed before the preliminary polishing process.
  • the lapping step is a step of polishing the polishing object by pressing the surface of the polishing surface plate (for example, cast iron surface plate) against the polishing object. Therefore, no polishing pad is used in the lapping process.
  • the lapping process is typically performed by supplying abrasive grains (typically diamond abrasive grains) between the polishing surface plate and the object to be polished.
  • the polishing method disclosed herein may include an additional process (a cleaning process or a polishing process) before the preliminary polishing process or between the preliminary polishing process and the finishing polishing process.
  • the technology disclosed herein can include, for example, providing a method for manufacturing an abrasive (eg, a substrate). That is, according to the technology disclosed herein, any polishing composition disclosed herein is supplied to a polishing object composed of a polishing object material having a Vickers hardness of at least 1500 Hv or more. There is provided a method for producing a polished object, comprising polishing an object to be polished.
  • the above manufacturing method can be implemented by preferably applying the contents of any of the polishing methods disclosed herein. According to the above manufacturing method, a polished object (for example, a substrate) having a high hardness material surface can be efficiently provided.
  • a polishing composition was prepared by mixing alumina (average secondary particle size: 500 nm) as abrasive grains, potassium permanganate (KMnO 4 ) as a polishing aid and deionized water.
  • the content (W) of abrasive grains in the polishing composition was 6%, and the content (C) of KMnO 4 was 1.2%.
  • the pH of the polishing composition was adjusted to 9.0 using KOH.
  • Example 2 Polishing composition in the same manner as in Example 1 except that sodium periodate (NaIO 4 ) was used instead of KMnO 4 and the content of NaIO 4 in the polishing composition was 1.2%. A product was prepared.
  • sodium periodate NaIO 4
  • Example 3 A polishing composition was prepared in the same manner as in Example 1 except that the abrasive grain content was 2%.
  • Example 2 Example 1 except that hydrogen peroxide (H 2 O 2 ) was used instead of KMnO 4 and the content of H 2 O 2 in the polishing composition was 1.2%. A polishing composition was prepared.
  • the oxidation-reduction potential ORP x [mV] relative to the standard hydrogen electrode was measured using the oxidation-reduction potentiometer (main body model: F-52, electrode model: 9300) manufactured by Horiba, Ltd. It measured on 25 degreeC conditions.
  • the oxidation-reduction potential of the slurry was measured, and the value was defined as the oxidation-reduction potential ORP y [mV] of SiC.
  • the oxidation-reduction potential ORP y of SiC was 607 mV. From these measured values and the composition of the polishing composition according to each example, ORP x -ORP y , W / C and ⁇ (that is, (ORP x -ORP y ) ⁇ W) were calculated.
  • polishing rate was computed according to the following formulas (1) and (2). The results are shown in the corresponding column of Table 1.
  • Model “EJ-380IN” Polishing pad “SUBA800” manufactured by Nitta Haas Polishing pressure: 300 g / cm 2 Surface plate rotation speed: 80 rotations / minute Polishing time: 1 hour Head rotation speed: 40 rotations / minute Polishing liquid supply rate: 20 mL / minute (flowing) Polishing liquid temperature: 25 ° C Polishing object: SiC wafer (conduction type: n-type, crystal type 4H 4 ° off) 2 inches
  • a polishing composition capable of improving the polishing rate can be provided.

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

Abstract

L'invention concerne une composition de polissage pour matériaux à polir ayant une dureté Vickers de 1 500 Hv ou plus. Cette composition de polissage permet d'obtenir une relation entre le potentiel d'oxydo-réduction ORPx [mV] de la composition de polissage et le potentiel d'oxydo-réduction ORPy [mV] du matériau à polir qui satisfait l'équation suivante : ORPx - ORPy ≥ 100 mV.
PCT/JP2015/080844 2014-11-07 2015-10-30 Composition de polissage WO2016072371A1 (fr)

Priority Applications (5)

Application Number Priority Date Filing Date Title
EP20209757.2A EP3800229B1 (fr) 2014-11-07 2015-10-30 Composition de polissage
EP15858037.3A EP3216839B1 (fr) 2014-11-07 2015-10-30 Composition de polissage
KR1020177014192A KR20170080616A (ko) 2014-11-07 2015-10-30 연마용 조성물
US15/524,989 US11015098B2 (en) 2014-11-07 2015-10-30 Polishing composition
CN201580060437.7A CN107109191B (zh) 2014-11-07 2015-10-30 研磨用组合物

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JP2014227388 2014-11-07
JP2014-227388 2014-11-07
JP2015130440A JP6656829B2 (ja) 2014-11-07 2015-06-29 研磨用組成物
JP2015-130440 2015-06-29

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CN118165701B (zh) * 2024-05-11 2024-07-26 山东天岳先进科技股份有限公司 一种金刚石用研磨液及金刚石衬底的研磨方法

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JP2007311586A (ja) * 2006-05-19 2007-11-29 Nippon Steel Corp 炭化珪素単結晶ウェハ表面の仕上げ研磨方法
JP2008068390A (ja) * 2006-09-15 2008-03-27 Noritake Co Ltd 結晶材料の研磨加工方法
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