US20110005143A1 - Polishing oil slurry for polishing hard crystal substrate - Google Patents
Polishing oil slurry for polishing hard crystal substrate Download PDFInfo
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- US20110005143A1 US20110005143A1 US12/886,810 US88681010A US2011005143A1 US 20110005143 A1 US20110005143 A1 US 20110005143A1 US 88681010 A US88681010 A US 88681010A US 2011005143 A1 US2011005143 A1 US 2011005143A1
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- 238000005498 polishing Methods 0.000 title claims abstract description 157
- 239000002002 slurry Substances 0.000 title claims abstract description 52
- 239000000758 substrate Substances 0.000 title claims abstract description 46
- 239000013078 crystal Substances 0.000 title claims abstract description 26
- 239000002245 particle Substances 0.000 claims abstract description 103
- 229910003460 diamond Inorganic materials 0.000 claims abstract description 58
- 239000010432 diamond Substances 0.000 claims abstract description 58
- 239000011164 primary particle Substances 0.000 claims abstract description 11
- 229930195733 hydrocarbon Natural products 0.000 claims description 18
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- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 abstract description 65
- 230000003746 surface roughness Effects 0.000 abstract description 34
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Images
Classifications
-
- 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 at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System 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
- 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
-
- 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
- C09K3/1436—Composite particles, e.g. coated particles
-
- 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
- C09K3/1472—Non-aqueous liquid suspensions
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L29/00—Semiconductor devices adapted for rectifying, amplifying, oscillating or switching, or capacitors or resistors with at least one potential-jump barrier or surface barrier, e.g. 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 System
- H01L29/1608—Silicon carbide
Definitions
- This invention relates to polishing oil slurry for use in a method of polishing a hard crystal substrate such as gallium nitride (GaN) and silicon carbide (SiC) substrates.
- a hard crystal substrate such as gallium nitride (GaN) and silicon carbide (SiC) substrates.
- GaN (Group III nitride semiconductor) and crystalline material of SiC are wide band-gap semiconductors, and a GaN substrate is usually manufactured by forming a GaN film on a sapphire substrate by a halide vapor phase epitaxy (HVPE) method, as disclosed in Japanese Patent Publication Tokkai 9-335580. Devices may be formed on this GaN film, for example, to produce a short-wavelength green or blue light-emitting elements and a purple-color semiconductor laser.
- HVPE halide vapor phase epitaxy
- SiC is coming to be used as the substrate of a high-function power device since it can be used in high-output, high-frequency and high-temperature operations and has a high insulation breakdown field.
- GaN substrates and SiC substrates are hard crystal substrates and since devices of specified kinds are formed on the surface of such a hard crystal substrate, high levels of flatness and smoothness are required of such surfaces.
- Polishing by free abrading particles is carried out by rotating a metallic lapping plate, supplying polishing slurry on the surface of this lapping plate, pressing the surface of a substrate held by a work holder onto the surface of the lapping plate and causing this work holder to rotate.
- aqueous slurry with abrading particles dispersed in an aqueous dispersant has been used.
- Polishing oil slurry of this invention may be characterized as comprising abrading particles including artificial diamond clusters and an oil dispersant for dispersing these abrading particles, and the hard crystal substrate to be polished may be a GaN or SiC substrate.
- the artificial diamond clusters comprise approximately spherical agglomerate particles with average particle diameter D50 of 20 nm or more and 50 nm or less, having primary particles with particle diameters of 2 nm or more and 10 nm or less.
- the oil dispersant includes synthetic isoparaffin hydrocarbons.
- a method of this invention for polishing a hard crystal substrate may be characterized as comprising a rough polishing process of polishing a surface of the substrate such that it will come to have an average surface roughness (Ra) of 0.5 nm or more and 1 nm or less and a finishing process, carried out after the rough polishing process, of polishing the substrate surface such that its average surface roughness (Ra) becomes 0.2 nm or less.
- the finishing process comprises the steps of rotating a lapping plate, supplying the polishing oil slurry of this invention described above to a surface of this lapping plate, pressing the surface of the hard crystal substrate onto the surface of the lapping plate and rotating the hard crystal substrate.
- the lapping plate comprises a soft metal such as tin or its alloy, having a groove formed thereon.
- the groove is preferably spiral, centered around the axis of rotation of the lapping plate and being sectionally V-shaped.
- the rough polishing process preferably comprises a first rough polishing step of polishing the surface of the hard crystal substrate such that its average surface roughness (Ra) becomes 1 nm or more and 3 nm or less and a second rough polishing step, carried out after the first rough polishing step, of polishing the substrate surface such that its average surface roughness (Ra) becomes 0.5 nm or more and 1 nm or less.
- the merit of the invention is that the surface of a hard crystal substrate can be mirror-polished so as to have an average surface roughness (Ra) of 0.2 nm or less without forming any scratches.
- FIG. 1 is a side view of an apparatus for pad-less polishing.
- FIG. 2A is a schematic sectional view of a lapping plate used in the rough polishing process.
- FIG. 2B is an enlarged photograph of a portion of its surface.
- FIG. 3A is a schematic sectional view of a lapping plate used in the finishing process.
- FIG. 3B is an enlarged photograph of a portion of its surface.
- FIG. 4 is a graph of particle size distribution of artificial diamond particles used in the first rough polishing step of Test Examples 1 and 2 and their microscopic (SEM) photograph.
- FIG. 5 is a graph of particle size distribution of artificial diamond particles used in the second rough polishing step of Test Examples 1 and 2 and their microscopic (SEM) photograph.
- FIG. 6 is a graph of particle size distribution of the artificial diamond clusters with average size of 27 nm in the polishing oil slurry of Test Example 1 and their microscopic (SEM and TEM) photographs.
- FIG. 7 is a graph of particle size distribution of the artificial diamond clusters with average size of 30 nm in the polishing oil slurry of Comparison Example 1 and their microscopic (TEM) photograph.
- FIG. 8 includes FIGS. 8A and 8B which are respectively an enlarged photograph of a plan view and a diagonal view of the surface of the GaN substrate after the first rough polishing step of Test Example 1.
- FIG. 9 includes FIGS. 9A and 9B which are respectively an enlarged photograph of a plan view and a diagonal view of the surface of the GaN substrate after the second rough polishing step of Test Example 1.
- FIG. 10 includes FIGS. 10A and 10B which are respectively an enlarged photograph of a plan view and a diagonal view of the surface of the GaN substrate after the finishing step of Test Example 1.
- FIG. 11 includes FIGS. 11A and 11B which are respectively an enlarged photograph of a plan view and a diagonal view of the surface of the GaN substrate after the first rough polishing step of Comparison Example 1.
- FIG. 12 includes FIGS. 12A and 12B which are respectively an enlarged photograph of a plan view and a diagonal view of the surface of the GaN substrate after the second rough polishing step of Comparison Example 1.
- FIG. 13 includes FIGS. 13A and 13B which are respectively an enlarged photograph of a plan view and a diagonal view of the surface of the GaN substrate after the finishing step of Comparison Example 1.
- FIG. 14 includes FIGS. 14A and 14B which are respectively an enlarged photograph of a plan view and a diagonal view of the surface of the GaN substrate after the first rough polishing step of Comparison Example 2.
- FIG. 15 includes FIGS. 15A and 15B which are respectively an enlarged photograph of a plan view and a diagonal view of the surface of the GaN substrate after the second rough polishing step of Comparison Example 2.
- FIG. 16 includes FIGS. 16A and 16B which are respectively an enlarged photograph of a plan view and a diagonal view of the surface of the GaN substrate after the finishing step of Comparison Example 2.
- FIG. 17 includes FIGS. 17A and 17B which are respectively an enlarged photograph of a plan view and a diagonal view of the surface of the GaN substrate after the first rough polishing step of Test Example 2.
- FIG. 18 includes FIGS. 18A and 18B which are respectively an enlarged photograph of a plan view and a diagonal view of the surface of the GaN substrate after the second rough polishing step of Test Example 2.
- FIG. 19 includes FIGS. 19A and 19B which are respectively an enlarged photograph of a plan view and a diagonal view of the surface of the GaN substrate after the finishing step of Test Example 2.
- the invention relates to polishing oil slurry for polishing a hard crystal substrate which may preferably be a GaN substrate or a SiC substrate.
- Polishing oil slurry of this invention comprises abrading particles and an oil dispersant that disperses these abrading particles, and the abrading particles according to this invention include artificial diamond clusters.
- the oil dispersant according to this invention includes oils, having the function of forming an oily film on the surfaces of the abrading particles and improving the particle lubricity on the target surface to be polished.
- oils include paraffin hydrocarbons and may preferably include synthesized isoparaffin hydrocarbons.
- the oil dispersants according to this invention include non-ionic surfactants as dispersants for improving dispersion of abrading particles and preferably include higher aliphatic monoglycerides or higher aliphatic diglycerides.
- the artificial diamond clusters according to this invention comprise approximately spherical agglomerate particles with average size D50 of 20 nm or more and 50 nm or less, having primary particles with particle diameters of 2 nm or more and 10 nm or less. Since the particle size distribution of the abrading particles dispersed in an oil dispersant cannot be measured, the average particle size D50 of the artificial diamond clusters is shown here by the measured value of the dispersion inside pure water.
- the artificial diamond clusters of this invention comprise artificial diamond obtained by an explosion synthesis method (also known as a shockwave method) of a known kind.
- explosion synthesis method also known as a shockwave method
- One is to use graphite powders as the material for diamond and to compress these graphite powders at a high temperature by providing a shock with the energy of explosion to thereby generate diamond artificially.
- the other method is to explode an explosive such as TNT or RDX and to artificially convert the carbon (as the material for diamond) contained in the explosive into diamond by the shock caused by the energy of explosion.
- reaction product that is obtained by such an explosion synthesis method contains carbon materials that have not reacted as well as metallic impurities
- such obtained product is chemically treated with nitric acid, sulfuric acid, hydrochloric acid or a mixture thereof to dissolve and remove these impurities. After the impurities are removed, water is used for washing.
- the artificial diamond thus obtained comprises primary particles and agglomerate particles of these primary particles.
- the diameters of the primary particles are within the range of 2 nm-20 nm, and they have the shape with more roundness than monocrystalline and polycrystalline diamond particles.
- Diamond films that have not reacted and diamond-like carbon films are formed on the surfaces of the primary particles.
- the agglomerate particles are formed as the primary particles agglomerate into a nearly spherical shape at the time of the explosion synthesis, and these agglomerate particles are referred to as artificial diamond clusters.
- Artificial diamond clusters are more easily breakable than agglomerate particles obtained by agglomerating natural (monocrystalline and polycrystalline) diamond particles within a liquid. In other words, if artificial diamond clusters are pressed to the surface of a target object to be polished, those of larger sizes break up to an appropriate degree such that the number of scratches formed by artificial diamond clusters can be reduced.
- the surface of the target object to be polished is polished too deeply as the clusters break up, and this may result in unwanted scratches. Since the average surface roughness of the target surface to be polished is 0.2 nm or less according to this invention, artificial diamond particles exceeding 50 nm are excluded.
- the product obtained by the explosion synthesis method is crushed by means of a ball mill or the like, the aforementioned chemical treatment is carried out, it is washed with water and then a centrifugal separator is used for sorting to collect artificial diamond particles of a desired size.
- Polishing oil slurry of this invention is produced by mixing oil with a dispersant and causing artificial diamond clusters to be dispersed in this liquid mixture.
- the amount of the dispersant to be used is 1 weight % or more and 10 weight % or less with respect to the whole of the oil.
- the amount of the artificial diamond cluster is 0.1 weight % or more and 3 weight % or less with respect to the whole of the polishing oil slurry.
- the method of this invention for polishing a hard crystal substrate comprises a rough polishing process for polishing a surface of the hard crystal substrate such that the average surface roughness (Ra) of the surface becomes 0.5 nm or more and 1 nm or less and a finishing process for polishing the surface after the rough polishing process such that its average surface roughness (Ra) becomes 0.2 nm or less.
- the target surface of the hard crystal substrate is polished in the rough polishing process such that the surface waviness (Wa) becomes 1 nm or less. This is because the correction of the surface waviness becomes difficult in the subsequent finishing process if it exceeds 1 nm because the stock removal is small during the finishing process.
- the rough polishing process is carried out by a known method of tape polishing, pad polishing or pad-less polishing such that the average surface roughness (Ra) of the target surface of the hard crystal substrate becomes 0.5 nm or more and 1 nm or less.
- the tape polishing method is carried out by rotating the substrate attached to a spindle, supplying polishing slurry on the surface of this substrate, pressing a tape of a woven or non-woven cloth or a foamed material and causing it to run.
- the pad polishing method is carried out by rotating a lapping plate with a pad of a woven or non-woven cloth or a foamed material adhered to its surface, supplying polishing slurry to the surface of this pad, pressing the surface of the substrate thereto and causing it to rotate.
- the pad-less polishing method may be carried out by using an apparatus 10 shown in FIG. 1 , rotating its lapping plate 11 in the direction of arrow R with no pad on its surface, supplying polishing slurry through a nozzle 13 directly to the surface of the lapping plate 11 , pressing the surface of the substrate W held by a work holder 12 onto the surface of the lapping plate 11 and rotating the work holder 12 in the direction of arrow r.
- the polishing slurry may be water-based or oil-based, having abrading particles dispersed in a water-based or oil-based dispersing medium.
- the abrading particles may be particles of polycrystalline diamond, monocrystalline diamond, aluminum oxide (Al 2 O 3 ), silicon oxide (SiO 2 ), chromium oxide (Cr 2 O 3 ) or cubic boron nitride (cBN). Of the above, polycrystalline diamond particles are preferable.
- water-based dispersing medium examples include water and aqueous solutions obtained by adding a dispersing agent such as glycols and alcohols to water.
- oil-based dispersing medium examples include oils and those obtained by adding a dispersing agent such as paraffin hydrocarbons to oil.
- the rough polishing process may consist of a single step or two or more steps of rough polishing process. If the target average surface roughness (Ra) (of 0.5 nm or more and 1 nm or less) is to be attained by a single step of rough polishing process, it will take a long time and the surface waviness (Wa) becomes large. If the rough polishing process includes three or more steps, on the other hand, the process becomes too cumbersome.
- the rough polishing process consists of a first step of polishing the target surface of a hard crystal substrate such that its average surface roughness (Ra) becomes 1 nm or more and 3 nm or less and a second step of polishing (carried out after the first step) the target surface such that its average surface roughness (Ra) becomes 0.5 nm or more and 1 nm or less).
- the hard crystal substrate is subjected to tape polishing, pad polishing or pad-less polishing (such as shown in FIG. 1 ) by using water-based or oil-based polishing slurry containing abrading particles (preferably comprising polycrystalline diamond particles) with average size D50 of 3 ⁇ m or more and 5 ⁇ m or less.
- abrading particles preferably comprising polycrystalline diamond particles
- the hard crystal substrate is subjected to tape polishing, pad polishing or pad-less polishing by using water-based or oil-based polishing slurry containing abrading particles (preferably comprising polycrystalline diamond particles) with average size D50 of 0.5 ⁇ m or more and 3 ⁇ m or less.
- abrading particles preferably comprising polycrystalline diamond particles
- Pad-less polishing is particularly preferred both for the first and second rough polishing steps.
- the lapping plate to be used in such pad-less polishing process is shown in FIG. 2 .
- This lapping plate 11 is made of a soft metallic material (such as tin or a tin alloy), and spiral grooves (shown by symbol g) with depth (indicated by symbol d) in the range of 50 nm-100 nm are formed on the surface (shown by symbol s) with average surface roughness (Ra) of 1 nm-50 nm, having a center matching the axis of rotation (shown at 14 in FIG. 1 ).
- These grooves (g) are sectionally V-shaped with the inner surfaces having a slope ⁇ within the range of 30°-90°.
- the pitch (indicated by symbol p) of the grooves (g) is 0.2 mm-0.5 mm.
- the target surface of the hard crystal substrate is subjected to a pad-less processing process (as shown in FIG. 1 ), inclusive of the steps of rotating the lapping plate 11 in the direction of arrow R, supplying polishing oil slurry of this invention through the nozzle 13 to the surface of the lapping plate 11 , pressing the surface of the hard crystal substrate W held by the work holder 12 onto the surface of the lapping plate 11 and rotating the work holder 12 holding the hard crystal substrate W in the direction of arrow r.
- a pad-less processing process as shown in FIG. 1 , inclusive of the steps of rotating the lapping plate 11 in the direction of arrow R, supplying polishing oil slurry of this invention through the nozzle 13 to the surface of the lapping plate 11 , pressing the surface of the hard crystal substrate W held by the work holder 12 onto the surface of the lapping plate 11 and rotating the work holder 12 holding the hard crystal substrate W in the direction of arrow r.
- FIG. 3 shows the lapping plate 11 used in this finishing process, made of a soft metallic material (such as tin or a tin alloy).
- Spiral grooves shown by symbol g) with depth (indicated by symbol d) in the range of 15 nm-30 ⁇ m are formed on the surface (shown by symbol s) with average surface roughness (Ra) of 10 nm-50 nm, having a center matching the axis of rotation (shown at 14 in FIG. 1 ).
- These grooves (g) are sectionally V-shaped with the inner surfaces having a slope ⁇ within the range of 30°-90°.
- the pitch (indicated by symbol p) of the grooves (g) is 0.05 mm-0.2 mm.
- FIG. 6 shows a graph of particle size distribution of the artificial diamond clusters in the polishing oil slurry of Test Example 1 and their microscopic (SEM and TEM) photographs.
- the first rough polishing step was carried out by the pad-less polishing method.
- the lapping plate was rotated and polishing slurry was supplied to its surface.
- the surface of a GaN substrate held by the work holder was pressed onto the surface of the lapping plate and the work holder was rotated to carry out the first rough polishing of the target surface.
- the conditions of this process were as shown in Table 2 below.
- a tin plate of diameter 15 inches was used as the lapping plate with its surface polished so as to have the average surface roughness of 20 nm and spiral grooves formed thereon with the center matching the axis of its rotation.
- the grooves were sectionally V-shaped with a depth of 100 ⁇ m and having inner surface sloped at an angle of 60°.
- the pitch of the grooves was 0.3 mm.
- the polishing slurry was as described in Table 4 below, having polycrystalline diamond particles with average size D50 of 3 ⁇ m dispersed in an oil dispersant.
- FIG. 4 shows a graph of particle size distribution of these artificial diamond particles and their microscopic (SEM) photograph.
- the second rough polishing step was also carried out by the pad-less polishing method.
- the lapping plate was rotated, polishing slurry was supplied to its surface, the surface of the GaN substrate held by the work holder was pressed onto the surface of the lapping plate and the work holder was rotated so as to carry out the second rough polishing process.
- FIG. 2 also shows the conditions of this second rough polishing step.
- paraffin hydrocarbons were used again, as was the case after the first rough polishing step, to wash away the abrading particles, alcohols are used to rinse the GaN substrate, and the average surface roughness (Ra) and the surface waviness (Wa) of the GaN substrate were measured by using a commercially available apparatus for the measurement (Product name: NewView 5000 produced by Zygo Company) under the conditions shown in Table 3 below.
- the same lapping plate as used in the first rough polishing was used also for the second rough polishing.
- the polishing slurry was as described in Table 5 below, having polycrystalline diamond particles with average size D50 of 1 ⁇ m dispersed in an oil dispersant of the same kind as used for the first rough polishing step.
- FIG. 5 shows a graph of particle size distribution of these artificial diamond particles and their microscopic (SEM) photograph.
- the finishing step was also carried out by the pad-less polishing method.
- the lapping plate was rotated, polishing slurry was supplied to its surface, the surface of the GaN substrate held by the work holder was pressed onto the surface of the lapping plate and the work holder was rotated so as to carry out the finishing process.
- Table 2 also shows the conditions of this finishing step.
- a tin plate of diameter 15 inches was used as the lapping plate with its surface polished so as to have the average surface roughness of 20 nm and spiral grooves formed thereon with the center matching the axis of its rotation.
- the grooves were sectionally V-shaped with a depth of 20 nm and having inner surface sloped at an angle of 60°.
- the pitch of the grooves was 0.1 mm.
- paraffin hydrocarbons were used again to wash off the abrading particles, alcohols were used for rinsing the GaN substrate and the average surface roughness (Ra) and the surface waviness (Wa) of the GaN substrate were measured by using a commercially available apparatus for the measurement (Product name: NewView 5000 produced by Zygo Company) under the conditions shown in Table 3 above.
- Polishing oil slurry of Comparison Example 1 contains as abrading particles polycrystalline diamond particles with nearly the same average size D50 of 30 nm as the artificial diamond clusters of Test Examples 1.
- the composition of polishing oil slurry of Comparison Example 1 is shown in Table 6 below.
- FIG. 7 shows a graph of particle size distribution of the artificial diamond particles in the polishing oil slurry of Comparison Example 1 and their microscopic (SEM and TEM) photographs. This polishing oil slurry of Comparison Example 1 was used to carry out the finishing process on a GaN substrate of diameter 2 inches.
- the average particle size D50 of the artificial diamond clusters is shown here by the measured value of the dispersion inside pure water.
- the measurement was made with a commercially available apparatus for the measurement of particle size distribution (Product name: UPA-150 produced by Nikkiso Kabushiki Kaisha).
- the same lapping plate and the same polishing oil slurry (described in Table 4) described above for the first rough polishing step of Test Example 1 were used under the same conditions described in Table 2 to polish the GaN substrate by the pad-less method.
- paraffin hydrocarbons were used to wash off the abrading particles
- alcohols were used to rinse the GaN substrate
- the average surface roughness (Ra) and the surface waviness (Wa) of the GaN substrate were thereafter measured by using a commercially available apparatus for the measurement (Product name: NewView 5000 produced by Zygo Company) under the conditions shown in Table 3 above.
- the same lapping plate and the same polishing oil slurry (described in Table 5) described above for the second rough polishing of Test Example 1 were used under the same conditions described in Table 2 to polish the GaN substrate by the pad-less method.
- paraffin hydrocarbons were used to wash off the abrading particles
- alcohols were used to rinse the GaN substrate
- the average surface roughness (Ra) and the surface waviness (Wa) of the GaN substrate were thereafter measured by using a commercially available apparatus for the measurement (Product name: NewView 5000 produced by Zygo Company) under the conditions shown in Table 3 above.
- the finishing process was also carried out by the pad-less polishing method as for the finishing process in Test Example 1.
- the same lapping plate used for the finishing process in Test Example 1 was rotated, the polishing oil slurry of Comparison Example 1 was supplied to its surface, the surface of the GaN substrate held by the work holder was pressed onto the surface of the lapping plate, and the work holder was rotated to carry out the finishing process on the GaN substrate under the conditions described in Table 2.
- paraffin hydrocarbons were used to wash off the abrading particles, alcohols were used to rinse the GaN substrate, and the average surface roughness (Ra) and the surface waviness (Wa) of the GaN substrate were thereafter measured by using a commercially available apparatus for the measurement (Product name: NewView 5000 produced by Zygo Company) under the conditions shown in Table 3 above.
- Polishing slurry of Comparison Example 2 is water-based and contains artificial diamond clusters of Test Examples 1 as abrading particles.
- the composition of the polishing slurry of Comparison Example 2 is shown in Table 7 below. This slurry was produced by mixing a dispersant with water, adding abrading particles to this liquid mixture (water-based dispersant) and dispersing the abrading particles in this water-based dispersant by using a homogenizer. A GaN substrate of diameter 2 inches was subjected to a finishing process by using this water-based polishing slurry. It is to be noted that polishing oil slurry was used in the first and second rough polishing steps of Test Example 1 and Comparison Example 1 but water-based polishing slurry was used in the first and second rough polishing steps of Comparison Example 2.
- the same lapping plate for the first rough polishing step of Test Example 1 was used under the same conditions described in Table 2 to polish a GaN substrate by the pad-less method.
- the GaN substrate was rinsed with pure water and the average surface roughness (Ra) and the surface waviness (Wa) of the GaN substrate were thereafter measured by using a commercially available apparatus for the measurement (Product name: NewView 5000 produced by Zygo Company) under the conditions shown in Table 3 above.
- FIG. 4 shows a graph of particle size distribution of these polycrystalline diamond particles and their microscopic (SEM) photograph.
- the same lapping plate described above for the second rough polishing of Test Example 1 was used under the same conditions described in Table 2 to polish the GaN substrate by the pad-less method.
- the GaN substrate was rinsed with pure water and the average surface roughness (Ra) and the surface waviness (Wa) of the GaN substrate were thereafter measured by using a commercially available apparatus for the measurement (Product name: NewView 5000 produced by Zygo Company) under the conditions shown in Table 3 above.
- FIG. 5 shows a graph of particle size distribution of these polycrystalline diamond particles and their microscopic (SEM) photograph.
- the finishing process was also carried out by the pad-less polishing method as for the finishing process in Test Example 1.
- the same lapping plate used for the finishing process in Test Example 1 was rotated, the polishing oil slurry of Comparison Example 2 was supplied to its surface, the surface of the GaN substrate held by the work holder was pressed onto the surface of the lapping plate, and the work holder was rotated to carry out the finishing process on the GaN substrate under the conditions described in Table 2.
- the GaN substrate was rinsed with pure water and the average surface roughness (Ra) and the surface waviness (Wa) of the GaN substrate were thereafter measured by using a commercially available apparatus for the measurement (Product name: NewView 5000 produced by Zygo Company) under the conditions shown in Table 3 above.
- Results of a comparison among Test Example 1 and Comparison Examples 1 and 2 are shown in Table 8 below.
- the surface conditions of the GaN substrate after the first rough polishing step, after the second rough polishing step and after the finishing step in Test Example 1 as described in Table 8 are shown respectively in FIGS. 8 , 9 and 10 .
- the surface conditions of the GaN substrate after the first rough polishing step, after the second rough polishing step and after the finishing step in Comparison Example 1 as described in Table 8 are shown respectively in FIGS. 11 , 12 and 13 .
- the surface conditions of the GaN substrate after the first rough polishing step, after the second rough polishing step and after the finishing step in Comparison Example 2 as described in Table 8 are shown respectively in FIGS. 14 , 15 and 16 .
- FIG. 10A shows that no scratches are formed on the surface of the GaN substrate in Test Example 1, while scratches are formed in Comparison Examples 1 and 2, as shown in FIGS. 13A and 16A .
- Table 8 also indicates that average surface roughness (Ra) of 0.2 nm or less is possible by Test Example 1 with the surface waviness (Wa) significantly reduced from Comparison Examples 1 and 2.
- the surface of a GaN substrate can be polished to be very flat (low in Wa) and very smooth (low in Ra) without scratches formed thereon according to Test Example 1.
- a finishing step was carried out on a SiC substrate of diameter 2 inches by using the polishing oil slurry of Test Example 1 described above.
- the first rough polishing step was carried out by the pad-less polishing method as in Test Example 1 under the conditions shown in Table 2.
- paraffin hydrocarbons were used to wash away the abrading particles and the GaN substrate was rinsed with alcohols.
- the average surface roughness (Ra) and the surface waviness (Wa) of the surface of the GaN substrate were measured by means of a commercially available measurement apparatus (Product name: NewView 5000 produced by Zygo Company) under the conditions shown in Table 3 above.
- a lapping plate as used in the first rough polishing step of Test Example 1 and the same polishing oil slurry described in Table 4 above were used.
- the second rough polishing step was carried out by the pad-less method under the same conditions as described in Table 2 for the second rough polishing step of Test Example 1.
- paraffin hydrocarbons were used to wash away the abrading particles and the GaN substrate was rinsed with alcohols.
- the average surface roughness (Ra) and the surface waviness (Wa) of the surface of the GaN substrate were measured by means of a commercially available measurement apparatus (Product name: NewView 5000 produced by Zygo Company) under the conditions shown in Table 3 above.
- a lapping plate as used in the first rough polishing step and the same polishing oil slurry used in the second rough polishing of Test Example 1 described in Table 5 above were used.
- the finishing step was carried out also by the pad-less polishing method as in the finishing step of Test Example 1 under the conditions described in Table 2 above.
- a lapping plate and polishing slurry as used in the finishing step of Test Example 1 were used.
- paraffin hydrocarbons were used to wash away the abrading particles and the GaN substrate was rinsed with alcohols. Thereafter, the average surface roughness (Ra) and the surface waviness (Wa) of the surface of the GaN substrate were measured by means of a commercially available measurement apparatus (Product name: NewView 5000 produced by Zygo Company) under the conditions shown in Table 3 above.
- Results of Test Example 2 are shown in Table 9 below.
- the surface condition of the GaN substrate after the first rough polishing step, after the second rough polishing step and after the finishing step in Test Example 2 as described in Table 9 are shown respectively in FIGS. 17 , 18 and 19 .
- FIG. 19A indicates that no scratches are formed on the surface of the SiC according to Test Example 2.
- Table 9 further indicates that average surface roughness (Ra) of 0.2 nm or less is possible according to Test Example 2 with reduced surface waviness (Wa).
- the surface of a SiC substrate can be polished to be very flat (low in Wa) and very smooth (low in Ra) without scratches formed thereon according to Test Example 2.
Abstract
A hard crystal substrate such as a GaN substrate or a SiC substrate is polished by using polishing oil slurry having abrading particles of artificial diamond clusters dispersed in a dispersant. The artificial diamond clusters include approximately spherical agglomerate particles with average particle size D50 of 20 nm or more and 50 nm or less, having primary particles with particle diameters of 2 nm or more and 10 nm or less. A rough polishing process is carried out first such that an average surface roughness of 0.5 nm or more and 1 nm or less is obtained, followed by a finishing process such that the average surface roughness of said surface becomes 0.2 nm or less.
Description
- This is a divisional of application Ser. No. 11/946,531 filed Nov. 28, 2007, currently pending.
- This invention relates to polishing oil slurry for use in a method of polishing a hard crystal substrate such as gallium nitride (GaN) and silicon carbide (SiC) substrates.
- GaN (Group III nitride semiconductor) and crystalline material of SiC are wide band-gap semiconductors, and a GaN substrate is usually manufactured by forming a GaN film on a sapphire substrate by a halide vapor phase epitaxy (HVPE) method, as disclosed in Japanese Patent Publication Tokkai 9-335580. Devices may be formed on this GaN film, for example, to produce a short-wavelength green or blue light-emitting elements and a purple-color semiconductor laser. On the other hand, SiC is coming to be used as the substrate of a high-function power device since it can be used in high-output, high-frequency and high-temperature operations and has a high insulation breakdown field.
- Since GaN substrates and SiC substrates are hard crystal substrates and since devices of specified kinds are formed on the surface of such a hard crystal substrate, high levels of flatness and smoothness are required of such surfaces.
- Conventional methods of polishing the surface of such a hard crystal substrate were to use free polishing particles, initially carrying out a rough polishing process by using somewhat larger abrading particles and reducing stepwise the size of the abrading particles such that the substrate surface will become flat and smooth, as disclosed in Japanese Patent Publication Tokkai 2001-322899.
- Polishing by free abrading particles is carried out by rotating a metallic lapping plate, supplying polishing slurry on the surface of this lapping plate, pressing the surface of a substrate held by a work holder onto the surface of the lapping plate and causing this work holder to rotate. In conventional polishing methods by free abrading particles, aqueous slurry with abrading particles dispersed in an aqueous dispersant has been used.
- In conventional polishing methods by free abrading particles, furthermore, the technical problem has been to reduce the required polishing time, and the limit reachable by such methods has been to polish the target surface of a substrate to an average surface roughness (Ra) of about 0.4 nm. By such a conventional polishing method, however, unwanted scratch lines are formed, as shown in
FIG. 16A , and it is presently not possible to sufficiently mirror-polish the surface of a hard crystal substrate. - It is therefore an object of this invention to provide polishing oil slurry for polishing the surface of a hard crystal substrate to a mirror surface with average surface roughness of 0.2 nm or less.
- Polishing oil slurry of this invention may be characterized as comprising abrading particles including artificial diamond clusters and an oil dispersant for dispersing these abrading particles, and the hard crystal substrate to be polished may be a GaN or SiC substrate.
- In the above, the artificial diamond clusters comprise approximately spherical agglomerate particles with average particle diameter D50 of 20 nm or more and 50 nm or less, having primary particles with particle diameters of 2 nm or more and 10 nm or less. The oil dispersant includes synthetic isoparaffin hydrocarbons.
- A method of this invention for polishing a hard crystal substrate may be characterized as comprising a rough polishing process of polishing a surface of the substrate such that it will come to have an average surface roughness (Ra) of 0.5 nm or more and 1 nm or less and a finishing process, carried out after the rough polishing process, of polishing the substrate surface such that its average surface roughness (Ra) becomes 0.2 nm or less.
- In the above, the finishing process comprises the steps of rotating a lapping plate, supplying the polishing oil slurry of this invention described above to a surface of this lapping plate, pressing the surface of the hard crystal substrate onto the surface of the lapping plate and rotating the hard crystal substrate. The lapping plate comprises a soft metal such as tin or its alloy, having a groove formed thereon. The groove is preferably spiral, centered around the axis of rotation of the lapping plate and being sectionally V-shaped.
- The rough polishing process preferably comprises a first rough polishing step of polishing the surface of the hard crystal substrate such that its average surface roughness (Ra) becomes 1 nm or more and 3 nm or less and a second rough polishing step, carried out after the first rough polishing step, of polishing the substrate surface such that its average surface roughness (Ra) becomes 0.5 nm or more and 1 nm or less.
- The merit of the invention is that the surface of a hard crystal substrate can be mirror-polished so as to have an average surface roughness (Ra) of 0.2 nm or less without forming any scratches.
-
FIG. 1 is a side view of an apparatus for pad-less polishing. -
FIG. 2A is a schematic sectional view of a lapping plate used in the rough polishing process, and -
FIG. 2B is an enlarged photograph of a portion of its surface. -
FIG. 3A is a schematic sectional view of a lapping plate used in the finishing process, and -
FIG. 3B is an enlarged photograph of a portion of its surface. -
FIG. 4 is a graph of particle size distribution of artificial diamond particles used in the first rough polishing step of Test Examples 1 and 2 and their microscopic (SEM) photograph. -
FIG. 5 is a graph of particle size distribution of artificial diamond particles used in the second rough polishing step of Test Examples 1 and 2 and their microscopic (SEM) photograph. -
FIG. 6 is a graph of particle size distribution of the artificial diamond clusters with average size of 27 nm in the polishing oil slurry of Test Example 1 and their microscopic (SEM and TEM) photographs. -
FIG. 7 is a graph of particle size distribution of the artificial diamond clusters with average size of 30 nm in the polishing oil slurry of Comparison Example 1 and their microscopic (TEM) photograph. -
FIG. 8 includesFIGS. 8A and 8B which are respectively an enlarged photograph of a plan view and a diagonal view of the surface of the GaN substrate after the first rough polishing step of Test Example 1. -
FIG. 9 includesFIGS. 9A and 9B which are respectively an enlarged photograph of a plan view and a diagonal view of the surface of the GaN substrate after the second rough polishing step of Test Example 1. -
FIG. 10 includesFIGS. 10A and 10B which are respectively an enlarged photograph of a plan view and a diagonal view of the surface of the GaN substrate after the finishing step of Test Example 1. -
FIG. 11 includesFIGS. 11A and 11B which are respectively an enlarged photograph of a plan view and a diagonal view of the surface of the GaN substrate after the first rough polishing step of Comparison Example 1. -
FIG. 12 includesFIGS. 12A and 12B which are respectively an enlarged photograph of a plan view and a diagonal view of the surface of the GaN substrate after the second rough polishing step of Comparison Example 1. -
FIG. 13 includesFIGS. 13A and 13B which are respectively an enlarged photograph of a plan view and a diagonal view of the surface of the GaN substrate after the finishing step of Comparison Example 1. -
FIG. 14 includesFIGS. 14A and 14B which are respectively an enlarged photograph of a plan view and a diagonal view of the surface of the GaN substrate after the first rough polishing step of Comparison Example 2. -
FIG. 15 includesFIGS. 15A and 15B which are respectively an enlarged photograph of a plan view and a diagonal view of the surface of the GaN substrate after the second rough polishing step of Comparison Example 2. -
FIG. 16 includesFIGS. 16A and 16B which are respectively an enlarged photograph of a plan view and a diagonal view of the surface of the GaN substrate after the finishing step of Comparison Example 2. -
FIG. 17 includesFIGS. 17A and 17B which are respectively an enlarged photograph of a plan view and a diagonal view of the surface of the GaN substrate after the first rough polishing step of Test Example 2. -
FIG. 18 includesFIGS. 18A and 18B which are respectively an enlarged photograph of a plan view and a diagonal view of the surface of the GaN substrate after the second rough polishing step of Test Example 2. -
FIG. 19 includesFIGS. 19A and 19B which are respectively an enlarged photograph of a plan view and a diagonal view of the surface of the GaN substrate after the finishing step of Test Example 2. - The invention relates to polishing oil slurry for polishing a hard crystal substrate which may preferably be a GaN substrate or a SiC substrate.
- Polishing oil slurry of this invention comprises abrading particles and an oil dispersant that disperses these abrading particles, and the abrading particles according to this invention include artificial diamond clusters.
- The oil dispersant according to this invention includes oils, having the function of forming an oily film on the surfaces of the abrading particles and improving the particle lubricity on the target surface to be polished. Examples of the oil include paraffin hydrocarbons and may preferably include synthesized isoparaffin hydrocarbons.
- The oil dispersants according to this invention include non-ionic surfactants as dispersants for improving dispersion of abrading particles and preferably include higher aliphatic monoglycerides or higher aliphatic diglycerides.
- The artificial diamond clusters according to this invention comprise approximately spherical agglomerate particles with average size D50 of 20 nm or more and 50 nm or less, having primary particles with particle diameters of 2 nm or more and 10 nm or less. Since the particle size distribution of the abrading particles dispersed in an oil dispersant cannot be measured, the average particle size D50 of the artificial diamond clusters is shown here by the measured value of the dispersion inside pure water.
- The artificial diamond clusters of this invention comprise artificial diamond obtained by an explosion synthesis method (also known as a shockwave method) of a known kind. There are two kinds of explosion synthesis method. One is to use graphite powders as the material for diamond and to compress these graphite powders at a high temperature by providing a shock with the energy of explosion to thereby generate diamond artificially. The other method is to explode an explosive such as TNT or RDX and to artificially convert the carbon (as the material for diamond) contained in the explosive into diamond by the shock caused by the energy of explosion.
- Since the reaction product that is obtained by such an explosion synthesis method contains carbon materials that have not reacted as well as metallic impurities, such obtained product is chemically treated with nitric acid, sulfuric acid, hydrochloric acid or a mixture thereof to dissolve and remove these impurities. After the impurities are removed, water is used for washing.
- The artificial diamond thus obtained comprises primary particles and agglomerate particles of these primary particles. The diameters of the primary particles are within the range of 2 nm-20 nm, and they have the shape with more roundness than monocrystalline and polycrystalline diamond particles. Diamond films that have not reacted and diamond-like carbon films are formed on the surfaces of the primary particles. The agglomerate particles are formed as the primary particles agglomerate into a nearly spherical shape at the time of the explosion synthesis, and these agglomerate particles are referred to as artificial diamond clusters.
- Artificial diamond clusters are more easily breakable than agglomerate particles obtained by agglomerating natural (monocrystalline and polycrystalline) diamond particles within a liquid. In other words, if artificial diamond clusters are pressed to the surface of a target object to be polished, those of larger sizes break up to an appropriate degree such that the number of scratches formed by artificial diamond clusters can be reduced.
- If the size of artificial diamond clusters is too large, however, the surface of the target object to be polished is polished too deeply as the clusters break up, and this may result in unwanted scratches. Since the average surface roughness of the target surface to be polished is 0.2 nm or less according to this invention, artificial diamond particles exceeding 50 nm are excluded. For this purpose, the product obtained by the explosion synthesis method is crushed by means of a ball mill or the like, the aforementioned chemical treatment is carried out, it is washed with water and then a centrifugal separator is used for sorting to collect artificial diamond particles of a desired size.
- Polishing oil slurry of this invention is produced by mixing oil with a dispersant and causing artificial diamond clusters to be dispersed in this liquid mixture. The amount of the dispersant to be used is 1 weight % or more and 10 weight % or less with respect to the whole of the oil. The amount of the artificial diamond cluster is 0.1 weight % or more and 3 weight % or less with respect to the whole of the polishing oil slurry.
- The method of this invention for polishing a hard crystal substrate comprises a rough polishing process for polishing a surface of the hard crystal substrate such that the average surface roughness (Ra) of the surface becomes 0.5 nm or more and 1 nm or less and a finishing process for polishing the surface after the rough polishing process such that its average surface roughness (Ra) becomes 0.2 nm or less.
- The target surface of the hard crystal substrate is polished in the rough polishing process such that the surface waviness (Wa) becomes 1 nm or less. This is because the correction of the surface waviness becomes difficult in the subsequent finishing process if it exceeds 1 nm because the stock removal is small during the finishing process.
- The rough polishing process is carried out by a known method of tape polishing, pad polishing or pad-less polishing such that the average surface roughness (Ra) of the target surface of the hard crystal substrate becomes 0.5 nm or more and 1 nm or less.
- The tape polishing method is carried out by rotating the substrate attached to a spindle, supplying polishing slurry on the surface of this substrate, pressing a tape of a woven or non-woven cloth or a foamed material and causing it to run. The pad polishing method is carried out by rotating a lapping plate with a pad of a woven or non-woven cloth or a foamed material adhered to its surface, supplying polishing slurry to the surface of this pad, pressing the surface of the substrate thereto and causing it to rotate.
- The pad-less polishing method may be carried out by using an
apparatus 10 shown inFIG. 1 , rotating itslapping plate 11 in the direction of arrow R with no pad on its surface, supplying polishing slurry through anozzle 13 directly to the surface of the lappingplate 11, pressing the surface of the substrate W held by awork holder 12 onto the surface of the lappingplate 11 and rotating thework holder 12 in the direction of arrow r. - In the above, the polishing slurry may be water-based or oil-based, having abrading particles dispersed in a water-based or oil-based dispersing medium.
- The abrading particles may be particles of polycrystalline diamond, monocrystalline diamond, aluminum oxide (Al2O3), silicon oxide (SiO2), chromium oxide (Cr2O3) or cubic boron nitride (cBN). Of the above, polycrystalline diamond particles are preferable.
- Examples of water-based dispersing medium include water and aqueous solutions obtained by adding a dispersing agent such as glycols and alcohols to water. Examples of oil-based dispersing medium include oils and those obtained by adding a dispersing agent such as paraffin hydrocarbons to oil.
- The rough polishing process may consist of a single step or two or more steps of rough polishing process. If the target average surface roughness (Ra) (of 0.5 nm or more and 1 nm or less) is to be attained by a single step of rough polishing process, it will take a long time and the surface waviness (Wa) becomes large. If the rough polishing process includes three or more steps, on the other hand, the process becomes too cumbersome.
- According to a preferred embodiment of this invention, the rough polishing process consists of a first step of polishing the target surface of a hard crystal substrate such that its average surface roughness (Ra) becomes 1 nm or more and 3 nm or less and a second step of polishing (carried out after the first step) the target surface such that its average surface roughness (Ra) becomes 0.5 nm or more and 1 nm or less).
- In the first of the rough polishing steps, the hard crystal substrate is subjected to tape polishing, pad polishing or pad-less polishing (such as shown in
FIG. 1 ) by using water-based or oil-based polishing slurry containing abrading particles (preferably comprising polycrystalline diamond particles) with average size D50 of 3 μm or more and 5 μm or less. - In the second rough polishing step, the hard crystal substrate is subjected to tape polishing, pad polishing or pad-less polishing by using water-based or oil-based polishing slurry containing abrading particles (preferably comprising polycrystalline diamond particles) with average size D50 of 0.5 μm or more and 3 μm or less.
- Pad-less polishing is particularly preferred both for the first and second rough polishing steps. The lapping plate to be used in such pad-less polishing process is shown in
FIG. 2 . This lappingplate 11 is made of a soft metallic material (such as tin or a tin alloy), and spiral grooves (shown by symbol g) with depth (indicated by symbol d) in the range of 50 nm-100 nm are formed on the surface (shown by symbol s) with average surface roughness (Ra) of 1 nm-50 nm, having a center matching the axis of rotation (shown at 14 inFIG. 1 ). These grooves (g) are sectionally V-shaped with the inner surfaces having a slope θ within the range of 30°-90°. The pitch (indicated by symbol p) of the grooves (g) is 0.2 mm-0.5 mm. - In the finishing process, the target surface of the hard crystal substrate is subjected to a pad-less processing process (as shown in
FIG. 1 ), inclusive of the steps of rotating the lappingplate 11 in the direction of arrow R, supplying polishing oil slurry of this invention through thenozzle 13 to the surface of the lappingplate 11, pressing the surface of the hard crystal substrate W held by thework holder 12 onto the surface of the lappingplate 11 and rotating thework holder 12 holding the hard crystal substrate W in the direction of arrow r. -
FIG. 3 (consisting ofFIGS. 3A and 3B ) shows the lappingplate 11 used in this finishing process, made of a soft metallic material (such as tin or a tin alloy). Spiral grooves (shown by symbol g) with depth (indicated by symbol d) in the range of 15 nm-30 μm are formed on the surface (shown by symbol s) with average surface roughness (Ra) of 10 nm-50 nm, having a center matching the axis of rotation (shown at 14 inFIG. 1 ). These grooves (g) are sectionally V-shaped with the inner surfaces having a slope θ within the range of 30°-90°. The pitch (indicated by symbol p) of the grooves (g) is 0.05 mm-0.2 mm. - The invention is described next by way of test and comparison examples.
- Polishing oil slurry with composition as shown in Table 1 below was used in Test Example 1 to carry out a finishing process on a GaN substrate with diameter=2 inches.
-
TABLE 1 Abrading particles Artificial diamond clusters: 0.5 weight % Diameter of primary particles = 4 nm-10 nm Average size of agglomerate particles D50 = 27 nm Oil-based dispersing Oil Synthetic isoparaffin 95.5 weight % medium hydrocarbons Dispersing agent Non-ionic surfactant (higher 4.0 weight % aliphatic monoglyceride - In the above, the artificial diamond clusters were those manufactured by the explosion synthesis method, including approximately spherically shaped agglomerate particles with average size D50=27 nm with primary particles of diameters in the range of 4 nm-10 nm.
- Since the particle size distribution of the abrading particles dispersed in the oil dispersant cannot be measured, the average particle size D50 of the artificial diamond clusters is shown here by the measured value of the dispersion inside pure water. The measurement was made with a commercially available apparatus for the measurement of particle size distribution (Product name: UPA-150 produced by Nikkiso Kabushiki Kaisha).
FIG. 6 shows a graph of particle size distribution of the artificial diamond clusters in the polishing oil slurry of Test Example 1 and their microscopic (SEM and TEM) photographs. - The first rough polishing step was carried out by the pad-less polishing method. The lapping plate was rotated and polishing slurry was supplied to its surface. The surface of a GaN substrate held by the work holder was pressed onto the surface of the lapping plate and the work holder was rotated to carry out the first rough polishing of the target surface. The conditions of this process were as shown in Table 2 below.
-
TABLE 2 Rotational speed of lapping plate 60 rpm Rotational speed of work holder 40 rpm Polishing pressure 0.5 kg/cm2 Supply rate of slurry 3 ml/minute Polishing time First rough polishing 40 minutes Second rough polishing 40 minutes Finishing 60 minutes - After the first rough polishing step, paraffin hydrocarbons were used to wash away the abrading particles and the GaN substrate was washed and rinsed with alcohols. Thereafter, the average surface roughness (Ra) and the surface waviness (Wa) of the surface of the GaN substrate were measured by means of a commercially available measurement apparatus (Product name: NewView 5000 produced by Zygo Company) under the conditions shown in Table 3 below.
-
TABLE 3 Average surface Surface waviness roughness (Ra) (Wa) Magnification of x10 x10 object lens Magnification of x0.8 x0.8 intermediate lens High pass filter 0.05 mm — Band pass filter — 0.05 mm-0.5 mm - A tin plate of
diameter 15 inches was used as the lapping plate with its surface polished so as to have the average surface roughness of 20 nm and spiral grooves formed thereon with the center matching the axis of its rotation. The grooves were sectionally V-shaped with a depth of 100 μm and having inner surface sloped at an angle of 60°. The pitch of the grooves was 0.3 mm. - The polishing slurry was as described in Table 4 below, having polycrystalline diamond particles with average size D50 of 3 μm dispersed in an oil dispersant.
FIG. 4 shows a graph of particle size distribution of these artificial diamond particles and their microscopic (SEM) photograph. -
TABLE 4 Abrading particles Polycrystalline diamond particles: 0.5 weight % Average particle size D50: 3 μm Oil dispersant Oil Synthetic isoparaffin 95.5 weight % hydrocarbons Dispersant Non-ionic surfactant 4.0 weight % (higher aliphatic monoglycerides) - The second rough polishing step was also carried out by the pad-less polishing method. As in the first rough polishing step, the lapping plate was rotated, polishing slurry was supplied to its surface, the surface of the GaN substrate held by the work holder was pressed onto the surface of the lapping plate and the work holder was rotated so as to carry out the second rough polishing process.
FIG. 2 also shows the conditions of this second rough polishing step. - After this second rough polishing step, paraffin hydrocarbons were used again, as was the case after the first rough polishing step, to wash away the abrading particles, alcohols are used to rinse the GaN substrate, and the average surface roughness (Ra) and the surface waviness (Wa) of the GaN substrate were measured by using a commercially available apparatus for the measurement (Product name: NewView 5000 produced by Zygo Company) under the conditions shown in Table 3 below.
- The same lapping plate as used in the first rough polishing was used also for the second rough polishing. The polishing slurry was as described in Table 5 below, having polycrystalline diamond particles with average size D50 of 1 μm dispersed in an oil dispersant of the same kind as used for the first rough polishing step.
FIG. 5 shows a graph of particle size distribution of these artificial diamond particles and their microscopic (SEM) photograph. -
TABLE 5 Abrading particles Polycrystalline diamond particles: 0.5 weight % Average particle size D50: 1 μm Oil dispersant Oil Synthetic isoparaffin 95.5 weight % hydrocarbons Dispersant Non-ionic surfactant 4.0 weight % (higher aliphatic monoglycerides) - The finishing step was also carried out by the pad-less polishing method. As in the first and second rough polishing steps, the lapping plate was rotated, polishing slurry was supplied to its surface, the surface of the GaN substrate held by the work holder was pressed onto the surface of the lapping plate and the work holder was rotated so as to carry out the finishing process. Table 2 also shows the conditions of this finishing step.
- A tin plate of
diameter 15 inches was used as the lapping plate with its surface polished so as to have the average surface roughness of 20 nm and spiral grooves formed thereon with the center matching the axis of its rotation. The grooves were sectionally V-shaped with a depth of 20 nm and having inner surface sloped at an angle of 60°. The pitch of the grooves was 0.1 mm. - After this finishing step, paraffin hydrocarbons were used again to wash off the abrading particles, alcohols were used for rinsing the GaN substrate and the average surface roughness (Ra) and the surface waviness (Wa) of the GaN substrate were measured by using a commercially available apparatus for the measurement (Product name: NewView 5000 produced by Zygo Company) under the conditions shown in Table 3 above.
- Polishing oil slurry of Comparison Example 1 contains as abrading particles polycrystalline diamond particles with nearly the same average size D50 of 30 nm as the artificial diamond clusters of Test Examples 1. The composition of polishing oil slurry of Comparison Example 1 is shown in Table 6 below.
FIG. 7 shows a graph of particle size distribution of the artificial diamond particles in the polishing oil slurry of Comparison Example 1 and their microscopic (SEM and TEM) photographs. This polishing oil slurry of Comparison Example 1 was used to carry out the finishing process on a GaN substrate of diameter 2 inches. -
TABLE 6 Abrading particles Polycrystalline diamond particles: 0.5 weight % Average particle size D50: 30 μm Oil dispersant Oil Synthetic isoparaffin 95.5 weight % hydrocarbons Dispersant Non-ionic surfactant 4.0 weight % (higher aliphatic monoglycerides) - In the above, as was the case in Test Example 1 discussed above, since the particle size distribution of the abrading particles dispersed in the oil dispersant cannot be measured, the average particle size D50 of the artificial diamond clusters is shown here by the measured value of the dispersion inside pure water. The measurement was made with a commercially available apparatus for the measurement of particle size distribution (Product name: UPA-150 produced by Nikkiso Kabushiki Kaisha).
- In the firsts rough polishing step, the same lapping plate and the same polishing oil slurry (described in Table 4) described above for the first rough polishing step of Test Example 1 were used under the same conditions described in Table 2 to polish the GaN substrate by the pad-less method. After the first rough polishing step, paraffin hydrocarbons were used to wash off the abrading particles, alcohols were used to rinse the GaN substrate, and the average surface roughness (Ra) and the surface waviness (Wa) of the GaN substrate were thereafter measured by using a commercially available apparatus for the measurement (Product name: NewView 5000 produced by Zygo Company) under the conditions shown in Table 3 above.
- In the second rough polishing step, the same lapping plate and the same polishing oil slurry (described in Table 5) described above for the second rough polishing of Test Example 1 were used under the same conditions described in Table 2 to polish the GaN substrate by the pad-less method. After the second rough polishing step, paraffin hydrocarbons were used to wash off the abrading particles, alcohols were used to rinse the GaN substrate, and the average surface roughness (Ra) and the surface waviness (Wa) of the GaN substrate were thereafter measured by using a commercially available apparatus for the measurement (Product name: NewView 5000 produced by Zygo Company) under the conditions shown in Table 3 above.
- The finishing process was also carried out by the pad-less polishing method as for the finishing process in Test Example 1. The same lapping plate used for the finishing process in Test Example 1 was rotated, the polishing oil slurry of Comparison Example 1 was supplied to its surface, the surface of the GaN substrate held by the work holder was pressed onto the surface of the lapping plate, and the work holder was rotated to carry out the finishing process on the GaN substrate under the conditions described in Table 2. After the finishing step, paraffin hydrocarbons were used to wash off the abrading particles, alcohols were used to rinse the GaN substrate, and the average surface roughness (Ra) and the surface waviness (Wa) of the GaN substrate were thereafter measured by using a commercially available apparatus for the measurement (Product name: NewView 5000 produced by Zygo Company) under the conditions shown in Table 3 above.
- Polishing slurry of Comparison Example 2 is water-based and contains artificial diamond clusters of Test Examples 1 as abrading particles. The composition of the polishing slurry of Comparison Example 2 is shown in Table 7 below. This slurry was produced by mixing a dispersant with water, adding abrading particles to this liquid mixture (water-based dispersant) and dispersing the abrading particles in this water-based dispersant by using a homogenizer. A GaN substrate of diameter 2 inches was subjected to a finishing process by using this water-based polishing slurry. It is to be noted that polishing oil slurry was used in the first and second rough polishing steps of Test Example 1 and Comparison Example 1 but water-based polishing slurry was used in the first and second rough polishing steps of Comparison Example 2.
-
TABLE 7 Abrading Artificial diamond clusters of 0.5 weight % particles Test Example 1 Water-based Pure water 55 weight % dispersant Dispersant Polyethylene glycol 400 16.8 weight % Polyethylene glycol 2000 23 weight % Ethylene glycol 5 weight % Glycerol 0.2 weight % - In the first rough polishing step of Comparison Example 2, the same lapping plate for the first rough polishing step of Test Example 1 was used under the same conditions described in Table 2 to polish a GaN substrate by the pad-less method. After the first rough polishing step, the GaN substrate was rinsed with pure water and the average surface roughness (Ra) and the surface waviness (Wa) of the GaN substrate were thereafter measured by using a commercially available apparatus for the measurement (Product name: NewView 5000 produced by Zygo Company) under the conditions shown in Table 3 above.
- Water-based polishing slurry having 0.5 weight % of polycrystalline diamond particles with average size D50 of 3 μm dispersed in pure water was used.
FIG. 4 shows a graph of particle size distribution of these polycrystalline diamond particles and their microscopic (SEM) photograph. - In the second rough polishing step, the same lapping plate described above for the second rough polishing of Test Example 1 was used under the same conditions described in Table 2 to polish the GaN substrate by the pad-less method. After the second rough polishing step, the GaN substrate was rinsed with pure water and the average surface roughness (Ra) and the surface waviness (Wa) of the GaN substrate were thereafter measured by using a commercially available apparatus for the measurement (Product name: NewView 5000 produced by Zygo Company) under the conditions shown in Table 3 above.
- Water-based polishing slurry having 0.5 weight % of polycrystalline diamond particles with average size D50 of 1 μm dispersed in pure water was used.
FIG. 5 shows a graph of particle size distribution of these polycrystalline diamond particles and their microscopic (SEM) photograph. - The finishing process was also carried out by the pad-less polishing method as for the finishing process in Test Example 1. The same lapping plate used for the finishing process in Test Example 1 was rotated, the polishing oil slurry of Comparison Example 2 was supplied to its surface, the surface of the GaN substrate held by the work holder was pressed onto the surface of the lapping plate, and the work holder was rotated to carry out the finishing process on the GaN substrate under the conditions described in Table 2. After the finishing step, the GaN substrate was rinsed with pure water and the average surface roughness (Ra) and the surface waviness (Wa) of the GaN substrate were thereafter measured by using a commercially available apparatus for the measurement (Product name: NewView 5000 produced by Zygo Company) under the conditions shown in Table 3 above.
- Results of a comparison among Test Example 1 and Comparison Examples 1 and 2 are shown in Table 8 below. The surface conditions of the GaN substrate after the first rough polishing step, after the second rough polishing step and after the finishing step in Test Example 1 as described in Table 8 are shown respectively in
FIGS. 8 , 9 and 10. The surface conditions of the GaN substrate after the first rough polishing step, after the second rough polishing step and after the finishing step in Comparison Example 1 as described in Table 8 are shown respectively inFIGS. 11 , 12 and 13. The surface conditions of the GaN substrate after the first rough polishing step, after the second rough polishing step and after the finishing step in Comparison Example 2 as described in Table 8 are shown respectively inFIGS. 14 , 15 and 16. -
TABLE 8 After first rough After second After finishing polishing step rough polishing step step Ra Wa Ra Wa Ra Wa (nm) (nm) (nm) (nm) (nm) (nm) Test Example 1 1.10 1.00 0.48 0.44 0.15 0.08 Comparison 1.10 1.20 0.46 0.40 0.28 0.17 Example 1 Comparison 3.15 1.56 1.02 0.94 0.47 0.15 Example 2 - If the conditions after the finishing steps are compared,
FIG. 10A shows that no scratches are formed on the surface of the GaN substrate in Test Example 1, while scratches are formed in Comparison Examples 1 and 2, as shown inFIGS. 13A and 16A . - Table 8 also indicates that average surface roughness (Ra) of 0.2 nm or less is possible by Test Example 1 with the surface waviness (Wa) significantly reduced from Comparison Examples 1 and 2. In other words, the surface of a GaN substrate can be polished to be very flat (low in Wa) and very smooth (low in Ra) without scratches formed thereon according to Test Example 1.
- A finishing step was carried out on a SiC substrate of diameter 2 inches by using the polishing oil slurry of Test Example 1 described above.
- The first rough polishing step was carried out by the pad-less polishing method as in Test Example 1 under the conditions shown in Table 2. After the first rough polishing step, paraffin hydrocarbons were used to wash away the abrading particles and the GaN substrate was rinsed with alcohols. Thereafter, the average surface roughness (Ra) and the surface waviness (Wa) of the surface of the GaN substrate were measured by means of a commercially available measurement apparatus (Product name: NewView 5000 produced by Zygo Company) under the conditions shown in Table 3 above.
- A lapping plate as used in the first rough polishing step of Test Example 1 and the same polishing oil slurry described in Table 4 above were used.
- The second rough polishing step was carried out by the pad-less method under the same conditions as described in Table 2 for the second rough polishing step of Test Example 1. After the second rough polishing step, paraffin hydrocarbons were used to wash away the abrading particles and the GaN substrate was rinsed with alcohols. Thereafter, the average surface roughness (Ra) and the surface waviness (Wa) of the surface of the GaN substrate were measured by means of a commercially available measurement apparatus (Product name: NewView 5000 produced by Zygo Company) under the conditions shown in Table 3 above.
- A lapping plate as used in the first rough polishing step and the same polishing oil slurry used in the second rough polishing of Test Example 1 described in Table 5 above were used.
- The finishing step was carried out also by the pad-less polishing method as in the finishing step of Test Example 1 under the conditions described in Table 2 above. A lapping plate and polishing slurry as used in the finishing step of Test Example 1 were used. After the finishing step, paraffin hydrocarbons were used to wash away the abrading particles and the GaN substrate was rinsed with alcohols. Thereafter, the average surface roughness (Ra) and the surface waviness (Wa) of the surface of the GaN substrate were measured by means of a commercially available measurement apparatus (Product name: NewView 5000 produced by Zygo Company) under the conditions shown in Table 3 above.
- Results of Test Example 2 are shown in Table 9 below. The surface condition of the GaN substrate after the first rough polishing step, after the second rough polishing step and after the finishing step in Test Example 2 as described in Table 9 are shown respectively in
FIGS. 17 , 18 and 19.FIG. 19A indicates that no scratches are formed on the surface of the SiC according to Test Example 2. Table 9 further indicates that average surface roughness (Ra) of 0.2 nm or less is possible according to Test Example 2 with reduced surface waviness (Wa). In other words, the surface of a SiC substrate can be polished to be very flat (low in Wa) and very smooth (low in Ra) without scratches formed thereon according to Test Example 2. -
TABLE 9 After first rough After second After finishing polishing step rough polishing step step Ra Wa Ra Wa Ra Wa (nm) (nm) (nm) (nm) (nm) (nm) Test Example 2 1.10 0.63 0.49 0.28 0.19 0.11
Claims (2)
1. Polishing oil slurry for polishing a hard crystal substrate, said polishing oil slurry comprising:
abrading particles that include artificial diamond clusters; and
an oil dispersant;
wherein said artificial diamond clusters comprise approximately spherical agglomerate particles with average particle size D50 of 20 nm or more and 50 nm or less, having primary particles with particle diameters of 2 nm or more and 10 nm or less.
2. The polishing oil slurry of claim 1 wherein said oil dispersant contains synthetic isoparaffin hydrocarbons.
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US11/946,531 US7828628B2 (en) | 2006-12-01 | 2007-11-28 | Method of polishing hard crystal substrate |
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KR101488987B1 (en) | 2015-02-02 |
JP5599547B2 (en) | 2014-10-01 |
US7828628B2 (en) | 2010-11-09 |
TWI409323B (en) | 2013-09-21 |
JP2008138097A (en) | 2008-06-19 |
TW200835781A (en) | 2008-09-01 |
KR20080050338A (en) | 2008-06-05 |
US20080139089A1 (en) | 2008-06-12 |
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