CN114673012A - Abrasive cloth - Google Patents

Abrasive cloth Download PDF

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Publication number
CN114673012A
CN114673012A CN202111607875.4A CN202111607875A CN114673012A CN 114673012 A CN114673012 A CN 114673012A CN 202111607875 A CN202111607875 A CN 202111607875A CN 114673012 A CN114673012 A CN 114673012A
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China
Prior art keywords
polishing
polishing cloth
cloth
nonwoven fabric
hardness
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CN202111607875.4A
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Chinese (zh)
Inventor
川端丈
山本惠司
岳田考司
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Nida Dupont Co ltd
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Nida Dupont Co ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B24—GRINDING; POLISHING
    • B24D—TOOLS FOR GRINDING, BUFFING OR SHARPENING
    • B24D3/00—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents
    • B24D3/02—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent
    • B24D3/20—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent and being essentially organic
    • B24D3/28—Resins or natural or synthetic macromolecular compounds
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
    • D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
    • D06N3/12—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins
    • D06N3/14—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins with polyurethanes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B24—GRINDING; POLISHING
    • B24D—TOOLS FOR GRINDING, BUFFING OR SHARPENING
    • B24D11/00—Constructional features of flexible abrasive materials; Special features in the manufacture of such materials
    • B24D11/001—Manufacture of flexible abrasive materials

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Dispersion Chemistry (AREA)
  • Textile Engineering (AREA)
  • Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
  • Mechanical Treatment Of Semiconductor (AREA)
  • Polishing Bodies And Polishing Tools (AREA)

Abstract

The polishing cloth of the present invention comprises a nonwoven fabric and a resin impregnated in the nonwoven fabric as a material for forming the polishing cloth, wherein the AsKer-C hardness is 80 or more, and the quartile distance of the average value of the longitudinal abundance ratios of the 100 [ mu ] m width of the material is 10.5 or less.

Description

Abrasive cloth
Cross reference to related applications
The present application claims priority from Japanese patent application No. 2020-.
Technical Field
The present invention relates to a polishing cloth.
Background
An object to be polished such as a silicon wafer is polished using a polishing cloth (for example, patent document 1). The polishing cloth includes a nonwoven fabric and a resin impregnated in the nonwoven fabric as a material for forming the polishing cloth.
It is known that, in such a polishing cloth, end sagging occurs when the flexibility is too high. Conventionally, the treatment of hardening the polishing cloth by increasing the amount of resin impregnated can reduce the end sagging by preventing excessive contact with the end.
Documents of the prior art
Patent document 1: japanese patent laid-open No. 2006-43811
Summary of the invention
Problems to be solved by the invention
However, if the resin content is increased, local unevenness tends to occur at intervals of about 100 to 200 μm in the entire polishing cloth. In particular, unevenness due to the longitudinal entanglement of the nonwoven fabric causes minute variations in hardness, and as a result, local excessive contact occurs, which leads to a problem of lowering the flatness of the object to be polished.
Disclosure of Invention
In view of the above problems, an object of the present invention is to provide a polishing cloth capable of suppressing fine variation in hardness.
The polishing cloth of the present invention comprises a nonwoven fabric and a resin impregnated in the nonwoven fabric as a material for forming the polishing cloth, wherein the polishing cloth has an AsKer-C hardness of 80 or more, and the quartering pitch of the average value of the longitudinal abundance ratios of 100 [ mu ] m width of the material for forming the polishing cloth is 10.5 or less.
Drawings
FIG. 1 is a graph showing the quartering distance of the average value of the longitudinal abundance ratio of the forming material at a width of 100 μm and the flatness of the object to be polished in the polishing cloths of comparative example 1 and examples 1 to 3.
FIG. 2 is a graph showing the quartering distance of the average value of the longitudinal abundance ratio of the forming material at a width of 100 μm and the flatness of the object to be polished in the polishing cloths of comparative example 2 and examples 4 to 5.
Detailed Description
Hereinafter, one embodiment of the present invention will be described.
The polishing pad of the present embodiment includes a nonwoven fabric and a resin impregnated in the nonwoven fabric as a material for forming the polishing pad. That is, the polishing cloth of the present embodiment has a forming material including a nonwoven fabric and a resin impregnated in the nonwoven fabric.
The abrasive cloth of the present embodiment has an AsKer-C hardness of 80 or more, preferably 85 or more. On the other hand, the AsKer-C hardness is preferably 95 or less from the viewpoint of being less likely to cause defects (e.g., scratches) in the object to be polished. The case where the AsKer-C hardness satisfies the above range means a case where two regions (N: 2) which do not overlap each other in one polishing cloth are measured, and the above range is satisfied in both regions.
AsKer－The C hardness is a hardness measured by a rubber hardness meter used in JIS K7312, and is generally used as an index of hardness in a polishing cloth. The AsKer-C hardness was measured on the surface of the cloth on one side, i.e., on the polishing surface. The shape of the pressing needle is as follows
Figure BDA0003426173030000021
5.08mm, a height of 2.54mm, for example, an AsKer-C hardness of 90, a measurement range of
Figure BDA0003426173030000022
The circle of (c). Therefore, only the AsKer-C hardness cannot reflect the minute hardness deviation generated in the interval of about 100 to 200 μm.
The inventors of the present invention have made extensive studies and found that the average value of the longitudinal abundance ratio obtained by analyzing an image in the thickness direction of the polishing cloth is proportional to the hardness. Moreover, the following conclusions were drawn from this finding: by narrowing the measurement range to a width of 100 μm and defining the longitudinal abundance ratio in a predetermined range, it is possible to suppress a slight variation in hardness.
That is, the polishing pad of the present embodiment is formed such that the quartering pitch of the average value of the longitudinal abundance ratios of the 100 μm width of the material is 10.5 or less. The quartile distance of the average value in the longitudinal abundance ratio is preferably 10.0 or less, and more preferably 9.0 or less. In the polishing cloth, the quartile distance of the average value in the longitudinal abundance ratio of the forming material having a width of 100 μm may be 7.2 or more. Note that the case where the quartering distance of the average value in the longitudinal abundance ratio satisfies the above range means a case where the above range is satisfied in any one region of two regions (N is 2) that do not overlap each other in one polishing cloth, and the above range is measured.
The quartile range of the average value in the longitudinal abundance ratio of the 100 μm width of the forming material can be determined in the following manner.
First, a measurement area in a thin section (cross section) perpendicular to the surface of the polishing cloth was imaged with a field of view of 2000 μm × 2000 μm, and in the measurement area, a plurality of small areas of 100 μm × 100 μm were extracted. For example, in the case of a polishing pad having a thickness of 1.3mm, 144 small regions of 100 μm × 100 μm are extracted in a measurement region of 1200 μm (a direction parallel to the surface of the polishing pad) × 1200 μm (a direction perpendicular to the surface of the polishing pad, that is, a thickness direction of the polishing pad). At this time, the measurement region in the thickness direction depends on the thickness of the polishing cloth.
The average value of the abundance ratios in the columns arranged from the front surface to the back surface of the polishing pad was defined as "the average value of the abundance ratios in the columns of 100 μm width" (1 column amount). In this measurement, 17 photographs were taken of the cross section of each polishing cloth at an interval of 100 μm in one measurement, the average value of the longitudinal abundance ratio of the 100 μm width for the amount of 12 rows × 17 to 204 rows was obtained, the quartile distance was obtained, and two regions (N: 2) not overlapping in one polishing cloth were measured.
The abundance ratio of the forming material in each small region of 100 μm × 100 μm is a ratio of the area of a portion where the forming material is present, in each small region of 100 μm × 100 μm, when the area of each small region is 100% as a whole.
In the measurement, the abrasive cloth was photographed by CT-scan. Specifically, in a field of view of 2000 μm × 2000 μm, two measurement regions were imaged at intervals of 100 μm for each of the measurement regions on a thin-cut surface (cross section) perpendicular to the surface of the polishing cloth (the two measurement regions do not overlap), a plurality of small regions of 100 μm × 100 μm were extracted from each measurement region, and an image of each small region of 100 μm × 100 μm was subjected to binarization processing for classifying into voids and portions other than voids (portions where the forming material exists), thereby measuring the abundance ratio (area ratio).
As the CT apparatus, a three-dimensional measuring X-ray CT apparatus (TDM 1000H-1) manufactured by Daihe scientific Co., Ltd. can be used. Further, as the CT image processing software, image processing software VG Studio max2.1 manufactured by Visual Science Volume Graphics, inc. Also, as image analysis software for calculating the abundance ratio (area ratio) of the formation material, ImageJ (Rasband, w.s., u.s.national Institutes of Health, Bethesda, Maryland, USA) can be used.
For example, the abundance ratio (area ratio) of the formation material is measured under the following conditions.
In the measurement, the measurement region of the polishing cloth was continuously measured with the following visual field size.
Size of visual field (vertical × horizontal × height): 2,000. mu. m.times.2, 000. mu. m.times.the whole region in the thickness direction
The measurement conditions are as follows.
Number of views per rotation (view): 1500
Frame number/view: 10
X-ray tube voltage [ KV ]: 28.000
Enlarged shaft position [ mm ]: 7.416
Reconstructed pixel size X [ mm ]: 0.003880
Reconstructed pixel size Y [ mm ]: 0.003880
Reconstructed pixel size Z [ mm ]: 0.003880
The binarization process for classifying the measurement regions into voids and other portions (portions where the forming material is present) is as follows.
In the binarization process, the contrast of the image in the measurement area is adjusted by the image processing software VG Studio Max so as to classify the image into voids and portions other than voids (portions where the forming material exists). The adjustment of the contrast is performed in Ramp mode.
In contrast adjustment, the difference between the void and a portion other than the void (a portion where the forming material exists) is clarified.
In VG Studio Max, the adjustment of contrast is labeled "opacity adjustment". Specifically, in the screen for opacity adjustment of VG Studio Max, the lower limit value of the gradation value is set to the peak, and the upper limit value of the gradation value is set to the range of "peak of the peak +100 ± 5". Since the transmittance of light differs depending on the material, the adjustment range of the contrast is not limited to this.
The 2D image with the contrast adjusted is obtained as an image of a thin section, which is a measurement region of the image. Further, since the angle of view of the measurement region must be set to be large, when the cross section is stored by the image, the position is set so that the surface layer of the polishing cloth comes into contact with the upper part of the image.
Next, the abundance ratio of the forming material was measured by the image processing software ImageJ for the obtained image of the measurement region.
Here, the measurement range in ImageJ was 1200 μm × thickness of the polishing cloth. For example, in the case of a polishing cloth having a thickness of 1.0mm, the upper left of the image data is set as the (x, y) — (0pix ) position, and the portion from the (120, 10) position toward the lateral direction 312pix (═ 1201.2 μm) and the longitudinal direction 234pix (═ 900.9 μm) is extracted as the measurement range. Then, the image type is converted from RGB color to 8bit, and the image is binarized. Under this binarization condition, the range of the gradation from "129" to "255" corresponds to the portion where the forming material exists. The image size of the image data is reduced to 12pix in horizontal direction by 9pix in vertical direction. The 1pix × 1pix of the reduced image is a plane of 100 μm × 100 μm. This operation was performed for 17 images per 100 μm in the vertical direction of the polished surface. In the binarization process in ImageJ, the portion having the gradation range of "129" to "255" is a portion other than the void (portion where the forming material exists).
The polishing cloth of the present embodiment preferably has a compressibility of 5% or less, more preferably 3.5% or less. The case where the compressibility satisfies the above range means a case where two regions (N is 2) of one polishing cloth which do not overlap each other are measured, and the above range is satisfied in any region.
The compressibility can be determined by the following method. That is, JIS L1096: 2010 compression elasticity tester (indenter area: 50 mm)2) Applying 300gf/cm to the polishing cloth in the thickness direction by a indenter2The thickness T1 of the polishing cloth was measured after holding for 60 seconds, and 1800gf/cm was then applied to the polishing cloth in the thickness direction by a indenter2The thickness T2 of the polishing pad was measured after the pressure was maintained for 60 seconds, and the compressibility can be determined by the following equation.
Compression ratio (T1-T2). times.100/T1
The polishing cloth of the present embodiment preferably has a thickness of 0.8mm or more and 3.0mm or less, and more preferably 1.0mm or more and 2.0mm or less. By making the thickness of the polishing cloth 0.8mm or more, the following advantages are obtained: the adverse effect on the polishing performance due to the fixed disk state of the polishing machine can be easily alleviated. In addition, this also has the following advantages, for example: the object to be polished can be easily stabilized and flattened. On the other hand, the polishing cloth has an advantage that the deformation amount of the polishing cloth during polishing can be reduced by making the thickness of the polishing cloth 3.0mm or less, and as a result, the object to be polished is less likely to have end sagging. The case where the thickness satisfies the above range means a case where two regions (N ═ 2) of one polishing cloth which do not overlap each other are measured, and the above range is satisfied in any region.
The polishing cloth of the present embodiment preferably has a compressibility of 5% or less and a thickness of 0.8mm to 3.0 mm. With this configuration, fine hardness variation can be further suppressed.
In the polishing cloth of the present embodiment, the apparent density of the forming material is preferably 0.30g/cm3Above and 0.50g/cm3Hereinafter, more preferably 0.40g/cm3Above and 0.50g/cm3The following. The apparent density of the formed material was 0.30g/cm3Above and 0.50g/cm3In the following, fine hardness variations can be more suppressed. Further, the apparent density can be based on JIS K7222: 2005. The case where the apparent density satisfies the above range means a case where the apparent density satisfies the above range in any two regions (N: 2) of one polishing cloth which do not overlap each other.
Examples of the fibers constituting the nonwoven fabric include polyester fibers and nylon fibers.
The nonwoven fabric preferably has a basis weight of 200g/m2 or more and 600g/m2 or less. When the basis weight of the nonwoven fabric is 200g/m2 or more, the hardness tends to be high, and as a result, the object to be polished is less likely to have end sagging. Further, the nonwoven fabric has a basis weight of 200g/m2 or more and 600g/m2 or less, and thus tends to have a void portion in a polishing surface at an appropriate ratio, and as a result, has the following advantages: the polishing performance is easily prevented from being changed due to the clogging of the gap by the polishing dust or the like.
Examples of the resin include a urethane resin.
Examples of the object to be polished by the polishing cloth of the present embodiment include a silicon wafer.
The polishing pad of the present embodiment is configured as described above, and a method for producing the polishing pad of the present embodiment will be described below.
Hereinafter, a method of manufacturing the polishing pad of the present embodiment will be described by taking as an example a two-stage impregnation method in which a nonwoven fabric is impregnated with a polyurethane resin in a wet state and the nonwoven fabric is further impregnated with the polyurethane resin in a dry state.
In the wet impregnation, a polyurethane resin is dissolved in a water-soluble organic solvent to obtain a first impregnation liquid.
Examples of the water-soluble organic solvent include dimethylformamide, dimethylsulfoxide, tetrahydrofuran, and dimethylacetamide.
The first impregnation fluid may further contain a filler. Examples of the filler include carbon black. In addition, the first impregnation fluid may further contain a dispersion stabilizer. Examples of the dispersion stabilizer include a surfactant.
Next, the nonwoven fabric is immersed in the first immersion liquid, and the nonwoven fabric immersed in the first immersion liquid is immersed in water. As a result, the water-soluble organic solvent in the first impregnation liquid attached to the nonwoven fabric is replaced with water, the polyurethane resin solidifies, and the polyurethane resin adheres to the surface of the nonwoven fabric.
In the dry impregnation, a prepolymer having an isocyanate group as an end group, a curing agent having active hydrogen as an organic compound, and an organic solvent are mixed to obtain a second impregnation liquid.
Examples of the organic solvent include methyl ethyl ketone, acetone, alcohol, and ethyl acetate.
Then, the wet-impregnated nonwoven fabric is immersed in the second impregnation solution, and the nonwoven fabric immersed in the second impregnation solution is heated in a drying furnace. As a result, the organic solvent evaporates, the prepolymer and the curing agent undergo a curing reaction to form a polyurethane resin, and as a result, the polyurethane resin further adheres to the surface of the nonwoven fabric.
The polishing pad of the present embodiment is configured as described above, and therefore has the following advantages.
That is, the polishing cloth of the present embodiment is a polishing cloth having a nonwoven fabric and a resin impregnated in the nonwoven fabric as a material for forming the polishing cloth, and has an AsKer-C hardness of 80 or more and a quartile range of 10.5 or less in an average value of a longitudinal abundance ratio of a 100 μm width of the material for forming.
Since the AsKer-C hardness of the polishing cloth is 80 or more and the quartering pitch of the average value of the longitudinal abundance ratios of 100 μm width of the forming material is 10.5 or less, unevenness due to longitudinal entanglement of the nonwoven fabric can be reduced. As a result, it is possible to suppress the minute hardness deviation which cannot be reflected by only AsKer-C hardness.
The polishing pad of the present invention is not limited to the above embodiment. The polishing pad of the present invention is not limited to the above-described effects. The polishing cloth of the present invention can be variously modified within a range not departing from the gist of the present invention.
Examples
The present invention will be further described with reference to examples and comparative examples.
Polishing cloths of examples having the physical properties shown in tables 1 and 2 were produced. Further, polishing cloths (commercially available products) of comparative examples having the physical properties shown in tables 1 and 2 were prepared. Further, the average value of the AsKer-C hardness, compressibility, apparent density of the formed material, longitudinal abundance ratio of 100 μm width of the formed material, and the quartile range of the average value were measured by the above-described methods.
The flatness of the polishing cloth with a thickness of 1.2 to 1.3mm and the polishing cloth with a thickness of 0.9 to 1.1mm was evaluated by changing the conditions as described below.
Grinding cloth with the thickness of 1.2-1.3 mm: comparative example 1 and examples 1 to 3
The GBIR was measured from the wafer shape when the wafer was polished with a polishing cloth. The polishing was performed after the polishing cloth was set on a double-side polishing machine and subjected to a dressing treatment before polishing. In addition, the GBIR and ESFQR of wafer are optimized to the GBIR/ESFQR values in the gap of 0 to 3 μm. The results are shown in table 1 and fig. 1.
The polishing conditions were as follows.
Grinding machine: speed FAM 20B
A trimmer: speed FAM pure trimmer #100/#120
Setting a clearance: 0 to 3 μm
Grinding load: 1500kg
Rotating speed: 10rpm
Wafer: 12inch P-wafer
Grinding fluid: a solution having a solid content (115 ℃ C.) of 36.6%, an average particle diameter of 108nm and a pH of 11.3.
A polishing pad having a thickness of 0.9 to 1.1 mm: comparative example 2, examples 4 to 5
Polishing is performed by setting a polishing cloth on a single-side machine, and then dressing the cloth before polishing. However, since the single facer is greatly affected by the shape before polishing, the difference between the shape before polishing and the shape after polishing is analyzed, and the flatness is evaluated as the difference GBIR. Since the difference GBIR is a parameter that is highly correlated with the polishing rate, the shape comparison is performed as the difference GBIR/polishing rate. The results are shown in table 2 and fig. 2.
Further, the polishing conditions were as follows.
Grinding machine: poli762
A trimmer: kinik System conditioner #150
Grinding pressure: 300gf/cm2
Speed of rotation Head/Platen: 40/43rpm
Wafer: 8' (P-)
Grinding fluid: NP6610 (manufactured by Nitta Dupont Co., Ltd.)
DIW (purified water) was used by adding 7.14% thereto
Flow rate of polishing liquid: 600mL/min
[ Table 1]
Figure BDA0003426173030000071
[ Table 2]
Figure BDA0003426173030000081
As shown in tables 1 and 2 and fig. 1 and 2, the polishing cloths of the respective examples satisfying all the constituent requirements of the present invention can suppress fine hardness variation, and as a result, the flatness of the wafer is good.

Claims (3)

1. A grinding cloth is characterized in that the cloth is provided with a plurality of grinding grooves,
the polishing pad is formed from a nonwoven fabric and a resin impregnated in the nonwoven fabric,
the abrasive cloth has an AsKer-C hardness of 80 or more,
the quartering pitch of the average value of the longitudinal abundance ratios of the forming material with a width of 100 [ mu ] m is 10.5 or less.
2. Abrasive cloth according to claim 1,
the polishing cloth has a compressibility of 5% or less and a thickness of 0.8mm to 3.0 mm.
3. Abrasive cloth according to claim 1 or 2,
the apparent density of the forming material was 0.30g/cm3Above and 0.50g/cm3The following.
CN202111607875.4A 2020-12-24 2021-12-22 Abrasive cloth Pending CN114673012A (en)

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JP2020215154A JP2022100894A (en) 2020-12-24 2020-12-24 Polishing cloth

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Publication number Priority date Publication date Assignee Title
JP4890751B2 (en) 2004-08-04 2012-03-07 ニッタ・ハース株式会社 Polishing cloth

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