WO2011125902A1 - 磁気ディスク用ガラス基板の製造方法 - Google Patents
磁気ディスク用ガラス基板の製造方法 Download PDFInfo
- Publication number
- WO2011125902A1 WO2011125902A1 PCT/JP2011/058332 JP2011058332W WO2011125902A1 WO 2011125902 A1 WO2011125902 A1 WO 2011125902A1 JP 2011058332 W JP2011058332 W JP 2011058332W WO 2011125902 A1 WO2011125902 A1 WO 2011125902A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- glass substrate
- polishing
- ultrasonic cleaning
- frequency
- magnetic disk
- Prior art date
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- 239000000758 substrate Substances 0.000 title claims abstract description 131
- 239000011521 glass Substances 0.000 title claims abstract description 123
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 25
- 239000002245 particle Substances 0.000 claims abstract description 96
- 238000005498 polishing Methods 0.000 claims abstract description 91
- 238000004506 ultrasonic cleaning Methods 0.000 claims abstract description 84
- 239000006061 abrasive grain Substances 0.000 claims abstract description 53
- 239000011163 secondary particle Substances 0.000 claims abstract description 31
- 238000000034 method Methods 0.000 claims description 49
- 230000008569 process Effects 0.000 claims description 36
- 238000004140 cleaning Methods 0.000 claims description 24
- 238000007517 polishing process Methods 0.000 claims description 18
- 239000002002 slurry Substances 0.000 claims description 17
- 239000007788 liquid Substances 0.000 claims description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 5
- 230000004931 aggregating effect Effects 0.000 claims 3
- 238000009210 therapy by ultrasound Methods 0.000 abstract description 29
- 239000010410 layer Substances 0.000 description 38
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 18
- 238000003426 chemical strengthening reaction Methods 0.000 description 11
- 239000000463 material Substances 0.000 description 11
- 230000007246 mechanism Effects 0.000 description 9
- 229910003460 diamond Inorganic materials 0.000 description 7
- 239000010432 diamond Substances 0.000 description 7
- 238000000227 grinding Methods 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 230000002776 aggregation Effects 0.000 description 6
- 238000004220 aggregation Methods 0.000 description 6
- 230000002093 peripheral effect Effects 0.000 description 6
- 229910000420 cerium oxide Inorganic materials 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 238000011156 evaluation Methods 0.000 description 5
- 238000007518 final polishing process Methods 0.000 description 5
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 5
- 238000012545 processing Methods 0.000 description 5
- 239000011347 resin Substances 0.000 description 5
- 229920005989 resin Polymers 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 230000002378 acidificating effect Effects 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 230000007547 defect Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000010408 film Substances 0.000 description 4
- 230000001050 lubricating effect Effects 0.000 description 4
- 239000011241 protective layer Substances 0.000 description 4
- 238000000527 sonication Methods 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 239000005354 aluminosilicate glass Substances 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 239000008119 colloidal silica Substances 0.000 description 3
- 239000003599 detergent Substances 0.000 description 3
- 239000002270 dispersing agent Substances 0.000 description 3
- 239000010419 fine particle Substances 0.000 description 3
- 230000007935 neutral effect Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229910018068 Li 2 O Inorganic materials 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 150000001721 carbon Chemical class 0.000 description 2
- 239000003112 inhibitor Substances 0.000 description 2
- 230000001678 irradiating effect Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 2
- 229910001415 sodium ion Inorganic materials 0.000 description 2
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 2
- 239000002344 surface layer Substances 0.000 description 2
- 230000003746 surface roughness Effects 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 229910000599 Cr alloy Inorganic materials 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 238000006124 Pilkington process Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000005388 borosilicate glass Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000005345 chemically strengthened glass Substances 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000003618 dip coating Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000003280 down draw process Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000005357 flat glass Substances 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000009499 grossing Methods 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 239000006249 magnetic particle Substances 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000007500 overflow downdraw method Methods 0.000 description 1
- 239000010702 perfluoropolyether Substances 0.000 description 1
- 229910001414 potassium ion Inorganic materials 0.000 description 1
- 239000004323 potassium nitrate Substances 0.000 description 1
- 235000010333 potassium nitrate Nutrition 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000005361 soda-lime glass Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000004317 sodium nitrate Substances 0.000 description 1
- 235000010344 sodium nitrate Nutrition 0.000 description 1
- 239000007779 soft material Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
- B08B3/12—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration by sonic or ultrasonic vibrations
-
- G—PHYSICS
- G11—INFORMATION STORAGE
- G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
- G11B5/00—Recording by magnetisation or demagnetisation of a record carrier; Reproducing by magnetic means; Record carriers therefor
- G11B5/84—Processes or apparatus specially adapted for manufacturing record carriers
- G11B5/8412—Processes or apparatus specially adapted for manufacturing record carriers treatment by ultrasonics
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C19/00—Surface treatment of glass, not in the form of fibres or filaments, by mechanical means
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C23/00—Other surface treatment of glass not in the form of fibres or filaments
- C03C23/0075—Cleaning of glass
-
- G—PHYSICS
- G11—INFORMATION STORAGE
- G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
- G11B5/00—Recording by magnetisation or demagnetisation of a record carrier; Reproducing by magnetic means; Record carriers therefor
- G11B5/84—Processes or apparatus specially adapted for manufacturing record carriers
- G11B5/8404—Processes or apparatus specially adapted for manufacturing record carriers manufacturing base layers
Definitions
- the present invention relates to a method for producing a glass substrate for a magnetic disk.
- a magnetic disk used for an HDD which is one of magnetic recording media, has been rapidly reduced in size, thinned, and increased in recording density and access speed.
- a magnetic disk having a magnetic layer on a disk-shaped substrate is rotated at high speed, and recording and reproduction are performed while a magnetic head is flying over the magnetic disk.
- the magnetic head Since the rotation speed of the magnetic disk increases as the access speed increases, a higher substrate strength is required for the magnetic disk. As the recording density increases, the magnetic head is also changing from a thin film head to a magnetoresistive head (MR head), a large magnetoresistive head (GMR head), and a DFH (Dynamic Flying Height) control mechanism. As a result, the flying height of the magnetic head from the magnetic disk (the narrowest distance of the gap between the magnetic head and the magnetic disk) has been reduced to about 2 nm. For this reason, if there are irregularities on the surface of the magnetic disk, there may be a crash failure in which the magnetic head collides, or a thermal asperity failure that causes a read error due to adiabatic compression or contact of air. In order to suppress such troubles in the magnetic head, it is important to finish the main surface of the magnetic disk as a very smooth surface.
- a glass substrate is used instead of a conventional aluminum substrate as a substrate for a magnetic disk. This is because a glass substrate made of glass which is a hard material is superior in flatness of the substrate surface compared to an aluminum substrate made of a metal which is a soft material. Further, since the glass substrate is harder than the aluminum substrate, it is possible to suppress distortion and fluttering of the substrate during high-speed rotation. Thereby, the risk of collision with the head can be reduced.
- Patent Document 1 For example, in Patent Document 1, 50 kHz ultrasonic cleaning is performed after polishing using 0.8 ⁇ m polishing abrasive grains. Therefore, when the abrasive grains are smaller than this, it is considered that the ultrasonic frequency needs to be set higher.
- DFH Dynamic Flying Height
- the main surface of the magnetic disk is smoother and more than conventional. It has been found that it is necessary to clean with few defects such as foreign matter.
- the DFH head instead of lowering the flying height of the head main body and approaching the magnetic disk surface, only the periphery of the head element portion is projected and brought closer to the medium surface. Is considered to be affected.
- the distance between the protruding head element portion and the magnetic disk is preferably 1 nm or less.
- This invention is made
- the method for producing a glass substrate for a magnetic disk according to the present invention comprises a polishing step of polishing using a polishing grain having a predetermined particle size on a glass substrate, and an ultrasonic wave for ultrasonically cleaning the glass substrate after the polishing step.
- a cleaning step wherein the ultrasonic cleaning step performs the first ultrasonic cleaning at a frequency at which particles having a predetermined particle size are aggregated to form secondary particles, and then sets the secondary particles to be cleaned.
- the second ultrasonic cleaning is performed.
- the method for manufacturing a glass substrate for a magnetic disk according to the present invention includes a polishing step for polishing a glass substrate, and an ultrasonic cleaning step for ultrasonically cleaning the glass substrate after the polishing step.
- the first ultrasonic cleaning is performed at a frequency of 300 KHz to 1000 KHz to form secondary particles, and then the second ultrasonic wave is generated at a frequency of 30 KHz to 100 KHz. It is characterized by performing cleaning.
- the method for producing a glass substrate for a magnetic disk of the present invention it is preferable to form secondary particles having a particle size of 1000 nm to 3000 nm by performing the first ultrasonic cleaning.
- the polishing step is preferably a final polishing step among a plurality of polishing steps performed on the glass substrate.
- the first ultrasonic cleaning is performed at a relatively high frequency, and then the second ultrasonic cleaning is performed at a relatively low frequency. Even when abrasive grains having a small particle diameter are used in the process, it is possible to suppress the aggregation particles caused by the abrasive grains and the like from remaining and effectively remove particles on the surface of the glass substrate.
- the present inventor reduced the grain size of the abrasive grains used in the polishing process for the purpose of further improving the smoothing of the glass substrate surface, and ultrasonic waves after polishing for the purpose of removing fine particles.
- particles particle size of 10 nm to 30 nm
- particles which has not been a problem in the past, aggregate and remain on the glass substrate surface. Faced a problem.
- ultrasonic waves are irradiated at a relatively high frequency (300 KHz to 1000 KHz) to agglomerate particles caused by the abrasive grains.
- a relatively high frequency 300 KHz to 1000 KHz
- a relatively low frequency (30 KHz or more and 100 KHz or less) and irradiating with ultrasonic waves, it is possible to effectively remove particles on the glass substrate surface and not to cause concave defects due to ultrasonic waves on the glass substrate.
- a relatively low frequency (30 KHz or more and 100 KHz or less
- the method for manufacturing a glass substrate for a magnetic disk shown in the present embodiment includes a polishing step in which polishing is performed using polishing abrasive grains having a predetermined particle size on at least a glass substrate, and an ultrasonic cleaning is performed on the glass substrate after the polishing step.
- the ultrasonic cleaning step performs the first ultrasonic cleaning at a frequency at which particles having a predetermined particle size are aggregated to form secondary particles, and then the secondary particles are cleaned.
- the second ultrasonic cleaning is performed at a frequency that is a target and does not cause a concave defect on the glass substrate surface.
- the first ultrasonic cleaning is performed at a frequency of 300 KHz to 1000 KHz
- the second ultrasonic cleaning is performed at a frequency of 30 KHz to 100 KHz. be able to.
- the first ultrasonic cleaning using a relatively high frequency removes particles having a particle size to be cleaned and reduces the particle size of 10 nm to 30 nm outside the target to be cleaned.
- the second ultrasonic treatment using a relatively low frequency (30 KHz to 100 KHz) is intended to form secondary particles (aggregates) by agglomerating particles (abrasive grains, etc.) having An object of the present invention is to prevent the generation of concave defects in the glass substrate while removing the secondary particles aggregated by the first ultrasonic treatment.
- the glass substrate after the polishing process is first subjected to ultrasonic treatment at a relatively high frequency to remove particles having a particle size to be cleaned attached to the surface of the glass substrate and Particles collide with large particles and agglomerate. Thereafter, ultrasonic treatment is performed at a relatively low frequency to remove the aggregated particles having a large particle diameter. In this case, even if ultrasonic treatment is performed at a relatively low frequency, most of the aggregated particles can be removed without being dispersed. This is presumably because organic substances are present at the interface of the aggregates and the bonding strength is increased.
- This organic substance is considered to be derived from a dispersant or a re-aggregation inhibitor added to the slurry as the abrasive grains become finer.
- These dispersants and anti-agglomeration inhibitors are added by selecting substances that are optimal according to the pH of the slurry. For example, dispersants that are effective in acidic slurries are sufficient under alkaline conditions. Unable to exert a good dispersion effect.
- the frequency of the first ultrasonic cleaning is such that particles having a particle size to be cleaned attached to the glass substrate surface can be removed, and particles that are not to be cleaned (here, particles such as abrasive grains of 10 nm to 30 nm) are removed. What is necessary is just to set to the frequency to aggregate.
- the frequency satisfying such a condition may be 300 KHz to 1000 KHz.
- the frequency is less than 300 KHz, particles with a particle size of 10 nm to 30 nm do not form a secondary particle size well, and when the frequency exceeds 1000 KHz, tertiary particles, quaternary particles, etc. are formed and removed. It becomes difficult.
- the frequency of the second ultrasonic cleaning may be set to a frequency for which the particle size of particles generated by aggregation by the frequency of the first ultrasonic cleaning is a cleaning target.
- the frequency of the first ultrasonic cleaning is 950 kHz
- the particle size of the aggregated particles varies depending on the application time of the ultrasonic wave, but is 1000 nm to 3000 nm. Therefore, the frequency of the second ultrasonic cleaning is the target. What is necessary is just to set to 30 kHz-100 KHz from which a particle size becomes 1000 nm-3000 nm.
- the frequency of ultrasonic cleaning and the particle size of particles to be cleaned can be obtained by the following equation (1) showing the relationship between the cleaning target diameter in the ultrasonic frequency band using the amplitude and the speed of sound.
- ⁇ ac (2 ⁇ / ⁇ ) 0.5 (in water) (1)
- ⁇ ac represents the thickness of the sound pressure boundary layer
- ⁇ represents the speed of sound
- ⁇ represents Hz (frequency).
- the frequency of the second ultrasonic cleaning is less than 30 KHz, particles are removed, but a strong impact is applied to the glass surface, and the surface roughness may be deteriorated.
- the frequency exceeds 100 KHz, It becomes difficult to remove particles.
- the first ultrasonic cleaning and the second ultrasonic cleaning can be performed separately in two different cleaning tanks, but can also be performed continuously by switching the frequency in the middle of one cleaning tank.
- the timing of switching from the frequency of the first ultrasonic cleaning to the frequency of the second ultrasonic cleaning is measured in advance for the time when secondary particles are formed by irradiating the frequency used in the first ultrasonic cleaning. It is preferable to feed back the conditions.
- the second ultrasonic cleaning can be performed after sufficiently forming secondary particles having a particle size to be subjected to the second ultrasonic cleaning by the first ultrasonic cleaning.
- ultrasonic cleaning is continuously performed on the polished glass substrate at different frequencies, and after the particles caused by the abrasive grains are aggregated to form secondary particles, the secondary particles are removed.
- fine polishing abrasive grains particles size: 10 nm to 30 nm
- ultrasonic treatment is performed at a relatively high frequency (300 KHz to 1000 KHz) in the ultrasonic cleaning process after the polishing process.
- particles on the glass substrate surface can be effectively removed.
- both the first ultrasonic cleaning and the second ultrasonic cleaning are performed in a liquid adjusted to be alkaline.
- the secondary particles generated by the first ultrasonic cleaning are decomposed during the second ultrasonic cleaning.
- the cleaning liquid of the ultrasonic cleaning and the second ultrasonic cleaning is made alkaline, it cannot be removed well.
- the pH of the cleaning solution for the first ultrasonic cleaning and the second ultrasonic cleaning is preferably in the range of 12 to 14, and more preferably in the range of 13 to 14.
- the method for manufacturing a glass substrate for a magnetic disk according to the present embodiment includes an agglomeration process for agglomerating abrasive grains adhering to the surface of the glass substrate to form secondary particles, and a cleaning process for removing the secondary particles. It can be considered that the combination process is included. Specifically, after performing a polishing process for polishing the surface of the glass substrate using a slurry containing abrasive grains, the abrasive grains adhering to the surface of the glass substrate are aggregated to form secondary particles ( Aggregation treatment), and then the secondary particles are removed by washing (washing treatment).
- the aggregation treatment can be a treatment in which ultrasonic waves are applied to the abrasive grains in a liquid adjusted to be alkaline.
- cleaning treatment scrub cleaning or the like can be used, but it is preferable to use ultrasonic cleaning.
- the polishing step is preferably a slurry containing silicon oxide abrasive grains. If silicon oxide is used, it is possible to obtain abrasive grains having a very small particle size with a center particle size of 10 to 30 nm and having the same main component as the glass substrate to be polished. Since the difference in hardness is small, it is optimal for polishing the glass substrate surface very smoothly.
- the polishing step uses a slurry containing silicon oxide abrasive grains under acidic conditions.
- the polishing rate can be improved by the etching effect of the acid or the like.
- plate-like glass can be used.
- aluminosilicate glass soda lime glass, borosilicate glass, or the like can be used.
- an aluminosilicate glass in that a glass substrate for a magnetic disk excellent in flatness of the main surface and substrate strength can be provided.
- the plate-like glass can be manufactured by using a known manufacturing method such as a press method, a float method, a downdraw method, a redraw method, or a fusion method using these glasses as materials. Of these methods, if a press method is used, a sheet glass can be produced at a low cost.
- the first lapping step can be performed using alumina loose abrasive grains by a double-side grinding apparatus using a planetary gear mechanism. Specifically, the lapping platen is pressed on both sides of the disk-shaped glass substrate from above and below, and a grinding liquid containing loose abrasive grains is supplied onto the main surface of the glass substrate, and these are moved relatively to perform lapping. I do. By this lapping process, a glass substrate having a flat main surface can be obtained.
- Shape processing step (coring step for forming a hole, chamfering step for forming a chamfered surface at the end (outer peripheral end and inner peripheral end) (chamfered surface forming step))
- an inner hole can be formed in the central portion of the disk-shaped glass substrate using a cylindrical diamond drill to obtain an annular glass substrate.
- the inner peripheral end surface and the outer peripheral end surface are ground with a diamond grindstone, and a predetermined chamfering process is performed on the glass substrate.
- Second lapping step a second lapping process is performed on both main surfaces of the obtained glass substrate.
- the fine uneven shape formed on the main surface of the glass substrate in the shape processing step, which is the previous step can be removed, and the polishing step for the subsequent main surface is completed in a short time. It becomes possible.
- the second lapping process can be performed by using a fixed abrasive polishing pad made of a diamond sheet by a double-side grinding apparatus using a planetary gear mechanism.
- the diamond sheet only needs to have diamond particles as abrasive grains.
- a diamond sheet in which diamond particles are provided on a base material made of PET can be used.
- End surface polishing step In the end surface polishing step, the outer peripheral end surface and the inner peripheral end surface of the glass substrate are mirror-polished by a brush polishing method. At this time, as the abrasive grains, for example, a slurry containing cerium oxide abrasive grains can be used. By this end surface polishing step, the end surface of the glass substrate becomes a mirror surface.
- abrasive grains for example, a slurry containing cerium oxide abrasive grains can be used.
- Main surface polishing step As the main surface polishing step, first, a first polishing step is performed.
- the first polishing process is a process whose main purpose is to remove scratches and distortions remaining on both main surfaces in the lapping process described above.
- both main surfaces are polished using a hard resin polisher by a double-side polishing apparatus having a planetary gear mechanism.
- the abrasive cerium oxide abrasive grains can be used.
- a pair of polishing cloth (a polishing pad of a hard resin polisher) can be attached to the main surface portion of the upper and lower surface plates.
- a glass substrate can be installed between polishing cloths attached to the upper and lower surface plates, and one or both of the upper and lower surface plates can be moved to polish both main surfaces of the glass substrate. .
- Chemical strengthening process a glass substrate is immersed in a chemical strengthening liquid and a chemical strengthening process is performed.
- the chemical strengthening solution used for the chemical strengthening treatment for example, a mixed solution of potassium nitrate (60%) and sodium nitrate (40%) can be used.
- the chemical strengthening solution is heated to 300 ° C. to 400 ° C.
- the glass substrate is preheated to 200 ° C. to 300 ° C., and immersed in the chemical strengthening solution for 3 hours to 4 hours.
- the lithium ions and sodium ions in the surface layer of the glass substrate are respectively replaced with sodium ions and potassium ions having a relatively large ion radius in the chemical strengthening solution.
- the chemically strengthened glass substrate may be cleaned with sulfuric acid and then with pure water, IPA, or the like.
- Main surface polishing step (final polishing step) As the final polishing step, a second polishing step is performed.
- the second polishing step is a step aimed at finishing both main surfaces into a mirror shape.
- both main surfaces are mirror-polished using a soft foam resin polisher by a double-side polishing apparatus having a planetary gear mechanism.
- the polishing abrasive grains it is possible to use a slurry having colloidal silica having a particle diameter of 10 nm to 30 nm, which is finer than the cerium oxide abrasive grains used in the first polishing step.
- a double-side polishing apparatus using a planetary gear mechanism can be used in the same manner as in the first polishing step.
- the glass substrate is subjected to a cleaning process using ultrasonic waves after the final polishing process.
- the ultrasonic cleaning process is a process aimed at removing particles adhering to the surface of the glass substrate after the final polishing process using two or more types of ultrasonic frequency bands.
- the glass substrate subjected to the final polishing process is immersed in pure water, a KOH aqueous solution, or the like, and then irradiated with ultrasonic waves. Specifically, first, the first ultrasonic cleaning is performed at a relatively high frequency (300 KHz to 1000 KHz) to form secondary particles, and then the second is performed at a relatively low frequency (30 KHz to 100 KHz). By performing the ultrasonic cleaning of 2, the particles including the secondary particles aggregated by the first ultrasonic cleaning are removed from the glass substrate surface.
- the first ultrasonic cleaning and the second ultrasonic cleaning can be performed by switching the frequency in one ultrasonic cleaning process.
- the timing of switching from the frequency of the first ultrasonic cleaning to the frequency of the second ultrasonic cleaning is the size of secondary particles formed when ultrasonic waves are irradiated at a relatively high frequency in advance (for example, 1000 nm). It is preferable to define the relationship between the ultrasonic cleaning time and the like, and to feed back the conditions. Thereby, after sufficiently forming secondary particles by the first ultrasonic cleaning, the second ultrasonic cleaning can be performed.
- a perpendicular magnetic layer is formed by sequentially forming, for example, an adhesion layer, a soft magnetic layer, a nonmagnetic underlayer, a perpendicular magnetic recording layer, a protective layer, and a lubricating layer on the main surface of the glass substrate obtained through the above-described steps.
- a recording disk can be manufactured.
- the material constituting the adhesion layer include a Cr alloy.
- the material constituting the soft magnetic layer include a CoTaZr-based alloy.
- the nonmagnetic underlayer include a granular nonmagnetic layer.
- An example of the perpendicular magnetic recording layer is a granular magnetic layer.
- Examples of the material constituting the protective layer include hydrogenated carbon.
- Examples of the material constituting the lubrication layer include a fluororesin.
- these recording layers and the like are more specifically formed by using an in-line sputtering apparatus on a glass substrate, a CrTi adhesion layer, a CoTaZr / Ru / CoTaZr soft magnetic layer, and a CoCrSiO 2 nonmagnetic granular material.
- An underlayer, a CoCrPt—SiO 2 ⁇ TiO 2 granular magnetic layer, and a hydrogenated carbon protective film can be sequentially formed, and a perfluoropolyether lubricating layer can be formed by dipping.
- a Ru underlayer may be used in place of the CoCrSiO 2 nonmagnetic granular underlayer. Further, a NiW seed layer may be added between the soft magnetic layer and the underlayer. Further, a CoCrPtB magnetic layer may be added between the granular magnetic layer and the protective layer.
- the size and the number of particles remaining on the glass substrate surface were evaluated. .
- SiO 2 58 wt% to 75 wt%
- Al 2 O 3 5 wt% to 23 wt%
- Li 2 O 3 wt% to 10 wt%
- Na 2 O 4 wt% to 13 wt%
- Aluminosilicate glass containing wt% as the main component was used.
- Li 2 O may be greater than 0% by weight and 7% by weight or less.
- a main surface polishing step As a main surface polishing step, first, a first polishing step was performed. In the first polishing step, the main surface was polished using a hard resin polisher by a double-side polishing apparatus having a planetary gear mechanism. As the abrasive, a slurry containing cerium oxide having a particle size of 0.2 nm to 4.5 nm was used.
- the glass substrate after the first polishing step was sequentially immersed in each washing tank of neutral detergent, pure water, and IPA (isopropyl alcohol) and washed.
- a second polishing step was performed as the main surface polishing step.
- the purpose of this second polishing step is to finish the main surface into a mirror surface.
- mirror polishing of the main surface was performed using a soft foamed resin polisher by a double-side polishing apparatus having a planetary gear mechanism.
- a slurry containing colloidal silica abrasive grains (average particle diameter of 10 nm to 30 nm) finer than the cerium oxide abrasive grains used in the first polishing step was used.
- polishing was performed with the pH of the slurry set to 2. At this time, polishing is performed by adding an additive containing acetic acid and acetate to the slurry. This is for controlling the pH of the slurry constant during the polishing process.
- polishing liquid a mixed liquid obtained by adding the colloidal silica particles to ultrapure water and 0.5% by weight of citric acid as an additive was used.
- the generation of cracks in the glass substrate is suppressed when the first ultrasonic treatment frequency is in the range of 300 kHz to 1000 kHz and the second ultrasonic treatment frequency is in the range of 30 kHz to 100 kHz.
- the number of remaining particles could be reduced (Example 1 to Example 10, Example 17 to Example 21). This is because the first sonication is performed in the frequency range of 300 kHz to 1000 kHz to effectively agglomerate particles caused by the abrasive grains, and then the second sonication is performed in the frequency range of 30 kHz to 100 kHz. This is probably because the aggregated particles on the surface of the glass substrate could be effectively removed.
- the frequency of the first ultrasonic treatment is in the range of 300 kHz to 1000 kHz
- the second When the ultrasonic treatment was performed at a frequency of 30 kHz to 100 kHz, it was possible to suppress the generation of cracks in the glass substrate and reduce the number of remaining particles (Examples 20 and 21).
- the frequency of the second ultrasonic treatment is performed within the range of 30 kHz to 100 kHz
- the frequency of the first ultrasonic treatment is out of the range of 300 kHz to 1000 kHz.
- Table 2 shows the evaluation results when the first ultrasonic treatment and the second ultrasonic treatment were performed using different cleaning liquids.
- the treatment when the treatment is performed in the range of the frequency of the first ultrasonic treatment in the range of 300 kHz to 1000 kHz and the frequency of the second ultrasonic treatment in the range of 30 kHz to 100 kHz, a different treatment liquid is used. Even so, the number of remaining particles could be reduced to 1000 or less.
- the cleaning solution for the first ultrasonic treatment and the second ultrasonic treatment was made alkaline, the number of remaining particles was the smallest (Example 22).
- the pH of the cleaning liquid is preferably in the range of 12 to 14, and more preferably in the range of 13 to 14.
- Magnetic disk A 2.5-inch (inner diameter 20 mm, outer diameter 65 mm, plate thickness 0.8 mm) glass substrate is manufactured, and a recording layer or the like is formed on the glass substrate. Evaluation radius: 22 mm Magnetic disk rotation speed: 5400 RPM Temperature: 25 ° C Humidity: 60%
- the recording layer was formed on the glass substrate as follows. First, an adhesion layer / soft magnetic layer / pre-underlayer / main layer / main recording layer / auxiliary recording layer / protection on a substrate in a Ar atmosphere by a DC magnetron sputtering method using a vacuum-deposited film forming apparatus A layer / lubricating layer was sequentially formed. Unless otherwise noted, the Ar gas pressure during film formation was 0.6 Pa. As the adhesion layer, Cr-50Ti was formed to a thickness of 10 nm. As the soft magnetic layer, 92 Co-3Ta-5Zr was formed to a thickness of 20 nm with a 0.7 nm Ru layer interposed therebetween.
- Ni-5W was deposited to 8 nm.
- Ru was formed to a thickness of 10 nm at 0.6 Pa, and then Ru was deposited to a thickness of 10 nm at 5 Pa.
- 90 nm (72Co-10Cr-18Pt) -5 (SiO 2 ) -5 (TiO 2 ) was formed to a thickness of 15 nm at 3 Pa.
- 62Co-18Cr-15Pt-5B was formed to a thickness of 6 nm.
- the protective layer a film of 4 nm was formed using C 2 H 4 by a CVD method, and the surface layer was nitrided. The lubricating layer was formed to 1 nm using PFPE by dip coating.
- Table 1 The results of the DFH touchdown test are shown in Table 1.
- Table 1 the following evaluation was made according to the distance (x) where the head element portion and the magnetic disk contacted. ⁇ : x ⁇ 1.0 nm ⁇ : 1.0 nm ⁇ x
- the substrate that can suppress the occurrence of cracks in the glass substrate and can effectively reduce the number of remaining particles (Examples 1 to 10, Example 17 to Example 21).
- the distance that the head element portion and the magnetic disk contacted could be reduced to 1.0 nm or less.
- the first ultrasonic treatment frequency is in the range of 300 kHz to 1000 kHz and the second ultrasonic treatment frequency is in the range of 30 kHz to 100 kHz. It is considered that particles on the surface of the glass substrate can be effectively removed without causing them.
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Abstract
Description
なお、上記式(1)において、δacは音圧境界層の厚さ、νは音速、ωはHz(周波数)を示す。
素材加工工程では、板状のガラスを用いることができる。ガラスとしては、アルミノシリケートガラス、ソーダライムガラス、ボロシリケートガラスなどを用いることができる。特に、主表面の平坦性及び基板強度において優れた磁気ディスク用ガラス基板を提供することができるという点では、アルミノシリケートガラスを用いることが好ましい。板状ガラスは、これらのガラスを材料として、プレス法やフロート法、ダウンドロー法、リドロー法、フュージョン法など、公知の製造方法を用いて製造することができる。これらの方法うち、プレス法を用いれば、板状ガラスを廉価に製造することができる。
第1ラッピング工程では、ディスク状のガラス基板の主表面をラッピング加工し、ガラス基板の形状を整える。第1のラッピング工程は、遊星歯車機構を利用した両面研削装置により、アルミナ系遊離砥粒を用いて行うことができる。具体的には、ディスク状のガラス基板の両面に上下からラップ定盤を押圧させ、遊離砥粒を含む研削液をガラス基板の主表面上に供給し、これらを相対的に移動させてラッピング加工を行う。このラッピング加工により、平坦な主表面を有するガラス基板を得ることができる。
コアリング工程では、例えば、円筒状のダイヤモンドドリルを用いて、ディスク状のガラス基板の中心部に内孔を形成し、円環状のガラス基板とすることができる。チャンファリング工程においては、内周端面及び外周端面をダイヤモンド砥石によって研削し、ガラス基板に所定の面取り加工を施す。
第2ラッピング工程では、得られたガラス基板の両主表面について、第2ラッピング加工を行う。第2ラッピング工程を行うことにより、前工程である形状加工工程においてガラス基板の主表面に形成された微細な凹凸形状を除去することができ、後続の主表面に対する研磨工程を短時間で完了させることが可能となる。
端面研磨工程では、ガラス基板の外周端面及び内周端面について、ブラシ研磨方法により、鏡面研磨を行う。このとき、研磨砥粒としては、例えば、酸化セリウム砥粒を含むスラリーを用いることができる。この端面研磨工程により、ガラス基板の端面は、鏡面状態になる。
主表面研磨工程として、まず第1研磨工程を施す。第1研磨工程は、前述のラッピング工程で両主表面に残留したキズや歪みの除去を主たる目的とする工程である。この第1研磨工程においては、遊星歯車機構を有する両面研磨装置により、硬質樹脂ポリッシャを用いて、両主表面の研磨を行う。研磨剤としては、酸化セリウム砥粒を用いることができる。また、第1研磨工程を終えたガラス基板は、中性洗剤、純水、IPA等で洗浄することが好ましい。
化学強化工程においては、ガラス基板を化学強化液に浸漬して化学強化処理を施す。化学強化処理に用いる化学強化液としては、例えば、硝酸カリウム(60%)と硝酸ナトリウム(40%)の混合溶液などを用いることができる。化学強化処理においては、化学強化液を300℃~400℃に加熱し、ガラス基板を200℃~300℃に予熱し、化学強化溶液中に3時間~4時間浸漬することによって行う。この浸漬の際には、ガラス基板の両表面全体が化学強化されるようにするため、複数のガラス基板が端面で保持されるように、ホルダに収納した状態で行うことが好ましい。
最終研磨工程として、第2研磨工程を施す。第2研磨工程は、両主表面を鏡面状に仕上げることを目的とする工程である。第2研磨工程においては、遊星歯車機構を有する両面研磨装置により、軟質発泡樹脂ポリッシャを用いて、両主表面の鏡面研磨を行う。研磨砥粒としては、第1研磨工程で用いた酸化セリウム砥粒よりも微細な粒径10nm~30nmのコロイダルシリカなどを有するスラリーを用いることがきる。この最終研磨工程において、遊星歯車機構を利用した両面研磨装置を用いて上記第1研磨工程と同様に行うことができる。
最終研磨工程後にガラス基板に超音波を用いた洗浄工程を施す。超音波洗浄工程は、最終研磨工程後にガラス基板の表面に付着したパーティクルを2種類以上の超音波周波数帯を用いて除去することを目的とする工程である。
上述した工程を経て得られたガラス基板の主表面に、例えば、付着層、軟磁性層、非磁性下地層、垂直磁気記録層、保護層、及び潤滑層を順次成膜することにより、垂直磁気記録ディスクを製造することができる。付着層を構成する材料としては、Cr合金などを挙げることができる。軟磁性層を構成する材料としては、CoTaZr基合金などを挙げることができる。非磁性下地層としては、グラニュラー非磁性層などを挙げることができる。垂直磁気記録層としては、グラニュラー磁性層などを挙げることができる。保護層を構成する材料としては、水素化カーボンなどを挙げることができる。潤滑層を構成する材料としては、フッ素樹脂などを挙げることができる。例えば、これらの記録層等は、より具体的には、インライン型スパッタリング装置を用いて、ガラス基板の上に、CrTiの付着層、CoTaZr/Ru/CoTaZrの軟磁性層、CoCrSiO2の非磁性グラニュラー下地層、CoCrPt-SiO2・TiO2のグラニュラー磁性層、水素化カーボン保護膜を順次成膜し、さらに、ディップ法によりパーフルオロポリエーテル潤滑層を成膜することができる。なお、CoCrSiO2の非磁性グラニュラー下地層の替わりにRuの下地層を用いてもよい。また、軟磁性層と下地層の間にNiWのシード層を追加してもよい。また、グラニュラー磁性層と保護層の間にCoCrPtBの磁性層を追加してもよい。
主表面研磨工程として、まず第1研磨工程を施した。第1研磨工程においては、遊星歯車機構を有する両面研磨装置により、硬質樹脂ポリッシャを用いて、主表面の研磨を行った。研磨剤としては、粒径0.2nm~4.5nmの酸化セリウムを含むスラリーを用いた。
次に、主表面研磨工程として、第2研磨工程を施した。この第2研磨工程は、主表面を鏡面状に仕上げることを目的とする。第2研磨工程においては、遊星歯車機構を有する両面研磨装置により、軟質発泡樹脂ポリッシャを用いて、主表面の鏡面研磨を行った。研磨剤としては、第1研磨工程で用いた酸化セリウム砥粒よりも微細なコロイダルシリカ砥粒(平均粒子径10nm~30nm)を含むスラリーを使用した。
最終研磨工程を終えたガラス基板を、濃度2重量%のKOH水溶液に浸漬して表1に示す各条件にて超音波洗浄工程を行った。その後、中性洗剤、純水、純水、IPA、IPA(蒸気乾燥)の各洗浄槽に順次浸漬して洗浄した後に、光学測定機を用いてガラス基板表面に残存しているパーティクルの個数及び基板表面のクラックの有無について評価した。
評価結果を表1に示す。
次に、上記表1に示した条件で洗浄工程を行ったガラス基板を用いて磁気ディスクを作製し、クボタコンプス社製HDFテスター(Head/Disk Flyability Tester)を用いて、DFHヘッド素子部のタッチダウン試験を行った。この試験は、DFH機構によって素子部を徐々に突き出していき、AEセンサーによって磁気ディスク表面との接触を検知することによって、ヘッド素子部が磁気ディスク表面と接触するときの距離を評価するものである。ヘッドは320GB/P磁気ディスク(2.5インチサイズ)向けのDFHヘッドを用いた。素子部の突き出しがない時の浮上量は10nmである。また、その他の条件は以下の通り設定した。
評価半径:22mm
磁気ディスクの回転数:5400RPM
温度:25℃
湿度:60%
○:x≦1.0nm
△:1.0nm<x
Claims (10)
- ガラス基板に対して所定の粒径を有する研磨砥粒を用いて研磨を行う研磨工程と、前記研磨工程後に前記ガラス基板に超音波洗浄を行う超音波洗浄工程を有し、
前記超音波洗浄工程は、前記所定の粒径を有するパーティクルを凝集させる周波数で第1の超音波洗浄を行って二次粒子を形成した後、前記二次粒子を洗浄対象とする周波数で第2の超音波洗浄を行うことを特徴とする磁気ディスク用ガラス基板の製造方法。 - 前記研磨工程で粒径が10nm~30nmの研磨砥粒を用い、
前記超音波洗浄工程において、300KHz~1000KHzの周波数で第1の超音波洗浄を行って二次粒子を形成した後、30KHz~100KHzの周波数で第2の超音波洗浄を行うことを特徴とする請求項1に記載の磁気ディスク用ガラス基板の製造方法。 - 前記第1の超音波洗浄を行うことにより、粒径が1000nm~3000nmの前記二次粒子を形成することを特徴とする請求項1又は請求項2に記載の磁気ディスク用ガラス基板の製造方法。
- 前記研磨工程は、前記ガラス基板に対して複数行われる研磨工程のうち最終の研磨工程であることを特徴とする請求項1から請求項3のいずれかに記載の磁気ディスク用ガラス基板の製造方法。
- ガラス基板の表面を研磨砥粒を含むスラリーを利用して研磨する研磨処理の後、前記研磨砥粒を除去する洗浄処理を含む磁気ディスク用ガラス基板の製造方法であって、
前記研磨処理の後、前記ガラス基板の表面に付着した研磨砥粒を凝集させて二次粒子を形成する凝集処理を行なった後、前記二次粒子を前記洗浄処理で除去することを特徴とする、磁気ディスク用ガラス基板の製造方法。 - 前記研磨砥粒は、珪素酸化物からなることを特徴とする請求項5に記載の磁気ディスク用ガラス基板の製造方法。
- 前記凝集処理は、前記研磨砥粒に超音波を印加して二次粒子を生成させることを特徴とする請求項5又は請求項6に記載の磁気ディスク用ガラス基板の製造方法。
- 前記凝集処理は、アルカリ性に調整された液体中で、前記研磨砥粒に超音波を印加する処理であることを特徴とする請求項5から請求項7のいずれかに記載の磁気ディスク用ガラス基板の製造方法。
- 前記スラリーは、珪素酸化物の研磨砥粒を含む酸性に調整されたスラリーであることを特徴とする請求項5から請求項8のいずれかに記載の磁気ディスク用ガラス基板の製造方法。
- 前記洗浄処理は、超音波洗浄であることを特徴とする請求項5から請求項9のいずれかに記載の磁気ディスク用ガラス基板の製造方法。
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CN102812514B (zh) | 2016-05-25 |
US8821735B2 (en) | 2014-09-02 |
JPWO2011125902A1 (ja) | 2013-07-11 |
MY155778A (en) | 2015-11-30 |
CN102812514A (zh) | 2012-12-05 |
US20130119015A1 (en) | 2013-05-16 |
JP5813628B2 (ja) | 2015-11-17 |
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