CN104918752A - Resin-bond wire saw - Google Patents
Resin-bond wire saw Download PDFInfo
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- CN104918752A CN104918752A CN201380070217.3A CN201380070217A CN104918752A CN 104918752 A CN104918752 A CN 104918752A CN 201380070217 A CN201380070217 A CN 201380070217A CN 104918752 A CN104918752 A CN 104918752A
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- Prior art keywords
- resin
- scroll saw
- resinoid bond
- weight portion
- bonded
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Classifications
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- 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
- B24B27/00—Other grinding machines or devices
- B24B27/06—Grinders for cutting-off
- B24B27/0633—Grinders for cutting-off using a cutting wire
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23D—PLANING; SLOTTING; SHEARING; BROACHING; SAWING; FILING; SCRAPING; LIKE OPERATIONS FOR WORKING METAL BY REMOVING MATERIAL, NOT OTHERWISE PROVIDED FOR
- B23D61/00—Tools for sawing machines or sawing devices; Clamping devices for these tools
- B23D61/18—Sawing tools of special type, e.g. wire saw strands, saw blades or saw wire equipped with diamonds or other abrasive particles in selected individual positions
- B23D61/185—Saw wires; Saw cables; Twisted saw strips
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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
Abstract
To provide a resin-bond wire saw having good cutting performance and a long lifespan. [Solution] A resin-bond wire saw in which abrasive grains are fixed to the surface of the wire by a resin bond containing a novolac-type phenol resin, a resol-type phenol resin, and an amine-based silane coupling agent. The resin bond shows a plurality of peaks at intervals of 208 (m/z) that represent fragments in positive ions in MALDI-TOF-MS (mass spectrometry), and a peak that corresponds to a softening point at 175 DEG C to 182 DEG C in TG-DTA (differential thermal analysis).
Description
Technical field
The present invention relates to the resin-bonded scroll saw (resin bond wire saw) used in the cutting of silicon ingot etc.Abrasive particle is fixed on line and forms by resin-bonded scroll saw resinoid bond (resin adhesive).Line for cutting is also referred to as " sawline ", is called " scroll saw " in present specification.
Background technology
Up to now, in the cutting of silicon ingot, use inside diameter saw slicer (inner diameter saw dicer) always.But along with the maximization of silicon ingot, inner circumferential sword slicer there will be the problems such as productivity ratio reduces, generation affected layer, dimensional accuracy are low, the maximization of device.Therefore, the cutting using scroll saw is implemented in recent years gradually.The cutting of scroll saw is used to be easy to tackle the maximization of ingot casting.In addition, multiple wafer can be obtained by 1 cutting.
Free abrasive scroll saw and bonded-abrasive scroll saw is had in scroll saw.Free abrasive scroll saw uses the lines such as piano wire and makes abrasive particle be scattered in the abrasive particle liquid of liquid.Abrasive particle is diamond particle, silicon-carbide particles etc.Free abrasive scroll saw, while abrasive particle drop is added to cutting part, makes line move and carry out cutting (patent document 1: Japanese Unexamined Patent Publication 2008-103690).Free abrasive scroll saw cuts ingot casting by the abrasive particle be clipped between line and ingot casting.
In free scroll saw, change due to the viscosity with temperature of abrasive particle liquid, therefore, the uneven thickness of wafer or the flatness of wafer are deteriorated.In addition, the line of free abrasive scroll saw also can wear and tear because of abrasive particle, therefore, is difficult to use thin line.And then, for free abrasive scroll saw, there is the worry that can form thick affected layer at crystal column surface.
In order to solve the problem of free abrasive scroll saw, proposing and abrasive particle being fixed on line surface and the scheme of bonded-abrasive scroll saw that obtains.As method abrasive particle being fixed on line surface, there are electrodeposition process, braze welding, resin-bonded method.
Electrodeposition process is the method (patent document 2: Japanese Patent Publication 4-4105, patent document 3: Japanese Unexamined Patent Publication 2003-334763) by nickel plating etc., abrasive particle being fixed on line surface.In electrodeposition process, in nickel plating liquid, nickel is made to separate out in line surface, while be embedded in nickel film by abrasive particle.Electrodeposition process is fixing comparatively firm due to abrasive particle, and therefore, the cutting performance of ingot casting is excellent.
In electrodeposition process, fix buried for abrasive particle in coating layer.Electrodeposition process, owing to needing thick plating epithelium, is therefore produced rate variance, cost is increased.And then line is thicker because of nickel coating layer, and therefore, line easily produces fatigue fracture.
In braze welding, online surface forms braze layer, and abrasive particle is imbedded the braze layer to melting, makes braze layer solidify and be fixed by abrasive particle (patent document 4: Japanese Unexamined Patent Publication 2006-123024).When the fusing point of hard solder is high, during braze layer melting, line is overheated, thus causes the intensity of line to reduce.Therefore, in braze welding, the selection of wire material is difficult.Be difficult to be used in piano wire, hard steel line that intensity under low temperature reduces, and use stainless steel wire, tungsten line.Otherwise in the low-melting situation of hard solder, frictional heat when having the cutting of hard solder because of ingot casting and melting, cause the worry of Grain Falling Off.
In resin-bonded method, the resinoid bond (resin adhesive) of liquid state and the mixture of abrasive particle are coated line surface, and utilizes sintering furnace to carry out heating (patent document 4: Japanese Unexamined Patent Publication 2006-123024).Utilize the resinoid bond that solidifies by heating and abrasive particle fixed (patent document 5: Japanese Unexamined Patent Publication 2000-263452, patent document 6: Japanese Unexamined Patent Publication 2000-271872, patent document 7: public table patent WO98/35784 again).As sintering furnace, there will be a known hot-air drying stove (patent document 8: Japanese Unexamined Patent Publication 09-35556, patent document 9: Japanese Unexamined Patent Publication 2010-267533).
Resin-bonded method is applicable to make cheap and rectangular scroll saw.And then, because the vibration of the scroll saw produced in the cutting of ingot casting can be absorbed by the resinoid bond of softness, therefore, scroll saw can be made stable mobile at high speed.In addition, thin wafer can be obtained.On the other hand, the confining force of the abrasive particle of resin-bonded scroll saw is lower, and therefore, in cutting, abrasive particle easily comes off.When using the resinoid bond of thermohardening type, the solidification due to resinoid bond needs long-time, and therefore the manufacture of scroll saw can spended time.In addition, if at high temperature carry out the solidification of resinoid bond, then bubble can be produced because of volatile ingredient.
Prior art document
Patent document
Patent document 1: Japanese Unexamined Patent Publication 2008-103690 publication
Patent document 2: Japanese Patent Publication 4-4105 publication
Patent document 3: Japanese Unexamined Patent Publication 2003-334763 publication
Patent document 4: Japanese Unexamined Patent Publication 2006-123024 publication
Patent document 5: Japanese Unexamined Patent Publication 2000-263452 publication
Patent document 6: Japanese Unexamined Patent Publication 2000-271872 publication
Patent document 7: public table patent WO98/35784 publication again
Patent document 8: Japanese Unexamined Patent Publication 09-35556 publication
Patent document 9: Japanese Unexamined Patent Publication 2010-267533 publication
Summary of the invention
the problem that invention will solve
The object of the invention is to, provide cutting performance good and long-life resin-bonded scroll saw.
for the scheme of dealing with problems
The discoveries such as the present inventor, can reach object of the present invention: (1) uses the resin comprising phenolic varnish type (novolak type) phenolic resins, resol type (resol type) phenolic resins and amine silane coupler as resinoid bond by the following method; (2) by infrared radiation, resinoid bond is solidified.By the present invention, few long-life resin-bonded scroll saw that comes off of cutting performance excellence, abrasive particle can be manufactured expeditiously.
In resin-bonded scroll saw of the present invention, utilize the resinoid bond using phenolic resins as principal component and online surperficial bonded-abrasive.By utilizing the mass spectral analysis of MALDI-TOF-MS method to detect, cation represents the peak of the fragment at 208 (m/z) interval to the resinoid bond used in the present invention.In addition, by TG-DT A spectrum (TG-DTA) method, detect at 175 DEG C ~ 182 DEG C the peak being equivalent to softening point.(MALDI: substance assistant laser desorpted ionized method, TOF-MS: flying time mass spectrum analysis method).
The resinoid bond used in the present invention comprises novolak phenolics: 100 weight portions, resol type phenol resin: 10 weight portion ~ 30 weight portions, amine silane coupler: 0.1 weight portion ~ 5 weight portion.
the effect of invention
According to the present invention, achieve the good and long-life resin-bonded scroll saw of cutting performance.
Accompanying drawing explanation
Fig. 1 is the key diagram of the method for the paste coated on line being carried out to infrared heating.
Fig. 2 is that the energy of lamp divides Light distribation.
Fig. 3 is the cation mensuration figure (comparative example) of the mass spectral analysis utilizing MALDI-TOF-MS method.
Fig. 4 is the cation mensuration figure (embodiment 1) of the mass spectral analysis utilizing MALDI-TOF-MS method.
Fig. 5 is the anion mensuration figure (comparative example) of the mass spectral analysis utilizing MALDI-TOF-MS method.
Fig. 6 is the anion mensuration figure (embodiment 1) of the mass spectral analysis utilizing MALDI-TOF-MS method.
Fig. 7 is the differential thermal analysis curve of embodiment 1 and comparative example.
Detailed description of the invention
Resin-bonded scroll saw of the present invention utilizes the resinoid bond comprising novolak phenolics, resol type phenol resin and amine silane coupler that abrasive particle is fixed on line surface.
Novolak phenolics is the resin making the aldehyde such as phenolic compounds and formaldehyde such as phenol, cresols, bisphenol-A that condensation reaction occur under acidic catalyst.Resol type phenol resin is the resin making the aldehyde such as phenolic compounds and formaldehyde such as phenol, cresols, bisphenol-A that condensation reaction occur under base catalyst.
Resinoid bond can also comprise curing agent.Relative to novolak phenolics 100 weight portion, curing agent preferably comprises 5 weight portion ~ 20 weight portions.
Relative to novolak phenolics 100 weight portion, when curing agent is more than 20 weight portion, produces gas because of the decomposition of curing agent and can cause the generations such as expansion, be full of cracks.Relative to novolak phenolics 100 weight portion, when curing agent is lower than 5 weight portion, when resol type phenol resin compounding few, there is the worry that the solidification of novolac resin becomes insufficient.Now, although increment can be carried out to resol type phenol resin, in contrast to this, the compounding amount of curing agent is preferably increased in the scope of 5 weight portion ~ 20 weight portions.If add curing agent with aforementioned proportion, then shorten the hardening time of paste described later (paste).
As curing agent, such as, can enumerate: methenamine, melamine methylol, methylolurea etc.Wherein, methenamine because hardening time is short preferably.
Resinoid bond can also contain phenolic compounds 5 weight portion ~ 15 weight portions such as phenol, cresols, bisphenol-A.In addition, also can containing below aldehyde 1 weight portions such as formaldehyde.And then, as long as be also can contain base catalyst, moisture on a small quantity.
Resinoid bond comprises resol type phenol resin 10 weight portion ~ 30 weight portion relative to novolak phenolics 100 weight portion, therefore, utilizes crosslinked and forms fine and close three dimensional network structure.Thus, resinoid bond engages securely with abrasive particle.Relative to novolak phenolics 100 weight portion, when resol type phenol resin is more than 30 weight portion, the viscosity of paste becomes too low, can become and be difficult to paste to be coated on line.Relative to novolak phenolics 100 weight portion, when resol type phenol resin is lower than 10 weight portion, the curing rate of resinoid bond is slack-off.Therefore, make paste curing become difficult at short notice, the speed of production of resin-bonded scroll saw is slack-off.
During the amine silane coupler of 0.1 weight portion ~ 5 weight portion compounding relative to novolak phenolics 100 weight portion, the adhesive strength of resinoid bond and line increases.Relative to novolak phenolics 100 weight portion, when amine silane coupler is lower than 0.1 weight portion, the increase of adhesive strength cannot be expected.Relative to novolak phenolics 100 weight portion, when amine silane coupler is more than 5 weight portion, harmful effect can be caused to the solidification of novolak phenolics.
As amine silane coupler, can enumerate: 3-TSL 8330, N-2-(amino-ethyl)-3-TSL 8330, N-2-(amino-ethyl)-3-amino propyl methyl dimethoxysilane APTES etc.
Resinoid bond comprises novolak phenolics: 100 weight portions, resol type phenol resin: 10 weight portion ~ 30 weight portions, amine silane coupler: 0.1 weight portion ~ 5 weight portion.By using this resinoid bond, the good and long-life resin-bonded scroll saw of cutting performance can be obtained.
The manufacture method manufacturing resin-bonded scroll saw of the present invention comprises: (a) prepares the operation of paste (comprising resinoid bond, solvent, abrasive particle, filler); The operation of (b) ready line; C the operation on the surface of line coated by paste by (); D () carries out infrared heating to be coated with paste and the operation making it solidify.
By infrared heating, the dehydrating condensation of resinoid bond can promptly carry out, thus forms fine and close three-dimensional crosslinking structure.
Utilize distributor method or floating die general laws etc., paste is coated on the line of movement.The mode that the coating weight of paste reaches 50 ~ 120 with the concentration degree of abrasive particle sets.The concentration degree of abrasive particle refers to the ratio shared by area of abrasive particle in the projected area on line surface.In this manual, when the projected area in total projection area shared by abrasive particle is 15%, concentration degree is denoted as 100.Such as, when the projected area in total projection area shared by abrasive particle is 30%, concentration degree is 200, and when the projected area in total projection area shared by abrasive particle is 7.5%, concentration degree is 50.
About the viscosity of paste, in resinoid bond, add solvent and be set to 3Pas ~ 6Pas.The scope of the amount of solvent preferred 100 weight portion ~ 200 weight portions relative to resinoid bond 100 weight portion.Solvent is not particularly limited, but when considering reactivity, preferred lower boiling orthoresol.
Abrasive particle is not particularly limited, can uses: diamond abrasive grain, CBN abrasive particle, alumina abrasive grain, silicon carbide abrasive particles etc.
The thermal conductivity of diamond abrasive grain is high, and therefore, when carrying out infrared heating, the dash area of abrasive particle also can promptly heat up.Thus, in order to the solidification of resinoid bond is carried out equably, preferably diamond abrasive grain is used.The size of abrasive particle can be selected according to target or according to wire diameter, but in order to reduce saw kerf loss (cutting loss), is preferably several μm ~ 25 μm.As abrasive particle, also preferably by diamond abrasive grain that the metal film such as nickel, titanium is coating.But, the efficiency of silicon solar cell can be caused to reduce because of copper atom by the diamond abrasive grain that copper film is coated to, thus not preferred.Compared with electrodeposition process scroll saw, warpage, the kerf (saw mark) of the Silicon Wafer that the resin-bonded scroll saw using nickel film to be coated to diamond abrasive grain cuts are few.
In order to avoid being considered to be worth doing the blocking caused by silicon, it is desirable to abrasive particle and be moderately scattered in line surface.Preferably, abrasive particle 50 weight portion ~ 120 weight portions compounding relative to resinoid bond 100 weight portion.
As line, be preferably steel wire.To wire diameter, there is no particular limitation, but be preferably 0.05mm φ ~ 0.3mm φ.As steel wire, be suitably: the wire rod be made up of the heat treatment such as high-carbon steel, medium carbon low alloy steel spring steel; The wire rod be made up of processed springs steel such as hard steel line, piano wire, stainless steel wire, cold rolling steel wire, oil-temper steel wires; The steel wire rod of the high tenacity/high-fatigue strengths such as low-alloy steel, medium alloy steel, high-alloy steel, Maraging steel.
While make the line being coated with paste move limit carry out infrared heating, make paste curing.When utilizing enamelling kiln etc. in the past to carry out Hot-blast Heating, start heat cure occurs from the surface of paste, therefore, the water generated because of reaction is closed in paste inside, produces bubble sometimes.On the other hand, when infrared heating is carried out to paste, because the near infrared ray of wavelength about 1 μm can be absorbed expeditiously by water, therefore can complete cross-linked polymeric at short notice.When carrying out infrared heating to paste, because water evaporates at short notice, therefore paste not easily produces bubble.Infrared ray preferably has the peak of spectrum in the near infrared frequency band of wavelength 0.7 μm ~ 2.5 μm.The near infrared ray of wavelength about 1 μm (0.9 μm ~ 1.3 μm) can suppress the bubble produced along with the gasification of the water generated, therefore particularly preferably.
When utilizing infrared heating, to be cured reaction at a high speed, uniform higher structure can be obtained compared with Hot-blast Heating.Its result, in resinoid bond after hardening, by utilizing the mass spectral analysis of MALDI-TOF-MS method, cation detection goes out the peak of the fragment at expression 208 (m/z) interval.In addition, utilize differential thermal analysis (DTA) method, detect at 175 DEG C ~ 182 DEG C the clear and definite peak being equivalent to softening point.It should be noted that, the temperature at peak is slightly different because of programming rate during differential thermal analysis etc.Peak in differential thermal analysis also reflects uniform higher structure while the peak of fragment belonging to expression 208 (m/z) interval.By uniform higher structure, the hardness of resinoid bond increases, thus keeps abrasive particle securely.Thus, the resin-bonded scroll saw of cutting performance excellence can be obtained.
Fig. 1 is the key diagram line being coated with paste being carried out to infrared heating.In the method for Fig. 1, the infrared heater 4 of the linearity of the concave mirror 2 using half cartridge type and the length direction being configured at concave mirror 2.Make the line 3 being coated with paste mobile along the length direction (vertical direction of paper) of concave mirror 2.Reflect the infrared ray from infrared heater 4 by reflecting surface 8, make the light collecting part 6 (heating region) that it is concentrated on about 10mm φ.Also multiple concave mirror 2 and infrared heater 4 can be configured in the mode of the mobile route surrounding line 3.
The length of light collecting part 6 depends on infrared heater 4, the size of concave mirror 2, number.The line 3 being coated with paste is moved, and infrared heating is carried out to paste.The length of light collecting part 6 is set to such as 400mm ~ 1000mm.In order to increase light collecting part 6, also can online 3 the upper multiple infrared heater 4 of arranged in series of moving direction (vertical direction of paper).
As infrared heater 4, preferably there is near infrared range the infrared lamp at peak.As infrared lamp, such as, can use: xenon short-act lamp (short-arcxenon lamp), in quartz glass tube, enclose the lamp of tungsten filament.
The temperature measuring the line 3 of movement in light collecting part 6 is difficult.Therefore, the situation that the fracture strength being conceived to the line 3 caused because of heating reduces, arranges the heating-up temperature of 95% of the fracture strength before can guaranteeing heating.By experiment, utilize the temperature of the sheath thermocouple measurement light collecting part 6 of 1mm diameter, result is 500 DEG C ~ 800 DEG C.Use the infrared heating device of Fig. 1, make line with 1000mm/ second ~ speed of 2000mm/ second moves, and it can be made to solidify and resinoid bond can not be made to foam.
As infrared heating method, can for irradiating the method for infrared laser.
In paste, compounding have the filler (filler) formed by inorganic particle.Filler can suppress the thermal expansion/thermal contraction of resinoid bond, reduces the Grain Falling Off in cutting.Filler relative to resinoid bond 100 weight portion, preferably compounding 20 weight portion ~ 100 weight portions, further preferred compounding 30 weight portion ~ 60 weight portions.As filler, the diamond particle being of a size of 2 μm ~ about 3 μm is applicable, but also can use other inorganic material (such as silicon-carbide particles).
If heat again the resin-bonded scroll saw implementing infrared heating, then stable performance.By heating again, the thermal deformation that line and paste produce when infrared heating can be eliminated.Exist hardly cause the fracture strength of resin-bonded scroll saw because heating again, the molecular structure of resinoid bond changes.
Heating preferably carries out 1 hour ~ 5 hours at temperature 100 DEG C ~ 200 DEG C again.Although the time of heating again is long, owing to multiple volume can be had the bobbin of resin-bonded scroll saw (bobbin) heat again in the lump, therefore will the productivity ratio of resin-bonded scroll saw be caused significantly to reduce because heating again.By by infrared heating and heating in combination again, the high production rate of resin-bonded scroll saw can be obtained.
Resin-bonded scroll saw of the present invention penetraction depth compared with resin-bonded scroll saw is in the past large." penetraction depth " refer to test sheet (piece) is cut, scroll saw broken string time penetraction depth.The broken string of scroll saw mainly causes because of coming off of abrasive particle.Resin-bonded scroll saw of the present invention is compared with resin-bonded scroll saw in the past, and the constant intensity of abrasive particle is large, and therefore penetraction depth is large.
Any person in the warpage of the wafer of resin-bonded scroll saw of the present invention, expansion, thickness deviation (TTV) is compared with resin-bonded scroll saw in the past all excellent more than 25%.Utilize resin-bonded scroll saw of the present invention, compared with resin-bonded scroll saw in the past, the wafer of the value little about 20% of surface roughness (Ra, Ry) can be obtained.Utilize resin-bonded scroll saw of the present invention, the wafer that the processing upgrading layer on surface is few can be obtained.Utilize resin-bonded scroll saw of the present invention, the wafer that bending strength is high can be obtained.
Embodiment
The cutting performance of resin-bonded scroll saw of the present invention is confirmed by following experiment.
Use the resinoid bond of following formula, modulate the paste of following formula, and manufacture resin-bonded scroll saw by following production line.
[embodiment 1]
(1) formula of resinoid bond
(2) formula of paste
(3) production line of resin-bonded scroll saw
The summary of (a) line
Line conveyer → apparatus for coating → heater → coiling machine → reheating furnace
(b) line conveyer: feeding wrapper is in the device of the line of bobbin.
(c) apparatus for coating: utilize the mould of water jet (water jet) shape to be uniformly coated with the device of paste online.
(d) heater: the device that the line being coated with paste is heated.
Infrared gilded image furnace (gold image furnace) by ULVAC-RIKO, Inc. manufacture: connect 3 uses model RHL-E410-N (heated length 265mm, maximum output 4kw).Fig. 2 illustrates that the energy of lamp divides Light distribation.
(e) coiling machine: resin-bonded scroll saw is batched the device in bobbin.
(f) reheating furnace: utilize coiling machine to batching the convection oven heated in the resin-bonded scroll saw of bobbin.
(4) material and manufacturing condition
(a) line: piano wire (wire diameter: 120 μm, fracture strength: about 42N).
The translational speed of (b) line: 1200mm/ second.
The coating weight of (c) paste: 0.01g/m.
The temperature of (d) infrared gilded image furnace: 720 DEG C ~ 750 DEG C (thermocouple measurement).
(do not make the temperature of fracture strength lower than 40N of resin-bonded scroll saw.)
Temperature and time in (e) reheating furnace: 180 DEG C, 2 hours.
[embodiment 2]
(1) formula of resinoid bond
(2) formula of paste
Apart from the above, resin-bonded scroll saw has been manufactured similarly to Example 1.
[comparative example]
As resinoid bond, use commercially available novolak phenolics (manufacture of Sumitomo Bakelite Co., Ltd.); As heater, use vertical enamel sintering furnace.Vertical enamel sintering furnace is by circulating in adding hot-air and heating line in furnace core tube.Heater is nichrome wire.In vertical enamel sintering furnace, carry out furnace temperature 300 DEG C, the heating of 20 minutes heat times.In addition, resin-bonded scroll saw is obtained similarly to Example 1.
The penetraction depth of the penetraction depth of the resin-bonded scroll saw of embodiment 1,2 and the resin-bonded scroll saw of comparative example is compared.
(1) penetraction depth test method
The polycrystal silicon sheet of 1cm × 1cm × 2mm is arranged at the top of the resin-bonded scroll saw of horizontal development, polycrystal silicon sheet is declined mobile, measure penetraction depth.The decrease speed of sheet: 0.9mm/ minute.
(2) condition is cut
Resinoid bond line moves: the reciprocating motion of amplitude 80mm, speed 400mm/ minute.
(3) cut-in timing: until broken string.
Table 1 illustrates the result that penetraction depth is tested.Table 2 illustrates the abrasive particle residual rate of the line after test.
[table 1]
| Sample | Embodiment 1 | Embodiment 2 | Comparative example |
| Penetraction depth (mm) | 11.0 | 11.0 | 6.5 |
[table 2]
| Sample | Embodiment 1 | Comparative example |
| Abrasive particle residual rate (%) | 92 | 50 |
As shown in table 1, the penetraction depth of the resin-bonded scroll saw of embodiment 1,2 is about 1.7 times of the penetraction depth of the resin-bonded scroll saw of comparative example.As shown in table 2, the abrasive particle residual rate of the resin-bonded scroll saw of embodiment 1 is about 1.8 times of the abrasive particle residual rate of the resin-bonded scroll saw of comparative example.
In order to study the reason of this difference, the hardness of the resinoid bond that have cured is studied.
Example 1: the resinoid bond used in embodiment 1 is heating and curing.Heating condition: with 15 DEG C/h from room temperature to 180 DEG C, keeps 2 hours at 180 DEG C.
Example 2: under the heating condition identical with situation 1 to comparative example in the novolak phenolics that uses be heating and curing.
Use the hardometer (ATK-F3000 manufactured by Co., Ltd.'s alum making; Use 1/4 cun of steel ball, load 100kgf), the Rockwell hardness of the hardness of the solidfied material obtained is measured.Show the result in table 3.
[table 3]
| Sample | Example 1 | Example 2 |
| Rockwell hardness (HRM) | 111.6 | 109.7 |
As shown in Table 3: compared with the resinoid bond of comparative example, the hardness of the resinoid bond of embodiment 1 is high.This is one of reason that the penetraction depth of resin-bonded scroll saw of the present invention is large.
[analysis]
The network molecular structure of the resinoid bond of embodiment 1 and the resinoid bond of comparative example and physical property are studied.
MALDI-TOF-MS method is utilized to carry out mass spectral analysis.(MALDI: substance assistant laser desorpted ionization method, TOF-MS: flying time mass spectrum analysis method).
Use equipment: the AXIMA-CFR that Shimadzu Seisakusho Ltd. manufactures
+(SHIMADZU).
Analytical model: linear model (cation, Anionic recognition).
Vacuum: 10
-5below Pa.
Matrix: DHB.
Optical maser wavelength: 337nm (N_2 laser).
Fig. 3 ~ Fig. 6 represents the mensuration figure of the mass spectral analysis utilizing MALDI-TOF-MS method.Fig. 3 is the cation detection figure of the resinoid bond of comparative example.Fig. 4 is the cation detection figure of the resinoid bond of embodiment 1.Fig. 5 is the Anionic recognition figure of the resinoid bond of comparative example.Fig. 6 is the Anionic recognition figure of the resinoid bond of embodiment 1.
The peak (arrow) of the fragment at expression 208 (m/z) interval is observed in Fig. 4 (embodiment 1).Infer and: the fragment at 208 (m/z) interval is at following structural formula (construction unit; C
14h
12o
2: molecular weight 212) in, because of what produce 4 site cross fracture (fragment) containing aromatic rings.
It demonstrates in the resinoid bond of embodiment 1, and following structure arranges in net high-polymer structure regularly with the form repeating fragment.
The peak (arrow) of the fragment representing fixed intervals is not detected in Fig. 3, Fig. 5, Fig. 6.Therefore, think: in the resinoid bond of comparative example, there is not the structure that chemical formula 1 represents.
The above results from relevant with Fig. 3 ~ Fig. 6: represent that the molecular structure of the fragment at 208 (m/z) interval produces because carrying out infrared heating to resinoid bond.
Fig. 7 represents the differential thermal analysis curve of the resinoid bond of embodiment 1 and the resinoid bond of comparative example.
Operative installations: TG8120 (Rigaku).
Programming rate: 10 DEG C/min (minute).
Atmosphere: N
2air-flow.
Standard substance: aluminium oxide (Al
2o
3).
Sample weight: about 10mg.
In the figure of the resinoid bond of the embodiment 1 shown in Fig. 7, observe the peak of clear and definite softening point at 175 DEG C ~ 182 DEG C.On the other hand, the resinoid bond of comparative example only observes the peak of indefinite softening point near 190 DEG C.Think the resinoid bond of comparative example due to higher structure uneven, therefore can not occur with structure change transfer, do not observe the peak of clear and definite softening point.Think that the resinoid bond of embodiment 1 is owing to possessing the higher structure of the fragment based on 208 (m/z) interval, therefore hardness is high.Think that the low reason of the hardness of resinoid bond of comparative example is because higher structure is uneven.
utilizability in industry
If use resin-bonded scroll saw of the present invention, then can cut out the wafer of high-quality expeditiously from silicon ingot.
Claims (2)
1. a resin-bonded scroll saw, in order to utilize phenolic resins, as the resinoid bond of principal component, online surface is fixed with the resin-bonded scroll saw of abrasive particle for it,
Described resinoid bond is in the mass spectral analysis utilizing MALDI-TOF-MS method, and cation demonstrates multiple peaks of the fragment at expression 208 (m/z) interval,
In the differential thermal analysis utilizing TG-DTA method, demonstrate at 175 DEG C ~ 182 DEG C the peak being equivalent to softening point.
2. resin-bonded scroll saw according to claim 1, wherein, described resinoid bond comprises: novolak phenolics 100 weight portion, resol type phenol resin 10 weight portion ~ 30 weight portion, amine silane coupler 0.1 weight portion ~ 5 weight portion.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2013002792A JP5792208B2 (en) | 2013-01-10 | 2013-01-10 | Resin bond wire saw |
| JP2013-002792 | 2013-01-10 | ||
| PCT/JP2013/082639 WO2014109149A1 (en) | 2013-01-10 | 2013-12-04 | Resin-bond wire saw |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104918752A true CN104918752A (en) | 2015-09-16 |
| CN104918752B CN104918752B (en) | 2016-04-20 |
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| CN201380070217.3A Expired - Fee Related CN104918752B (en) | 2013-01-10 | 2013-12-04 | Resin-bonded scroll saw |
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| JP (1) | JP5792208B2 (en) |
| KR (1) | KR101594747B1 (en) |
| CN (1) | CN104918752B (en) |
| MY (1) | MY168372A (en) |
| SG (1) | SG11201504210SA (en) |
| TW (1) | TWI519366B (en) |
| WO (1) | WO2014109149A1 (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2016171018A1 (en) * | 2015-04-20 | 2016-10-27 | 株式会社Tkx | Method for producing fine silicon powder, and method for producing fine silicon nitride powder |
| JP7002935B2 (en) * | 2015-05-21 | 2022-01-20 | 三井化学東セロ株式会社 | Manufacturing method of gas barrier laminate |
| SG11201804316UA (en) * | 2016-05-24 | 2018-06-28 | Tkx Corp | Device for manufacturing coated wire |
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| JP2001259993A (en) * | 2000-03-10 | 2001-09-25 | Noritake Diamond Ind Co Ltd | Resin bond wire saw |
| CN1784292A (en) * | 2003-05-09 | 2006-06-07 | 戴蒙得创新股份有限公司 | Abrasive particles having coatings with tortuous surface topography |
| CN101445587A (en) * | 2008-12-26 | 2009-06-03 | 南京师范大学 | Resin binding agent for a diamond wire saw and preparation method thereof |
| CN101712135A (en) * | 2008-09-30 | 2010-05-26 | 日本则武超精密磨料磨具有限公司 | Resin bonder wire saw |
| CN102513609A (en) * | 2011-12-28 | 2012-06-27 | 山东大学 | Resin bond consolidation abrasive wire saw production system |
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| KR940001070B1 (en) * | 1990-12-29 | 1994-02-12 | 고려화학 주식회사 | Preparation of epoxy resin compositions for encapsulating semiconductor |
| JP3734854B2 (en) | 1995-07-18 | 2006-01-11 | 古河電気工業株式会社 | Hot air circulation type individual multiple enamel wire baking furnace and method for producing enamel wire using the same |
| US6070570A (en) * | 1997-02-14 | 2000-06-06 | Sumitomo Electric Industries, Ltd. | Wire-saw and its manufacturing method |
| JP2000263452A (en) | 1999-03-12 | 2000-09-26 | Osaka Diamond Ind Co Ltd | Super-abrasive grain wire saw |
| JP2000271872A (en) | 1999-03-23 | 2000-10-03 | Osaka Diamond Ind Co Ltd | Super abrasive grain resin bond wire saw |
| JP2008006584A (en) * | 2000-05-15 | 2008-01-17 | Allied Material Corp | Cutting method using super-abrasive grain wire saw |
| JP2003334763A (en) | 2002-05-16 | 2003-11-25 | Read Co Ltd | Fixed abrasive grain wire saw |
| JP2006123024A (en) | 2004-10-26 | 2006-05-18 | Nakamura Choko:Kk | Fixed abrasive grain type wire saw and its manufacturing method |
| JP4703448B2 (en) * | 2006-03-22 | 2011-06-15 | 株式会社ノリタケスーパーアブレーシブ | Resin bond wire saw |
| JP2008103690A (en) | 2007-08-24 | 2008-05-01 | Mitsubishi Electric Corp | Slurry used for cutting silicon ingot |
| JP5443825B2 (en) | 2009-05-15 | 2014-03-19 | 古河電気工業株式会社 | Enamel wire printing equipment |
-
2013
- 2013-01-10 JP JP2013002792A patent/JP5792208B2/en not_active Expired - Fee Related
- 2013-12-04 CN CN201380070217.3A patent/CN104918752B/en not_active Expired - Fee Related
- 2013-12-04 KR KR1020157011316A patent/KR101594747B1/en not_active IP Right Cessation
- 2013-12-04 SG SG11201504210SA patent/SG11201504210SA/en unknown
- 2013-12-04 MY MYPI2015001761A patent/MY168372A/en unknown
- 2013-12-04 WO PCT/JP2013/082639 patent/WO2014109149A1/en active Application Filing
- 2013-12-18 TW TW102146989A patent/TWI519366B/en not_active IP Right Cessation
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001259993A (en) * | 2000-03-10 | 2001-09-25 | Noritake Diamond Ind Co Ltd | Resin bond wire saw |
| CN1784292A (en) * | 2003-05-09 | 2006-06-07 | 戴蒙得创新股份有限公司 | Abrasive particles having coatings with tortuous surface topography |
| CN101712135A (en) * | 2008-09-30 | 2010-05-26 | 日本则武超精密磨料磨具有限公司 | Resin bonder wire saw |
| CN101445587A (en) * | 2008-12-26 | 2009-06-03 | 南京师范大学 | Resin binding agent for a diamond wire saw and preparation method thereof |
| CN102513609A (en) * | 2011-12-28 | 2012-06-27 | 山东大学 | Resin bond consolidation abrasive wire saw production system |
Also Published As
| Publication number | Publication date |
|---|---|
| KR101594747B1 (en) | 2016-02-16 |
| CN104918752B (en) | 2016-04-20 |
| SG11201504210SA (en) | 2015-07-30 |
| TW201433391A (en) | 2014-09-01 |
| KR20150102946A (en) | 2015-09-09 |
| JP5792208B2 (en) | 2015-10-07 |
| JP2014133288A (en) | 2014-07-24 |
| WO2014109149A1 (en) | 2014-07-17 |
| TWI519366B (en) | 2016-02-01 |
| MY168372A (en) | 2018-10-31 |
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