CN104955601B - There is the fixed abrasive sawline at nickel oxide interface between nickel subgrade - Google Patents
There is the fixed abrasive sawline at nickel oxide interface between nickel subgrade Download PDFInfo
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- CN104955601B CN104955601B CN201480006664.7A CN201480006664A CN104955601B CN 104955601 B CN104955601 B CN 104955601B CN 201480006664 A CN201480006664 A CN 201480006664A CN 104955601 B CN104955601 B CN 104955601B
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- nickel
- subgrade
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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
- 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
- B23D65/00—Making tools for sawing machines or sawing devices for use in cutting any kind of material
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- Polishing Bodies And Polishing Tools (AREA)
Abstract
The fixed abrasive sawline of invention is described, it includes metal core wire, attachment is in the abrasive grain in electroless nickel layer in the metal core wire.The electroless nickel layer includes the subgrade of two or more stackings, wherein there is the interface containing nickel oxide between at least one pair of continuous subgrade.Nickel oxide layer serves as preferred fracture plane during sawing.Therefore, compared with such conventional fixed abrasive sawline, it is easier to disclose abrasive grain in use first.This does not cause increased total abrasion of the line.Therefore the fixed abrasive sawline of the present invention need not be repaired before the use.In addition, describing different illustrative methods to introduce nickel oxide layer between nickel dam.
Description
Specification
Technical field
The present invention relates to available for the fixed abrasive sawline for cutting hard and crisp material, the wherein sawline has by electrolysis
The nickel dam of storing and the abrasive grain for being attached to metal base line.
Background technology
Hard and crisp material such as sapphire, silicon, quartz, carborundum, GaAs, the magnetic material or other high for cutting
The major technique of expensive material is always to use internal diameter saw blade.Article to be cut is introduced to the tension of rotation in such saw
Saw blade centre bore in.The inner edge of the saw blade is coated with diamond nickel composite material.The technology have saw kerf loss (due to
The loss of material that cutting width is caused) and productivity ratio (because its concern sequence of maneuvers) in terms of shortcoming.
Destructive technology gushes with the development of the single scroll saw of multiloop (known generally with the title " multi-wire saw " of mistake)
It is existing.In such " multi-wire saw ", above one group of two or more groove capstan winch in the loop arranged parallel to each other
Very thin steel wire is guided, gauze is consequently formed.(for example poly- second of resisting medium can be usually suspended in by using abrasive slurries
Carborundum in glycol, loose abrasive saw) or by abrasive material be attached to line in itself (fixed abrasive saw) come obtain saw effect.Pass through
Capstan winch drives the line with reciprocating pattern or single direction movement.Multi-wire saw allows very thin saw kerf (being less than 150 μm) and single
The parallel processing chip of more than 1000 (be processed into sometimes specific loading) of individual ingot, causes increased productivity ratio and material cost
Big saving.
Although the use of abrasive slurries is now widely used for the silicon that will be used in solar cell industry or semi-conductor industry
Wafer slice, but it brings some disadvantages associateds of slurry management aspect really, cause increased Environmental costs (must with by
The mode of control abandons slurry), technology controlling and process cost (silicon and iron from steel wire are loaded with due to slurry, it is necessary to it is carried out often
Update) and running stores cost (abrasive material and line that are worn and torn in technique).
Abrasive material is wherein fixed on to the use of " the fixed abrasive sawline " of base material line has these lesser degree of shortcomings, only
It is that cooling agent must be used to wash away the bits cut away.The cooling agent is mainly comprising material to be cut, and the material is therefore
Readily available recycling.However, the requirement for line in itself is severeer：
- abrasive grain must be well attached in base material line, because the effect reduces when abrasive material loses in saw effect；
- for size, shape, hardness and acutance, the selection of abrasive grain is important；
- the line do not merely have to by force enough to keep cutting tension force (normally about 25N) and also it enter workpiece in when it is necessary
Dynamically good operating ratio loose abrasive saw is more about hundred times.
The distinct methods that abrasive grain is attached to base material line are developed, wherein most prominent method is by bonding
Metal or welding metal, by resin, by mechanical indentation or by including abrasive material is adhered in electrolytic metal retaining layer.To the greatest extent
The technology that pipe is won is not clear, but later approach must be good candidate.Abrasive material is maintained at and provided well
In abrasive material confining force and the electrolytic nickel coatings of good wearability.The related application for describing this technology is
US7704127, EP1886753 and EP2277660.
Mainly diamond is used for abrasive grain.In order to very well keep diamond particles, with semi-conducting layers (example
Such as titanium carbide TiC, carborundum SiC, referring to US 7704127) or conducting shell (nickel, nickel-phosphor Ni-P, referring to EP2277660) plating
The diamond particles.So, also with the diamond particles are coated outside metal level, thus it is further kept in the coating.
But the diamond particles must be had this of nickel before the diamond particles can actually start cutting
External coating is removed from diamond particles.Starting saw process when the external coating is still suffered from causes initial increased saw frame.By nickel
After external coating is removed from the top of diamond particles, the particle can start effectively to cut.Sometimes this is referred to as：" line is repaiied
Whole (dress ing) " is the adjustment that line is used to saw.
The different ideas that " offline " prepares the line for service are suggested, for example, guide the line to pass through " finishing stone " (JP
181701) 2006 or pass through " inverse electrolysis " (JP 2011042561).Alternatively, it is proposed that line on the saw device it is specific
Intersection threading so that the line " self-training " before saw：Referring to JP 2011079073.However, these processes are not related to line
Independent processing, the adaptation of machine, or do not work simply.
The content of the invention
The main object of the present invention is to improve existing abrasive material sawline.It is easier present invention is primarily concerned with pre-shaping step is made.
Describe improved products and the method for preparing the product.
According to the first aspect of the invention, fixed abrasive sawline has been claimed.The invention product is related to such as claim 1
Described combinations of features.The special characteristic of the preferred embodiments of the invention is listed in the dependent claims.
In the first preferred embodiment of the present invention, fixed abrasive sawline is attached comprising metal core wire and in electroless nickel layer
The abrasive grain in metal core wire.The electroless nickel layer includes the nickel subgrade of two or more stackings.It is continuous at least one pair of
Subgrade between exist the interface containing nickel oxide.Illustrate alternatively but equivalently：The electroless nickel layer contains comprising at least one
There is the inner boundary layer of nickel oxide.
50 μm of size can be used until 300 μm of round wire is used as metal core wire.Generally by with the work(of material to be cut
Linear diameter can be selected.For example for monocrystalline silicon is cut into chip, small size diameter is favourable for example from 80 to 150 μm.
For cutting sapphire, the large-size of 150 μm to 250 μm (such as 175 μm) is preferred.For ingot cutting (such as crop)
Use even more big diameter：More than 250 μm, such as 300 μm.
The cored wire can be made by any metal with enough tensile strengths.Particularly preferably also show relatively high lead
Electrical metal, because electrolytic coating electric current passes through the cored wire (adding any layer that may be deposited) in coating procedure.
Ordinary carbon steel in terms of this particularly preferably with least 0.70wt% carbon, because the tensile strength that they are well combined
(being higher than 3000MPa) (is higher than 4.10 with relatively good electrical conductivity6S/m).With increased carbon content, electric conductivity is reduced, together
Shi Qiangdu increases.Although copper cash can hardly realize the tensile strength higher than 1000MPa with good electric conductivity.Can
High tensile can be drawn into but then lack sufficiently high electric conductivity by very well resisting the tungsten wire of heat.
Actual ordinary carbon steel composition not only includes iron and carbon, and comprising many other alloys and trace element, wherein
Some have profound influence to property of the steel in terms of intensity, ductility, formability, corrosion resistance.On the application, by force
Degree is important, and following element composition is preferred for ordinary carbon steel cored wire：
- at least 0.70wt% carbon, the upper limit depends on being formed other alloy element (see below)s of the line
- 0.30 to the manganese content between 0.70wt%；
- 0.15 to the silicone content between 0.30wt%；
- deposit element such as aluminium, sulphur (be less than 0.03wt%), phosphorus (being less than 0.30wt%), copper (being less than 0.60wt%)
Keeping to minimum value.
The surplus of-steel is iron and other elements
Carbon content for constituting (0.80%wt C) higher than eutectoid, chromium (0.005 to 0.30%wt), vanadium (0.005 to
0.30%wt), nickel (0.05-0.30%wt), molybdenum (0.05-0.25%wt) and boron trace can reduce the formation of crystal boundary cementite,
And thus improve the formability of the line.Such alloying make it possible 0.90 to 1.20%wt carbon content, lead
Cause can be the 4000MPa of higher tensile strength, such as steel core wire level.
Generally, with N/mm2The tensile strength " TS " of the steel core wire of expression necessarily be greater than：
TS >=4700-7.4 × d
Wherein " d " is the core line diameter represented with micron.
It also can use suitable metal coating to coat the metal core wire, it is more suitable for its purpose.For example can use by copper, silver,
The coating of good conductive coats the line made from any alloy of zinc or cobalt or these metals.When it is sufficiently thick (such as line it is total
Diameter 2%) when, the coating contribute to reduce metal core wire online resistance rate.Referring to WO 20122055712.Also it can use
The metal coating of copper, zinc or tin or its alloy (such as brass or bronze) coats the line to improve the machinability of the line.At this
Individual aspect, it is found that the ordinary carbon steel line for being coated with brass for loose abrasive sawline is very suitable.
Abrasive grain is attached to by the metal core wire by electroless nickel layer.In addition to specially the existing of oxide, the electricity
Other elements such as sulphur, phosphorus, boron, cobalt, iron, copper, zinc or this layer can be polluted during being formed that nickel coating can also include trace
Other elements (such as caused by their presence in the electrolyte).
The electroless nickel layer is accumulated by least two subgrades overlie one another.This is due to the mode of layer growth：In a layer
Another layer above.The layer in metallographic cross section is recognizable after following etching：
● first with the nitric acid (HNO of 38ml 65%3), 100ml glacial acetic acid (CH3COOH) and 10ml distilled water solution etching
About 10 seconds；
● and then in the nitric acid (HNO of 50ml 65%3) in 50ml glacial acetic acid (CH3COOH etched in the solution in) other 5 seconds.
Characteristic on the sawline of the present invention is exist between at least one pair of continuous subgrade and contain nickel oxide now
Interface.
Prior art fixed abrasive sawline has the nickel dam consolidated on abrasive grain, and therebetween without nickel oxide
Layer.This means abrasive grain can be used for saw before must remove on abrasive grain nickel dam (nickel be in itself it is stone and
Wear-resisting), i.e., the line is necessary " finishing ", and this causes increased disposal and/or saw loss of efficiency.
Inventor find nickel oxide interface have the advantages that bring some unexpected to it.Nickel oxide interface is in the saw phase
Between serve as preferred fracture plane.Because due to they small radius of curvature and contact is highest on abrasive grain
, so while the presence of nickel oxide boundary layer, nickel subgrade is easily worn and torn there compared with existing fixed abrasive sawline.
Although the wearability of intergranular electroless nickel layer also reduces, generally this does not cause the increased abrasion of line.In fact, mill
Radius of curvature (it is about the radius of line in itself) between material particle is much higher and therefore contact is relatively low there.This
Outside, the less contact workpiece of layer between abrasive grain, because line is pressed on abrasive grain.
The thickness ratio 50nm of boundary layer containing nickel oxide is thin, and preferably smaller than 20nm or even better is less than 10nm.Too
Thick boundary layer will cause the nickel subgrade when distortion or bending to be peeled off.In order to which for what be can recognize that, the nickel oxide interface must be at least
For 0.5nm.The required effect that abrasion is easier on abrasive grain is expected under the thickness.
Energy dispersion X-ray spectroscopic methodology (EDX) can be combined with scanning transmission electron microscope method (STEM) best to determine
The presence of oxygen in boundary layer.EDX devices are to confirm the presence of oxygen in interface.Generally can not be true in SEM
Recognize nickel oxide interface.
" thickness at interface " means " full width under half height " at the oxygen K lines peak in EDX spectrum.Relative to unintentionally
The oxygen K line background signals of neighbouring nickel subgrade of the ground comprising some oxygen obtain the height.
The thickness of subgrade in itself can change between 0.05 μm and 20 μm.Preferably, the thickness of subgrade is at 0.1 μm and 10
Between μm, or 0.2 μm to 5 μm or 0.2 μm to 1 μm.The amount of the thickness of layer and the atom deposited during the deposition of single subgrade
Directly relevant, due to electrolytic deposition subgrade, the amount of electric charge of the amount of the atom of the deposition with being transmitted during depositing is directly relevant
(by Faraday's law).The amount of the electric charge of the transmission will depend on current density, ionic charge and dip time.
In the second preferred embodiment, radially outer of the interface comprising nickel oxide in abrasive grain is found." radially
Outside " means the axis relative to fixed abrasive sawline.Therefore, the interface containing nickel oxide is present at least at the outer of abrasive grain
Side.Therefore, then with least two nickel subgrade coated abrasive particles, separate this at least with least one interface for containing nickel oxide
Two nickel subgrades.The number of the subgrade of abrasive grain radially outer can be big.Such as five to ten or even more.It is many
The radially outer of abrasive grain is may be present in up to 60 layers.
The total thickness of all subgrades of abrasive grain radially outer is between 2 and 20 μm, preferably between 3 and 10 μm.
Thicker top layer helps preferably to keep particle.However, too thick top layer is intended to abrasive grain being imbedded in electroless nickel layer
In so that they are inert for saw.
In the 3rd preferred embodiment, the number for being present in the subgrade between metal core wire and abrasive grain is limited in
Between one and ten, or even more preferably between one and three or even it is limited to a layer.In the heavy of abrasive grain
These subgrades or this subgrade are deposited in metal core wire before or during product.
The total thickness of subgrade between metal core wire and abrasive grain is between 0.05 μm and 15 μm, preferably at 0.1 μm
And between 5 μm, such as 0.3 μm to 1.0 μm.The presence of at least one nickel subgrade between metal core wire and abrasive grain contributes to
Increase consolidation of the abrasive grain in electroless nickel layer.
The gross thickness of electroless nickel layer is between 1 and 40 μm." gross thickness " means the institute in the region without abrasive grain
There is the total thickness of subgrade.The gross thickness of electroless nickel layer preferably abrasive grain middle position size 1/3rd and 2/3rds
Between.For example, the particle with 30 μm of middle position crystallite dimension is most preferably maintained at the total thickness between 10 and 20 μm
In the electronickelling of degree.In the case of saw is sapphire, preferably larger abrasive grain highest is up to 60 μm, and therefore electroplates
The gross thickness of nickel dam then amounts to 20 to 40 μm.When sawing sapphire, abrasive grain is more typically measured as 30 μm, the total thickness of nickel dam
Degree is between 10 and 20 μm.Conversely, for cutting monocrystalline silicon, the smaller abrasive grain less than 20 μm of middle position sizes is preferred
's.Typical middle position size is 11 μm in the purposes.The gross thickness of electroless nickel layer is between 3 and 8 μm.It is preferred that passing through basis
ANSI B74.20-2004 " laser diffractometry " (or " low-angle laser light scattering ") determines the middle position crystal grain chi of abrasive grain
It is very little.
The preferred superabrasive particles of abrasive grain such as diamond or cubic boron nitride or its mixture.Although it is also possible to consider
Other hard materials such as tungsten carbide, carborundum, aluminum oxide or silicon nitride, but they are rarely used in fixed abrasive sawline.For
For both its low cost and fragility, the diamond of size is most preferably broken and sieved.
Advantageously, abrasive grain has at least a portion precoated shet, and the precoated shet has conducting compound, otherwise will not
Or hardly with nickel subgrade electrolysis covering abrasive grain." part precoated shet " means before being included into electroless nickel layer extremely
The surface of few a part of abrasive grain shows coating.
Exemplary precoated shet come self-contained nickel, nickel-phosphor, nickel-boron, titanium, titanium carbide, zirconium, zirconium carbide, tungsten, tungsten carbide,
Any of vanadium, vanadium carbide, niobium, niobium carbide, molybdenum, molybdenum carbide, chromium, chromium carbide, silicon, group of carborundum.Most preferably nickel
Phosphorus, because abrasive grain can electrically be applied it to non-.Precoating layer weight should be less than gross weight, and (abrasive grain is added
Coating) 60%, preferably smaller than 35%.Too thick precoated shet must be also worn away before abrasive grain can play its effect,
Aggravate finishing problem.5% particle that precoating layer weight is less than gross weight is more difficult to be embedded in electroless nickel layer.
In the further preferred embodiment of fixed abrasive sawline, first in the precoated shet of abrasive grain and thereon
Deposition and the therefore interface between nickel subgrade adjacent thereto are substantially free of oxygen." substantially free of oxygen " means at interface
Difference between oxygen in the STEM-EDX distribution maps of place and adjacent interface is counted is interior in measurement limitation.Preferably, it is at least first
The layer being first deposited on abrasive grain adheres well to abrasive grain with good confining force.
According to the second aspect of the invention, the continuous method for preparing fixed abrasive sawline is disclosed.This method causes such as production
The fixed abrasive sawline limited in product claim.This method comprises the following steps：
(A) by the metal core wire for example described in the fourth paragraph on page three and the 4th section of page 4 ([0013] and [0018] section) from
Carrier unreel；
(B) line is guided to be bathed by cleaning.Alkalescence is preferably used or neutral bath cleans organic remains from the line, then
Using acid bath to remove oxide and inorganic pollution.
(C) then by the way that the line repeated impregnations are electroplated into the line in electrolytic ni plating bath.In each of electrolytic ni plating bath
In bath, nickel subgrade is deposited.The bath of at least one electrolytic coating includes abrasive grain.Abrasive grain is included into electroless nickel layer in the bath
In.
(D) fixed abrasive sawline is wrapped on carrier after common flushing and drying steps.
Term " before " and " afterwards " mean the time sequencing of the event that line undergoes during processing.
This method is different from known method：By at that time between a sequence of at least twice nickel plating bath dipping of the line
The oxidation of outer nickel dam forms nickel oxide layer.
Nickel plating bath is known in the art.There is Watts nickel plating solutions (nickel sulfate, nickel chloride, boric acid), based on amino
Solution (nickel sulfamic acid, nickel chloride, boric acid), perchloro- compound solution (nickel chloride, boric acid), the sulfate-chloride of nickel sulphonic acid
Solution (nickel sulfate, nickel chloride, boric acid, but the concentration to be bathed different from Watt), fluorborate solution (nickel fluoborate, chlorination
Nickel, boric acid) and many other nickel plating baths.For its high deposition rate, nickel sulfamic acid bath is most preferred.
Following improvement can be made to this method：
First, the oxidation of outer nickel dam at that time can be carried out after at least one bath comprising abrasive grain at this.In the feelings
Under condition, the interface containing nickel oxide will be present in above abrasive grain.Interface containing nickel oxide preferably exists only in abrasive material
Grain radially outer and be not present between metal core wire and abrasive grain, be not thus a priori to exclude the possibility.
Second, abrasive grain is preferably provided with the conduction precoating that 3-4 sections of page 7 ([0034] and [0035] sections) are explained
Layer.Preferably note preventing the formation of the oxide surface layer of self-assembling formation on conductibility precoated shet.It thus avoid pre-
The presence at the interface containing nickel oxide between coating and neighbouring nickel subgrade.
3rd, the oxidation of outer nickel dam at that time can be substantially carried out in three different ways：
● by the oxygen present in the air, it can be improved by adding heat.For this must by the line drying with
Just outer nickel subgrade at that time is made to be exposed to atmosphere；
● pass through the electrochemical oxidation in aqueous electrolyte medium.The line is biased to anode, thus occurs oxidation anti-
Answer (oxygen is formed).
● in the alkalescence bath of oxidation for causing outer nickel dam at that time by being immersed in.
Further open actual embodiment and the explanation in ensuing part.
Brief Description Of Drawings
Fig. 1 schematically depict the first preferred embodiment according to the present invention.
Fig. 2 describes the second preferred embodiment of the present invention in a schematic manner.
Fig. 3 a show according to the present invention fixed abrasive sawline electroless nickel layer layer structure STEM pictures, and
The EDX spectrum of the oxygen of correlation are shown in Fig. 3 b.
Fig. 4 a and 4b are the STEM pictures and EDX spectrum obtained on another sample.
Fig. 5 schematically shows the equipment that the line of the present invention can be prepared thereon.
Fig. 6 illustrates the saw behavior of conventional sawline and sawline of the invention under first time cutting.
Embodiment
As explained in the schematic diagram of the coating equipment shown in Figure 5, fixed abrasive sawline can be prepared.For understanding this
The display not in the schematic diagram such as pump, wiper, driver, filter of the unwanted servicing unit of invention institute, but
It is known to those skilled in the art.
120 μm of diameter had into the general of Brass coating (65wt%Cu, 3g/kg coating weight) in the equipment 501
Lead to carbon steel line 500 from the continuous unreel of spool 502.
The organic remains for removing the line using alkaline cleaner in bracket 504 is for example remained from previous draw step
Lubricant.Acid clean removes all other pollutant from the line surface and activates the surface and is used to plate in bracket 506
Cover.
Contact roller 510 ensures to supply from power supply 512 to the continuous current of line 500, and it is then following thus to make line 500
The first nickel plating bath 508 in negative electrode.Deposit the first nickel dam.There is dry station 522 in the exit of the first nickel plating bath 508, can
Arbitrarily it is turned on and off the dry station 522.In dry station 522, the line is heated by drying, thus in outer nickel dam at that time
Upper formation oxide interface.The line can be heated by resistance heating as substituting.More identical nickel plating stages can be introduced next
Make this layer it is thickening.
The plating bath includes the nickel sulfamic acid plating electrolyte of consisting of：
Table 1
Subsequent nickel plating bath 514 includes nickel plating electrolyte, wherein making abrasive grain keep suspension by mechanical splash bar.The line
Roller 510 ' is made electrical contact with again and passes through current and power supply 512 ' supplies.Abrasive grain is with 12 μm of middle position chis in this case
Very little broken diamond, the diamond is pre-coated with nickel phosphorus (about 12 to 13wt% phosphorus), in an amount of from the diamond of Unit Weight
About 16wt% nickel phosphorus, thus notes preventing the formation of natural nickel oxide layer.The diamond that is deposited on the line is measured certainly
In the line intended application and can change between 0.10 to 2.5 gram/km lines.For thin line (120 μ for sawing silicon ingot
M), target is 0.15 gram/km value.Thin nickel dam keeps diamond particles before the next stop is gone to enough.Include sodium hydroxide
Bath 520 provide oxidation source, cause to form the interface containing nickel oxide on outer layer at that time.
In the multiloop stage 519, then repeat the line being directed to each other two tops of trench line roller 516,516 '
In parallel multiple loops.The line repeatedly enters in identical nickel plating bath 509.Acid is for example passed through by electrolyte 518 now
Such as sulfuric acid makes the line be contacted with current and power supply 512 ".At negative electrode, it will be reduced in electrolyte 518, and in the line
The surface oxidation of nickel dam of the place by generation at that time.(can for example it be changed by adjusting the current density in electrolyte 518 at the line
Its steeping length) or by the way that the nickel oxide layer of formation is dissolved into (not shown) in subsequent acid bath adjust the oxide table
Layer.Finally the line is wrapped on tension spool 524.
By this way, the interfacial structure of different nickel subgrades can arbitrarily be adjusted.Fig. 1 shows the example according to the present invention
The schematic accumulation of different layers near the abrasive grain of property fixed abrasive sawline 100.Coated and cleaned with the first nickel dam 104 first
Line base material 102, with rear oxidation first nickel dam 104, hereafter form nickel oxide layer 106 and (indicated with hacures to aoxidize in figure
The presence at nickel interface).Then it is coated with the second nickel subgrade 108, oxygen is formed again on the second nickel subgrade 108
Change nickel interface 110.Form the 3rd nickel subgrade 112 with the interface 114 (being indicated in figure with solid line) without nickel oxide and the
Four nickel subgrades 116.In the growth period of the 4th subgrade, abrasive diamond particle 130 is included in the layer.The particle has nickel phosphorus
Pre-coat layer 132.Notice that the outer surface of the pre-coat layer is free of nickel oxide, to prevent the weak attachment of the third and fourth nickel subgrade.
After the 4th layer of deposition, growth nickel oxide interface 118 then deposits the therebetween with the interface 122 containing nickel oxide
Five nickel subgrades 120 and the 6th nickel subgrade 124.Atmospheric oxidn nickel dam 126 will grow as time go by outer layer.
Alternative practical embodiments 200 are schematically showed in fig. 2.Identical tens and units are indicated such as
Same characteristic features in Fig. 1, unless be described additionally below.As in the embodiment in fig. 1, there is the layer of same number and arrangement.
Here only nickel oxide boundary layer 214,218 and 222 is present in the radially outer of abrasive grain, in Fig. 5 multi-loop device 519
It deposited these nickel oxide boundary layers.Close other nickel oxide formation mechanism 522 and 520 and therefore boundary layer 206,210 is not
Containing nickel oxide.In addition, the implication of the other accompanying drawings mark in Fig. 2 is as follows：
202：The line base material of cleaning；
204：First nickel dam；
208：Second nickel subgrade；
212：3rd nickel subgrade；
216：4th nickel subgrade；
220：5th nickel subgrade；
224：6th nickel subgrade；
226：Atmospheric oxidn nickel dam；
230：Abrasive diamond particle；
232：Nickel phosphorus pre-coat layer.
Energy dispersion X-ray probe unit (EDX) can be combined by scanning transmission electron microscope (STEM) to determine to aoxidize
The presence of nickel boundary layer.Fig. 3 or 4 shows the figure of the real-time stacking of the layer by being obtained according to the fixed abrasive sawline of the present invention
Piece.Sample is polished to 25 μm of gross thickness and it carried out further by ion beam grinding with Baltec RES101 machines
Prepare.High-resolution pictures and EDX spectrum are obtained on the Tecnai G2 microscopes operated under 200kV.For these pictures
Detector be high angle annular dark field detector (HAADF detectors), its detect scattering deviation beam electronics (off-beam
electron)。
The coating sample obtained by the plane perpendicular to the outer surface of fixed abrasive sawline is shown in fig. 3 a
HAADF pictures.Layer structure is clearly visible.These layers have 300nm thickness.There is different boundary layers and EDX
Spectrum (Fig. 3 b)-be configured with oxygen, K lines-be clearly illustrated in intersection along indicated trace (being white in Fig. 3 a)
Four interface oxygen presence.Due in the absence of other metals, can only form nickel oxide interface.Boundary layer comprising nickel oxide
Thickness be estimated as 6+/- 4nm.The another of same sample is shown in Fig. 4 a (HAADF-STEM pictures) and 4b (EDX spectrum)
One cross section.
With 3410N/mm2The making on the ordinary carbon steel line of brass that is coated with of tensile strength is intended as sapphire saw
Another sample of the invention of line.The nickel precoated shet of 5 μm of application on offline line.It is not given to the extra precoating of nickel
Layer, i.e., the nickel bath 508 and the line for not using Fig. 5 is immediately entered in nickel sulfamic acid diamond suspension.Deposit precoating
Diamond, it has 25-35 μm of middle position size and 30wt%Ni-P (in terms of diamond weight).The layer of first deposition has
0.1 μm of thickness, and oxygen is not present between the precoated shet of diamond and the nickel subgrade deposited thereon.In multiloop system
In, pass through 56 nickel subgrades for guiding them to be deposited by multiloop system comprising aerobic intermediate layer for 56 times.Electronickelling thickness
Degree is about 10 μm, and the thickness of subgrade is 0.179 μm.Use anode liquid contact system.By the sample " IS " of the present invention with having
Same metal core but contrasted without the commercially available fixed abrasive sawline (conventional sample " CS ") of nickel oxide boundary layer.
Fig. 6 shows the first time cast-cutting saw result of the single scroll saw test of two kinds of samples.Single scroll saw is obtained by DWT
RTS-480 types.It cut A2 " (50.8mm) circular sapphire ingot.With 400m/ points under 22N line tension in reciprocating pattern
The average linear velocity of clock operates the machine under the table top speed of 0.42mm/ minutes.Monitor and applied on ingot support during cutting
Plus power ' F (being counted using N) ' over time ' t (in seconds) ' change and the power measuring as required saw active force.This
Outside when cutting force increase, it was observed that larger bending.
Fig. 6 shows that two kinds of lines show the increased active force when first time, cutting started.This shows that diamond does not have also
There are their complete cutting performances of acquisition and show that they are remained as " finishing " during sawing.Significantly, the present invention's
Active force extra after about 2000 seconds reduces in the case of sample " IS ", and this lasts about 3400 for conventional sample " CS "
Second.In addition, compared with ensuing stability force platform, initial cutting force is flat higher than this in the case of conventional sample
Platform about 35%, and its corresponding platform only than the sample of the present invention is high by 17%.Therefore the present invention line finishing faster and than
Under the smaller active force of conventional line.This is attributed to by inventor has the beyond expectation excellent of nickel oxide interface between nickel subgrade
Point.
Claims (13)
1. fixed abrasive sawline, the abrasive grain of metal core wire is attached to comprising metal core wire and in electroless nickel layer, its feature
It is
The electroless nickel layer includes the nickel subgrade of two or more stackings, contains wherein existing between at least one pair of continuous subgrade
There is the interface of nickel oxide, wherein the interface containing nickel oxide is thinner than 50nm.
2. fixed abrasive sawline according to claim 1, wherein relative to the metal core wire center in the footpath of abrasive grain
To the outside interface for containing nickel oxide in the presence of at least one.
3. fixed abrasive sawline according to claim 1, wherein the thickness of each nickel subgrade is between 0.05 and 20 micron.
4. the nickel subgrade of fixed abrasive sawline according to claim 3, the wherein radially outer of abrasive grain is thinner than 10 μm.
5. fixed abrasive sawline according to claim 1, wherein abrasive grain are diamond particles.
6. fixed abrasive sawline according to claim 5, wherein diamond particles have precoated shet, the precoated shet has from bag
Nickeliferous, nickel-phosphor, nickel-boron, titanium, titanium carbide, zirconium, zirconium carbide, tungsten, vanadium, vanadium carbide, niobium, niobium carbide, tungsten carbide, molybdenum, molybdenum carbide,
Any of chromium, chromium carbide, silicon, group of carborundum.
7. the interface between fixed abrasive sawline according to claim 6, the wherein precoated shet and neighbouring nickel subgrade is substantially
Without nickel oxide.
8. continuously preparing the method for fixed abrasive sawline, comprise the following steps：
- by metal core wire from carrier unreel；
- guiding the metal core wire is bathed through cleaning；
- by the way that the metal core wire repeated impregnations are electroplated into the metal core wire with nickel in nickel plating bath
Nickel plating bath described in wherein at least one is the nickel plating bath comprising abrasive grain；
- obtained fixed abrasive sawline is wound on carrier；
It is characterized in that
Nickel oxide layer is formed by the oxidation of outer nickel dam at that time between the dipping of nickel plating bath at least twice.
9. method according to claim 8, wherein carrying out at that time outer after at least one described bath comprising abrasive grain
The oxidation of nickel dam.
10. according to the method for any one of claim 8 to 9, wherein by carrying out outer nickel dam at that time exposed to air
The oxidation.
11. according to the method for any one of claim 8 to 9, wherein being carried out by the electrochemical oxidation in water-bearing media
The oxidation of outer nickel dam at that time.
12. according to the method for any one of claim 8 to 9, wherein carrying out outer nickel at that time by impregnating through alkalescence bath
The oxidation of layer.
13. method according to claim 8, wherein by guiding the metal core wire to pass through at least one phase in multiple loops
With nickel plating bath carry out the repeated impregnations of the metal core wire in the nickel plating bath.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| EP13153257 | 2013-01-30 | ||
| EP13153257.4 | 2013-01-30 | ||
| PCT/EP2014/050715 WO2014118003A1 (en) | 2013-01-30 | 2014-01-15 | A fixed abrasive sawing wire with nickel oxide interfaces between nickel sub-layers |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104955601A CN104955601A (en) | 2015-09-30 |
| CN104955601B true CN104955601B (en) | 2017-09-12 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201480006664.7A Active CN104955601B (en) | 2013-01-30 | 2014-01-15 | There is the fixed abrasive sawline at nickel oxide interface between nickel subgrade |
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| Country | Link |
|---|---|
| CN (1) | CN104955601B (en) |
| WO (1) | WO2014118003A1 (en) |
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Also Published As
| Publication number | Publication date |
|---|---|
| CN104955601A (en) | 2015-09-30 |
| WO2014118003A1 (en) | 2014-08-07 |
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Effective date of registration: 20170216 Address after: No. 358 East Binjiang Road, Jiangyin, Jiangsu, China Applicant after: Jiangyin Bekaert Alloy Materials Co., Ltd. Address before: Belgium, Graham Weaver Applicant before: NV Bekaert SA |
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