CN107299378A - A kind of manufacture method of high efficiency cutting silicon chip diamond wire - Google Patents
A kind of manufacture method of high efficiency cutting silicon chip diamond wire Download PDFInfo
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- CN107299378A CN107299378A CN201710386862.6A CN201710386862A CN107299378A CN 107299378 A CN107299378 A CN 107299378A CN 201710386862 A CN201710386862 A CN 201710386862A CN 107299378 A CN107299378 A CN 107299378A
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- bus
- diadust
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D15/00—Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/10—Electroplating with more than one layer of the same or of different metals
- C25D5/12—Electroplating with more than one layer of the same or of different metals at least one layer being of nickel or chromium
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D7/00—Electroplating characterised by the article coated
- C25D7/06—Wires; Strips; Foils
- C25D7/0607—Wires
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- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention provides a kind of manufacture method of high efficiency cutting silicon chip diamond wire, the manufacture method comprises the following steps：（1）Unwrapping wire, impurity elimination,（2）Cleaning,（3）Surface preparation,（4）Preplating,（5）Upper sand,（6）Secondary plating,（7）Cleaning, drying, take-up.The present invention by the CURRENT DISTRIBUTION to electroplate liquid, PH sizes, viscosity, flow rate of liquid regulation, control to bus run speed and the additive addition manner using uniqueness, it ensure that diamond particles density is in 200 350/mm on diamond wire, the 6um of height of protrusion 5, and diamond particles are dispersed on bus, adhesive force is stable, without agglomeration.The diamond wire produced using the present invention can be completed to 8.0inch, 8.2inch, 8.4inch within 2 hours, the high efficiency cutting of long 650 700mm crystalline silicon rods, existing clipping time is shortened more than half, reduction silicon chip surface, seamed edge are bad, effectively improve production efficiency.
Description
Technical field
The invention belongs to electroplate diamond wire manufacturing technology field, and in particular to a kind of system of high efficiency cutting silicon chip diamond wire
Make method.
Background technology
Hard brittle material applies increasingly extensive, and it mainly includes silicon crystal, sapphire, glass, stone material, quartz, ceramics, hard
Alloy, rareearth magnetic material etc..Because most of hard brittle materials are expensive, therefore, the general requirement processed to hard brittle material
For low, efficiency high is lost, cost is low, pollution is small etc., and cutting processing is the most frequently used one in current hard brittle material processing method
Kind, common cutting mode has laser cutting, machine cuts, and machine cuts are divided into rigidity cutting and flexible cutting.With solar energy
The gradually expansion of photovoltaic industry, the processing of silicon crystal is increasingly taken seriously.The cutting processing of silicon crystal is mainly using machinery
Flexibility in cutting cuts to complete.Flexibility cutting is that silicon crystal is cut using a kind of high-carbon steel wire combination abrasive particle, soft
Property cutting according to abrasive particle existence form be divided into free abrasive cutting and fixed grain cut, free abrasive cutting be to use filament bus
A diameter of 8-20um SiC slurries are driven, realize that the grinding to crystalline silicon is cut, also known as abrasive wire sawing；Fixed grain is cut
First the diamond to the upper molecule of plating around filament bus, then uses the filament sliced crystal rod electroplated, also known as Buddha's warrior attendant
Wire cutting.Free abrasive cutting is that the high-speed motion based on filament bus takes abrasive particle to cutting zone, and the rolling for passing through abrasive particle
The removal of material is realized in dynamic-impression effect, due to entering the abrasive particle number of cutting zone by grinding fluid viscosity and its behavior
Influence, therefore certain influence is produced to cutting efficiency.With the improvement of technology, the market demand is increasing, because efficiency is low,
Oiliness cutting liquid causes very big pollution to environment, and abrasive wire sawing is gradually eliminated.Buddha's warrior attendant wire cutting is due to efficiency
Height, cost is low, and environmental protection pressure is small and rapid is favored by market.
However, using existing Buddha's warrior attendant wire cutting, often cutting a workpiece, the required time is 3-4h, either from
Enterprise itself profit direction, or from the point of view of the market demand, efficiency can not meet requirement.Cause existing diamond wire cutting efficiency low
The reason for mainly have：Diadust diameter skewness, bus tensile strength stability are poor, diamond exposure distribution
Uneven, diadust distribution density is low, agglomeration is obvious etc..In order to ensure distribution density of the diadust on bus
It is high and not reunite be relatively difficult, it may then reduce grain density to reduce to reunite；In order to improve diamond
Granule density, may bring agglomeration serious.
The content of the invention
To solve on the diamond wire prepared in the prior art, diamond particles density is low, and diamond adhesive force is small, Yi Jijin
Hard rock grain density height but skewness and the technical problem for occurring agglomeration, the present invention disclose a kind of high efficiency cutting silicon chip and used
The manufacture method of diamond wire.
The present invention by the additive formula of electroplate liquid, CURRENT DISTRIBUTION, PH sizes, viscosity, flow rate of liquid regulation, it is right
Using more stable additive addition manner during the control of bus run speed and upper sand, it ensure that on diamond wire
Diamond particles density is 200-350/mm, height of protrusion 5-6um, and diamond particles are dispersed on bus, attachment
Power is stable, without agglomeration.Using the diamond wire that produces of the present invention can be completed within 2 hours to 8.0inch,
8.2inch, 8.4inch, the high efficiency cutting of long 650~700mm crystalline silicon rods, more than half is shortened by existing clipping time, is dropped
Low silicon chip surface, seamed edge are bad, effectively improve production efficiency.
To achieve the above object, the technical solution adopted by the present invention is：
A kind of manufacture method of high efficiency cutting silicon chip diamond wire, the manufacture method comprises the following steps：(1) unwrapping wire,
Impurity elimination, (2) cleaning, (3) surface preparation, (4) preplating, sand on (5), (6) secondary plating, (7) cleaning, drying, take-up；
Sand on the step (5), is that diadust is electroplated onto into bus matrix surface：Preplating in step (4) is good
Diadust is mixed with plating solution and is put into a mixing bowl, by being pumped into bath trough, and bus is wrapped on roller, is immersed into
Plating solution lower section 5-10mm is simultaneously at the uniform velocity passed through with 12-20m/min, and bus is connected with power cathode, and bath trough bottom even is distributed with
Nickel block, nickel block switches on power positive pole, plating solution 200-280L in upper sand launder, wherein, nickel sulfamic acid 0.4-0.6L/L (every liter of amino
Nickel sulphonic acid stoste contains nickel ion 140-160g), boric acid 20-30g/L, nickel chloride 9-12g/L, diadust input amount 3.7-
Electric current 12-15A in 4.3g/L, additive proportion 20-30, electroplating process, 50 ± 2 DEG C of bath temperature, plating fluid viscosity 1.1-
1.3mPa s, plating solution circular flow 150L/min, PH4.6-5.1；
The electroplating process of the secondary plating of the step (6) is identical with step (5), plating solution 250-300L, wherein, nickel sulfamic acid
0.5-0.6L/L (every liter of nickel sulfamic acid stoste contains nickel ion 150-180g), boric acid 25-30g/L, nickel chloride 9-12g/L,
Electric current 28-30A in brightener 0.01-0.02g/L, plating, 52 ± 2 DEG C of bath temperature plates fluid viscosity 1.3-1.4mPa s, plating solution
Circular flow 150L/min, PH 3.8-4.4.
Further, additive includes complexing agent, dispersant and brightener in the step (5), and above-mentioned substance is according to quality
Than for 3: 2: 1-3: 3: 1, preferably 3: 3: 1, mixing.In the step (5) additive can also include complexing agent, dispersant,
Brightener, surfactant and wetting agent, wherein, complexing agent is ethylenediamine tetraacetic methene sodium phosphate (EDTMPS), the methene phosphorus of amine three
Hydrochlorate, polyacrylamide, the one or more of poly- hydroxy acrylic acid；Dispersant is BASF phenolsulfonate；Brightener is ten
Glycol sulfuric acid vinegar sodium (K-12), the one or more of cetyl trimethyl glycine betaine (Am)；Surfactant is aromatic series sulphur
Barbiturates；Wetting agent is sodium sulfosuccinic diester or phosphate diester sodium salt.
Further, 10mm below step (5) the bus immersion plating solution, diamond particles bury to bus nickel dam 2-3um.
Further, the addition manner of additive is that additive formula is good in the step (5), is added in container, makes
Addition is completed with titration, enables to additive more uniformly to act in whole electroplating process, and then ensures Buddha's warrior attendant
Stone particle is dispersed on bus, without agglomeration.
Further, current control accuracy requirement is in ± 0.1A in the step (5), the thinner bus of line footpath, it is desirable to control
Precision is higher；The running stability requires bus electroplating velocity precision controlling in 0.01-0.03m/min.
Further, diamond particles integrally bury depth 4-5um, diamond particles height of protrusion 4- in the step (6)
6um。
Further, the impurity elimination in the step (1) includes diadust impurity elimination and bus impurity elimination, diadust impurity elimination
Be by diadust in 70-80 DEG C, mass concentration is 15%-20% NaOH solutions ultrasound 120-360s, then in quality
Concentration is 15%-20%HNO3Ultrasound 120-360s in solution；Bus impurity elimination is that bus is put into except in oil solution, ultrasonic 3-
5s, except degreasing powder concentration is 20-40g/L in oil solution, proportion is 3-4, and temperature is 60 ± 2 DEG C.
Further, step (2) cleaning, including ultrasonic cleaning, once rinsing, pickling, secondary rinsing.
Wherein, it is described be cleaned by ultrasonic, once rinsing, it is secondary rinsing be pure water supersound washing, water temperature is maintained at 60 ± 2
DEG C, pickling is the sulfamic acid that 30-50g/L is added in descaling bath, and temperature is washing at 20 ± 2 DEG C, diadust and mother
Line passes sequentially through ultrasonic cleaning, once rinsing, pickling and secondary rinsing.
Further, step (3) surface preparation, locates in advance comprising diadust surface preparation with bus surface
Reason.
Wherein, diadust surface preparation：Diadust is first sequentially placed into NaOH and HNO3Solution is soaked
Bubble corrosion, soak time 10-30min, then by ultrasound rinsing, finally filter and dry using filter paper, improve diamond surface
Activity, is conducive to nickel dam to be combined with diamond surface in chemical plating；Surface corrosion is carried out with hydrochloric acid using dilute sulfuric acid to bus
Pretreatment, etching time 3-5s, then by pure water cleaning, drying, said process removes bus surface oxide layer, in pre- cross,
Strengthen nickel dam and belong to one with electroplating assembly line with bus pretreatment described in the adhesion on bus surface, be directly entered after having pre-processed
Electroplated in electroplating assembly line.
Wherein, described NaOH, HNO3The concentration of solution, dilute sulfuric acid and hydrochloric acid is 20-35%.
Described that diadust surface is pre-processed, i.e., Strong oxdiative is handled, the oxidation processes mechanism：Make diamond
Micro mist surface carbon atom obtains the groups such as oxidation generation hydroxyl (- OH), carboxyl (- COOH) and carbonyl (C=O), so as to improve gold
The hydrophily of hard rock particle.
Described that surface preparation is carried out to bus, roller drives bus to sequentially pass through pretreatment tank, and pretreatment tank includes 2
Acid tank (dilute sulfuric acid tank and hydrochloric acid trough), ultrasonic pure water rinse bath, pretreatment cause bus surface to form the other pit of micro/nano level,
Increase the contact area between nickel dam and bus, further enhance the adhesion between coating and bus, further strengthen nickel
Metallic bond connection between ion and bus.
Further, step (4) preplating, including diadust preplating and bus preplating.
Wherein, diadust preplating：Diadust after surface preparation is added in plating fluid cylinder, had in plating fluid cylinder
Agitating device, mixing speed 20-30 turns/min, the composition of the chemical plating fluid：Nickel sulfate 19-25g/L, boric acid 8-10g/L, chlorine
Change nickel 4-6g/L, absolute ethyl alcohol sodium 12-20g/L, naphthalene trisulfonic acid sodium 2-5g/L, pH=3.8~4.4.
Bus preplating：Bus after surface preparation is driven through electric bath groove by roller, bus is immersed in plating solution
Lower section 5-10mm, bus access power cathode, wherein bath trough plating liquid measure 100-120L, bath trough bottom even laying nickel block,
Access nickel sulfamic acid 0.2-0.5L/L (every liter of nickel sulfamic acid stostes in positive source, electric current 0.7-0.8A, the electroplate liquid
Contain nickel ion 100-130g), boric acid 15-20g/L, nickel chloride 3-6g/L, lauryl sodium sulfate 0.2-0.3g/L, plating bath temperature
50 ± 2 DEG C of degree, plating fluid viscosity 1.0-1.2mPa s, PH3.8-4.2.
Further, diadust pre-plating layer thickness is 0.5-1.5um in the step (4), and bus pre-plating layer thickness is
1-1.5um。
Further, the diamond wire of the secondary thickening of the step (7) removes surface residue by potcher, by drying
Case, oven temperature is set in 150-300 DEG C, after drying by guide wheel according to the winding department of setting away from being wound on take-up pulley, take-up
Tension force is set in 4-10N.
Further, diadust diameter screening used is 5-10um in step (1)-(7), is further 8-
10um。
The method of the present invention mainly includes the improvement of three aspects：1st, by being pre-processed to diadust and bus surface
Form relatively rough surface so that surface both product increase, in electroplating process, have more nickel ions and be restored to gold
Hard rock and bus surface form nickel dam, then by increasing diadust content in plating solution, not only increase diamond particles in
The adhesive force of bus, also improves diamond particles density on diamond wire so as to improve diamond wire cutting force；2nd, by step
(5) proportioning of additive in, especially in upper sand ring section, its uniqueness of complexing agent, dispersant, the proportioning of brightener and use
Addition manner, it is ensured that the uniformity consistency that diamond particles are distributed on bus, and soilless sticking phenomenon；3rd, control roller is synchronous
Property, bus extensional vibration and oscillation crosswise are reduced, control bus speed of service in liquid is crossed is stable, it is ensured that bus is crossed, added in advance
The nickel layer thickness of thickness plating is uniform and mechanical stress is small, wherein, control flow of the electrolyte is in laminar condition, and (bus passes through liquid height
Setpoint distance liquid level 10mm), it is ensured that different size of diamond particles can be evenly distributed crossing liquid different depth, control electricity
The stability of stream size enables to ensure during bus cabling diamond particles density one at least 50km length ranges
Cause.
Compared with prior art, beneficial effects of the present invention are：
(1) present invention preferably evengranular diadust, diameter average is 8-10um, effectively sets diadust
Preplating thickness 0.5-1.5um, bus pre-nickel plating thickness 1-1.5um, bus is obtained with diadust by surface preparation
The pit of micro/nano level, can strengthen bond area of the nickel ion on bus, and then improve nickel dam and diamond particle surfaces
Adhesive force, the final adhesion for improving diamond particles and bus.
(2) present invention dexterously sets secondary bath concentration more than pre-plating solution concentration, thickeies coating, and diamond particles are overall
Bury depth 4-5um, diamond particles height of protrusion 5-6um, it is ensured that while the strong adhesive force of diamond particles, improve Buddha's warrior attendant
Stone particle height of protrusion, improves the cutting force of diamond wire.
(3) present invention makes especially by the regulation of the allotment of additive addition manner and the mixing speed unique with it
Obtain liquid and keep Uniform Flow state, by being effectively controlled 1.1-1.3mPa s to viscosity, so as to control diadust to exist
The reasonable cooperation of sinking speed and the bus speed of travel in plating solution, while adjusting bus passes through liquid height setpoint distance liquid level
10mm, ensure that bus flows more stable aspect in liquid all the time, is evenly distributed so as to obtain diamond particles, and
For the diamond wire of agglomeration.
(4) present invention is by adding conduction liquid, and regulation voltage carrys out stabling current, is subject to so as to ensureing diamond particles
Electric current is uniform, and diamond particles density on diamond wire is further made and reaches 300/mm, and diamond particles are evenly distributed nothing
Agglomeration.
(5) silicon crystal is cut using diamond wire product produced by the present invention, unit interval internal cutting can be effectively improved and set
Standby production capacity, reduces cost, realizes existing process time by 3-4h/ knives, is reduced to 1.6-2h/ knives, is directly realized by production capacity
It is double.
Brief description of the drawings
Fig. 1 is diamond wire manufacturing process flow schematic diagram of the present invention；
Fig. 2 is the diameter 80um diamond wire electron microscope pictures that the embodiment of the present invention 1 is manufactured；
Fig. 3 is the diameter 70um diamond wire electron microscope pictures that the embodiment of the present invention 2 is manufactured；
Fig. 4 is the diameter 65um diamond wire electron microscope pictures that the embodiment of the present invention 3 is manufactured；
Fig. 5 is the diameter 60um diamond wire electron microscope pictures that the embodiment of the present invention 4 is manufactured；
Fig. 6 is surface topography electron microscope picture after the diadust surface preparation of the embodiment of the present invention 2；
Fig. 7 is surface topography electron microscope picture after the diadust preplating of the embodiment of the present invention 2；
Fig. 8 is the secondary plating surface topography electron microscope picture of the diadust of the embodiment of the present invention 2.
Embodiment
With reference to embodiment, the present invention is described in further detail.
Used chemical raw material is diadust used in commercially available prod, the embodiment of the present invention in embodiment 1-4
Particle is uniform, and particle diameter average is 8-10um, and bus used is high-carbon steel wire.
Embodiment 1
The bus diameter used in the present embodiment is 80um, as shown in figure 1, making the signal of diamond wire equipment for the present invention
Figure.Manufacture method of the present invention is comprised the steps of：(1) impurity elimination, (2) cleaning, (3) surface preparation, (4) preplating, sand on (5),
(6) secondary plating, (7) cleaning, drying, take-up, is comprised the following steps that：
(1) impurity elimination, includes diadust impurity elimination and bus impurity elimination.Diadust impurity elimination is in temperature 70 C, concentration
Surface and oil contaminant, then the HNO through over-richness 15% are removed in 15%NaOH solution3Compound, both of which ultrasound 300s are deoxygenated in solution；
Bus is to release to enter by guide wheel from actinobacillus wheel 1 to go to degrease in ultrasonic tank 2, and degreasing powder concentration is 20g/ in ultrasonic tank 2
L, proportion is 3, and water temperature is controlled in 60 ± 2 DEG C, ultrasonic time 3s.
(2) clean, diadust is cleaned by ultrasonic with bus using pure water, and water temperature is controlled at 60 ± 2 DEG C.The bus
First pass through in ultrasonic pure water rinse bath 3, it is desirable to be immersed in liquid level 10mm depths, water temperature is controlled at 60 ± 2 DEG C；Sequentially pass through drift
Washing trough 4, descaling bath 5, secondary potcher 6 thoroughly remove impurity, potcher 4 and the secondary drifts such as bus oxide on surface, residue
It is three grooves in washing trough 6, inside fills pure water, water temperature controls to fill 30g/L sulfamic acid, temperature in 60 ± 2 DEG C, descaling bath 5
Spend for 20 ± 2 DEG C.
(3) surface preparation, to diadust using concentration 30%NaOH and concentration 30%HNO3Solution soaks respectively
10min, corrosion treatment is carried out to surface and forms micro/nano level pit, then through over cleaning, drying；30% dilute sulphur is used to bus
Acid, salt acid soak 3s carry out surface corrosion processing, then through over cleaning, 150 DEG C of drying.
(4) preplating, diadust preplating：Plating solution formula：Contain nickel sulfate 21g, boric acid 8g, chlorination in 1L plating solution
Nickel 4g, absolute ethyl alcohol sodium 16g, naphthalene trisulfonic acid sodium 3g, mixing speed 20 turns/min, pH3.8；
The preplating of bus：(every liter of nickel sulfamic acid stoste contains nickel ion by electroplate liquid 120L, nickel sulfamic acid 0.3L/L
120g), boric acid 18g/L, nickel chloride 3g/L, lauryl sodium sulfate 0.2g/L.Bus connects negative pole, and positive pole uniformly lays nickel plate,
Electric current 0.72A, 50 ± 2 DEG C of bath temperature, plating fluid viscosity 1.0mPa s, PH3.8.
(5) sand on, the upper solution composition of sand launder 8：Plating solution 250L, nickel sulfamic acid 0.5L/L (every liter of nickel sulfamic acid stoste
Contain nickel ion 140g), boric acid 25g/L, nickel chloride 9g/L, diadust particle diameter average 10um, diadust 3.8g/L,
Additive weight in mass ratio is 20 additions, and electric current 12.5A, 50 ± 2 DEG C of bath temperature plates fluid viscosity 1.1mPa s, plating solution circulation
Flow 150L/min, PH4.6.
(6) secondary plating, carries out plating thickening, purpose enhancing diamond exists by the bus of upper complete sand by secondary thickening groove 9
Adhesive force on bus.Solution composition in secondary coating bath：Electroplate liquid：260L, nickel sulfamic acid 0.6L/L (every liter of nickel sulfamic acid
Stoste contains nickel ion 150g), boric acid 28g/L, nickel chloride 11.5g/L, brightener 3g, electric current 28A, 52 ± 2 DEG C of bath temperature,
Plate fluid viscosity 1.3mPa s, plating solution circular flow 150L/min, PH3.8.
(7) cleaning, drying, take-up, the diamond wire of secondary thickening removes surface residue by potcher 10, by drying
Case 11, oven temperature is set in 200 DEG C, after drying by guide wheel according to the winding department of setting away from being wound on take-up pulley 12, take-up
Tension force is set in 8.5N.
Embodiment 2
The bus diameter used in the present embodiment is 70um.Manufacture method of the present invention is comprised the steps of：(1) impurity elimination, (2)
Cleaning, (3) surface preparation, (4) preplating, sand on (5), (6) secondary plating, (7) cleaning, drying, take-up are comprised the following steps that：
(1) impurity elimination, includes diadust impurity elimination and bus impurity elimination.Diadust impurity elimination is in temperature 70 C, concentration
Surface and oil contaminant, then the HNO through over-richness 17% are removed in 17%NaOH solution3Compound, ultrasonic time 300s are deoxygenated in solution；It is female
Line is to release to enter by guide wheel from actinobacillus wheel 1 to go to degrease in ultrasonic tank 2, and degreasing powder concentration is 23g/L in ultrasonic tank 2,
Water temperature is controlled at 60 ± 2 DEG C, is, ultrasonic time 3s.
(2) clean, diadust is cleaned by ultrasonic with bus using pure water, and water temperature is controlled at 60 ± 2 DEG C.The bus
First pass through in ultrasonic pure water rinse bath 3, it is desirable to be immersed in liquid level 10mm depths, water temperature is controlled at 60 ± 2 DEG C；Sequentially pass through drift
Washing trough 4, descaling bath 5, secondary potcher 6 thoroughly remove impurity, potcher 4 and the secondary drifts such as bus oxide on surface, residue
It is three grooves in washing trough 6, inside fills pure water, water temperature controls to fill 40g/L sulfamic acid, temperature in 60 ± 2 DEG C, descaling bath 5
Spend for 20 ± 2 DEG C.
(3) surface preparation, to diadust using concentration 33%NaOH and concentration 33%HNO3Solution, soaks respectively
15min, corrosion treatment is carried out to surface and forms micro/nano level pit, then through over cleaning, drying；33% dilute sulphur is used to bus
Acid, salt acid soak 3.5s carry out surface corrosion processing, then through over cleaning, 150 DEG C of drying.
(4) preplating, diadust preplating：Plating solution formula：Contain nickel sulfate 21g, boric acid 8g, chlorination in 1L plating solution
Nickel 4g, absolute ethyl alcohol sodium 16g, naphthalene trisulfonic acid sodium 3g, mixing speed 20 turns/min, pH=3.8；
The preplating of bus：(every liter of nickel sulfamic acid stoste contains nickel ion by electroplate liquid 120L, nickel sulfamic acid 0.3L/L
120g), boric acid 18g/L, nickel chloride 3g/L, lauryl sodium sulfate 0.2g/L.Bus connects negative pole, and positive pole uniformly lays nickel plate,
Electric current 0.72A, 50 ± 2 DEG C of bath temperature, plating fluid viscosity 1.0mPa s, PH3.8.
(5) sand on, the upper solution composition of sand launder 8：Plating solution 250L, nickel sulfamic acid 0.51L/L (every liter of nickel sulfamic acid stoste
Contain nickel ion 140g), boric acid 28g/L, nickel chloride 10g/L, diadust particle diameter average 10um, diadust 4.0g/
L, additive weight in mass ratio is 23, electric current 12.5A, and 50 ± 2 DEG C of bath temperature plates fluid viscosity 1.1mPa s, plates liquid recycle stream
Measure 150L/min, PH4.6.
(6) secondary plating, carries out plating thickening, purpose enhancing diamond exists by the bus of upper complete sand by secondary thickening groove 9
Adhesive force on bus.Solution composition in secondary coating bath：Electroplate liquid 260L, nickel sulfamic acid 0.6L/L (every liter of nickel sulfamic acid
Stoste contains nickel ion 160g), boric acid 34g/L, nickel chloride 11.5g/L, brightener 3g, electric current 28A, 52 ± 2 DEG C of bath temperature,
Plate fluid viscosity 1.3mPa s, plating solution circular flow 150L/min, PH 3.9.
(7) cleaning, drying, take-up, the diamond wire of secondary thickening removes surface residue by potcher 10, by drying
Case 11, oven temperature is set in 200 DEG C, after drying by guide wheel according to the winding department of setting away from being wound on take-up pulley 12, take-up
Tension force is set in 7.5N.
Embodiment 3
The bus diameter used in the present embodiment is 65um.Manufacture method of the present invention is comprised the steps of：(1) impurity elimination, (2)
Cleaning, (3) surface preparation, (4) preplating, sand on (5), (6) secondary plating, (7) cleaning, drying, take-up are comprised the following steps that：
(1) impurity elimination, includes diadust impurity elimination and bus impurity elimination.Diadust impurity elimination is in 80 DEG C of temperature, concentration
Surface and oil contaminant, then the HNO through over-richness 15% are removed in 15%NaOH solution3Compound, ultrasonic time 360s are deoxygenated in solution；It is female
Line is to release to enter by guide wheel from actinobacillus wheel 1 to go to degrease in ultrasonic tank 2, and degreasing powder concentration is 20g/L in ultrasonic tank 2,
Water temperature is controlled in 60 ± 2 DEG C, ultrasonic time 4s.
(2) clean, diadust is cleaned by ultrasonic with bus using pure water, and water temperature is controlled at 60 ± 2 DEG C.The bus
First pass through in ultrasonic pure water rinse bath 3, it is desirable to be immersed in liquid level 10mm depths, water temperature is controlled at 60 ± 2 DEG C；Sequentially pass through drift
Washing trough 4, descaling bath 5, secondary potcher 6 thoroughly remove impurity, potcher 4 and the secondary drifts such as bus oxide on surface, residue
It is three grooves in washing trough 6, inside fills pure water, water temperature controls to fill 45g/L sulfamic acid, temperature in 60 ± 2 DEG C, descaling bath 5
Spend for 20 ± 2 DEG C.
(3) surface preparation, to diadust using concentration 32%NaOH and concentration 32%HNO3Solution, soaks respectively
20min, corrosion treatment is carried out to surface and forms micro/nano level pit, then through over cleaning, drying；Dilute sulfuric acid, salt are used to bus
Acid soak 4s carries out surface corrosion processing, then through over cleaning, 150 DEG C of drying.
(4) preplating, diadust preplating：Plating solution formula：Contain nickel sulfate 21g, boric acid 8g, chlorination in 1L plating solution
Nickel 4g, absolute ethyl alcohol sodium 16g, naphthalene trisulfonic acid sodium 3g, mixing speed 20 turns/min, pH3.8；
The preplating of bus：(every liter of nickel sulfamic acid stoste contains nickel ion by electroplate liquid 120L, nickel sulfamic acid 0.3L/L
120g), boric acid 18g/L, nickel chloride 3g/L, lauryl sodium sulfate 0.2g/L, bus connects negative pole, and positive pole uniformly lays nickel plate,
Electric current 0.72A, 50 ± 2 DEG C of bath temperature, plating fluid viscosity 1.0mPa s, PH3.8.
(5) sand on, the upper solution composition of sand launder 8：Plating solution 250L, nickel sulfamic acid 0.5L/L (every liter of nickel sulfamic acid stoste
Contain nickel ion 150g), boric acid 30g/L, nickel chloride 10g/L, diadust particle diameter average 8um, diadust 4.1g/L,
Additive weight in mass ratio is 23, electric current 12.5A, and 50 ± 2 DEG C of bath temperature plates fluid viscosity 1.2mPa s, plating solution circular flow
150L/min, PH4.4.
(6) secondary plating, carries out plating thickening, purpose enhancing diamond exists by the bus of upper complete sand by secondary thickening groove 9
Solution composition in adhesive force on bus, secondary coating bath：Electroplate liquid 260L, nickel sulfamic acid 0.55L/L (every liter of nickel sulfamic acid
Stoste contains nickel ion 170g), boric acid 30g/L, nickel chloride 10g/L, brightener 3g, electric current 28A, 52 ± 2 DEG C of bath temperature, plating
Fluid viscosity 1.3mPa s, plating solution circular flow 150L/min, PH3.8.
The step (7), the diamond wire of secondary thickening removes surface residue by potcher 10, by drying baker 11,
Oven temperature is set in 200 DEG C, after drying by guide wheel according to the winding department of setting away from being wound on take-up pulley 12, takeup tension is set
It is scheduled on 4.5N.
Embodiment 4
The bus diameter used in the present embodiment is 60um.Manufacture method of the present invention is comprised the steps of：(1) impurity elimination, (2)
Cleaning, (3) surface preparation, (4) preplating, sand on (5), (6) secondary plating, (7) cleaning, drying, take-up are comprised the following steps that：
(1) impurity elimination, includes diadust impurity elimination and bus impurity elimination.Diadust impurity elimination is in 80 DEG C of temperature, concentration
Surface and oil contaminant, then the HNO through over-richness 15% are removed in 15%NaOH solution3Deoxygenate compound in solution, ultrasonic time 360s,；
Bus is to release to enter by guide wheel from actinobacillus wheel 1 to go to degrease in ultrasonic tank 2, and degreasing powder concentration is 20g/ in ultrasonic tank 2
L, water temperature is controlled in 60 ± 1 DEG C, ultrasonic time 4s.
(2) clean, diadust is cleaned by ultrasonic with bus using pure water, and water temperature is controlled at 60 ± 2 DEG C.The bus
First pass through in ultrasonic pure water rinse bath 3, it is desirable to be immersed in liquid level 10mm depths, water temperature is controlled at 60 ± 2 DEG C；Sequentially pass through drift
Washing trough 4, descaling bath 5, secondary potcher 6 thoroughly remove impurity, potcher 4 and the secondary drifts such as bus oxide on surface, residue
It is three grooves in washing trough 6, inside fills pure water, water temperature controls to fill 50g/L sulfamic acid, temperature in 60 ± 2 DEG C, descaling bath 5
Spend for 20 ± 2 DEG C.
(3) surface preparation, to diadust using concentration 32%NaOH and concentration 32%HNO3Solution, soaks respectively
30min carries out corrosion treatment to surface and forms micro/nano level pit, then through over cleaning, drying；Dilute sulfuric acid, hydrochloric acid are used to bus
Soak 5s and carry out surface corrosion processing, then through over cleaning, 150 DEG C of drying.
(4) preplating, diadust preplating：Plating solution formula：Contain nickel sulfate 21g, boric acid 8g, chlorination in 1L plating solution
Nickel 4g, absolute ethyl alcohol sodium 16g, naphthalene trisulfonic acid sodium 3g, mixing speed 20 turns/min, pH=3.8；
The preplating of bus：(every liter of nickel sulfamic acid stoste contains nickel ion by electroplate liquid 120L, nickel sulfamic acid 0.3L/L
120g), boric acid 18g/L, nickel chloride 3g/L, lauryl sodium sulfate 0.2g/L, bus connects negative pole, and positive pole uniformly lays nickel plate,
Electric current 0.72A, 50 ± 2 DEG C of bath temperature, plating fluid viscosity 1.0mPa s, PH3.8.
(5) sand on, the upper solution composition of sand launder 8：Plating solution 250L, nickel sulfamic acid 0.5L/L (every liter of nickel sulfamic acid stoste
Contain nickel ion 150g), boric acid 30g/L, nickel chloride 10.5g/L, diadust particle diameter average 8um, diadust 4.3g/
L, additive weight in mass ratio is 24, electric current 13A, 50 ± 2 DEG C of bath temperature, plating fluid viscosity 1.1mPa s, PH4.8.
(6) secondary plating, carries out plating thickening, purpose enhancing diamond exists by the bus of upper complete sand by secondary thickening groove 9
Solution composition in adhesive force on bus, secondary coating bath：Electroplate liquid 260L, nickel sulfamic acid 0.55L/L (every liter of nickel sulfamic acid
Stoste contains nickel ion 175g), boric acid 30g/L, nickel chloride 10.5g/L, brightener 3g, electric current 29A, 52 ± 2 DEG C of bath temperature,
Plate fluid viscosity 1.4mPa s, plating solution circular flow 150L/min, PH4.0.
(7) cleaning, drying, take-up, the diamond wire of secondary thickening removes surface residue by potcher 10, by drying
Case 11, oven temperature is set in 200 DEG C, after drying by guide wheel according to the winding department of setting away from being wound on take-up pulley 12, take-up
Tension force is set in 3.5N.
Major parameter is contrasted in the manufacture method of diamond wire in above-mentioned 4 embodiments, as shown in table 1.Table 1 is embodiment 1-
The parameter of diamond wire manufacture method in 4.
The parameter of diamond wire manufacture method in the embodiment 1-4 of table 1
Although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of changes, modification can be carried out to these embodiments, replace without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (10)
1. a kind of manufacture method of high efficiency cutting silicon chip diamond wire, it is characterised in that the manufacture method comprises the following steps：
（1）Unwrapping wire, impurity elimination,（2）Cleaning,（3）Surface preparation,（4）Preplating,（5）Upper sand,（6）Secondary plating,（7）Cleaning, drying, receipts
Line；
The step（5）Upper sand, is that diadust is electroplated onto into bus matrix surface：By step（4）The good Buddha's warrior attendant of middle preplating
Stone micro mist is mixed with plating solution to be put into a mixing bowl, and by being pumped into bath trough, bus is wrapped on roller, is immersed into plating solution
Lower section 5-10mm is simultaneously at the uniform velocity passed through with 12-20m/min, and bus is connected with power cathode, and nickel block is distributed with bath trough bottom even,
Nickel block switches on power positive pole, plating solution 200-280L in upper sand launder, wherein, nickel sulfamic acid 0.4-0.6L/L, boric acid 20-30g/L,
Electric current 12- in nickel chloride 9-12g/L, diadust input amount 3.7-4.3g/L, additive proportion 20-30, electroplating process
15A, 50 ± 2 DEG C of bath temperature plates fluid viscosity 1.1-1.3mPa s, liquid circulation flow 150L/min, PH4.6-5.1；
The step（6）Secondary plating, its electroplating process and step（5）It is identical, secondary solution composition：Electroplate liquid 250-300L, ammonia
Base nickel sulphonic acid 0.5-0.6L/L, boric acid 25-30g/L, nickel chloride 9-12g/L, brightener 0.01-0.02g/L, electric current 28-30A,
52 ± 2 DEG C of bath temperature, plates fluid viscosity 1.3-1.4mPa s, liquid circulation flow 150L/min, PH 3.8-4.4.
2. a kind of manufacture method of high efficiency cutting silicon chip diamond wire according to claim 1, it is characterised in that the step
Suddenly（1）Middle impurity elimination includes diadust impurity elimination and bus impurity elimination, and diadust impurity elimination is in 70-80 by diadust
DEG C, mass concentration for 15%-20% NaOH solution in ultrasound 120-360s, then mass concentration be 15%-20%HNO3In solution
Ultrasonic 120-360s；Bus impurity elimination is that bus is put into except in oil solution, ultrasonic 3-5s, except degreasing powder concentration is in oil solution
20-40g/L, proportion is 3-4, and temperature is 60 ± 2 DEG C.
3. a kind of manufacture method of high efficiency cutting silicon chip diamond wire according to claim 1, it is characterised in that the step
Suddenly（2）Middle cleaning includes diadust and bus cleaning, including ultrasonic cleaning, once rinsing, pickling, secondary rinsing.
4. a kind of manufacture method of high efficiency cutting silicon chip diamond wire according to claim 1, it is characterised in that the step
Suddenly（3）Surface preparation, includes diadust surface preparation and bus surface preparation；Wherein, diadust surface
Pretreatment：Diadust is first sequentially placed into NaOH and HNO3Solution carries out immersion corrosion, soak time 10-30min, then passes through
Ultrasound rinsing is crossed, finally filters and dries using filter paper；Surface corrosion pretreatment is carried out using dilute sulfuric acid and hydrochloric acid to bus, it is rotten
Erosion time 3-5s, then by pure water cleaning, drying.
5. a kind of manufacture method of high efficiency cutting silicon chip diamond wire according to claim 1, it is characterised in that the step
Suddenly（4）Preplating, including diadust preplating and bus preplating；
Wherein, diadust preplating：Diadust after surface preparation is added in plating fluid cylinder, has stirring in plating fluid cylinder
Device, mixing speed 20-30 turns/min, the composition of the chemical plating fluid：Nickel sulfate 19-25g/L, boric acid 8-10g/L, nickel chloride
4-6g/L, absolute ethyl alcohol sodium 12-20g/L, naphthalene trisulfonic acid sodium 2-5g/L, pH3.8 ~ 4.4；
Bus preplating：Bus after surface preparation is driven through electric bath groove by roller, bus is immersed in below plating solution
5-10mm, bus access power cathode plates liquid measure 100-120L wherein in bath trough, bath trough bottom even laying nickel block connects
Enter positive source, electric current 0.7-0.8A, the composition of the electroplate liquid：Nickel sulfamic acid 0.2-0.5L/L, boric acid 15-20g/L, chlorine
Change nickel 3-6g/L, lauryl sodium sulfate 0.2-0.3g/L, 50 ± 2 DEG C of bath temperature plates fluid viscosity 1.0-1.2mPa s,
PH3.8-4.2。
6. the manufacture method of a kind of high efficiency cutting silicon chip diamond wire according to claim 1, it is characterised in that described
Step（5）10mm below bus immersion plating solution, diamond particles bury to bus nickel dam 2-3um.
7. a kind of manufacture method of high efficiency cutting silicon chip diamond wire according to claim 1, it is characterised in that the step
Suddenly（5）Middle additive includes complexing agent, dispersant and brightener, and above-mentioned substance is 3: 2: 1-3: 3: 1 mixing according to mass ratio.
8. a kind of manufacture method of high efficiency cutting silicon chip diamond wire according to claim 1, it is characterised in that the step
Suddenly（5）The addition manner of middle additive is added using titration.
9. a kind of manufacture method of high efficiency cutting silicon chip diamond wire according to claim 1, it is characterised in that the step
Suddenly（5）Middle current control accuracy requirement is in ± 0.1A；The running stability requires bus electroplating velocity precision controlling in 0.01-
0.03m/min。
10. the manufacture method of a kind of high efficiency cutting silicon chip diamond wire according to claim 1, it is characterised in that described
Step（7）The diamond wire of secondary thickening removes surface residue by potcher, and by drying baker, oven temperature is set in 150-
300 DEG C, after drying by guide wheel according to the winding department of setting away from being wound on take-up pulley, takeup tension is set in 4-10N.
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