CN105185877A - Sapphire LED filament preparation method - Google Patents

Sapphire LED filament preparation method Download PDF

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Publication number
CN105185877A
CN105185877A CN201510339646.7A CN201510339646A CN105185877A CN 105185877 A CN105185877 A CN 105185877A CN 201510339646 A CN201510339646 A CN 201510339646A CN 105185877 A CN105185877 A CN 105185877A
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Prior art keywords
crystal
wafer
speed
polishing
sapphire
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Inventor
苏凤坚
刘俊
郝正平
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Jiangsu Sue And Optical Equipment Co Ltd
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Jiangsu Sue And Optical Equipment Co Ltd
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Priority to CN201510339646.7A priority Critical patent/CN105185877A/en
Publication of CN105185877A publication Critical patent/CN105185877A/en
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/005Processes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B24GRINDING; POLISHING
    • B24BMACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B37/00Lapping machines or devices; Accessories
    • B24B37/04Lapping machines or devices; Accessories designed for working plane surfaces
    • B24B37/042Lapping machines or devices; Accessories designed for working plane surfaces operating processes therefor
    • B24B37/044Lapping machines or devices; Accessories designed for working plane surfaces operating processes therefor characterised by the composition of the lapping agent
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B24GRINDING; POLISHING
    • B24BMACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B37/00Lapping machines or devices; Accessories
    • B24B37/04Lapping machines or devices; Accessories designed for working plane surfaces
    • B24B37/07Lapping machines or devices; Accessories designed for working plane surfaces characterised by the movement of the work or lapping tool
    • B24B37/08Lapping machines or devices; Accessories designed for working plane surfaces characterised by the movement of the work or lapping tool for double side lapping
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B24GRINDING; POLISHING
    • B24BMACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B9/00Machines or devices designed for grinding edges or bevels on work or for removing burrs; Accessories therefor
    • B24B9/02Machines or devices designed for grinding edges or bevels on work or for removing burrs; Accessories therefor characterised by a special design with respect to properties of materials specific to articles to be ground
    • B24B9/06Machines or devices designed for grinding edges or bevels on work or for removing burrs; Accessories therefor characterised by a special design with respect to properties of materials specific to articles to be ground of non-metallic inorganic material, e.g. stone, ceramics, porcelain
    • B24B9/065Machines or devices designed for grinding edges or bevels on work or for removing burrs; Accessories therefor characterised by a special design with respect to properties of materials specific to articles to be ground of non-metallic inorganic material, e.g. stone, ceramics, porcelain of thin, brittle parts, e.g. semiconductors, wafers
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2933/00Details relating to devices covered by the group H01L33/00 but not provided for in its subgroups
    • H01L2933/0008Processes
    • H01L2933/0033Processes relating to semiconductor body packages

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Computer Hardware Design (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Power Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Led Devices (AREA)
  • Mechanical Treatment Of Semiconductor (AREA)

Abstract

The invention relates to a sapphire LED filament preparation method specifically comprising the steps of crystal growing, bar hollowing-out from crystal, crystal cutting, grinding, chamfering, annealing, double-sided polishing, wafer cutting through laser, circuit printing, chip welding, encapsulation, and the like. Sapphire LED filaments prepared by the method of the invention are of high quality, the rejection rate is low, and the production efficiency is high.

Description

The preparation method of sapphire LED silk
Technical field
The present invention relates to a kind of preparation method of sapphire sheet, particularly relate to a kind of preparation method of sapphire LED silk, belong to technical field of sapphire treatment.
Background technology
Advantages such as LED silk is energy-conservation with it, full angle is luminous and being widely used.At present, the material of LED silk substrate is generally glass, silicones or carborundum, but glass hard (HRC65Yi Shang) is poor, poor thermal conductivity; Silicones poor thermal conductivity; Carborundum then cost of manufacture is large.
Along with the progress of science and technology, sapphire substrate is used widely in LED technology.Sapphire has good thermal characteristics, fabulous electrical characteristic and dielectric property, at high temperature can keep high strength, excellent hot attribute and transmitance, and anti-chemical corrosion.Be the LED silk that raw material is made with sapphire, brightness is high, and hardness is high and thermal conductivity good, deeply by consumer satisfaction.
Chinese patent literature ZL201420699840.7 discloses a kind of LED silk of all-round luminescence, comprise the substrate being mixed with fluorescent material, be arranged at the electrode on described substrate, at least one LED chip be on the substrate installed, and be covered in the packaging plastic on described LED chip.By the substrate that the silicones containing fluorescent material is formed, eliminate glass or the sapphire cost as substrate.The substrate that the silicones being mixed with fluorescent material is formed instead of glass and sapphire substrate, and use the filament of described substrate manufacture to avoid glass or sapphire to the impact of chip light-emitting, achieve 360 degree of bright dippings, light-emitting uniformity and light efficiency improve greatly.But the method process step design is reasonable not, quality and the rate of finished products of LED silk directly can be affected.
Summary of the invention
The technical problem that the present invention solves is: propose a kind of one-tenth tablet quality high, percent defective is low, the preparation method of the sapphire LED silk that production efficiency is high.
In order to solve the problems of the technologies described above, the technical scheme that the present invention proposes is: a kind of preparation method of sapphire LED silk, comprises following concrete steps:
Step one, crystal growth; Pure Al is loaded in the crucible of crystal growing furnace 2o 3raw material, is provided with lifting rod that is rotatable and lifting above described crucible, the lower end of lifting rod is folded with the seed crystal in A crystal orientation, M crystal orientation or C crystal orientation; To vacuumize in crystal growing furnace and pass into protective gas, be warming up to 2100 ~ 2200 DEG C, make Al 2o 3melting, the liquid level temperature controlling melt is 2055 DEG C, and seed crystal is placed in Al 2o 3the upper surface of melt makes itself and melt contacts, continues 0.5 ~ 1h; After seed crystal and melt are fully stained with profit, lift and rotate seed crystal, thus realizing necking down-expansion shoulder-isodiametric growth; In the necking down stage, the liquid level temperature controlling melt is 2050 DEG C, upwards lifts seed crystal with the speed of 3 ~ 5mm/h, rotates seed crystal with the speed of 45 ~ 48r/min; Expand the shoulder stage, the liquid level temperature controlling melt is 2048 DEG C, upwards lifts seed crystal with the speed of 8 ~ 10mm/h, rotates seed crystal with the speed of 50 ~ 55r/min; In the isometrical stage, the liquid level temperature controlling melt is 2052 DEG C, upwards lifts seed crystal with the speed of 5 ~ 8mm/h, rotates seed crystal with the speed of 48 ~ 50r/min; After crystal growth terminates, the temperature in crystal growing furnace is down to 1580 ~ 1680 DEG C, then carries out annealing in process to crystal, control temperature also continues 18 ~ 22h with the speed slow cooling of 80 ~ 100 DEG C/h, thus obtains crystal;
Step 2, crystal draw rod; Orientation is carried out to crystal, then uses and draw excellent machine and carry out drawing rod, thus obtain crystal bar;
Step 3, crystal-cut; Adopt carborundum line cutting equipment to cut crystal bar, thus obtain wafer;
Step 4, grinding; Grinder is adopted to grind wafer; During grinding, add lapping liquid, abrasive disk is forced into 0.02 ~ 0.022Mpa to wafer, and the rotating speed of abrasive disk is 1000 ~ 1200rpm/min; Grind rear washes of absolute alcohol; Described lapping liquid component comprises: the granular size of 0.5 ~ 2% is the cubic boron nitride powder of 10 ~ 20 μm, the APES of 14 ~ 16%, the glycerine of 4 ~ 6%, the polypropylene glycol 400 of 9 ~ 11%, and all the other are deionized water;
Step 5, chamfering; The skive of Digit Control Machine Tool is adopted to carry out chamfered to the corner of wafer;
Step 6, annealing; Wafer is put into annealing furnace, carry out heating up with the speed of 180 ~ 220 DEG C/h and temperature risen to 1600 DEG C, 2 ~ 6h is incubated respectively at 300 DEG C, 800 DEG C, 1600 DEG C during intensification, then lower the temperature with the temperature of 200 DEG C, be incubated 2 ~ 3h respectively at 1000 DEG C, 500 DEG C during cooling and be cooled to room temperature taking-up;
Step 7, double side chemical polishing; First with absolute ethyl alcohol, wafer is cleaned, then the wafer after cleaning is put into Twp-sided polishing machine and fix; During polishing, add polishing fluid, polishing disk is forced into 0.12 ~ 0.15Mpa to wafer, and the rotating speed of polishing disk is 1000 ~ 1500rpm/min, by after polished wafer washes of absolute alcohol, at room temperature carries out nature cooling; Described polishing fluid component comprises: the granular size of 0.5 ~ 2% is the cubic boron nitride powder of 1 ~ 6 μm, the APES of 14 ~ 16%, the glycerine of 4 ~ 6%, the polypropylene glycol 400 of 9 ~ 11%, the nano silicon of 0.5 ~ 2%, make polishing fluid pH value be 11.0 ~ 13.0 alkaline solution, all the other are deionized water; Alkaline solution is constantly supplemented to keep the pH value of polishing fluid in polishing process;
Step 8, laser get sheet; Wafer after polishing is put into laser cutting machine and passes into protective gas, wafer is cut into corresponding size by demand;
Step 9, printed circuit; Laser is got the silver of the Sapphire wafer surface after sheet slurry printed circuit, be then heated to 400 ~ 500 degrees Celsius and circuit is sintered on sapphire wafer;
Step 10, welding chip; LED chip scaling powder is fixed on printed circuit, is heated to 400 ~ 450 degrees Celsius by chips welding on printed circuit;
Step 11, encapsulation; Fluorescent glue is used sapphire wafer and LED chip to be encapsulated.
Being improved to technique scheme: in described step one, the temperature in crystal growing furnace is down to 1600 DEG C, then annealing in process is carried out to crystal, control temperature also continues 22h with the speed slow cooling of 100 DEG C/h.
Being improved to technique scheme: in described step 3, the diameter of carborundum line is 0.14 ~ 0.16mm, on carborundum line, adamantine particle diameter is 30 ~ 40 μm, carborundum line moves with the speed of 12 ~ 15m/s when cutting, crystal is 0.2 ~ 0.3mm/min relative to the translational speed of carborundum line, constantly cutting liquid is sprayed to carborundum line, containing particle diameter to be the diamond particles of 20 ~ 30 μm and particle diameter the be corundum in granules of 50 ~ 60 μm in described cutting liquid during cutting.
Being improved to technique scheme: in described step 4 is the alumina particle of 3 ~ 6 μm containing particle diameter in described lapping liquid.
Being improved to technique scheme: in described step 6, during intensification, at 300 DEG C of insulation 2h, at 800 DEG C of insulation 3h, at 1600 DEG C of insulation 4h.
Being improved to technique scheme: in described step 7, described alkaline solution is KOH.
Being improved to technique scheme: in described step 7, described polishing fluid pH value is 12.0.
Being improved to technique scheme: in described step 7, polishing disk is forced into 0.135Mpa to wafer.
Being improved to technique scheme: in described step 8, the diameter of laser beam is 0.015 ~ 0.02mm, and cutting speed is 3 ~ 5mm/s.
Being improved to technique scheme: protective gas described in step 8 is nitrogen.
The present invention has positive effect:
(1) LED silk preparation method of the present invention, sheet is got in first grinding, polishing again laser, the production efficiency of grinding, polishing can be improved, because sapphire hardness is large, larger pressure must be applied during polishing, annealing is conducive to the internal stress that machining operation such as elimination Linear cut, grinding etc. produces before polishing., makes wafer unsuitable cracked when polishing, effectively improves rate of finished products.
(2) LED silk preparation method of the present invention, interface temperature during strict control crystal growth, draw high speed, rotary speed and annealing parameter, interface temperature is controlled at 2048 ~ 2052 DEG C, draw high speeds control at 3 ~ 10mm/h, rotary speed controls at 45 ~ 55r/min, annealing temperature controls at 1580 ~ 1680 DEG C (preferably 1600 DEG C), also 18 ~ 22h is continued with the speed slow cooling of 80 ~ 100 DEG C/h, thus make the production capacity of crystal high, defect concentration is low, quality is good, and rate of finished products is high, can reduce production cost widely.
(3) LED silk preparation method of the present invention, strict control grinding and the parameter of polishing and the composition of lapping liquid and polishing fluid, be conducive to the efficiency improving grinding and polishing, improve the rate of finished products of grinding and polishing, the chip architecture prepared is complete, and without physical damnification, surface is fine and smooth, smooth, deformation is little.In lapping liquid and polishing fluid, appropriate cubic boron nitride powder serves as abrasive material, and hardness is high, and resistance to wear is good; The suspension viscosity that APES, glycerine, polypropylene glycol 400 and deionized water are formed and interfacial film stable in properties, abrasive suspension is stablized, and good evenness, can not glue also, is conducive to the quality and the efficiency that improve grinding and polishing.Appropriate APES is a kind of non-ionic surface active agent, its stable in properties, and having dispersion, emulsification, the multiple performance such as wetting, is that suspension obtains the topmost composition of excellent properties; Glycerine proportion is suitable, has good dissolubility with water and organic solution, very applicable as auxiliary dispersants; Polypropylene glycol 400 has emulsification, wetting effect, and can effectively thickening, effectively promotes viscosity and the interfacial film character of suspension.In addition, appropriate Nano-meter SiO_2 is contained in polishing fluid 2, epigranular, good dispersion, planarization efficiency are high.Alkaline solution KOH makes polishing fluid be alkalescence, assists polishing by chemical corrosion, thus polishing effect is better, and polishing efficiency is better.In order to keep the stability of polishing fluid, thus ensureing efficiency and the quality of polishing, constantly must supplement alkaline solution, maintaining polishing fluid pH value substantially constant.
(4) LED silk of the present invention adopts sapphire to be that substrate is made, and because sapphire hardness is high, resistance to wear is good, does not make substrate easy to wear and scratch.By the filament that LED silk preparation method of the present invention makes, luminous efficiency is high, and optical property is up to standard, and becomes tablet quality high, and percent defective is low, and production efficiency is high, has a extensive future.
Embodiment
Embodiment 1
The preparation flow of the sapphire LED silk of the present embodiment comprises the steps:
Step one, crystal growth; Pure Al is loaded in the crucible of crystal growing furnace 2o 3raw material, is provided with lifting rod that is rotatable and lifting above described crucible, the lower end of lifting rod is folded with the seed crystal in A crystal orientation, M crystal orientation or C crystal orientation; To vacuumize in crystal growing furnace and pass into protective gas, be warming up to 2200 DEG C, make Al 2o 3melting, the liquid level temperature controlling melt is 2055 DEG C, and seed crystal is placed in Al 2o 3the upper surface of melt makes itself and melt contacts, continues 1h; After seed crystal and melt are fully stained with profit, lift and rotate seed crystal, thus realizing necking down-expansion shoulder-isodiametric growth; In the necking down stage, the liquid level temperature controlling melt is 2050 DEG C, upwards lifts seed crystal with the speed of 5mm/h, rotates seed crystal with the speed of 48r/min; Expand the shoulder stage, the liquid level temperature controlling melt is 2048 DEG C, upwards lifts seed crystal with the speed of 10mm/h, rotates seed crystal with the speed of 55r/min; In the isometrical stage, the liquid level temperature controlling melt is 2052 DEG C, upwards lifts seed crystal with the speed of 8mm/h, rotates seed crystal with the speed of 50r/min; After crystal growth terminates, the temperature in crystal growing furnace is down to 1680 DEG C, then carries out annealing in process to crystal, control temperature also continues 22h with the speed slow cooling of 100 DEG C/h, thus obtains crystal;
Step 2, crystal draw rod; Orientation is carried out to crystal, then uses and draw excellent machine and carry out drawing rod, thus obtain crystal bar;
Step 3, crystal-cut; Adopt carborundum line cutting equipment to cut crystal bar, thus obtain wafer;
Step 4, grinding; Grinder is adopted to grind wafer; During grinding, add lapping liquid, abrasive disk is forced into 0.022Mpa to wafer, and the rotating speed of abrasive disk is 1200rpm/min; Grind rear washes of absolute alcohol; Described lapping liquid component comprises: the granular size of 2% is the cubic boron nitride powder of 20 μm, the APES of 16%, the glycerine of 6%, the polypropylene glycol 400 of 11%, and all the other are deionized water;
Step 5, chamfering; The skive of Digit Control Machine Tool is adopted to carry out chamfered to the corner of wafer;
Step 6, annealing; Wafer is put into annealing furnace, carry out heating up with the speed of 220 DEG C/h and temperature risen to 1600 DEG C, be incubated 6h respectively at 300 DEG C, 800 DEG C, 1600 DEG C during intensification, then lower the temperature with the temperature of 200 DEG C, be incubated 3h respectively at 1000 DEG C, 500 DEG C during cooling and be cooled to room temperature taking-up;
Step 7, double side chemical polishing; First with absolute ethyl alcohol, wafer is cleaned, then the wafer after cleaning is put into Twp-sided polishing machine and fix; During polishing, add polishing fluid, polishing disk is forced into 0.15Mpa to wafer, and the rotating speed of polishing disk is 1500rpm/min, by after polished wafer washes of absolute alcohol, at room temperature carries out nature cooling; Described polishing fluid component comprises: the granular size of 2% is the cubic boron nitride powder of 6 μm, the APES of 16%, the glycerine of 6%, the polypropylene glycol 400 of 11%, the nano silicon of 2%, make polishing fluid pH value be 13.0 alkaline solution, all the other are deionized water; Alkaline solution is constantly supplemented to keep the pH value of polishing fluid in polishing process;
Step 8, laser get sheet; Wafer after polishing is put into laser cutting machine and passes into protective gas, wafer is cut into corresponding size by demand;
Step 9, printed circuit; Laser is got the silver of the Sapphire wafer surface after sheet slurry printed circuit, be then heated to 500 degrees Celsius and circuit is sintered on sapphire wafer;
Step 10, welding chip; LED chip scaling powder is fixed on printed circuit, is heated to 450 degrees Celsius by chips welding on printed circuit;
Step 11, encapsulation; Fluorescent glue is used sapphire wafer and LED chip to be encapsulated.
Embodiment 2
The preparation flow of the sapphire LED silk of the present embodiment comprises the steps:
Step one, crystal growth; Pure Al is loaded in the crucible of crystal growing furnace 2o 3raw material, is provided with lifting rod that is rotatable and lifting above described crucible, the lower end of lifting rod is folded with the seed crystal in A crystal orientation, M crystal orientation or C crystal orientation; To vacuumize in crystal growing furnace and pass into protective gas, be warming up to 2100 DEG C, make Al 2o 3melting, the liquid level temperature controlling melt is 2055 DEG C, and seed crystal is placed in Al 2o 3the upper surface of melt makes itself and melt contacts, continues 0.5 ~ 1h; After seed crystal and melt are fully stained with profit, lift and rotate seed crystal, thus realizing necking down-expansion shoulder-isodiametric growth; In the necking down stage, the liquid level temperature controlling melt is 2050 DEG C, upwards lifts seed crystal with the speed of 3mm/h, rotates seed crystal with the speed of 45r/min; Expand the shoulder stage, the liquid level temperature controlling melt is 2048 DEG C, upwards lifts seed crystal with the speed of 8mm/h, rotates seed crystal with the speed of 50r/min; In the isometrical stage, the liquid level temperature controlling melt is 2052 DEG C, upwards lifts seed crystal with the speed of 5mm/h, rotates seed crystal with the speed of 48r/min; After crystal growth terminates, the temperature in crystal growing furnace is down to 1580 DEG C, then carries out annealing in process to crystal, control temperature also continues 18h with the speed slow cooling of 80 ~ 100 DEG C/h, thus obtains crystal;
Step 2, crystal draw rod; Orientation is carried out to crystal, then uses and draw excellent machine and carry out drawing rod, thus obtain crystal bar;
Step 3, crystal-cut; Adopt carborundum line cutting equipment to cut crystal bar, thus obtain wafer;
Step 4, grinding; Grinder is adopted to grind wafer; During grinding, add lapping liquid, abrasive disk is forced into 0.02Mpa to wafer, and the rotating speed of abrasive disk is 1000rpm/min; Grind rear washes of absolute alcohol; Described lapping liquid component comprises: the granular size of 0.5% is the cubic boron nitride powder of 10 μm, the APES of 14%, the glycerine of 4%, the polypropylene glycol 400 of 9%, and all the other are deionized water;
Step 5, chamfering; The skive of Digit Control Machine Tool is adopted to carry out chamfered to the corner of wafer;
Step 6, annealing; Wafer is put into annealing furnace, carry out heating up with the speed of 180 DEG C/h and temperature risen to 1600 DEG C, be incubated 2h respectively at 300 DEG C, 800 DEG C, 1600 DEG C during intensification, then lower the temperature with the temperature of 200 DEG C, be incubated 2h respectively at 1000 DEG C, 500 DEG C during cooling and be cooled to room temperature taking-up;
Step 7, double side chemical polishing; First with absolute ethyl alcohol, wafer is cleaned, then the wafer after cleaning is put into Twp-sided polishing machine and fix; During polishing, add polishing fluid, polishing disk is forced into 0.12Mpa to wafer, and the rotating speed of polishing disk is 1000rpm/min, by after polished wafer washes of absolute alcohol, at room temperature carries out nature cooling; Described polishing fluid component comprises: the granular size of 0.5% is the cubic boron nitride powder of 1 μm, the APES of 14%, the glycerine of 4%, the polypropylene glycol 400 of 9%, the nano silicon of 0.5%, make polishing fluid pH value be 11.0 alkaline solution, all the other are deionized water; Alkaline solution is constantly supplemented to keep the pH value of polishing fluid in polishing process;
Step 8, laser get sheet; Wafer after polishing is put into laser cutting machine and passes into protective gas, wafer is cut into corresponding size by demand;
Step 9, printed circuit; Laser is got the silver of the Sapphire wafer surface after sheet slurry printed circuit, be then heated to 400 degrees Celsius and circuit is sintered on sapphire wafer;
Step 10, welding chip; LED chip scaling powder is fixed on printed circuit, is heated to 400 degrees Celsius by chips welding on printed circuit;
Step 11, encapsulation; Fluorescent glue is used sapphire wafer and LED chip to be encapsulated.
Embodiment 3
The preparation flow of the sapphire LED silk of the present embodiment comprises the steps:
Step one, crystal growth; Pure Al is loaded in the crucible of crystal growing furnace 2o 3raw material, is provided with lifting rod that is rotatable and lifting above described crucible, the lower end of lifting rod is folded with the seed crystal in A crystal orientation, M crystal orientation or C crystal orientation; To vacuumize in crystal growing furnace and pass into protective gas, be warming up to 2100 DEG C, make Al 2o 3melting, the liquid level temperature controlling melt is 2055 DEG C, and seed crystal is placed in Al 2o 3the upper surface of melt makes itself and melt contacts, continues 0.5h; After seed crystal and melt are fully stained with profit, lift and rotate seed crystal, thus realizing necking down-expansion shoulder-isodiametric growth; In the necking down stage, the liquid level temperature controlling melt is 2050 DEG C, upwards lifts seed crystal with the speed of 4mm/h, rotates seed crystal with the speed of 45r/min; Expand the shoulder stage, the liquid level temperature controlling melt is 2048 DEG C, upwards lifts seed crystal with the speed of 8mm/h, rotates seed crystal with the speed of 50r/min; In the isometrical stage, the liquid level temperature controlling melt is 2052 DEG C, upwards lifts seed crystal with the speed of 5mm/h, rotates seed crystal with the speed of 48r/min; After crystal growth terminates, the temperature in crystal growing furnace is down to 1600 DEG C, then carries out annealing in process to crystal, control temperature also continues 18h with the speed slow cooling of 80 DEG C/h, thus obtains crystal;
Step 2, crystal draw rod; Orientation is carried out to crystal, then uses and draw excellent machine and carry out drawing rod, thus obtain crystal bar;
Step 3, crystal-cut; Adopt carborundum line cutting equipment to cut crystal bar, thus obtain wafer;
Step 4, grinding; Grinder is adopted to grind wafer; During grinding, add lapping liquid, abrasive disk is forced into 0.02Mpa to wafer, and the rotating speed of abrasive disk is 1100rpm/min; Grind rear washes of absolute alcohol; Described lapping liquid component comprises: the granular size of 1% is the cubic boron nitride powder of 15 μm, the APES of 15%, the glycerine of 5%, the polypropylene glycol 400 of 10%, and all the other are deionized water;
Step 5, chamfering; The skive of Digit Control Machine Tool is adopted to carry out chamfered to the corner of wafer;
Step 6, annealing; Wafer is put into annealing furnace, carry out heating up with the speed of 200 DEG C/h and temperature risen to 1600 DEG C, be incubated 4h respectively at 300 DEG C, 800 DEG C, 1600 DEG C during intensification, then lower the temperature with the temperature of 200 DEG C, be incubated 3h respectively at 1000 DEG C, 500 DEG C during cooling and be cooled to room temperature taking-up;
Step 7, double side chemical polishing; First with absolute ethyl alcohol, wafer is cleaned, then the wafer after cleaning is put into Twp-sided polishing machine and fix; During polishing, add polishing fluid, polishing disk is forced into 0.13Mpa to wafer, and the rotating speed of polishing disk is 1200rpm/min, by after polished wafer washes of absolute alcohol, at room temperature carries out nature cooling; Described polishing fluid component comprises: the granular size of 1% is the cubic boron nitride powder of 3 μm, the APES of 15%, the glycerine of 5%, the polypropylene glycol 400 of 10%, the nano silicon of 1%, make polishing fluid pH value be 12.0 alkaline solution, all the other are deionized water; Alkaline solution is constantly supplemented to keep the pH value of polishing fluid in polishing process;
Step 8, laser get sheet; Wafer after polishing is put into laser cutting machine and passes into protective gas, wafer is cut into corresponding size by demand;
Step 9, printed circuit; Laser is got the silver of the Sapphire wafer surface after sheet slurry printed circuit, be then heated to 450 degrees Celsius and circuit is sintered on sapphire wafer;
Step 10, welding chip; LED chip scaling powder is fixed on printed circuit, is heated to 400 degrees Celsius by chips welding on printed circuit;
Step 11, encapsulation; Fluorescent glue is used sapphire wafer and LED chip to be encapsulated.
The preparation method of sapphire LED silk of the present invention is not limited to the concrete technical scheme described in above-described embodiment, and all employings are equal to replaces the protection range that the technical scheme formed is application claims.

Claims (10)

1. a preparation method for sapphire LED silk, is characterized in that, comprises following concrete steps:
Step one, crystal growth; Pure Al is loaded in the crucible of crystal growing furnace 2o 3raw material, is provided with lifting rod that is rotatable and lifting above described crucible, the lower end of lifting rod is folded with the seed crystal in A crystal orientation, M crystal orientation or C crystal orientation; To vacuumize in crystal growing furnace and pass into protective gas, be warming up to 2100 ~ 2200 DEG C, make Al 2o 3melting, the liquid level temperature controlling melt is 2055 DEG C, and seed crystal is placed in Al 2o 3the upper surface of melt makes itself and melt contacts, continues 0.5 ~ 1h; After seed crystal and melt are fully stained with profit, lift and rotate seed crystal, thus realizing necking down-expansion shoulder-isodiametric growth; In the necking down stage, the liquid level temperature controlling melt is 2050 DEG C, upwards lifts seed crystal with the speed of 3 ~ 5mm/h, rotates seed crystal with the speed of 45 ~ 48r/min; Expand the shoulder stage, the liquid level temperature controlling melt is 2048 DEG C, upwards lifts seed crystal with the speed of 8 ~ 10mm/h, rotates seed crystal with the speed of 50 ~ 55r/min; In the isometrical stage, the liquid level temperature controlling melt is 2052 DEG C, upwards lifts seed crystal with the speed of 5 ~ 8mm/h, rotates seed crystal with the speed of 48 ~ 50r/min; After crystal growth terminates, the temperature in crystal growing furnace is down to 1580 ~ 1680 DEG C, then carries out annealing in process to crystal, control temperature also continues 18 ~ 22h with the speed slow cooling of 80 ~ 100 DEG C/h, thus obtains crystal;
Step 2, crystal draw rod; Orientation is carried out to crystal, then uses and draw excellent machine and carry out drawing rod, thus obtain crystal bar;
Step 3, crystal-cut; Adopt carborundum line cutting equipment to cut crystal bar, thus obtain wafer;
Step 4, grinding; Grinder is adopted to grind wafer; During grinding, add lapping liquid, abrasive disk is forced into 0.02 ~ 0.022Mpa to wafer, and the rotating speed of abrasive disk is 1000 ~ 1200rpm/min; Grind rear washes of absolute alcohol; Described lapping liquid component comprises: the granular size of 0.5 ~ 2% is the cubic boron nitride powder of 10 ~ 20 μm, the APES of 14 ~ 16%, the glycerine of 4 ~ 6%, the polypropylene glycol 400 of 9 ~ 11%, and all the other are deionized water;
Step 5, chamfering; The skive of Digit Control Machine Tool is adopted to carry out chamfered to the corner of wafer;
Step 6, annealing; Wafer is put into annealing furnace, carry out heating up with the speed of 180 ~ 220 DEG C/h and temperature risen to 1600 DEG C, 2 ~ 6h is incubated respectively at 300 DEG C, 800 DEG C, 1600 DEG C during intensification, then lower the temperature with the temperature of 200 DEG C, be incubated 2 ~ 3h respectively at 1000 DEG C, 500 DEG C during cooling and be cooled to room temperature taking-up;
Step 7, double side chemical polishing; First with absolute ethyl alcohol, wafer is cleaned, then the wafer after cleaning is put into Twp-sided polishing machine and fix; During polishing, add polishing fluid, polishing disk is forced into 0.12 ~ 0.15Mpa to wafer, and the rotating speed of polishing disk is 1000 ~ 1500rpm/min, by after polished wafer washes of absolute alcohol, at room temperature carries out nature cooling; Described polishing fluid component comprises: the granular size of 0.5 ~ 2% is the cubic boron nitride powder of 1 ~ 6 μm, the APES of 14 ~ 16%, the glycerine of 4 ~ 6%, the polypropylene glycol 400 of 9 ~ 11%, the nano silicon of 0.5 ~ 2%, make polishing fluid pH value be 11.0 ~ 13.0 alkaline solution, all the other are deionized water; Alkaline solution is constantly supplemented to keep the pH value of polishing fluid in polishing process;
Step 8, laser get sheet; Wafer after polishing is put into laser cutting machine and passes into protective gas, wafer is cut into corresponding size by demand;
Step 9, printed circuit; Laser is got the silver of the Sapphire wafer surface after sheet slurry printed circuit, be then heated to 400 ~ 500 degrees Celsius and circuit is sintered on sapphire wafer;
Step 10, welding chip; LED chip scaling powder is fixed on printed circuit, is heated to 400 ~ 450 degrees Celsius by chips welding on printed circuit;
Step 11, encapsulation; Fluorescent glue is used sapphire wafer and LED chip to be encapsulated.
2. the preparation method of sapphire LED silk according to claim 1, it is characterized in that: in described step one, temperature in crystal growing furnace is down to 1600 DEG C, then carries out annealing in process to crystal, control temperature also continues 22h with the speed slow cooling of 100 DEG C/h.
3. the preparation method of sapphire LED silk according to claim 1, it is characterized in that: in described step 3, the diameter of carborundum line is 0.14 ~ 0.16mm, on carborundum line, adamantine particle diameter is 30 ~ 40 μm, carborundum line moves with the speed of 12 ~ 15m/s when cutting, crystal is 0.2 ~ 0.3mm/min relative to the translational speed of carborundum line, constantly cutting liquid is sprayed to carborundum line, containing particle diameter to be the diamond particles of 20 ~ 30 μm and particle diameter the be corundum in granules of 50 ~ 60 μm in described cutting liquid during cutting.
4. the preparation method of sapphire LED silk according to claim 1, is characterized in that: in described step 4, is the alumina particle of 3 ~ 6 μm in described lapping liquid containing particle diameter.
5. the preparation method of sapphire LED silk according to claim 1, is characterized in that: in described step 6, during intensification, at 300 DEG C of insulation 2h, at 800 DEG C of insulation 3h, at 1600 DEG C of insulation 4h.
6. the preparation method of sapphire LED silk according to claim 1, it is characterized in that: in described step 7, described alkaline solution is KOH.
7. the preparation method of sapphire LED silk according to claim 1, it is characterized in that: in described step 7, described polishing fluid pH value is 12.0.
8. the preparation method of sapphire LED silk according to claim 1, is characterized in that: in described step 7, polishing disk is forced into 0.135Mpa to wafer.
9. the preparation method of sapphire LED silk according to claim 1, it is characterized in that: in described step 8, the diameter of laser beam is 0.015 ~ 0.02mm, and cutting speed is 3 ~ 5mm/s.
10. the preparation method of sapphire LED silk according to claim 1, is characterized in that: protective gas described in step 8 is nitrogen.
CN201510339646.7A 2015-06-18 2015-06-18 Sapphire LED filament preparation method Pending CN105185877A (en)

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CN111515792A (en) * 2020-04-28 2020-08-11 福建晶安光电有限公司 Substrate material suitable for graphene growth and manufacturing method thereof

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Application publication date: 20151223