CN104966664A - Recycling method for sapphire substrate - Google Patents
Recycling method for sapphire substrate Download PDFInfo
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- CN104966664A CN104966664A CN201510378725.9A CN201510378725A CN104966664A CN 104966664 A CN104966664 A CN 104966664A CN 201510378725 A CN201510378725 A CN 201510378725A CN 104966664 A CN104966664 A CN 104966664A
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- Prior art keywords
- sapphire substrate
- epitaxial loayer
- cavity
- chlorine
- substrate surface
- Prior art date
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- 239000000758 substrate Substances 0.000 title claims abstract description 94
- 229910052594 sapphire Inorganic materials 0.000 title claims abstract description 57
- 239000010980 sapphire Substances 0.000 title claims abstract description 57
- 238000000034 method Methods 0.000 title claims abstract description 35
- 238000004064 recycling Methods 0.000 title abstract description 6
- 229910052751 metal Inorganic materials 0.000 claims abstract description 13
- 239000002184 metal Substances 0.000 claims abstract description 13
- 238000004140 cleaning Methods 0.000 claims abstract description 12
- 238000002161 passivation Methods 0.000 claims abstract description 12
- 238000006263 metalation reaction Methods 0.000 claims abstract description 10
- 239000012530 fluid Substances 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims abstract description 5
- 239000000376 reactant Substances 0.000 claims abstract description 4
- 239000000460 chlorine Substances 0.000 claims description 21
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 19
- 229910052801 chlorine Inorganic materials 0.000 claims description 19
- 238000011084 recovery Methods 0.000 claims description 16
- 238000005530 etching Methods 0.000 claims description 14
- 238000001039 wet etching Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 6
- FAQYAMRNWDIXMY-UHFFFAOYSA-N trichloroborane Chemical compound ClB(Cl)Cl FAQYAMRNWDIXMY-UHFFFAOYSA-N 0.000 claims description 6
- 230000003628 erosive effect Effects 0.000 claims description 5
- 238000000605 extraction Methods 0.000 claims description 2
- 238000005260 corrosion Methods 0.000 abstract description 8
- 230000007797 corrosion Effects 0.000 abstract description 8
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 abstract 3
- 238000007599 discharging Methods 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 description 13
- 238000009616 inductively coupled plasma Methods 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 238000000227 grinding Methods 0.000 description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 238000001020 plasma etching Methods 0.000 description 4
- 229910002601 GaN Inorganic materials 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000000407 epitaxy Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000005498 polishing Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 238000007517 polishing process Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000012958 reprocessing Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910002704 AlGaN Inorganic materials 0.000 description 1
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 1
- -1 InGaN Inorganic materials 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000008034 disappearance Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- MUJOIMFVNIBMKC-UHFFFAOYSA-N fludioxonil Chemical compound C=12OC(F)(F)OC2=CC=CC=1C1=CNC=C1C#N MUJOIMFVNIBMKC-UHFFFAOYSA-N 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- NICDRCVJGXLKSF-UHFFFAOYSA-N nitric acid;trihydrochloride Chemical compound Cl.Cl.Cl.O[N+]([O-])=O NICDRCVJGXLKSF-UHFFFAOYSA-N 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02002—Preparing wafers
- H01L21/02005—Preparing bulk and homogeneous wafers
- H01L21/02032—Preparing bulk and homogeneous wafers by reclaiming or re-processing
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor 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
Landscapes
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Drying Of Semiconductors (AREA)
- Led Devices (AREA)
Abstract
The invention discloses a recycling method for a sapphire substrate. The surface of the sapphire substrate comprises an AlxInyGa1-x-yN epitaxial layer with the x being greater than or equal to 0 and the y is less than or equal to 1 and a metal and/or passivation layer. The recycling method comprises the steps of cleaning the surface of the sapphire substrate by using a cleaning fluid, and removing the metal and/or passivation layer. The characteristics lie in that a PSS substrate to be recycled is placed in an equipment cavity, a chlorine gas is pumped into the equipment cavity, the chlorine gas is heated at a temperature between 700 DEG C and 1500 DEG C in the cavity, the heated chlorine gas carries out corrosion removal on the surface of the sapphire substrate to be recycled in the cavity until the AlxInyGa1-x-yN epitaxial layer with the x being greater than or equal to 0 and the y is less than or equal to 1 is completely corroded; and gas reactants generated by the reaction are discharged out of the cavity through a gas discharging system.
Description
The present invention relates to field of photoelectric technology, particularly relate to the recovery method of substrate in the photoelectric device with Sapphire Substrate.
Technical background
Along with the progress of gallium nitride based LED technology and the raising of light efficiency, LED has become the lighting source of a new generation, is widely used in backlight, display screen, decorative lighting, and progresses into home lighting, outdoor lighting field.There are Sapphire Substrate, GaN epitaxy, chip manufacture in the production upstream of LED.Wherein saphire substrate material is main raw material(s), and especially graphical sapphire substrate (Patterned Sapphire Substrate, abbreviation PSS substrate) is the main substrate of industry.At present, the plane sapphire substrate price of 2 inches is at 8-10 dollar/sheet, and the price of generally use on the market 2 inches of PSS substrates is more than twices of planar substrate, so, Sapphire Substrate accounts for about 20% of whole LED chip cost, size along with Sapphire Substrate increases to the more large scales such as 4 inches, 8 inches, and the ratio that Sapphire Substrate accounts for chip cost also can increase.
Therefore, reclaim Sapphire Substrate, particularly reclaim PSS substrate and to its recycling, significantly can reduce LED extension and chip manufacturing cost, LED manufacture field is reduced costs and has great importance
Also some are had to reclaim the method for Sapphire Substrate in prior art, such as in LED production process, to the waste product produced in extension processing and chip manufacture process or defect ware, generally give sapphire producer and carry out reprocessing, the key step of reprocessing is first cleaned, and then ground away by epitaxial loayer, then polishing again, last processing and manufacturing PSS substrate further, then gives LED chip factory and carries out production and application by product.
Prior art needs by grinding and polishing process, more consuming time, causes production efficiency lower; And, the figure of PSS substrate surface can be caused to disappear after grinding and polishing, also need again to form figure by extra preparation technology, add operation, consuming time and cost is higher.
Summary of the invention
The invention provides a kind of method reclaiming Sapphire Substrate, especially a kind of method reclaiming PSS substrate, described sapphire substrate surface comprises Al
xin
yga
1-x-yn (0≤x, y≤1) epitaxial loayer, metal and/or passivation layer, it comprises the steps:
Use cleaning fluid cleaning sapphire substrate surface, remove metal and/or passivation layer; It is characterized in that, in ICP or RIE equipment, adopt chlorine or boron trichloride gas etching to remove sapphire substrate surface Al
xin
yga
1-x-yn (0≤x, y≤1) epitaxial loayer; Form the Sapphire Substrate of recoverable.
Alternatively, described Sapphire Substrate is the PSS substrate that surface has figure.
Alternatively, the method for described recovery Sapphire Substrate is also included in and adopts chlorine or boron trichloride gas etching to remove sapphire substrate surface Al
xin
yga
1-x-yin N (0≤x, y≤1) epitaxial loayer process, residual thickness is the epitaxial loayer of 1-2um, the step of wet etching residue epitaxial loayer.
Present invention also offers the recovery method of another Sapphire Substrate, described sapphire substrate surface comprises Al
xin
yga
1-x-yn (0≤x, y≤1) epitaxial loayer, metal and/or passivation layer, it comprises the steps:
Use cleaning fluid cleaning sapphire substrate surface, remove metal and/or passivation layer; It is characterized in that, be placed in equipment cavity by PSS substrate to be recycled, chlorine is passed into this equipment cavity, chlorine is heated between 700-1500 DEG C in cavity, and the chlorine of heating carries out erosion removal to sapphire substrate surface to be recycled in cavity, until Al
xin
yga
1-x-yn (0≤x, y≤1) epitaxial loayer is corroded totally; Reaction generates gas reactant and discharges cavity through gas extraction system.
Alternatively, wherein said Sapphire Substrate is the PSS substrate that surface has figure.
Alternatively, the recovery method of described Sapphire Substrate, is also included in and adopts chlorine heating erosion removal sapphire substrate surface Al
xin
yga
1-x-yin N (0≤x, y≤1) epitaxial loayer process, wet etching remains the step of epitaxial loayer.
Adopt the method for recovery Sapphire Substrate provided by the present invention, do not need grinding and polishing process, improve production efficiency, reduce production cost; And, etching or corrosion after, the original figure of sapphire substrate surface can remain, avoid grinding and polishing after can cause PSS substrate surface figure disappearance, further reduce operation, improve efficiency and significantly reduce cost.
Accompanying drawing explanation
Fig. 1 is PSS substrate cross-section schematic diagram to be recycled;
Fig. 2 is for according to the PSS substrate schematic diagram reclaimed after method process described in first embodiment of the invention;
Fig. 3 is for reclaiming the schematic diagram of PSS substrate according to method described in second embodiment of the invention.
Execution mode
Below, the method for recovery PSS substrate of the present invention is described with reference to Fig. 1 and 2.
According to the first embodiment of the present invention, as shown in Figure 1, the Sapphire Substrate 1 with figure 2 has epitaxial loayer 3, alternatively, not shown below, the passivation layer that described epitaxial loayer 3 is made up of oxide, nitride or organic substance, and/or as wiring metal level and/or other metal conductive oxide layers, also can have other by Al
xin
yga
1-x-yn (0≤x, y≤1) material forms the structures such as the table top on epitaxial loayer 3.That is, the PSS substrate to be recycled in the present invention can be did epitaxy technique, is alternatively after finishing epitaxy technique, have also been made a part of chip technology, but do not carry out grinding reduction process.
Carry out suitable cleaning, especially for the epitaxial wafer carried out after chip manufacture, cleaned up by the adjuncts such as metal level above and passivation layer, cleaning fluid can be acid, alkali, organic solvent, and water etc.Such as, adopt the acid solution such as chloroazotic acid, hydrochloric acid, and ethanol, acetone and other organic solvent, finally use deionized water rinsing.
Adopt chlorine (Cl
2) or boron chloride (BCl
3) or its mist by ICP (Inductive CoupledPlasma, inductively coupled plasma) equipment or RIE (reactive ion etching) equipment, etch, by Al in certain temperature
xin
yga
1-x-yn (0≤x, y≤1) epitaxial loayer 3 etches away, and leaves substrate.If flat substrate, after etching, also flat substrate will be left; If PSS substrate, after etching, by the PSS substrate formed with pattern is very close before, the substrate after recovery does not affect follow-up use.
The gas flow of adjustment ICP or RIE equipment and ICP power and DC bias power, ICP power 100-1000W, lower electrode power 20-200W, relevant with state with device therefor model.Make in etching initial stage physical bombardment effect comparatively strong, when figure 2 about about the 2um close to PSS substrate, increase gas flow, reduce DC bias power, make the composition material Al of gaseous plasma and epitaxial loayer 3
xin
yga
1-x-ythe chemical reaction of N (0≤x, y≤1) accounts for leading, and the Al of PSS substrate surface is removed in etching
xin
yga
1-x-yn (0≤x, y≤1) semi-conducting material.
Al herein
xin
yga
1-x-yn (0≤x, y≤1) semi-conducting material, comprises the binary such as AlGaN, GaN, InGaN, AlN or ternary system III-nitride semiconductor material.
This etching gas is independent chlorine or independent BCl
3gas.Temperature in equipment is normal temperature, also can be high temperature, as 200 DEG C ~ 600 DEG C.
Alternatively, the method for described recovery Sapphire Substrate is also included in and adopts chlorine or boron trichloride gas etching to remove sapphire substrate surface Al
xin
yga
1-x-yin N (0≤x, y≤1) epitaxial loayer 3 process, residual thickness is the epitaxial loayer of about 2um, just has increase Cl
2ratio, the technique reducing lower power etches, the step of wet etching remaining residue epitaxial loayer afterwards.Wet etching can adopt phosphoric acid and sulfuric acid hybrid corrosion liquid, and corrosion temperature is between 80 ~ 240 DEG C, and the ratio of phosphoric acid and sulfuric acid is between 1:3 ~ 3:1.
Substrate after corrosion etching as shown in Figure 2, leaves Sapphire Substrate 1 and figure 2, cleans, checks, packs the substrate after corrosion etching, in order to recycling.
According to a second embodiment of the present invention, as shown in Figure 3, the method step reclaiming PSS substrate is as follows:
The PSS substrate 10 with figure 2 to be recycled is placed in equipment cavity 20, chlorine is passed in this equipment cavity 20 by air inlet 4, chlorine is heated to (not shown heater) between 700-1500 DEG C in cavity, preferably be heated between 700-900 DEG C, more preferably, be heated between 700-900 DEG C, the chlorine of heating corrodes PSS substrate surface to be recycled in cavity, removes Al
xin
yga
1-x-yn (0≤x, y≤1) epitaxial loayer 3, until Al
xin
yga
1-x-yn (0≤x, y≤1) epitaxial loayer 3 is corroded totally, by air-extractor after the reactant gasification that corrosion generates, as pump, by exhaust outlet 5 device for transferring cavity 20.
Alternatively, the recovery method of the present embodiment is also included in and adopts chlorine heating erosion removal sapphire substrate surface Al
xin
yga
1-x-yin N (0≤x, y≤1) epitaxial loayer 3 process, the step of the remaining epitaxial loayer 3 of wet etching.Wet etching condition is similar to the first embodiment.
Substrate after corrosion etching is cleaned, checks, packed, in order to recycling.
Technical scheme of the present invention low cost can reclaim Sapphire Substrate, especially PSS substrate, reduces LED production cost.
The above; be only the embodiment in the present invention, but protection scope of the present invention is not limited thereto, any people being familiar with this technology is in the technical scope disclosed by the present invention; the conversion that can expect easily or replacement, all should be encompassed in of the present invention comprising within scope.Therefore, protection scope of the present invention should be as the criterion with the protection range of claims.
Claims (6)
1. a recovery method for Sapphire Substrate, described sapphire substrate surface comprises Al
xin
yga
1-x-yn (0≤x, y≤1) epitaxial loayer, metal and/or passivation layer, it comprises the steps:
Use cleaning fluid cleaning sapphire substrate surface, remove metal and/or passivation layer; It is characterized in that,
In ICP or RIE equipment, chlorine or boron trichloride gas etching is adopted to remove sapphire substrate surface Al
xin
yga
1-x-yn (0≤x, y≤1) epitaxial loayer;
Form the Sapphire Substrate of recoverable.
2. the recovery method of Sapphire Substrate as claimed in claim 1, described Sapphire Substrate is the PSS substrate that surface has figure.
3. the recovery method of Sapphire Substrate as claimed in claim 1, is also included in and adopts chlorine or boron trichloride gas etching to remove sapphire substrate surface Al
xin
yga
1-x-yin N (0≤x, y≤1) epitaxial loayer process, residual thickness is the epitaxial loayer of 1-2um, the step of wet etching residue epitaxial loayer.
4. a recovery method for Sapphire Substrate, described sapphire substrate surface comprises Al
xin
yga
1-x-yn (0≤x, y≤1) epitaxial loayer, metal and/or passivation layer, it comprises the steps:
Use cleaning fluid cleaning sapphire substrate surface, remove metal and/or passivation layer; It is characterized in that,
Be placed in equipment cavity by PSS substrate to be recycled, chlorine passed into this equipment cavity, chlorine is heated between 700-1500 DEG C in cavity, and the chlorine of heating carries out erosion removal to sapphire substrate surface to be recycled in cavity, until Al
xin
yga
1-x-yn (0≤x, y≤1) epitaxial loayer is corroded totally;
Reaction generates gas reactant and discharges cavity through gas extraction system.
5. the recovery method of Sapphire Substrate as claimed in claim 4, described Sapphire Substrate is the PSS substrate that surface has figure.
6. the recovery method of Sapphire Substrate as claimed in claim 4, is also included in and adopts chlorine heating erosion removal sapphire substrate surface Al
xin
yga
1-x-yin N (0≤x, y≤1) epitaxial loayer process, residual thickness is the epitaxial loayer of 1-2um, the step of wet etching residue epitaxial loayer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510378725.9A CN104966664A (en) | 2015-07-01 | 2015-07-01 | Recycling method for sapphire substrate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510378725.9A CN104966664A (en) | 2015-07-01 | 2015-07-01 | Recycling method for sapphire substrate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104966664A true CN104966664A (en) | 2015-10-07 |
Family
ID=54220687
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510378725.9A Pending CN104966664A (en) | 2015-07-01 | 2015-07-01 | Recycling method for sapphire substrate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104966664A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107578981A (en) * | 2016-07-04 | 2018-01-12 | 伯思达绿能科技股份有限公司 | The gallium nitride film remove device and method of LED manufacture patterned sapphire substrates |
| CN111063615A (en) * | 2019-12-30 | 2020-04-24 | 徐州同鑫光电科技股份有限公司 | Method for removing AlN coating of PSS substrate in dry etching |
| CN113782648A (en) * | 2021-08-31 | 2021-12-10 | 佛山市国星半导体技术有限公司 | Regeneration method of waste sapphire substrate and sapphire substrate |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101771115A (en) * | 2009-01-06 | 2010-07-07 | 北京大学 | Method for treating nitrogen surface after laser lift-off of gallium nitride-based material |
| US20120097184A1 (en) * | 2010-10-20 | 2012-04-26 | Ki Ho Park | Method for recycling wafer |
| CN102593285A (en) * | 2012-03-06 | 2012-07-18 | 华灿光电股份有限公司 | Method for recovering pattern sapphire substrate |
-
2015
- 2015-07-01 CN CN201510378725.9A patent/CN104966664A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101771115A (en) * | 2009-01-06 | 2010-07-07 | 北京大学 | Method for treating nitrogen surface after laser lift-off of gallium nitride-based material |
| US20120097184A1 (en) * | 2010-10-20 | 2012-04-26 | Ki Ho Park | Method for recycling wafer |
| CN102593285A (en) * | 2012-03-06 | 2012-07-18 | 华灿光电股份有限公司 | Method for recovering pattern sapphire substrate |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107578981A (en) * | 2016-07-04 | 2018-01-12 | 伯思达绿能科技股份有限公司 | The gallium nitride film remove device and method of LED manufacture patterned sapphire substrates |
| CN111063615A (en) * | 2019-12-30 | 2020-04-24 | 徐州同鑫光电科技股份有限公司 | Method for removing AlN coating of PSS substrate in dry etching |
| CN113782648A (en) * | 2021-08-31 | 2021-12-10 | 佛山市国星半导体技术有限公司 | Regeneration method of waste sapphire substrate and sapphire substrate |
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Application publication date: 20151007 |
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