CN103633201A - Regeneration method of graphical sapphire substrate - Google Patents

Regeneration method of graphical sapphire substrate Download PDF

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Publication number
CN103633201A
CN103633201A CN201210311752.0A CN201210311752A CN103633201A CN 103633201 A CN103633201 A CN 103633201A CN 201210311752 A CN201210311752 A CN 201210311752A CN 103633201 A CN103633201 A CN 103633201A
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sapphire substrate
time
drying
renovation process
graphic
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张简庆华
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JINGHAN PHOTOELECTRIC MATERIAL Co Ltd
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JINGHAN PHOTOELECTRIC MATERIAL Co Ltd
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02002Preparing wafers
    • H01L21/02005Preparing bulk and homogeneous wafers
    • H01L21/02032Preparing bulk and homogeneous wafers by reclaiming or re-processing
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50Manufacturing or production processes characterised by the final manufactured product

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  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Computer Hardware Design (AREA)
  • Microelectronics & Electronic Packaging (AREA)
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  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

The invention provides a regeneration method of a graphical sapphire substrate; the method comprises the following steps: baking a sapphire substrate with high temperature, sinking the sapphire substrate in highly basic corrosion liquid so as to remove an epitaxy layer on the sapphire substrate, cleaning and drying the sapphire substrate, cleaning the sapphire substrate with strong acid corrosion liquid, removing epitaxy layer particles remained on a graphical surface of the sapphire substrate, re-cleaning and drying the sapphire substrate, and completing the regeneration of the graphical sapphire substrate, thereby forming the invention. By employing the method of recovering and regenerating the sapphire substrate, the epitaxy layer particles remained on the graphical surface can be completely removed; compared with a conventional recovery regeneration method, the method can improve recovery regeneration yield of the sapphire substrate; compared with a conventional etching recovery regeneration method, the preparation process can be carried out in a faster and more efficient method, thereby effectively improving production power of recovery regeneration of the sapphire substrate.

Description

Graphic sapphire substrate renovation process
Technical field
The present invention relates to a kind of manufacture of semiconductor, espespecially a kind of graphic sapphire substrate renovation process.
Background technology
Artificial stone is the material of the normal application of a kind of product in fields such as bathroom and kitchen tools, its easy plastotype and outward appearance are imitated nature rock, after plastotype sclerosis, there is no pore, therefore be difficult for adhering to greasy dirt, easy cleaning arranges surface, if scratch or breakage also can be through repairings and reinstatement, useful life can be relatively more of a specified duration, because of these advantages, therefore many products are to take artificial stone as material making, such as kitchen cabinet, wash platform, dining table and tank etc. on the market.
At present artificial stone according to the difference of processing procedure can rough classification be Du Pont's artificial stone, have glue shell artificial stone, glue-free shell artificial stone and a BMC artificial stone.Described Du Pont artificial stone, is all made for bulk flat board, sees through dull and stereotyped gluing and finishing and the shape that forms predetermined moulding forms; Described have a glue shell artificial stone, is to insert after thicker resin among glue shell, then the mixture that pours into resin and stone flour forms; Described glue-free shell artificial stone is that sclerosis mode can be divided into thermosetting heat hardening, and the natural drying sclerosis of thermoplasticity with glass fibre reinforced plastic (Fiberglass Reinforced Plastics, FRP) mould molding; Described BMC artificial stone is with bulk moulding material (Bulk Molding Compound, BMC) steel mold pressing moulding.
Yet, though above-mentioned artificial stone method for making has otherness on processing procedure, all there is following common problem, comprising:
1, cost is expensive: according to the cost of artificial stone manufacturing process, the stone material more general by the price of its raw material itself is expensive, and make stone except outward appearance, its structural strength must can be taken into account, therefore must there is certain thickness when making, cannot save the consumption of artificial stone material, add that the price of mould is originally just quite expensive, so the made product price of artificial stone material relatively remain high.
2, processing procedure trouble: the product that artificial stone is made when hardened forming, conventionally must be again through measuring, engage and the operation such as grinding beginning to complete its finished product, if the surface of finished product must have the structural design of decorative pattern or concaveconvex shape, the operation of moulding will be more complicated.
Therefore, how to solve the above-mentioned problem that artificial stone manufacturing process causes of commonly using, be main emphasis of the present invention place.By known sapphire (Al 2o 3english Sapphire by name), for making the main substrate material of gallium nitride (GaN) trichite photosphere of heap of stone, due to sapphire substrate low price, and have high rigidity, can high temperature resistant and resistance to chemical attack characteristic, therefore be applied in the production of light-emitting diode quite general with sapphire substrate.
Press the manufacture of semiconductor of light-emitting diode, no matter brilliant growth course of heap of stone on sapphire substrate, or on sapphire substrate, process in the manufacturing process of light-emitting diode chip for backlight unit, have unavoidably bad crystalline substance and scrapped processing, because avoid the consideration of waste of material and saving member cost, there is the technology of the reclaiming of sapphire substrate to generate.
According to TaiWan, China Announcement Number I366894 patent of invention case, disclose a kind of sapphire substrate renovation process, be mainly on sapphire substrate, to see through dipping and high-temperature process to remove epitaxial layer, and carry out polishing on the surface of sapphire substrate, with the available sapphire substrate of regenerating.Yet the method instrument is useful in surface for smooth sapphire substrate, if graphic sapphire substrate (Pattern Sapphire Substrate, PSS), because the surface of the sapphire substrate of this kenel presents graphical structure of arrays, if in addition polishing can destroy this patterned surface.
Again according to No. 102593285 patents of invention of Chinese patent Announcement Number CN, disclose a kind of method that reclaims graphic sapphire substrate, adopt the dry etching method of inductively coupled plasma and utilize strong acid and wet etching that highly basic corrodes, to remove the epitaxial layer on graphic sapphire substrate.Yet, according to practical experience, discuss, graphic sapphire substrate utilizes the etching mode reclaiming of aforementioned dry etching method and wet etching, still cannot remove the residual particulates of epitaxial layer completely, therefore the yield of the method reclaiming of commonly using with this is not good, and must accurate Calculation in the etching period of reclaiming process and reduced efficiency, and be subject to the limitation of etching machines and cannot expand output, cause the production capacity of the reclaiming of process for sapphire-based slab integral not cite, the space remaining to be further improved.
Therefore, how to solve the above-mentioned problem of commonly using sapphire substrate regeneration, be main emphasis of the present invention place.
Summary of the invention
Main purpose of the present invention is to solve the above problems and a kind of graphic sapphire substrate renovation process is provided, to reach the effect that yield is good and production capacity is high of graphic sapphire substrate regeneration.
For reaching aforesaid object, the present invention by the following technical solutions:
A graphic sapphire substrate renovation process, it comprises the following steps:
Baking: utilize the temperature of 950 ℃ to 1500 ℃ to toast sapphire substrate, tentatively remove the epitaxial layer on sapphire substrate;
Highly basic immerses: the sapphire substrate after baking is immersed in the corrosive liquid of highly basic, is further removed the epitaxial layer on sapphire substrate;
Clean for the first time: sapphire substrate is cleaned for the first time, to clean the corrosive liquid of highly basic;
Dry for the first time: sapphire substrate, after cleaning, is dried for the first time;
Strong acid rinses: the corrosive liquid by dried sapphire substrate with strong acid is rinsed, to remove at the residual epitaxial layer particulate of the patterned surface of sapphire substrate;
Clean for the second time: sapphire substrate is cleaned for the second time, to clean the corrosive liquid of strong acid;
Dry for the second time: sapphire substrate, after cleaning, is dried for the second time.
In said method, described baking procedure is with high-temperature baking stove, sapphire substrate to be toasted, and baking time is 500min to 800min.
In said method, described oven is 1360 ℃ to the temperature of sapphire substrate baking.
In said method, described highly basic immerses the corrosive liquid in step, and one of them is corrosive substance to comprise potassium hydroxide and NaOH; Corrosive liquid in described strong acid rinsing step, take sulfuric acid as corrosive substance.
Corrosive liquid be take potassium hydroxide during as corrosive substance, at the temperature of 40 ℃ to 120 ℃, immerses 120min to 240min; Corrosive liquid be take sulfuric acid during as corrosive substance, rinses 30min to 90min.
In said method, described cleaning step for the first time and for the second time cleaning step, any one in the two is Quick drainage clean or ultrasonic waves clean.
Preferably, described cleaning step is for the first time Quick drainage clean, and scavenging period is 60min to 180min.
In said method, described drying steps for the first time and for the second time drying steps, any one in the two is that drying and processing or Rotary drying are processed.
Preferably, described drying steps is for the first time at the temperature of 40 ℃ to 120 ℃, and be 10min to 50min drying time.
Preferably, in described drying steps for the first time and for the second time drying steps, any one is processed with this Rotary drying, and be 60min drying time.
The invention has the advantages that:
Utilize the sapphire substrate of method reclaiming of the present invention, the residual epitaxial layer particulate of patterned surface more intactly can be removed, therefore can promote the yield of sapphire substrate reclaiming compared to the reclaiming method of commonly using, and compared to known with engraving method reclaiming, can be relatively with faster and efficient method is carried out processing procedure, can effectively promote the production capacity of sapphire substrate reclaiming.
Above-mentioned and other object of the present invention and advantage, be not difficult, from the detailed description and accompanying drawing of following selected embodiment, to gain in-depth understanding.
Accompanying drawing explanation
Fig. 1 is renovation process flow chart of the present invention.
Fig. 2 is the structural representation of graphic sapphire substrate of the present invention.
Embodiment
Refer to Fig. 1 to Fig. 2, shown in figure, for the selected example structure of the present invention, this instrument for explanation, is not subject to the restriction of this kind of structure in patent application.
The present embodiment provides a kind of graphic sapphire substrate renovation process, it is as shown in Figure 1, comprise that baking 10, highly basic immerse 11, clean for the first time 12, dry 13, strong acid rinses 14, cleans for the second time the steps such as 15 and for the second time dry 16 for the first time, mainly be the epitaxial layer on the sapphire substrate shown in Fig. 223 to remove, wherein:
In the step of baking 10, utilize the temperature of 950 ℃ to 1500 ℃ to toast this sapphire substrate 2, tentatively remove the epitaxial layer 3 on sapphire substrate 2.This baking step of 10 is with high-temperature baking stove to these sapphire substrate 2 bakings, and baking time is 500min to 800min, be made as 1360 ℃, and baking time is 690min in the baking temperature of the present embodiment.
In highly basic immerses 11 step, the sapphire substrate 2 after baking is immersed in the corrosive liquid of highly basic, further remove the epitaxial layer 3 on sapphire substrate 2.This states highly basic and immerses the corrosive liquid in 11 step, can be potassium hydroxide (KOH) and one of them corrosive substance of NaOH (NaOH), in the present embodiment, take potassium hydroxide as corrosive substance, at the temperature of 40 ℃ to 120 ℃, immerse 120min to 240min, and the present embodiment is at the temperature of 80 ℃, in corrosive liquid, to immerse 180min.
In cleaning for the first time 12 steps, sapphire substrate 2 is carried out to primary cleaning, to clean the corrosive liquid of highly basic.This states and cleans for the first time 12 steps, can be Quick drainage and clean (Quick Dump Rinse, QDR) process, or for cleaning (HDI Ultrasonic), processes ultrasonic waves, with Quick drainage clean, scavenging period is 60min to 180min, and in the present embodiment, scavenging period is 120min.
In dry 13 step for the first time, sapphire substrate 2, after cleaning, carries out primary dry.Described dry 13 step for the first time, can be drying and processing, or be Rotary drying processing, with drying and processing, dry at the temperature of 40 ℃ to 120 ℃, and be 10min to 50min drying time, and the present embodiment dry 13 is dry at the temperature of 80 ℃ for the first time, and be 30min drying time.
In the step of strong acid flushing 14, the corrosive liquid by dried sapphire substrate 2 with strong acid is rinsed, to remove at the residual epitaxial layer particulate of the patterned surface 20 of sapphire substrate 2.In the present embodiment, the corrosive liquid in the step of strong acid flushing 14, with sulfuric acid (H 2sO 4) be corrosive substance.In the present embodiment, the time that the strong acid of take rinses is 30min to 90min.
In cleaning for the second time 15 steps, sapphire substrate 2 is carried out to secondary cleaning, to clean the corrosive liquid of strong acid.This states and cleans for the second time 15 steps, can be Quick drainage clean, or is ultrasonic waves clean, clean 12 equally with Quick drainage clean, and scavenging period is 120min in the present embodiment Yu for the first time.
In dry 16 step for the second time, sapphire substrate 2, after cleaning, carries out secondary dry.Described dry 16 step for the second time, can be drying and processing, or is Rotary drying processing, and the present embodiment utilizes spinner to process with Rotary drying, and be 60min drying time.
As shown in table 1, yield comparison sheet for the sapphire substrate of new product and the sapphire substrate of reclaiming, wherein in table, in hurdle, the left side " wafer numbering " listed " 6,7,8,9 and 10 " five, be all the new product of sapphire substrate, from institute's column data, the yield average out to 95.47% of sapphire substrate; In this table, separately have numbering " JINR05B0758 " and " JINR03B0486 " the two, the finished product of this two method reclaiming of the present invention for sapphire substrate utilizes, wherein from institute's column data, the average yield of sapphire substrate is 78.95%.Therefore, utilize the sapphire substrate of method reclaiming of the present invention, average yield still has 82.69% of new product sapphire substrate, therefore have suitable reliability with the yield of the sapphire substrate of method reclaiming of the present invention.
The yield comparison of the sapphire substrate of the sapphire substrate of table 1 new product and method reclaiming of the present invention
Figure BDA00002068968200051
By above-mentioned explanation, be not difficult to find advantage of the present invention, be to utilize the sapphire substrate of method reclaiming of the present invention, the residual epitaxial layer particulate of patterned surface more intactly can be removed, therefore can promote the yield of sapphire substrate reclaiming compared to the reclaiming method of commonly using, and compared to known with engraving method reclaiming, can be relatively with faster and efficient method is carried out processing procedure, and in processing procedure, be unlikely to limit to the output of sapphire substrate reclaiming, therefore can effectively promote the production capacity of sapphire substrate reclaiming.
The announcement system of the above embodiment is in order to the present invention to be described, not in order to limit the present invention, therefore the change of numerical value or the displacement of equivalent elements must be subordinate to category of the present invention such as.
By describing in detail above, can make those skilled in the art understand that the present invention can reach aforementioned object really, the real regulation that has met Patent Law, whence proposes patent application.

Claims (10)

1. a graphic sapphire substrate renovation process, is characterized in that: it comprises the following steps:
Baking: utilize the temperature of 950 ℃ to 1500 ℃ to toast sapphire substrate, tentatively remove the epitaxial layer on sapphire substrate;
Highly basic immerses: the sapphire substrate after baking is immersed in the corrosive liquid of highly basic, is further removed the epitaxial layer on sapphire substrate;
Clean for the first time: sapphire substrate is cleaned for the first time, to clean the corrosive liquid of highly basic;
Dry for the first time: sapphire substrate, after cleaning, is dried for the first time;
Strong acid rinses: the corrosive liquid by dried sapphire substrate with strong acid is rinsed, to remove at the residual epitaxial layer particulate of the patterned surface of sapphire substrate;
Clean for the second time: sapphire substrate is cleaned for the second time, to clean the corrosive liquid of strong acid;
Dry for the second time: sapphire substrate, after cleaning, is dried for the second time.
2. according to graphic sapphire substrate renovation process claimed in claim 1, it is characterized in that: described baking procedure is with high-temperature baking stove, sapphire substrate to be toasted, and baking time is 500min to 800min.
3. according to graphic sapphire substrate renovation process claimed in claim 2, it is characterized in that: described oven is 1360 ℃ to the temperature of sapphire substrate baking.
4. according to graphic sapphire substrate renovation process claimed in claim 1, it is characterized in that: described highly basic immerses the corrosive liquid in step, one of them is corrosive substance to comprise potassium hydroxide and NaOH; Corrosive liquid in described strong acid rinsing step, take sulfuric acid as corrosive substance.
5. according to graphic sapphire substrate renovation process claimed in claim 4, it is characterized in that: corrosive liquid be take potassium hydroxide during as corrosive substance, at the temperature of 40 ℃ to 120 ℃, immerses 120min to 240min; Corrosive liquid be take sulfuric acid during as corrosive substance, rinses 30min to 90min.
6. according to graphic sapphire substrate renovation process claimed in claim 1, it is characterized in that: described cleaning step for the first time and for the second time cleaning step, any one in the two is Quick drainage clean or ultrasonic waves clean.
7. according to graphic sapphire substrate renovation process claimed in claim 6, it is characterized in that: described cleaning step is for the first time Quick drainage clean, scavenging period is 60min to 180min.
8. according to graphic sapphire substrate renovation process claimed in claim 1, it is characterized in that: described drying steps for the first time and for the second time drying steps, any one in the two is that drying and processing or Rotary drying are processed.
9. according to graphic sapphire substrate renovation process claimed in claim 8, it is characterized in that: described drying steps is for the first time at the temperature of 40 ℃ to 120 ℃, and be 10min to 50min drying time.
10. according to graphic sapphire substrate renovation process claimed in claim 8, it is characterized in that: in described drying steps for the first time and for the second time drying steps, any one is processed with this Rotary drying, and be 60min drying time.
CN201210311752.0A 2012-08-29 2012-08-29 Regeneration method of graphical sapphire substrate Pending CN103633201A (en)

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104925742A (en) * 2014-03-20 2015-09-23 中芯国际集成电路制造(上海)有限公司 Forming method of MEMS semiconductor device
CN105845786A (en) * 2015-01-15 2016-08-10 广东量晶光电科技有限公司 Graphical sapphire substrate recycling method
CN106206279A (en) * 2016-07-28 2016-12-07 常州亿晶光电科技有限公司 A kind of chemically polishing method of sapphire filament wafer
CN107946179A (en) * 2017-11-27 2018-04-20 上海超硅半导体有限公司 A kind of recovery method of the graphical wafer formed with integrated circuit and polycrystal layer
CN109513677A (en) * 2018-10-09 2019-03-26 东莞市希尔金属材料有限公司 Silk-screen sapphire strip cleaning method
CN109887878A (en) * 2019-02-28 2019-06-14 保定中创燕园半导体科技有限公司 A method of recycling graphical sapphire substrate
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
CN114373836A (en) * 2021-12-29 2022-04-19 南通同方半导体有限公司 Method for recycling sapphire substrate

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Publication number Priority date Publication date Assignee Title
CN102255013A (en) * 2011-08-01 2011-11-23 华灿光电股份有限公司 Method for making light-emitting diode with vertical structure through stripping GaN based epitaxial layer and sapphire substrate by using wet process
TWI366894B (en) * 2008-07-22 2012-06-21 Crystalwise Technology Inc A method of reclaiming sapphire 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

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TWI366894B (en) * 2008-07-22 2012-06-21 Crystalwise Technology Inc A method of reclaiming sapphire wafer
CN102255013A (en) * 2011-08-01 2011-11-23 华灿光电股份有限公司 Method for making light-emitting diode with vertical structure through stripping GaN based epitaxial layer and sapphire substrate by using wet process
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 (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104925742A (en) * 2014-03-20 2015-09-23 中芯国际集成电路制造(上海)有限公司 Forming method of MEMS semiconductor device
CN104925742B (en) * 2014-03-20 2016-09-07 中芯国际集成电路制造(上海)有限公司 The forming method of MEMS semiconductor devices
CN105845786A (en) * 2015-01-15 2016-08-10 广东量晶光电科技有限公司 Graphical sapphire substrate recycling method
CN106206279A (en) * 2016-07-28 2016-12-07 常州亿晶光电科技有限公司 A kind of chemically polishing method of sapphire filament wafer
CN107946179A (en) * 2017-11-27 2018-04-20 上海超硅半导体有限公司 A kind of recovery method of the graphical wafer formed with integrated circuit and polycrystal layer
CN107946179B (en) * 2017-11-27 2020-05-08 上海超硅半导体有限公司 Method for recycling patterned wafer with integrated circuit and polycrystalline layer
CN109513677A (en) * 2018-10-09 2019-03-26 东莞市希尔金属材料有限公司 Silk-screen sapphire strip cleaning method
CN109513677B (en) * 2018-10-09 2020-06-19 东莞市希尔金属材料有限公司 Screen printing sapphire deplating and cleaning method
CN109887878A (en) * 2019-02-28 2019-06-14 保定中创燕园半导体科技有限公司 A method of recycling graphical sapphire substrate
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
CN114373836A (en) * 2021-12-29 2022-04-19 南通同方半导体有限公司 Method for recycling sapphire substrate

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Application publication date: 20140312