WO2018018894A1 - Process for chemical polishing of sapphire filament wafers - Google Patents
Process for chemical polishing of sapphire filament wafers Download PDFInfo
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- WO2018018894A1 WO2018018894A1 PCT/CN2017/076571 CN2017076571W WO2018018894A1 WO 2018018894 A1 WO2018018894 A1 WO 2018018894A1 CN 2017076571 W CN2017076571 W CN 2017076571W WO 2018018894 A1 WO2018018894 A1 WO 2018018894A1
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- 238000005498 polishing Methods 0.000 title claims abstract description 36
- 239000000126 substance Substances 0.000 title claims abstract description 32
- 229910052594 sapphire Inorganic materials 0.000 title claims abstract description 28
- 239000010980 sapphire Substances 0.000 title claims abstract description 28
- 235000012431 wafers Nutrition 0.000 title abstract description 53
- 238000000034 method Methods 0.000 title abstract description 22
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000004140 cleaning Methods 0.000 claims abstract description 20
- 230000007797 corrosion Effects 0.000 claims abstract description 16
- 238000005260 corrosion Methods 0.000 claims abstract description 16
- 239000002253 acid Substances 0.000 claims abstract description 15
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 15
- 238000007517 polishing process Methods 0.000 claims abstract description 15
- 238000005520 cutting process Methods 0.000 claims abstract description 8
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 239000003513 alkali Substances 0.000 claims description 9
- 238000002791 soaking Methods 0.000 claims description 8
- 238000005530 etching Methods 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 6
- 238000005507 spraying Methods 0.000 claims description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 5
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 4
- 239000002585 base Substances 0.000 claims description 3
- 239000012459 cleaning agent Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000007654 immersion Methods 0.000 claims 3
- 230000003746 surface roughness Effects 0.000 abstract description 5
- 238000007605 air drying Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000003795 chemical substances by application Substances 0.000 description 10
- 238000000227 grinding Methods 0.000 description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000002245 particle Substances 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000003672 processing method Methods 0.000 description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 description 2
- 235000017550 sodium carbonate Nutrition 0.000 description 2
- FGUUSXIOTUKUDN-IBGZPJMESA-N C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 Chemical compound C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 FGUUSXIOTUKUDN-IBGZPJMESA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000003486 chemical etching Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
Classifications
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- 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
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
- H01L21/30604—Chemical etching
-
- 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
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
Definitions
- the invention relates to a chemical polishing process of a sapphire filament wafer, and belongs to the technical field of LED substrate processing.
- LED semiconductor lighting
- LED technology is developing rapidly, with wide application fields, strong industrial driving, and great potential for energy saving. It meets the requirements of low carbon and ecological economy and the development trend of modern high-tech industries, and is recognized by all countries as the most promising high-efficiency lighting industry.
- Sapphire has become an important mainstream substrate in the development of LED technology. At present, more than 90% of the world's LED products are epitaxially grown from sapphire substrate.
- LED filament lamps will replace traditional lamps. The structure is to install an LED chip on a slender strip sapphire wafer, and the sapphire high-temperature thermal stability and high light transmittance characteristics make the filament lamp have high luminous efficiency and low energy consumption.
- the sapphire crystal is obtained by melting and recrystallizing high-purity alumina at high temperature.
- the processing process of the sapphire filament in the industry is to process the crystal into a 30mm*40mm square ingot, and then process it through multiple processes. , including: head and tail, directional grinding, multi-line slicing, double-sided rough grinding, cleaning, double-sided fine grinding, cleaning coarse/fine polishing, cleaning into square pieces, and then cutting the square pieces to form 30 * 0.8*0.4mm sapphire filament.
- the processing steps are long, and most of them are rigid processing, the residual stress on the surface of the wafer is large, the coarse and fine polishing is easy to cause problems such as debris, and the processing cost is high. Therefore, the processing method and process technology of the sapphire filament wafer need to be further improved.
- the invention discloses a low-cost, high-efficiency LED sapphire filament preparation technical method, which will replace the double-face rough grinding, cleaning, double-side fine grinding, cleaning, rough/fine polishing and cleaning in the traditional processing method. Process. Its technical solutions are as follows:
- a chemical polishing process for a sapphire filament wafer comprising the steps of: a. cleaning the cut square piece and air drying; b. alkali high temperature corrosion; c. cleaning; d. phosphoric acid corrosion; e. mixed acid chemical polishing; f. Cleaning.
- the step a is to clean the square piece of 30mm*40mm*0.8mm after multi-line cutting, using a 5%-10% volume ratio hydrofluoric acid cleaning agent, and ultrasonic cleaning, the ultrasonic frequency is 40Hz, and the time is 4-10min. , preferably 5 min; after ultrasonic cleaning, rinse with water, and air dry or blow dry with dry air;
- This step is to remove residual metal ions, base complexes and alumina powder particles on the surface of the wafer after multi-line cutting, and with ultrasound, it can more completely remove particles such as particles on the wafer surface; provide the basis for the next process.
- the surface of the wafer must be rinsed with clean water and then dried by drying or drying compressed gas;
- the step b is to completely immerse the dried wafer in a high temperature strong alkali, preferably NaOH strong base, heating temperature is 300-350 ° C, preferably temperature 320 ° C, high temperature etching time is 10-30 min, preferably time 12 min; Corrosion, C is basically corroded to the cutting line marks and exhibits partial specular reflection. At the same time, removing the growth stress, processing stress and processing damage layer of the crystal;
- a high temperature strong alkali preferably NaOH strong base
- the step c is immersed in water and then sprayed to rinse the wafer to remove residual alkali on the surface of the wafer. Soaking time 1-8min, spraying time 20-60s, preferred time is 5min and 30s respectively;
- the step d is to soak the wafer at a high temperature with 85% concentrated phosphoric acid, the soaking temperature is 200-245 ° C, the soaking time is 1-12 h, the preferred temperature is 238 ° C, and the preferred time is 4 h. Further preferentially etching the surface of the crystal by high-temperature concentrated phosphoric acid to further remove the sub-damage layer and present the wafer C to the surface Obvious specular reflection.
- the step e is mixed with 95% concentrated sulfuric acid and 85% concentrated phosphoric acid in a ratio of 1:5 to 5:1, and 5%-30% hydrofluoric acid is added to prepare a mixed acid chemical polishing liquid on the surface of the wafer.
- the polishing temperature is 120 ° C - 240 ° C, and the polishing time is 15-45 min.
- the step f is immersed in water and then sprayed to rinse the wafer to remove residual polishing liquid on the surface of the wafer.
- the soaking time is 1-6 min
- the spraying time is 20-60 s
- the preferred time is 2 min and 45 s, respectively.
- the surface of the wafer surface is accelerated and etched to remove the damage layer on the surface of the wafer, reducing the roughness and residual stress on the surface of the wafer; soda ash is the initial rapid removal of the damage layer; Cleaned before entering the next pickling process; using high-concentration phosphoric acid high-temperature selective corrosion characteristics, further removing the damage layer and residual stress on the surface of the wafer C, further reducing the roughness of the wafer C to the surface, for the next chemical polishing process Provide preparation conditions.
- the wafer polished by the mixed acid chemical polishing agent has a C-direction surface roughness of 1 nm, which fully meets the requirements of the filament lamp wafer.
- the invention discloses a chemical polishing process for a sapphire filament wafer, and proposes a new process flow capable of meeting the surface requirements of the LED filament lamp wafer for a high cost and low efficiency processing process such as sapphire wafer grinding and polishing;
- the invention accelerates the corrosion rate of the wafer surface by using high temperature and strong alkali corrosion, but in the process of rapid corrosion, the surface of the wafer is microscopically easy to generate small pits, so , further etching by acid to remove pits, increasing the surface finish of the wafer, When the stress is removed, the flatness, warpage, bending and other indexes of the wafer are improved, and the strength of the wafer is increased, so that the wafer is not easily cracked during subsequent reworking; the surface of the wafer is coated with a mixed acid chemical polishing agent.
- the method can effectively reduce the processing cost of the sapphire wafer, greatly improve the production efficiency, shorten the processing process, and at the same time, remove the damage layer of the wafer surface and its residual stress to the greatest extent, and the equipment investment is small, the processing procedure is short, and the processing yield is high. Large, easy to operate, suitable for promotion.
- the chemical polishing process of the sapphire filament wafer disclosed by the invention refers to a new processing technology of the filament square wafer after sapphire multi-wire cutting, and adopts the following process flow:
- soda NaOH is heated to a high temperature of 320 ° C completely melted, the wafer is slowly preheated in a molten alkali, soaking time is 12min;
- step e concentrated phosphoric acid and concentrated sulfuric acid are mixed in a ratio of 2:1, and 15% hydrofluoric acid is added to be mixed to prepare a mixed acid chemical polishing agent, and the polishing agent is heated and mixed to 150 ° C, and the wafer is immersed therein for 20 minutes. Chemical polishing is completed; other processes are unchanged.
- step e concentrated phosphoric acid and concentrated sulfuric acid are mixed in a ratio of 5:1, and hydrofluoric acid 10% is added to be mixed to prepare a mixed acid chemical polishing agent, and the polishing agent is heated and mixed to 150 ° C, and the wafer is immersed therein for 20 minutes to complete. Chemical polishing; other processes are unchanged.
- Example 1 Example 2
- Example 3 C-direction surface roughness 1nm 1nm 1nm
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- Engineering & Computer Science (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Chemical & Material Sciences (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
Disclosed is a process for chemical polishing of sapphire filament wafers, comprising the following technological processes: a. cleaning and cutting into square pieces, and air-drying; b. alkaline high-temperature corrosion; c. cleaning; d. phosphoric acid corrosion; e. mixed acid chemical polishing; and f. cleaning. By using the chemical polishing process, the surface residual stress of the wafers can be effectively eliminated, the surface roughness of the wafers is reduced, and the production cost is greatly reduced.
Description
本发明涉及一种蓝宝石灯丝晶片的化学抛光工艺,属LED衬底加工技术领域。The invention relates to a chemical polishing process of a sapphire filament wafer, and belongs to the technical field of LED substrate processing.
LED(半导体照明)技术发展迅速、应用领域广泛、产业带动性强、节能潜力大,符合低碳与生态经济要求和当代高新技术产业发展趋势,被各国公认为最有发展前景的高效照明产业。而蓝宝石则成为LED技术发展中重要的主流衬底片,目前全世界90%以上的LED产品均由蓝宝石衬底片上外延生长得到。当前,LED灯丝灯将替代传统灯。其结构是在细长条形的蓝宝石晶片上安装LED芯片,利用蓝宝石高温热稳定性以及高透光率的特性,使得灯丝灯发光效率高,能耗低。LED (semiconductor lighting) technology is developing rapidly, with wide application fields, strong industrial driving, and great potential for energy saving. It meets the requirements of low carbon and ecological economy and the development trend of modern high-tech industries, and is recognized by all countries as the most promising high-efficiency lighting industry. Sapphire has become an important mainstream substrate in the development of LED technology. At present, more than 90% of the world's LED products are epitaxially grown from sapphire substrate. Currently, LED filament lamps will replace traditional lamps. The structure is to install an LED chip on a slender strip sapphire wafer, and the sapphire high-temperature thermal stability and high light transmittance characteristics make the filament lamp have high luminous efficiency and low energy consumption.
预计2016年LED灯丝灯需求量约为2.2亿只,同比2015年增长367%,未来几年,LED灯丝灯需求量将快速增加。因此,低成本的LED灯丝灯将有助于该产品的应用普及。It is estimated that the demand for LED filament lamps in 2016 will be about 220 million, an increase of 367% compared with 2015. In the next few years, the demand for LED filament lamps will increase rapidly. Therefore, low-cost LED filament lamps will contribute to the popularity of the product.
蓝宝石晶体是由高纯氧化铝在高温下熔化再结晶生长所得,当前,行业内对蓝宝石灯丝的加工流程是将晶体经开方加工成30mm*40mm的方形晶块,之后再经多道工序加工,包括:去头尾、定向磨面、多线切片、双面粗磨、清洗、双面精磨、清洗粗/精抛光、清洗制成方片,再将方片进行粘胶切割,形成30*0.8*0.4mm的蓝宝石灯丝片。加工工序较长,且多为刚性加工,晶片表面加工残余应力较大,粗精抛容易导致碎片等问题,且加工成本较高。因此,蓝宝石灯丝晶片加工方法及工艺技术有待进一步完善。
The sapphire crystal is obtained by melting and recrystallizing high-purity alumina at high temperature. At present, the processing process of the sapphire filament in the industry is to process the crystal into a 30mm*40mm square ingot, and then process it through multiple processes. , including: head and tail, directional grinding, multi-line slicing, double-sided rough grinding, cleaning, double-sided fine grinding, cleaning coarse/fine polishing, cleaning into square pieces, and then cutting the square pieces to form 30 * 0.8*0.4mm sapphire filament. The processing steps are long, and most of them are rigid processing, the residual stress on the surface of the wafer is large, the coarse and fine polishing is easy to cause problems such as debris, and the processing cost is high. Therefore, the processing method and process technology of the sapphire filament wafer need to be further improved.
发明内容Summary of the invention
本发明公开了一种低成本、高效率的LED蓝宝石灯丝的制备技术方法,将取代传统加工方法中的双面粗磨、清洗、双面精磨、清洗、粗/精抛光及清洗等多道工序。其技术方案如下:The invention discloses a low-cost, high-efficiency LED sapphire filament preparation technical method, which will replace the double-face rough grinding, cleaning, double-side fine grinding, cleaning, rough/fine polishing and cleaning in the traditional processing method. Process. Its technical solutions are as follows:
一种蓝宝石灯丝晶片的化学抛光工艺,其特征在于,包括以下步骤:a.清洗切割方片,并风干;b.碱高温腐蚀;c.清洗;d.磷酸腐蚀;e.混合酸化学抛光;f.清洗。A chemical polishing process for a sapphire filament wafer, comprising the steps of: a. cleaning the cut square piece and air drying; b. alkali high temperature corrosion; c. cleaning; d. phosphoric acid corrosion; e. mixed acid chemical polishing; f. Cleaning.
所述步骤a是清洗多线切割后的30mm*40mm*0.8mm的方片,采用5%-10%体积比的氢氟酸清洗剂,配合超声清洗,超声频率为40Hz,时间为4-10min,优选时间为5min;超声清洗后,用清水冲洗,并风干或用干燥空气吹干;The step a is to clean the square piece of 30mm*40mm*0.8mm after multi-line cutting, using a 5%-10% volume ratio hydrofluoric acid cleaning agent, and ultrasonic cleaning, the ultrasonic frequency is 40Hz, and the time is 4-10min. , preferably 5 min; after ultrasonic cleaning, rinse with water, and air dry or blow dry with dry air;
该步骤是为了去除多线切割加工后晶片表面的残余金属离子、碱基络合物以及氧化铝粉末颗粒,配合超声,可以更加彻底的去除晶片表面的颗粒等污染物;为下一步工艺提供基础条件;清洗结束后,晶片表面必须用清水冲洗干净,再用烘干或干燥压缩气体吹干;This step is to remove residual metal ions, base complexes and alumina powder particles on the surface of the wafer after multi-line cutting, and with ultrasound, it can more completely remove particles such as particles on the wafer surface; provide the basis for the next process. Condition; after cleaning, the surface of the wafer must be rinsed with clean water and then dried by drying or drying compressed gas;
所述步骤b是将干燥的晶片完全浸没在高温强碱中,优选NaOH强碱,加热温度为300-350℃,优选温度320℃,高温腐蚀时间为10-30min,优选时间12min;通过晶体择优腐蚀,C向切割线痕基本腐蚀,并呈现局部镜面反射。同时,去除晶体的生长应力、加工应力及加工损伤层;The step b is to completely immerse the dried wafer in a high temperature strong alkali, preferably NaOH strong base, heating temperature is 300-350 ° C, preferably temperature 320 ° C, high temperature etching time is 10-30 min, preferably time 12 min; Corrosion, C is basically corroded to the cutting line marks and exhibits partial specular reflection. At the same time, removing the growth stress, processing stress and processing damage layer of the crystal;
所述步骤c是采用清水浸泡后再喷淋冲洗晶片,去除晶片表面残余碱。浸泡时间1-8min,喷淋时间20-60s,优选时间分别为5min和30s;The step c is immersed in water and then sprayed to rinse the wafer to remove residual alkali on the surface of the wafer. Soaking time 1-8min, spraying time 20-60s, preferred time is 5min and 30s respectively;
所述步骤d是用85%浓磷酸对晶片进行高温浸泡,浸泡温度为200-245℃,浸泡时间为1-12h,优选温度为238℃,优选时间为4h。通过高温浓磷酸进一步对晶体表面进行择优取向腐蚀,进一步去除亚损伤层,并使晶片C向表面呈现
明显的镜面反射。The step d is to soak the wafer at a high temperature with 85% concentrated phosphoric acid, the soaking temperature is 200-245 ° C, the soaking time is 1-12 h, the preferred temperature is 238 ° C, and the preferred time is 4 h. Further preferentially etching the surface of the crystal by high-temperature concentrated phosphoric acid to further remove the sub-damage layer and present the wafer C to the surface
Obvious specular reflection.
所述步骤e是采用95%浓硫酸加85%的浓磷酸按照1:5至5:1比例混合,同时加入5%-30%的氢氟酸,制成混和酸化学抛光液,对晶片表面进行化学腐蚀抛光,抛光温度为120℃-240℃,抛光时间为15-45min。The step e is mixed with 95% concentrated sulfuric acid and 85% concentrated phosphoric acid in a ratio of 1:5 to 5:1, and 5%-30% hydrofluoric acid is added to prepare a mixed acid chemical polishing liquid on the surface of the wafer. For chemical etching, the polishing temperature is 120 ° C - 240 ° C, and the polishing time is 15-45 min.
所述步骤f采用清水浸泡后再喷淋冲洗晶片,去除晶片表面残余抛光液。浸泡时间1-6min,喷淋时间20-60s,优选时间分别为2min和45s。The step f is immersed in water and then sprayed to rinse the wafer to remove residual polishing liquid on the surface of the wafer. The soaking time is 1-6 min, the spraying time is 20-60 s, and the preferred time is 2 min and 45 s, respectively.
利用纯碱高温腐蚀速度快的优势,将晶片表面切割线痕等突出部分进行加速腐蚀,去除晶片表面损伤层,降低晶片表面的粗糙度和残余应力;纯碱是初步快速去除损伤层;腐蚀结束后必须清洗干净,才能进入下一道酸洗工序;利用高浓度磷酸高温择优腐蚀的特性,进一步去除晶片C向表面的损伤层和残余应力,进一步降低晶片C向表面的粗糙度,为下道化学抛光工序提供准备条件。Using the advantage of high-speed corrosion of soda ash, the surface of the wafer surface is accelerated and etched to remove the damage layer on the surface of the wafer, reducing the roughness and residual stress on the surface of the wafer; soda ash is the initial rapid removal of the damage layer; Cleaned before entering the next pickling process; using high-concentration phosphoric acid high-temperature selective corrosion characteristics, further removing the damage layer and residual stress on the surface of the wafer C, further reducing the roughness of the wafer C to the surface, for the next chemical polishing process Provide preparation conditions.
利用混和酸化学抛光剂,对晶片表面进行完全的择优取向抛光;利用高温电化学原理,对晶片C向表面突出部位高势能区进行加速腐蚀,进一步降低晶片C向表面粗糙度,以达到晶片表面抛光的效果;Using the mixed acid chemical polishing agent to completely polish the surface of the wafer; using the high-temperature electrochemical principle to accelerate the corrosion of the high energy region of the wafer C to the surface protrusion, further reducing the surface roughness of the wafer C to reach the surface of the wafer Polishing effect;
最后,进行清水浸泡清洗和喷淋清洗,去除残留抛光液。经混酸化学抛光剂抛光后的晶片,其C向表面粗糙度可达到1nm,完全能符合灯丝灯晶片的要求。Finally, rinse with water and spray to remove residual slurry. The wafer polished by the mixed acid chemical polishing agent has a C-direction surface roughness of 1 nm, which fully meets the requirements of the filament lamp wafer.
与现有技术相比,本发明的有益效果在于:Compared with the prior art, the beneficial effects of the present invention are:
本发明公开了一种蓝宝石灯丝晶片的化学抛光工艺,针对蓝宝石晶片磨抛清洗等高成本、低效率的加工工艺流程,提出了一种能满足LED灯丝灯晶片表面要求的新的工艺流程;The invention discloses a chemical polishing process for a sapphire filament wafer, and proposes a new process flow capable of meeting the surface requirements of the LED filament lamp wafer for a high cost and low efficiency processing process such as sapphire wafer grinding and polishing;
由于蓝宝石的硬度大,抗酸碱腐蚀能力强,本发明通过采用高温强碱腐蚀,加快了晶片表面的腐蚀速度,但在快速腐蚀的过程中,晶片表面微观上容易产生小的凹坑,因此,通过酸进一步腐蚀去除凹坑,增加晶片表面的光洁度,同
时达到去除应力的目的,使得晶片的平整度、翘曲、弯曲等指标得到提升,增加了晶片的强度,以便使晶片在后续再加工过程中不容易开裂;利用混合酸化学抛光剂对晶片表面进行完全的择优取向抛光,不需要借助机械力,直接通过高温腐蚀,并通过控制抛光温度和抛光时间,严格控制腐蚀速率,达到晶片表面抛光的效果。该工艺方法能够有效的降低蓝宝石晶片的加工成本,大幅度提高生产效率,缩短加工工序,同时,最大程度的去除了晶片表面损伤层及其残余应力,且设备投资小,加工工序短,加工产量大,操作简便,适合推广使用。Since the sapphire has high hardness and strong acid and alkali corrosion resistance, the invention accelerates the corrosion rate of the wafer surface by using high temperature and strong alkali corrosion, but in the process of rapid corrosion, the surface of the wafer is microscopically easy to generate small pits, so , further etching by acid to remove pits, increasing the surface finish of the wafer,
When the stress is removed, the flatness, warpage, bending and other indexes of the wafer are improved, and the strength of the wafer is increased, so that the wafer is not easily cracked during subsequent reworking; the surface of the wafer is coated with a mixed acid chemical polishing agent. Completely preferred orientation polishing, without the need of mechanical force, directly through high temperature corrosion, and by controlling the polishing temperature and polishing time, strictly control the corrosion rate to achieve the surface polishing effect of the wafer. The method can effectively reduce the processing cost of the sapphire wafer, greatly improve the production efficiency, shorten the processing process, and at the same time, remove the damage layer of the wafer surface and its residual stress to the greatest extent, and the equipment investment is small, the processing procedure is short, and the processing yield is high. Large, easy to operate, suitable for promotion.
实施例1:Example 1:
下面通过实施例对本发明作进一步详细说明:The present invention will be further described in detail below by way of examples:
本发明公开的蓝宝石灯丝晶片的化学抛光工艺,指的是蓝宝石多线切割后的灯丝方形晶片的新加工工艺,采用以下工艺流程:The chemical polishing process of the sapphire filament wafer disclosed by the invention refers to a new processing technology of the filament square wafer after sapphire multi-wire cutting, and adopts the following process flow:
a.自制5%的氢氟酸清洗剂,配合超声,清洗多线切割后的30mm*40mm*0.8mm的方片,其中,超声频率:40Hz,超声时间:5min,再用清水冲洗;a. Homemade 5% hydrofluoric acid cleaning agent, with ultrasonic, cleaning the square piece of 30mm*40mm*0.8mm after multi-line cutting, wherein the ultrasonic frequency: 40Hz, ultrasonic time: 5min, and then rinsed with water;
b.纯碱NaOH加热至高温320℃完全熔融,将晶片缓慢预热置于熔融的碱中,浸泡时间为12min;b. soda NaOH is heated to a high temperature of 320 ° C completely melted, the wafer is slowly preheated in a molten alkali, soaking time is 12min;
c.清水浸泡5min后,提出液面喷淋30s,去除残留碱;c. After soaking in water for 5 minutes, the liquid surface is sprayed for 30s to remove residual alkali;
d.将85%的浓磷酸加热至238℃,晶片缓慢预热放置浓磷酸中浸泡4h,取出;d. 85% concentrated phosphoric acid is heated to 238 ° C, the wafer is slowly preheated and placed in concentrated phosphoric acid for 4 hours, and taken out;
e.将85%的浓磷酸、95%的浓硫酸按1:5的比例混合,同时加入10%的氢氟酸进行混合制成混合酸化学抛光剂,加热混合抛光剂至150℃,晶片置于其中浸泡20min,完成化学抛光;e. Mix 85% concentrated phosphoric acid and 95% concentrated sulfuric acid in a ratio of 1:5, and add 10% hydrofluoric acid to mix to form a mixed acid chemical polishing agent, heat and mix the polishing agent to 150 ° C, and place the wafer. Soaking therein for 20 minutes to complete chemical polishing;
f.晶片置于清水中浸泡2min后提出液面,喷淋45s,去除表面残余抛光液。
f. After the wafer is immersed in clean water for 2 minutes, the liquid surface is lifted and sprayed for 45 s to remove the residual polishing liquid on the surface.
实施例2Example 2
步骤e中将浓磷酸、浓硫酸按2:1的比例混合,同时加入15%的氢氟酸进行混合制成混合酸化学抛光剂,加热混合抛光剂至150℃,晶片置于其中浸泡20min,完成化学抛光;其它工艺不变。In step e, concentrated phosphoric acid and concentrated sulfuric acid are mixed in a ratio of 2:1, and 15% hydrofluoric acid is added to be mixed to prepare a mixed acid chemical polishing agent, and the polishing agent is heated and mixed to 150 ° C, and the wafer is immersed therein for 20 minutes. Chemical polishing is completed; other processes are unchanged.
实施例3Example 3
步骤e中将浓磷酸、浓硫酸按5:1的比例混合,同时加入氢氟酸10%进行混合制成混合酸化学抛光剂,加热混合抛光剂至150℃,晶片置于其中浸泡20min,完成化学抛光;其它工艺不变。In step e, concentrated phosphoric acid and concentrated sulfuric acid are mixed in a ratio of 5:1, and hydrofluoric acid 10% is added to be mixed to prepare a mixed acid chemical polishing agent, and the polishing agent is heated and mixed to 150 ° C, and the wafer is immersed therein for 20 minutes to complete. Chemical polishing; other processes are unchanged.
表1经混合酸化学抛光剂抛光的蓝宝石灯丝晶片的表面粗糙度Table 1 Surface roughness of sapphire filament wafers polished by mixed acid chemical polishing agent
实施例1Example 1 | 实施例2Example 2 | 实施例3Example 3 | |
C向表面粗糙度C-direction surface roughness | 1nm1nm | 1nm1nm | 1nm1nm |
上述实施例仅为本发明的较佳的实施方式,除此之外,本发明还可以有其他实现方式。需要说明的是,在没有脱离本发明构思的前提下,任何显而易见的改进和修饰均应落入本发明的保护范围之内。
The above embodiments are merely preferred embodiments of the present invention, and other implementations of the present invention are possible. It should be noted that any obvious modifications and alterations are intended to fall within the scope of the present invention without departing from the spirit of the invention.
Claims (8)
- 一种蓝宝石灯丝晶片的化学抛光工艺,其特征在于:所述抛光工艺包括如下步骤:A chemical polishing process for a sapphire filament wafer, characterized in that the polishing process comprises the following steps:a.清洗切割方片,并风干;a. Clean the cut square pieces and air dry;b.碱高温腐蚀;b. alkali high temperature corrosion;c.清洗;c. cleaning;d.磷酸腐蚀;d. Phosphoric acid corrosion;e.混合酸化学抛光;e. mixed acid chemical polishing;f.清洗。f. Cleaning.
- 根据权利要求1所述的蓝宝石灯丝晶片的化学抛光工艺,其特征在于:步骤a所述清洗是指清洗多线切割后的30mm*40mm*0.8mm的方片,采用体积比为5%-10%的氢氟酸清洗剂,配合超声清洗,超声频率为40Hz,时间为4-10min;超声清洗后,用清水冲洗,并风干或用干燥空气吹干。The chemical polishing process for a sapphire filament wafer according to claim 1, wherein the cleaning in step a refers to cleaning a square piece of 30 mm*40 mm*0.8 mm after multi-line cutting, using a volume ratio of 5%-10. % hydrofluoric acid cleaning agent, combined with ultrasonic cleaning, ultrasonic frequency is 40Hz, time is 4-10min; after ultrasonic cleaning, rinse with water, air dry or dry with dry air.
- 根据权利要求1所述的蓝宝石灯丝晶片的化学抛光工艺,其特征在于:步骤b所述碱高温腐蚀是将干燥的晶片完全浸没在高温强碱中,加热温度为300-350℃,高温腐蚀时间为10-30min。The sapphire filament wafer chemical polishing process according to claim 1, wherein the alkaline high temperature etching in step b is to completely immerse the dried wafer in a high temperature and strong alkali, and the heating temperature is 300-350 ° C, and the high temperature etching time It is 10-30min.
- 根据权利要求3所述的蓝宝石灯丝晶片的化学抛光工艺,其特征在于:所述强碱为NaOH,加热温度为320℃,高温腐蚀时间为12min。The chemical polishing process for a sapphire filament wafer according to claim 3, wherein the strong base is NaOH, the heating temperature is 320 ° C, and the high temperature etching time is 12 min.
- 根据权利要求1所述的蓝宝石灯丝晶片的化学抛光工艺,其特征在于:步骤c所述清洗是采用清水浸泡后再喷淋冲洗晶片,清水浸泡时间为1-8min,喷淋时间为20-60s。The chemical polishing process for a sapphire filament wafer according to claim 1, wherein the cleaning in step c is performed by immersing in water and then spraying the wafer, the soaking time of the water is 1-8 min, and the spraying time is 20-60 s. .
- 根据权利要求1所述的蓝宝石灯丝晶片的化学抛光工艺,其特征在于:步骤d所述磷酸腐蚀是用85%浓磷酸对晶片进行高温浸泡,浸泡温度为200-245℃,浸泡时间为1-12h。 The sapphire filament wafer chemical polishing process according to claim 1, wherein the phosphoric acid etching in step d is performed by immersing the wafer at a high temperature with 85% concentrated phosphoric acid, the immersion temperature is 200-245 ° C, and the immersion time is 1- 12h.
- 根据权利要求1所述的蓝宝石灯丝晶片的化学抛光工艺,其特征在于:步骤e所述混合酸化学抛光是采用95%浓硫酸加85%的浓磷酸按照1:5-5:1的比例混合,同时加入5%-30%氢氟酸,制成混和酸化学抛光液,对晶片表面进行化学腐蚀抛光,抛光温度为120-240℃,抛光时间为15-45min。A chemical polishing process for a sapphire filament wafer according to claim 1, wherein the mixed acid chemical polishing in step e is carried out by mixing 95% concentrated sulfuric acid and 85% concentrated phosphoric acid in a ratio of 1:5 to 5:1. At the same time, 5%-30% hydrofluoric acid is added to prepare a mixed acid chemical polishing liquid, and the surface of the wafer is chemically polished, the polishing temperature is 120-240 ° C, and the polishing time is 15-45 min.
- 根据权利要求1所述的蓝宝石灯丝晶片的化学抛光工艺,其特征在于:步骤f所述清洗是采用清水浸泡后再喷淋冲洗晶片,浸泡时间为1-6min,喷淋时间为20-60s。 The sapphire filament wafer chemical polishing process according to claim 1, wherein the cleaning is performed by immersing in water and then rinsing the wafer, the immersion time is 1-6 min, and the spraying time is 20-60 s.
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