CN102021658A - Heavily doped monocrystalline silicon wafer corrosion technique by alkali corrosion before acid corrosion - Google Patents
Heavily doped monocrystalline silicon wafer corrosion technique by alkali corrosion before acid corrosion Download PDFInfo
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- CN102021658A CN102021658A CN2010105812500A CN201010581250A CN102021658A CN 102021658 A CN102021658 A CN 102021658A CN 2010105812500 A CN2010105812500 A CN 2010105812500A CN 201010581250 A CN201010581250 A CN 201010581250A CN 102021658 A CN102021658 A CN 102021658A
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- corrosion
- monocrystalline silicon
- acid
- heavily doped
- silicon wafer
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- 238000005260 corrosion Methods 0.000 title claims abstract description 89
- 230000007797 corrosion Effects 0.000 title claims abstract description 89
- 229910021421 monocrystalline silicon Inorganic materials 0.000 title claims abstract description 40
- 239000002253 acid Substances 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 22
- 239000003513 alkali Substances 0.000 title abstract description 6
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 18
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 15
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 12
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims abstract description 5
- 239000007864 aqueous solution Substances 0.000 claims abstract description 4
- 239000003518 caustics Substances 0.000 claims description 25
- 238000005530 etching Methods 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 10
- 238000004140 cleaning Methods 0.000 claims description 3
- 238000012797 qualification Methods 0.000 abstract description 2
- 238000005406 washing Methods 0.000 abstract 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 15
- 229910052710 silicon Inorganic materials 0.000 description 15
- 239000010703 silicon Substances 0.000 description 15
- 238000004519 manufacturing process Methods 0.000 description 5
- 230000003628 erosive effect Effects 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910021419 crystalline silicon Inorganic materials 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 125000000896 monocarboxylic acid group Chemical group 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention relates to a heavily doped monocrystalline silicon wafer corrosion technique by alkali corrosion before acid corrosion. The corrosion technique comprises the following steps: carrying out alkali corrosion on the monocrystalline silicon wafer by using a 30% potassium hydroxide aqueous solution at 84 DEG C for 7 minutes 12 seconds, wherein the removal amount of the alkali corrosion is about 20 mu m; washing the monocrystalline silicon wafer subject to alkali corrosion, and carrying out centrifugal drying; and carrying out acid corrosion by using an acid corrosion solution at 28 DEG C for 14 seconds, wherein the acid corrosion solution comprises 15-25% of hydrofluoric acid, 25-30% of nitric acid and 50-60% of acetic acid, and the removal amount of the acid corrosion is about 10 mu m. By utilizing the technique, the heavily doped monocrystalline silicon wafer with satisfactory surface can be produced, and the total thickness variation (TTV) added value of the heavily doped monocrystalline silicon wafer is less than 2.5 mu m; and the qualification rate of the product is higher than 98%, thus the market demands for low-TTV heavily doped monocrystalline silicon wafer can be satisfied, and the technique provided by the invention can be dominating in the market.
Description
Technical field
The present invention relates to the production method of monocrystalline silicon piece, particularly relate to the etching process of acid corrosion after the caustic corrosion of a kind of heavily doped monocrystalline silicon piece elder generation.
Background technology
Silicon polished main work flow comprises single crystal growing → barreling → section → chamfering → grinding → corrosion → polishing → cleaning → packing etc.Wherein corrosion is important production process, and its effect is that the stress that its surface produces because of mechanical workout is formed with the mechanical stress affected layer of certain depth after removing mechanical workouts such as the section of silicon single-crystal silicon chip process, grinding.Usual method is acid corrosion liquid or caustic corrosion liquid and the monocrystalline silicon piece generation chemical reaction that adopts under finite concentration and the certain temperature, thereby reaches the purpose of removing affected layer.The principle of wherein, caustic corrosion technology is: Si+2OH
-+ 4H
2O=Si (OH)
6 -2+ 2H
2, this is a kind of anisotropic etch process, corrosion back silicon chip surface is smooth; And because caustic corrosion technology is simple, corrosive fluid need not to stir, erosion rate is controlled; Environmental protection treatment is easier to relatively, nontoxic, advantage such as waste liquid can be recycled, and present domestic polished section production firm uses in this procedure multiselect caustic corrosion technology.
But the erosion rate of caustic corrosion technology is slower, and production capacity is not as sour technology; And the silicon wafer surface after its corrosion is coarse, adsorbs impurity easily; In addition, the more important thing is that the metal ion that alkali lye brought inevitably can remain in silicon wafer surface and to its lattice internal diffusion, have a strong impact on parameter indexs such as life-span after corrosion.And sour technology utilization acid corrosion liquid (HF, HNO
3And CH
3The mixing solutions of COOH) with the silicon chip top layer chemical reaction: Si+4HNO takes place
3+ 6HF=H
2SiF
6+ 4NO
2↑+4H
2O, its erosion rate is very fast, and silicon wafer roughness and glossiness after the corrosion are all higher, contain less metallic pollution again.Therefore, existing market is more favored the polished section that the acid corrosion operation is produced.
But regrettably, the technology of at present domestic acid corrosion exists limitation, embodies a concentrated reflection of to be silicon chip surface geometric parameter such as TTV(total thickness variations after the corrosion) difficult control; Adopt technology corrosion large size (more than the 6 inches) monocrystalline silicon piece of existing acid corrosion, because silicon chip surface is long-pending bigger, the removal amount difference of the different positions of monocrystalline silicon piece is bigger, causes the more difficult control of TTV; And the heavy doping monocrystalline silicon piece has reduced the interatomic bond energy because its a large amount of dopant atom has destroyed the crystalline network of crystalline silicon, makes the erosion removal amount more be difficult to control.Corrode heavily doped silicon slice corrosion front and back TTV increased value about 5 μ m with existing technology.Can not satisfy customer requirement.
Summary of the invention
The objective of the invention is at above-mentioned existing problems, the etching process of acid corrosion after the caustic corrosion of a kind of heavily doped monocrystalline silicon piece elder generation is provided.Because the corrosive purpose is to obtain the complete relatively monocrystalline silicon piece of lattice, so this technology takes to carry out earlier the method that acid corrosion is carried out in caustic corrosion again at heavily doped monocrystalline silicon piece.Take this method to corrode heavily doped monocrystalline silicon piece, its removal amount reaches about 20 μ m.The damage that utilizes caustic corrosion " stopping effect certainly " to remove monocrystalline silicon surface just; Utilize the technology of acid corrosion to corrode again, make the corrosion speed of different zones in the acid corrosion process even relatively; Its removal amount reaches about 10 μ m, and the monocrystalline silicon piece TTV increased value after the corrosion is below 2.5 μ m.Adopt this technology can stably produce the heavily doped silicon single crystal etched sheet of TTV increased value less than 2.5 μ m.
The technical scheme that the present invention takes is: the etching process of acid corrosion after the first caustic corrosion of a kind of heavily doped monocrystalline silicon piece, and it is characterized in that: its technology is as follows:
1) it is that 30% potassium hydroxide aqueous solution carries out caustic corrosion that the heavily doped monocrystalline silicon piece after will cleaning, is earlier put into concentration, and setting corrosion temperature is 84 ℃, and etching time is 7min12s;
2), the monocrystalline silicon piece after the caustic corrosion is cleaned drying afterwards;
3), the monocrystalline silicon piece after will drying puts into acid corrosion liquid and carries out acid corrosion, acid corrosion liquid is to carry out blended solution by hydrofluoric acid, nitric acid, acetic acid, the shared weight percent of each component is: hydrofluoric acid 15%～25%; Nitric acid 25%～30%; Acetic acid 50%～60%; Setting corrosion temperature is 28 ℃; Etching time is 14s.
The beneficial effect that the present invention produced is: takes this technology, can stably produce the TTV increased value less than 2.5 μ m, and the heavily doped corrosion monocrystalline silicon piece that the surface is good, product percent of pass is up to more than 98%.Thereby can satisfy the demand of market, and will in market, occupy vantage point the low heavily doped etched sheet of TTV.
Embodiment
The invention will be further described below in conjunction with embodiment:
Embodiment: 6 inches heavily doped monocrystalline silicon pieces, resistivity are 0.0004-0.0037 Ω. ㎝, and silicon chip TTV before the corrosion＜1, it is two-sided that removal amount requires to remove 60um/.Concrete etching process step is as follows:
1) configuration caustic corrosion liquid is poured solid potassium hydroxide in the caustic corrosion groove into earlier, injects pure water again in groove, is modulated into solid potassium hydroxide: the aqueous solution of water=30%:70%;
2) the caustic corrosion machine is warming up to 84 ℃;
3) silicon chip to be processed is put into the caustic corrosion machine, begin corrosion; Etching time is 7min12s; The caustic corrosion removal amount is about 20 μ m;
4) after caustic corrosion finishes, take out silicon chip, put into waterwheel; Monocrystalline silicon piece after the caustic corrosion is cleaned, dry afterwards;
The corrosion monocrystalline silicon piece that 5) will clean is poured in the acid corrosion machine;
6) selecting the acid corrosion liquid proportional is that corrosive fluid is a hydrofluoric acid: nitric acid: acetic acid=20%: 27%:53%; Process; It is 28 ℃ that corrosion temperature is set; Etching time is 14s;
7) monocrystalline silicon piece is put into the acid corrosion machine, begun corrosion; The acid corrosion removal amount is about 10 μ m;
8) after acid corrosion finishes, the monocrystalline silicon piece after the acid corrosion is poured in the sheet basket; After the sheet basket ultrasonic cleaning of monocrystalline silicon piece is housed, dry, send and test.
Technique effect detects: adopt above-mentioned acid corrosion to add 7095 of the heavily doped monocrystalline silicon pieces of caustic corrosion explained hereafter.To corrode back monocrystalline silicon piece TTV＜3.5, roughness is tested less than the inspecting standard of 0.5 μ m, and qualified 6983, qualification rate is 98.56%.
This detected result shows: this etching process can effectively improve acid corrosion monocrystalline silicon piece TTV by adopting the first caustic corrosion method corrosion monocrystalline silicon piece of acid corrosion again; This invention can realize the volume production of the low heavily doped silicon single crystal etched sheet of TTV.
Claims (1)
1. the etching process of acid corrosion after the heavily doped monocrystalline silicon piece elder generation caustic corrosion, it is characterized in that: its technology is as follows:
(1), earlier it is that 30% potassium hydroxide aqueous solution carries out caustic corrosion that the heavily doped monocrystalline silicon piece after will cleaning is put into concentration, and setting corrosion temperature is 84 ℃, and etching time is 7min12s;
(2), the monocrystalline silicon piece after the caustic corrosion is cleaned drying afterwards;
(3), the monocrystalline silicon piece after will drying puts into acid corrosion liquid and carries out acid corrosion, acid corrosion liquid is to carry out blended solution by hydrofluoric acid, nitric acid, acetic acid, the shared weight percent of each component is: hydrofluoric acid 15%～25%; Nitric acid 25%～30%; Acetic acid 50%～60%; Setting corrosion temperature is 28 ℃; Etching time is 14s.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105812500A CN102021658A (en) | 2010-12-10 | 2010-12-10 | Heavily doped monocrystalline silicon wafer corrosion technique by alkali corrosion before acid corrosion |
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|---|---|---|---|
| CN2010105812500A CN102021658A (en) | 2010-12-10 | 2010-12-10 | Heavily doped monocrystalline silicon wafer corrosion technique by alkali corrosion before acid corrosion |
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|---|---|
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|---|---|---|---|
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102324386A (en) * | 2011-09-15 | 2012-01-18 | 宜兴市环洲微电子有限公司 | Preparation method of silicon chip used for planar solid discharge tube chip manufacturing process |
| CN102418150A (en) * | 2011-12-15 | 2012-04-18 | 天津中环领先材料技术有限公司 | Processing technology of large-corrosion-line monocrystalline silicon alkaline corrosion wafer |
| CN102492947A (en) * | 2011-12-15 | 2012-06-13 | 天津中环领先材料技术有限公司 | Low-roughness silicon wafer alkali corrosion process |
| CN102569036A (en) * | 2012-03-09 | 2012-07-11 | 常州银河半导体有限公司 | Silicon wafer cleaning technology |
| CN102664149A (en) * | 2012-06-04 | 2012-09-12 | 扬州杰利半导体有限公司 | Method for preventing corrosion of grain side in caustic washing of OJ (Open Junction) chip |
| CN102866335A (en) * | 2011-07-05 | 2013-01-09 | 上海申和热磁电子有限公司 | Method for testing oxidation induced fault in czochralski silicon by minority carrier lifetime scanning method |
| CN103000544A (en) * | 2011-09-13 | 2013-03-27 | 康可电子（无锡）有限公司 | Recycling method of test strips for phosphorus and boron prediffusion process |
| CN105154268A (en) * | 2015-08-29 | 2015-12-16 | 江西赛维Ldk太阳能高科技有限公司 | Cleaning fluid capable of reducing thickness of damaged layer of surface of silicon wafer and cleaning method |
| CN105655248A (en) * | 2016-03-22 | 2016-06-08 | 河南芯睿电子科技有限公司 | Alkali corrosion processing method for photoetching alignment mark of non-polished monocrystal-silicon-based device |
| CN110047771A (en) * | 2019-03-07 | 2019-07-23 | 东方环晟光伏（江苏）有限公司 | The test method of monocrystalline silicon piece cutting damage thickness degree is obtained based on multiple weighing |
| CN111128714A (en) * | 2019-12-31 | 2020-05-08 | 杭州中欣晶圆半导体股份有限公司 | Acid etching process for reducing heavily boron-doped color spots |
| CN112951716A (en) * | 2021-03-22 | 2021-06-11 | 上海中欣晶圆半导体科技有限公司 | Method for improving flatness and roughness through mixed corrosion |
| CN113496886A (en) * | 2020-04-03 | 2021-10-12 | 重庆超硅半导体有限公司 | Method for controlling alkali corrosion removal amount of monocrystalline silicon wafer for integrated circuit |
-
2010
- 2010-12-10 CN CN2010105812500A patent/CN102021658A/en active Pending
Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102866335A (en) * | 2011-07-05 | 2013-01-09 | 上海申和热磁电子有限公司 | Method for testing oxidation induced fault in czochralski silicon by minority carrier lifetime scanning method |
| CN103000544A (en) * | 2011-09-13 | 2013-03-27 | 康可电子（无锡）有限公司 | Recycling method of test strips for phosphorus and boron prediffusion process |
| CN102324386A (en) * | 2011-09-15 | 2012-01-18 | 宜兴市环洲微电子有限公司 | Preparation method of silicon chip used for planar solid discharge tube chip manufacturing process |
| CN102492947B (en) * | 2011-12-15 | 2013-06-19 | 天津中环领先材料技术有限公司 | Low-roughness silicon wafer alkali corrosion process |
| CN102418150A (en) * | 2011-12-15 | 2012-04-18 | 天津中环领先材料技术有限公司 | Processing technology of large-corrosion-line monocrystalline silicon alkaline corrosion wafer |
| CN102492947A (en) * | 2011-12-15 | 2012-06-13 | 天津中环领先材料技术有限公司 | Low-roughness silicon wafer alkali corrosion process |
| CN102569036A (en) * | 2012-03-09 | 2012-07-11 | 常州银河半导体有限公司 | Silicon wafer cleaning technology |
| CN102664149B (en) * | 2012-06-04 | 2014-07-16 | 扬州杰利半导体有限公司 | Method for preventing corrosion of grain side in caustic washing of OJ (Open Junction) chip |
| CN102664149A (en) * | 2012-06-04 | 2012-09-12 | 扬州杰利半导体有限公司 | Method for preventing corrosion of grain side in caustic washing of OJ (Open Junction) chip |
| CN105154268A (en) * | 2015-08-29 | 2015-12-16 | 江西赛维Ldk太阳能高科技有限公司 | Cleaning fluid capable of reducing thickness of damaged layer of surface of silicon wafer and cleaning method |
| CN105655248A (en) * | 2016-03-22 | 2016-06-08 | 河南芯睿电子科技有限公司 | Alkali corrosion processing method for photoetching alignment mark of non-polished monocrystal-silicon-based device |
| CN105655248B (en) * | 2016-03-22 | 2018-06-05 | 河南芯睿电子科技有限公司 | A kind of caustic corrosion processing method of non-polished monocrystalline silicon-based devices photoetching alignment mark |
| CN110047771A (en) * | 2019-03-07 | 2019-07-23 | 东方环晟光伏（江苏）有限公司 | The test method of monocrystalline silicon piece cutting damage thickness degree is obtained based on multiple weighing |
| CN111128714A (en) * | 2019-12-31 | 2020-05-08 | 杭州中欣晶圆半导体股份有限公司 | Acid etching process for reducing heavily boron-doped color spots |
| CN111128714B (en) * | 2019-12-31 | 2022-06-03 | 杭州中欣晶圆半导体股份有限公司 | Acid etching process for reducing heavily boron-doped color spots |
| CN113496886A (en) * | 2020-04-03 | 2021-10-12 | 重庆超硅半导体有限公司 | Method for controlling alkali corrosion removal amount of monocrystalline silicon wafer for integrated circuit |
| CN113496886B (en) * | 2020-04-03 | 2022-10-25 | 重庆超硅半导体有限公司 | Method for controlling alkali corrosion removal amount of monocrystalline silicon wafer for integrated circuit |
| CN112951716A (en) * | 2021-03-22 | 2021-06-11 | 上海中欣晶圆半导体科技有限公司 | Method for improving flatness and roughness through mixed corrosion |
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Open date: 20110420 |