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CN109321253A - A kind of etching solution of Silicon Wafer - Google Patents

A kind of etching solution of Silicon Wafer Download PDF

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Publication number
CN109321253A
CN109321253A CN201811435355.8A CN201811435355A CN109321253A CN 109321253 A CN109321253 A CN 109321253A CN 201811435355 A CN201811435355 A CN 201811435355A CN 109321253 A CN109321253 A CN 109321253A
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CN
China
Prior art keywords
acid
etching solution
silicon wafer
etching
etch
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Pending
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CN201811435355.8A
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Chinese (zh)
Inventor
李少平
张庭
贺兆波
尹印
冯凯
万杨阳
王书萍
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Hubei Xingfa Chemicals Group Co Ltd
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Hubei Xingfa Chemicals Group Co Ltd
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Priority to CN201811435355.8A priority Critical patent/CN109321253A/en
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K13/00Etching, surface-brightening or pickling compositions
    • C09K13/04Etching, surface-brightening or pickling compositions containing an inorganic acid
    • C09K13/08Etching, surface-brightening or pickling compositions containing an inorganic acid containing a fluorine compound

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Weting (AREA)

Abstract

The invention discloses a kind of etching solution of Silicon Wafer, main component includes electronic grade nitric acid, electronic-stage hydrofluoric acid, electronic-grade sulfuric acid, electron-level phosphoric acid, electronic grade acetic acid, surfactant, ultrapure water.Wherein, silicon is oxidized to the oxide of silicon as oxidant by nitric acid;Oxide dissolution, the removal of silicon are realized the etching to Silicon Wafer as lytic agent by hydrofluoric acid;Solution viscosity can be improved in sulfuric acid, stablizes reaction rate, does not change etch profile, increases etch uniformity;Phosphoric acid can also be improved solution viscosity, improves mass transfer resistance, reduces etch-rate, do not change etch profile;Acetic acid reduces the degree of ionization of nitric acid as diluent, inhibits the oxidability of nitric acid, reduces reaction rate, the surface topography after influencing etching;Surfactant reduces the surface tension of solution, the surface topography after improving Silicon Wafer etching.The etch-rate of this etching solution is stably and controllable, etches surface uniform ground.

Description

A kind of etching solution of Silicon Wafer
Technical field
The present invention relates to the etching solution in a kind of Silicon Wafer manufacturing process, by the chemical treatment to silicon wafer surface, with Meet semiconductor chip designs and manufactures requirement.
Background technique
Semiconductor silicon wafer manufacture be multistage manufacturing process, crystal bar be processed into silicon wafer need by cutting, The processes such as chamfering, grinding, burn into polishing, in silicon wafer processing flow, the quality output of later process may be with preceding road work The manufacturing defect correlation of sequence or even certain quality problems can be inherited by many later process always, and client is eventually flowed to.
Silicon wafer used in semiconductor industry needs to have good flatness and lower surface defect, but passes through Cut, grinding obtained silicon wafer, often flatness is poor, surface have mechanical processing trauma, in chemically mechanical polishing Before need to completely remove these damages, silicon wafer manufacturing generally completes the corrosion of big removal amount using wet process acid corrosion Processing.It is influenced significantly by supplied materials quality since the quality of CMP process exports, the enabling objective of acid corrosion is not Only it is limited to that the mechanical damage of preceding working procedure is completely exfoliated, and needs to provide for later process and a kind of be beneficial to the flat of quality output Whole degree and geometry.
It is difficult to realize the regulation to etch-rate and surface using nitric acid and hydrofluoric acid system in the prior art, needs to add Other compositions improve the performance of etching solution.For example, patent document 1 using two-step wet etching backside of wafer is carried out it is thinned, Silicon substrate is etched to epitaxial layer is exposed using the mixture of hydrofluoric acid, nitric acid, phosphoric acid and sulfuric acid first, then uses hydrogen The mixture of fluoric acid, nitric acid and acetic acid carries out selective etch to the epitaxial layer of silicon substrate and exposing, completes ultra-thin and uniform The preparation of wafer, but two-step wet etching increases processing step, operates more complicated.Patent document 2 uses nitric acid, hydrogen fluorine The mixed solution of acid and sulfuric acid is etched silicon substrate, but the etching solution facilitates the surface roughening for making silicon substrate, no It can obtain the surface with satisfactory flatness.
A kind of patent document 1: 103077889 A of thinning method for backing side of wafer CN
Patent document 2: 106356296 A of method CN of the surface roughening of etching solution and silicon substrate.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of easy to operate, good flatness etching solution, etchings Rate stabilization is controllable, etches surface uniform ground, to meet semiconductor chip manufacture to the quality requirements of Silicon Wafer.
The present invention relates to a kind of etching solution of Silicon Wafer, the composition of the etching solution includes: to account for etching solution total weight 10- 50% electronic grade nitric acid, the electronic-stage hydrofluoric acid of 1-5%, the electronic-grade sulfuric acid of 5-20%, the electron-level phosphoric acid of 10-30%, 1-10% Electronic grade acetic acid, the surfactant of 0.001-3%, the water of 20-50%.The water is resistivity >=15.0M Ω * cm(25 DEG C) ultrapure water.
Further, the present invention relates to above-mentioned etching solution, silicon is oxidized to the oxidation of silicon as oxidant by the nitric acid Object;Hydrofluoric acid generates soluble H as lytic agent, with the oxide of silicon2SiF6.Its total reaction is as follows: 3Si+4HNO3 + 18HF → 3H2SiF6 + 4NO + 8H2O, acid processing described herein use nitric acid, hydrofluoric acid system, and nitric acid will Silicon is oxidized to the oxide of silicon, and the oxide of silicon is dissolved, removed by hydrofluoric acid.
The sulfuric acid is used to improve solution viscosity, reduces reaction rate, does not change etch profile, while keeping etching Stability and homogeneity.Phosphoric acid improves mass transfer resistance, reduces etch-rate, also do not change etch profile for improving solution viscosity.
The acetic acid inhibits nitric acid oxidation ability, slows down reaction rate as diluent, influences to etch rear surface shape Looks.
The surfactant can reduce the surface tension of solution, improve the wellability of solution, keep solution equal Even etching crystal column surface.
The surfactant is nonionic surfactant, preferably polyoxethylene octylphenyl phenol ether -10, poly alkyl alcohol One or more of ethylene oxide ether, polyoxyethylene sorbitan monooleate, ethylene oxide propylene oxide block polyether etc. Mixture.
Silicon wafer is etched using etching solution of the invention, the addition order by merging of each ingredient in etching solution are as follows: PFA bottles → ultrapure water → sulfuric acid → phosphoric acid → nitric acid → acetic acid → hydrofluoric acid → surfactant.
It the present invention relates to above-mentioned process for preparation is carried out in the container for filling a large amount of water, the temperature of solution is made using water-bath Stablize in room temperature;It is every a kind of ingredient is added to add a kind of lower ingredient after temperature is cooling, prevent effumability acid due to Solution temperature, which increases volatilization, causes content to reduce.
It is by preparation sequence that the raw material of etching solution is stand-by after mixing, the P-type wafer for being cut into 3cm*4cm is put into certainly It is placed on the top of etching solution in the card slot of system and by card slot, is immersed in silicon wafer in etching solution, and is added in the bottom of etching solution Magneton is placed on magnetic stirring apparatus and carries out soaking and stirring, guarantees uniform etching.Etch temperature and time are respectively 25 DEG C and 0- 5min。
The flatness of silicon wafer and etch-rate are detected after having etched.
Silicon is oxidized to the oxide of silicon as oxidant by nitric acid in technical solution of the present invention;Hydrofluoric acid is as dissolution Agent, by oxide dissolution, the removal of silicon;Solution viscosity can be improved in sulfuric acid, stablizes reaction rate, does not change etch profile, increases Add etch uniformity;Phosphoric acid can also be improved solution viscosity, improves mass transfer resistance, reduces etch-rate, also do not change etch profile; Acetic acid reduces the degree of ionization of nitric acid as diluent, inhibits the oxidability of nitric acid, reduces reaction rate, after influencing etching Surface topography;Surfactant reduces the surface tension of solution, the surface topography after improving Silicon Wafer etching.This etching solution can be with By regulating and controlling the content of each ingredient of etching solution, controllable etch-rate and etching surface are obtained, and keeps the stability, of etching Even property, planarization.
The present invention is added to sulfuric acid, phosphoric acid, acetic acid and surfactant in traditional nitric acid, hydrofluoric acid system, can be with Guarantee stable etch-rate, and etch-rate can be adjusted by the content of each component in regulation etching solution, realizes accurate Etch the requirement of different-thickness.In addition, may be implemented since the surface tension of etching solution is low, wellability is good to the equal of Silicon Wafer Even etching, crystal column surface is smooth after etching, has good controllable flatness.
Specific embodiment
Present invention will be further explained below with reference to specific examples.The present invention will be further described in detail, but unlimited In these embodiments.
Material concentration selects: electronic grade nitric acid can for 70% aqueous solution of nitric acid, electronic-stage hydrofluoric acid can be 50% hydrogen Aqueous fluorine acid solution, electronic-grade sulfuric acid can be 97% aqueous sulfuric acid, and electron-level phosphoric acid can be 90% aqueous sulfuric acid, electron level Acetic acid can be 99% aqueous acetic acid, but be not limited to above-mentioned each concentration value.
It is etched experiment using the P-type silicon wafer piece of twin polishing, the original thickness of P-type wafer is 725 μm.
Embodiment 1
The composition of etching solution 1: 38wt% electronic grade nitric acid, 3wt% electronic-stage hydrofluoric acid, 15wt% electronic-grade sulfuric acid, 15wt% electronics Grade phosphoric acid, 5wt% electronic grade acetic acid, 0.005wt% polyoxethylene octylphenyl phenol ether -10,23.995wt% ultrapure water.
It is by preparation sequence that etching solution 1 is stand-by after mixing, the P-type wafer for being cut into 3cm*4cm is put into homemade It is placed on the top of etching solution 1 in card slot and by card slot, is immersed in silicon wafer in etching solution 1, and magnetic is added in the bottom of etching solution 1 Son is placed on magnetic stirring apparatus and is stirred, and guarantees uniform etching.Etch temperature and time are respectively 25 DEG C and 2min.
The flatness of silicon wafer and etch-rate are detected after having etched, after the etched processing of liquid 1 can be obtained, flatness It is 0.40 μm, etch-rate is 7 μm/min.Etching solution 1 after circulation etching 5 times, distinguish by the flatness and etch-rate of silicon wafer For 0.42 μm and 6.79 μm/min.
Embodiment 2
The composition of etching solution 2: 38wt% electronic grade nitric acid, 3wt% electronic-stage hydrofluoric acid, 15wt% electronic-grade sulfuric acid, 15wt% electronics Grade phosphoric acid, 6wt% electronic grade acetic acid, 0.005wt% polyoxethylene octylphenyl phenol ether -10,22.995wt% ultrapure water.
It is by preparation sequence that etching solution 2 is stand-by after mixing, the P-type wafer for being cut into 3cm*4cm is put into homemade It is placed on the top of etching solution 2 in card slot and by card slot, is immersed in silicon wafer in etching solution 2, and magnetic is added in the bottom of etching solution 2 Son is placed on magnetic stirring apparatus and is stirred, and guarantees uniform etching.Etch temperature and time are respectively 25 DEG C and 3min.
The flatness of silicon wafer and etch-rate are detected after having etched, after the etched processing of liquid 2 can be obtained, flatness It is 0.34 μm, etch-rate is 6 μm/min.Etching solution 2 after circulation etching 5 times, distinguish by the flatness and etch-rate of silicon wafer For 0.37 μm and 5.82 μm/min.
Embodiment 3
The composition of etching solution 3: 30wt% electronic grade nitric acid, 5wt% electronic-stage hydrofluoric acid, 10wt% electronic-grade sulfuric acid, 15wt% electronics Grade phosphoric acid, 5wt% electronic grade acetic acid, 0.01wt% fatty alcohol polyoxyethylene ether, 34.99wt% ultrapure water.
It is by preparation sequence that etching solution 3 is stand-by after mixing, the P-type wafer for being cut into 3cm*4cm is put into homemade It is placed on the top of etching solution 3 in card slot and by card slot, is immersed in silicon wafer in etching solution 3, and magnetic is added in the bottom of etching solution 3 Son is placed on magnetic stirring apparatus and is stirred, and guarantees uniform etching.Etch temperature and time are respectively 25 DEG C and 2min.
The flatness of silicon wafer and etch-rate are detected after having etched, after the etched processing of liquid 3 can be obtained, flatness It is 0.53 μm, etch-rate is 10 μm/min.Etching solution 3 after circulation etching 5 times, distinguish by the flatness and etch-rate of silicon wafer For 0.58 μm and 9.7 μm/min.
Embodiment 4
The composition of etching solution 4: 30wt% electronic grade nitric acid, 2wt% electronic-stage hydrofluoric acid, 10wt% electronic-grade sulfuric acid, 10wt% electronics Grade phosphoric acid, 2wt% electronic grade acetic acid, 0.01wt% polyoxyethylene sorbitan monooleate, 45.99wt% ultrapure water.
It is by preparation sequence that etching solution 4 is stand-by after mixing, the P-type wafer for being cut into 3cm*4cm is put into homemade It is placed on the top of etching solution 4 in card slot and by card slot, is immersed in silicon wafer in etching solution 4, and magnetic is added in the bottom of etching solution 4 Son is placed on magnetic stirring apparatus and is stirred, and guarantees uniform etching.Etch temperature and time are respectively 25 DEG C and 1min.
The flatness of silicon wafer and etch-rate are detected after having etched, after the etched processing of liquid 4 can be obtained, flatness It is 0.67 μm, etch-rate is 12 μm/min.Etching solution 4 after circulation etching 5 times, distinguish by the flatness and etch-rate of silicon wafer For 0.71 μm and 11.8 μm/min.
Embodiment 5
The composition of etching solution 5: 30wt% electronic grade nitric acid, 2wt% electronic-stage hydrofluoric acid, 10wt% electronic-grade sulfuric acid, 10wt% electronics Grade phosphoric acid, 4wt% electronic grade acetic acid, 0.03wt% polyoxethylene octylphenyl phenol ether -10 and fatty alcohol polyoxyethylene ether mixture, 43.97wt% ultrapure water.
It is by preparation sequence that etching solution 5 is stand-by after mixing, the P-type wafer for being cut into 3cm*4cm is put into homemade It is placed on the top of etching solution 5 in card slot and by card slot, is immersed in silicon wafer in etching solution 5, and magnetic is added in the bottom of etching solution 5 Son is placed on magnetic stirring apparatus and is stirred, and guarantees uniform etching.Etch temperature and time are respectively 25 DEG C and 3min.
The flatness of silicon wafer and etch-rate are detected after having etched, after the etched processing of liquid 5 can be obtained, flatness It is 0.52 μm, etch-rate is 10 μm/min.Etching solution 5 after circulation etching 5 times, distinguish by the flatness and etch-rate of silicon wafer For 0.56 μm and 9.75 μm/min.
Obviously, above-described embodiment is just for the sake of clearly demonstrating made example, and is not the limitation to embodiment. To those of ordinary skill in the art, other various forms of variations or change can also be made on the basis of the above description Dynamic, there is no necessity and possibility to exhaust all the enbodiments.And the obvious changes or variations therefore amplified Within the protection scope of the invention.

Claims (8)

1. a kind of etching solution of Silicon Wafer, which is characterized in that the etching solution main component includes accounting for etching solution total weight 10- The surface of 50% nitric acid, the hydrofluoric acid of 1-5%, the sulfuric acid of 5-20%, the phosphoric acid of 10-30%, the acetic acid of 1-10%, 0.001-3% is living Property agent, the water of 20-50%.
2. the etching solution of Silicon Wafer according to claim 1, which is characterized in that the surfactant is nonionic table Face activating agent, specially polyoxethylene octylphenyl phenol ether -10, fatty alcohol polyoxyethylene ether, polyethenoxy sorbitan list oil The mixture of one or more of acid esters, ethylene oxide propylene oxide block polyether.
3. the etching solution of Silicon Wafer according to claim 1, which is characterized in that the water be at 25 DEG C resistivity >= The ultrapure water of 15.0M Ω * cm.
4. the etching solution of Silicon Wafer according to claim 1, which is characterized in that the nitric acid is electronic grade nitric acid, dense Degree is 68-72%.
5. the etching solution of Silicon Wafer according to claim 1, which is characterized in that the hydrofluoric acid is electron level hydrogen fluorine Acid, concentration 45-60%.
6. the etching solution of Silicon Wafer according to claim 1, which is characterized in that the sulfuric acid is electronic-grade sulfuric acid, dense Degree >=96%.
7. the etching solution of Silicon Wafer according to claim 1, which is characterized in that the phosphoric acid is electron-level phosphoric acid, dense Degree >=85%.
8. the etching solution of Silicon Wafer according to claim 1, which is characterized in that the acetic acid is electronic grade acetic acid, dense Degree >=98%.
CN201811435355.8A 2018-11-28 2018-11-28 A kind of etching solution of Silicon Wafer Pending CN109321253A (en)

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109913222A (en) * 2019-02-18 2019-06-21 湖北兴福电子材料有限公司 A kind of silicon wafer polishing liquid
CN110373719A (en) * 2019-08-13 2019-10-25 湖北兴福电子材料有限公司 A kind of polysilicon etch liquid of high selectivity ratio and preparation method thereof
CN112233967A (en) * 2020-10-15 2021-01-15 扬州扬杰电子科技股份有限公司 Processing method for improving abnormal shedding of back metal and substrate Si
CN112662401A (en) * 2020-11-25 2021-04-16 重庆臻宝实业有限公司 Etching solution for low-resistance silicon product and etching method thereof
CN113072306A (en) * 2021-04-08 2021-07-06 烟台远东精细化工有限公司 Preparation method of electronic grade mixed acid etching solution
CN114350367A (en) * 2021-12-16 2022-04-15 湖北兴福电子材料有限公司 Low-foam etching solution capable of etching uniformly
CN114891509A (en) * 2021-12-14 2022-08-12 湖北兴福电子材料有限公司 High-selectivity buffer oxide etching solution
CN115197706A (en) * 2022-06-27 2022-10-18 徐州鑫晶半导体科技有限公司 Acid etching solution, silicon wafer processing method and wafer packaging method
CN115537202A (en) * 2022-09-28 2022-12-30 重庆臻宝实业有限公司 Etching solution and etching method for etching silicon material micropores

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101130871A (en) * 2007-08-06 2008-02-27 江阴市润玛电子材料有限公司 Fluorine surface etchant for semiconductor and preparation method thereof
WO2011066029A3 (en) * 2009-09-10 2012-05-31 The Regents Of The University Of Michigan Methods of preparing flexible photovoltaic devices using epitaxial liftoff, and preserving the integrity of growth substrates used in epitaxial growth
CN103077889A (en) * 2013-01-14 2013-05-01 陆伟 Method for thinning back surface of wafer

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101130871A (en) * 2007-08-06 2008-02-27 江阴市润玛电子材料有限公司 Fluorine surface etchant for semiconductor and preparation method thereof
WO2011066029A3 (en) * 2009-09-10 2012-05-31 The Regents Of The University Of Michigan Methods of preparing flexible photovoltaic devices using epitaxial liftoff, and preserving the integrity of growth substrates used in epitaxial growth
CN103077889A (en) * 2013-01-14 2013-05-01 陆伟 Method for thinning back surface of wafer

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109913222A (en) * 2019-02-18 2019-06-21 湖北兴福电子材料有限公司 A kind of silicon wafer polishing liquid
CN110373719A (en) * 2019-08-13 2019-10-25 湖北兴福电子材料有限公司 A kind of polysilicon etch liquid of high selectivity ratio and preparation method thereof
CN112233967A (en) * 2020-10-15 2021-01-15 扬州扬杰电子科技股份有限公司 Processing method for improving abnormal shedding of back metal and substrate Si
CN112233967B (en) * 2020-10-15 2024-05-03 扬州扬杰电子科技股份有限公司 Processing method for improving abnormal falling of back metal and substrate Si
CN112662401A (en) * 2020-11-25 2021-04-16 重庆臻宝实业有限公司 Etching solution for low-resistance silicon product and etching method thereof
CN113072306A (en) * 2021-04-08 2021-07-06 烟台远东精细化工有限公司 Preparation method of electronic grade mixed acid etching solution
CN114891509A (en) * 2021-12-14 2022-08-12 湖北兴福电子材料有限公司 High-selectivity buffer oxide etching solution
CN114350367A (en) * 2021-12-16 2022-04-15 湖北兴福电子材料有限公司 Low-foam etching solution capable of etching uniformly
CN115197706A (en) * 2022-06-27 2022-10-18 徐州鑫晶半导体科技有限公司 Acid etching solution, silicon wafer processing method and wafer packaging method
CN115537202A (en) * 2022-09-28 2022-12-30 重庆臻宝实业有限公司 Etching solution and etching method for etching silicon material micropores
CN115537202B (en) * 2022-09-28 2023-09-05 重庆臻宝科技股份有限公司 Etching solution and etching method for etching micropores of silicon material

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