CN102827707A - Plasma etching residue cleaning fluid - Google Patents
Plasma etching residue cleaning fluid Download PDFInfo
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- CN102827707A CN102827707A CN2011101629587A CN201110162958A CN102827707A CN 102827707 A CN102827707 A CN 102827707A CN 2011101629587 A CN2011101629587 A CN 2011101629587A CN 201110162958 A CN201110162958 A CN 201110162958A CN 102827707 A CN102827707 A CN 102827707A
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Abstract
The invention discloses a fluorine-containing plasma etching residue cleaning fluid in the semiconductor industry. The cleaning fluid composition contains 5-75% of organic solvent, 10-50% of water, 0.1-20% of fluoride, 0.1-20% of organic amine, 0.1-10% of amino acid, 0.01-5% (preferably 0.05-2%) of carbamidines and 0.01-5% of benzotriazole and derivatives thereof. The cleaning fluid composition can effectively clean plasma etching residues in a semiconductor manufacturing process, has lower etching rate on a base material such as a low-dielectric material (SiO2 and PETEOS (plasma-enhanced tetraethoxysilane)) and some metal (such as Ti, Al and Cu), simultaneously has the capability of inhibiting galvanic corrosion of aluminum-copper alloy, and has excellent application prospects in the semiconductor chip cleaning and other micro-electronic fields.
Description
Technical field
The present invention relates to a kind of plasma etching residual washing liquid.
Background technology
In the semiconductor components and devices manufacturing processed, the coating of photoresist layer, exposure and imaging are necessary process steps to the pattern manufacturing of components and parts.Before last (promptly after coating, imaging, ion implantation and the etching at photoresist layer) of patterning carried out next process step, the residue of photoresist layer material need thoroughly be removed.So far the general two-step approach (dry ashing and wet etching) of using is removed this layer photoresistance tunic in semi-conductor industry.The first step utilizes dry ashing to remove the major part of photoresist layer (PR); Second step utilized composite corrosion inhibitor wet etching/cleaning to remove and wash remaining photoresist layer, and its step is generally scavenging solution cleaning/rinsing/rinsed with deionized water.In this process, can only remove residual polymkeric substance photoresist layer and inorganics, and can not attack infringement metal level such as aluminium lamination.
Typical scavenging solution has following several kinds in the prior art: amine scavenging solution, semi-aqueous amido (non-azanol class) scavenging solution and fluorochemical based cleaning liquid.Wherein preceding two based cleaning liquids need at high temperature to clean, and generally between 60 ℃ to 80 ℃, have the problem bigger to corrosion of metal speed; Though and existing fluorochemical based cleaning liquid can clean under lower temperature (room temperature to 50 ℃); But still exist various shortcomings; For example can not control the corrosion of metal and non-metallic substrate simultaneously; Cause the change of channel characteristics size after the cleaning easily, thereby change semiconductor structure; Owing to its big etch-rate, the cleaning operation window is smaller etc. on the other hand.US 6; 828,289 disclosed cleaning liquid compositions comprise: acidic buffer, organic polar solvent, fluorine-containing material and water, and the pH value is between 3～7; Acidic buffer wherein is made up of organic carboxyl acid or polyprotonic acid and pairing ammonium salt, and proportion of composing is between 10: 1 to 1: 10.Like US 5,698,503 disclose fluorine-containing scavenging solution, but make spent glycol in a large number, and the viscosity of its scavenging solution and surface tension are all very big, thereby influence cleaning performance.Like US 5,972,862 disclose the cleaning combination of fluorine-containing material, and it comprises fluorine-containing material, inorganic or organic acid, quaternary ammonium salt and organic polar solvent, and pH is 7～11, because its cleaning performance is not very stable, have various problem.For the problem of metal aluminum bronze stream electrocorrosion, preceding two based cleaning liquids, the main employing reduced in the scavenging solution moisture content and increased the solvent rinsing and solve, and the content that reduces water is unfavorable for the removal of inorganic residue.And the fluorine based cleaning liquid is shorter relatively owing to the time of its production and use, and the research of this respect is still waiting further exploration.
Although therefore disclosed the certain cleaning fluid composition; But need and need prepare more recently one type of more suitably cleaning combination or system; Adapt to new cleaning requirement, more friendly such as environment, low defect level, low etching rate, big action pane and the electrocorrosion of inhibition aluminum bronze stream or the like.
Summary of the invention
The objective of the invention is in order how to solve safety, healthy and effectively clean semi-conductor industry ionic medium etch residue, and a kind of cleaning liquid composition safely and effectively is provided.
The present invention is a kind of cleaning liquid composition that is used for semi-conductor industry ionic medium etch residue, and it comprises organic solvent, water, fluorochemical, organic amine, amino acid, guanidine class and benzotriazole and verivate thereof.Wherein the composite anticorrosive metal system of guanidine class and benzotriazole and verivate thereof has suppressed the stream electrocorrosion of metal aluminum bronze more effectively, and described cleaning liquid composition weight percent content is:
A) organic solvent 5%～75%;
B) water 10%～50%;
C) fluorochemical 0.1%～20%;
D) organic amine 0.1%～20%;
E) amino acid 0.1%～10%;
F) the guanidine class 0.01%～5%, and preferred 0.05%～2%;
G) benzotriazole and verivate 0.01%～5% thereof, above content is weight percent content.
Organic solvent of the present invention is preferable is in sulfoxide, sulfone, imidazolidone, pyrrolidone, imidazolone, acid amides and the ether one or more.Described sulfoxide is preferable is in DMSO 99.8MIN., diethyl sulfoxide and the first and second basic sulfoxides one or more; Described sulfone is preferable is in methyl sulfone, ethyl sulfone and the tetramethylene sulfone one or more; What described imidazolidone was preferable is 2-imidazolidone, 1,3-dimethyl--2-imidazolidone and 1, one or more in 3-diethylammonium-2-imidazolidone; Described pyrrolidone is preferable is in N-Methyl pyrrolidone, N-ethyl pyrrolidone, N-cyclohexyl pyrrolidone and the N-hydroxyethyl-pyrrolidone one or more; What described imidazolone was preferable is 1,3-dimethyl--2-imidazolone; What described acid amides was preferable is N, N,N-DIMETHYLACETAMIDE; Described ether is preferable is in ethylene glycol monoalkyl ether, Diethylene Glycol monoalky lether, propylene-glycol monoalky lether, dipropylene glycol monoalky lether and the tripropylene glycol monoalky lether one or more.Wherein, described ethylene glycol monoalkyl ether is preferable is in ethylene glycol monomethyl ether, ethylene glycol monoethyl ether and the ethylene glycol monobutyl ether one or more; Described Diethylene Glycol monoalky lether is preferable is in diethylene glycol monomethyl ether, diethylene glycol monoethyl ether and the diethylene glycol monobutyl ether one or more; Described propylene-glycol monoalky lether is preferable is in propylene glycol monomethyl ether, dihydroxypropane single-ether and the propylene glycol monobutyl ether one or more; Described dipropylene glycol monoalky lether is preferable is in dipropylene glycol monomethyl ether, dipropylene glycol list ether and the dipropylene glycol monobutyl ether one or more; What described tripropylene glycol monoalky lether was preferable is the tripropylene glycol monomethyl ether.What the content of described solvent was preferable is mass percent 5～75%.
Fluorochemical of the present invention preferably is the salt that hydrogen fluoride or hydrogen fluoride and alkali form.This alkali can be ammoniacal liquor, quaternary ammonium hydroxide and hydramine.Fluorochemical preferably is hydrogen fluoride (HF), Neutral ammonium fluoride (NH
4F), matt salt (NH
4HF
2), Methanaminium, N,N,N-trimethyl-, fluoride (N (CH3)
4F) or trihydroxyethyl Neutral ammonium fluoride NCH2OH
3Among the HF one or more.What the content of described fluorochemical was preferable is mass percent 0.1～20%.
The present invention also can further contain water.
Organic amine of the present invention is diethylenetriamine, pentamethyl-diethylenetriamine, polyethylene polyamine, ethamine, diethylamine, triethylamine, tripropyl amine; N; N-dimethylethanolamine, N, N-methylethyl thanomin, N methyldiethanol amine and trolamine one or more.One or more of preferred pentamethyl-diethylenetriamine, triethylamine and trolamine.What the content of described organic amine was preferable is mass percent 0.1～20%.
Amino acid of the present invention is 2-Padil, 2-benzaminic acid, iminodiethanoic acid, one or more in nitrilotriacetic acid(NTA) or the YD 30.Preferred 2-Padil and iminodiethanoic acid.What content of amino acids of the present invention was preferable is mass percent 0.1～10%.
Guanidine class of the present invention is meant the material that contains guanidine radicals.So-called guanidine radicals is meant that a carbon atom is connected with three nitrogen-atoms, and one of them nitrogen-atoms links to each other with carbon with two keys, and all the other two continuous with singly-bound.Shown in 1:
Formula 1
Preferably be tetramethyl guanidine, Guanidinium carbonate, guanidine acetate, 3-guanidine radicals propionic acid, polyhexamethylene guanidine and to guanidinobenzoic acid.What the content of guanidine class of the present invention was preferable is mass percent 0.01%～5%, preferred 0.05%～2%.
Benzotriazole corrosion inhibitor described in the present invention is one or more in benzotriazole, methyl benzotriazazole, 1-hydroxy benzo triazole, the 5-carboxy benzotriazole.
Positive progressive effect of the present invention is: cleaning liquid composition of the present invention can play a role in the bigger scope of temperature; Generally in room temperature to 55 ℃ scope; And can be used for very wide field, such as batch immersion type/batch rotary/monolithic is rotary, has adopted the composite anticorrosive metal system of guanidine class and benzotriazole and verivate thereof; Suppressed the stream electrocorrosion of metal aluminum bronze more effectively, bigger rinsing window is provided.
Cleaning liquid composition of the present invention is clean metal and semiconductor fabrication ionic medium etch residue effectively also, and can not corrode SiO
2, ion strengthen tetraethoxysilane silicon-dioxide (PETEOS), silicon, low dielectric material and some metallicses (like Ti, Al, Cu).
Embodiment
Come further to set forth the present invention through embodiment below.Simple mixing of component according to table 1 is enumerated allotted solution.
Table 1: embodiment 1～26
We have selected for use, and some embodiment have carried out performance test in the last table, and the result sees the following form.
The guide look of table 2 part embodiment The performance test results
The rate of metal corrosion testing method of solution:
1) utilize Napson four-point probe appearance to test the resistance initial value (Rs1) of the blank silicon chip of 4*4cm aluminium;
2) the blank silicon chip of this 4*4cm aluminium is immersed in advance in the solution of constant temperature to 35 ℃ 30 minutes;
3) take out the blank silicon chip of this 4*4cm aluminium, use washed with de-ionized water, high pure nitrogen dries up, and utilizes the resistance value (Rs2) of the blank silicon chip of Napson four-point probe appearance test 4*4cm aluminium again;
4) repeated for the second and the 3rd step and test once, resistance value is designated as Rs3;
5) be input to suitable procedure to above-mentioned resistance value and soak time and can calculate its erosion rate.
The nonmetal erosion rate testing method of solution:
1) utilize the Nanospec6100 thickness tester to test the thickness (T1) of 4*4cm PETEOS silicon chip;
2) this 4*4cmPETEOS silicon chip is immersed in advance in the solution of constant temperature to 35 ℃ 30 minutes;
3) take out this 4*4cmPETEOS silicon chip, use washed with de-ionized water, high pure nitrogen dries up, and utilizes the thickness (T2) of Nanospec6100 thickness tester test 4*4cmPETEOS silicon chip again;
4) the second and the 3rd step of repetition tests a thickness again and is designated as T3;
5) be input to suitable procedure to above-mentioned one-tenth-value thickness 1/10 and soak time and can calculate its erosion rate.
The method that wafer cleans:
1) wafer to be cleaned is put in advance the solution of constant temperature to 35 ℃;
The principle of 2) soaking 30 minutes according to metal wire immersion 20 minutes, passage and metal gasket is soaked wafer;
3) after soak time arrives, take out this wafer, use washed with de-ionized water, after high pure nitrogen dries up; Send SEM test.
From table 2, can find out: cleaning liquid composition of the present invention during semi-conductor is processed used metal (like metallic aluminium) and nonmetal (like PETEOS) can not corrode basically, its erosion rate is all less than the common desired 2 dust PMs of semi-conductor industry.Clean discovery with this solution article on plasma etch residue, its plasma etching residues all is removed, and does not have corroding metal and nonmetal.
To sum up, advantage of the present invention is:
1. the cleansing power of solution is strong, can clean metal wire (Metal)/passage (Via)/metal gasket (Pad) wafer
2. can control metal and nonmetallic erosion rate simultaneously,
3. have the ability that suppresses the electrocorrosion of aluminum-copper alloy stream, bigger rinsing window is provided
4. bigger action pane can be applicable to immersion type (wet Batch)/batch rotating spraying formula (Batch-spray)/monolithic rotary (single wafer tool) in batches simultaneously.
Claims (16)
1. the scavenging solution of a plasma etching residues, it comprises: organic solvent, water, fluorochemical, organic amine, amino acid, guanidine class and benzotriazole and verivate thereof.
2. scavenging solution according to claim 1 is characterized in that the content of said organic solvent is 5～75wt%; The content of said water is 10～50wt%; The content of said fluorochemical is 0.1～20wt%; The content of said organic amine is 0.1～20wt%; Said content of amino acids is 0.1～10wt%; The content of said guanidine class is 0.01～5wt%; The content of said benzotriazole and verivate thereof is 0.01～5wt%.
3. like the said scavenging solution of claim 2, it is characterized in that the content of said guanidine class is 0.05～2wt%.
4. scavenging solution according to claim 1 is characterized in that, said organic solvent is to be selected from sulfoxide, sulfone, imidazolidone, pyrrolidone, imidazolone, acid amides and the ether one or more.
5. like the said scavenging solution of claim 4, it is characterized in that said sulfoxide is one or more in DMSO 99.8MIN., diethyl sulfoxide and the first and second basic sulfoxides; Said sulfone is one or more in methyl sulfone, ethyl sulfone and the tetramethylene sulfone; Said imidazolidone is a 2-imidazolidone, 1,3-dimethyl--2-imidazolidone and 1, one or more in 3-diethylammonium-2-imidazolidone; Said pyrrolidone is one or more in N-Methyl pyrrolidone, N-ethyl pyrrolidone, N-cyclohexyl pyrrolidone and the N-hydroxyethyl-pyrrolidone; Said imidazolone is 1,3-dimethyl--2-imidazolone; Said acid amides is N, N,N-DIMETHYLACETAMIDE; Said ether is one or more in ethylene glycol monoalkyl ether, Diethylene Glycol monoalky lether, propylene-glycol monoalky lether, dipropylene glycol monoalky lether and the tripropylene glycol monoalky lether.
6. like the said scavenging solution of claim 5, it is characterized in that said ethylene glycol monoalkyl ether is one or more in ethylene glycol monomethyl ether, ethylene glycol monoethyl ether and the ethylene glycol monobutyl ether; Said Diethylene Glycol monoalky lether is one or more in diethylene glycol monomethyl ether, diethylene glycol monoethyl ether and the diethylene glycol monobutyl ether; Said propylene-glycol monoalky lether is one or more in propylene glycol monomethyl ether, dihydroxypropane single-ether and the propylene glycol monobutyl ether; Said dipropylene glycol monoalky lether is one or more in dipropylene glycol monomethyl ether, dipropylene glycol list ether and the dipropylene glycol monobutyl ether; Said tripropylene glycol monoalky lether is the tripropylene glycol monomethyl ether.
7. scavenging solution according to claim 1 is characterized in that, said fluorochemical is the salt that hydrogen fluoride or hydrogen fluoride and alkali form.
8. like the said scavenging solution of claim 7, it is characterized in that said alkali is ammoniacal liquor, quaternary ammonium hydroxide and hydramine.
9. like the said scavenging solution of claim 7, it is characterized in that said fluorochemical is hydrogen fluoride, Neutral ammonium fluoride, matt salt, Methanaminium, N,N,N-trimethyl-, fluoride or trihydroxyethyl Neutral ammonium fluoride NCH2OH
3Among the HF one or more.
10. scavenging solution according to claim 1; It is characterized in that; Said organic amine is diethylenetriamine, pentamethyl-diethylenetriamine, polyethylene polyamine, ethamine, diethylamine, triethylamine, tripropyl amine; N, N-dimethylethanolamine, N, N-methylethyl thanomin, N methyldiethanol amine and trolamine one or more.
11., it is characterized in that said organic amine is one or more of pentamethyl-diethylenetriamine, triethylamine and trolamine like the said scavenging solution of claim 10.
12. scavenging solution is characterized in that according to claim 1, said amino acid is 2-Padil, 2-benzaminic acid, iminodiethanoic acid, one or more in nitrilotriacetic acid(NTA) or the YD 30.
13., it is characterized in that said amino acid is 2-Padil and iminodiethanoic acid like the said scavenging solution of claim 12.
14. scavenging solution is characterized in that according to claim 1, said guanidine class is the material that contains guanidine radicals; So-called guanidine radicals is that a carbon atom is connected with three nitrogen-atoms; And one of them nitrogen-atoms links to each other with carbon with two keys, and all the other two are continuous with singly-bound, shown in 1:
Formula 1.
15., it is characterized in that said guanidine class is tetramethyl guanidine, Guanidinium carbonate, guanidine acetate, 3-guanidine radicals propionic acid, polyhexamethylene guanidine and to guanidinobenzoic acid like the said scavenging solution of claim 14.
16. scavenging solution is characterized in that according to claim 1, said benzotriazole and verivate thereof are one or more in benzotriazole, methyl benzotriazazole, 1-hydroxy benzo triazole, the 5-carboxy benzotriazole.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011101629587A CN102827707A (en) | 2011-06-16 | 2011-06-16 | Plasma etching residue cleaning fluid |
| PCT/CN2012/000766 WO2012171324A1 (en) | 2011-06-16 | 2012-06-04 | Solution for removing plasma etching residue |
| TW101120380A TW201300523A (en) | 2011-06-16 | 2012-06-07 | Solution for removing plasma etching residue |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011101629587A CN102827707A (en) | 2011-06-16 | 2011-06-16 | Plasma etching residue cleaning fluid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102827707A true CN102827707A (en) | 2012-12-19 |
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ID=47331021
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011101629587A Pending CN102827707A (en) | 2011-06-16 | 2011-06-16 | Plasma etching residue cleaning fluid |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103695190A (en) * | 2013-12-31 | 2014-04-02 | 镇江市港南电子有限公司 | Novel silicon wafer cleaning liquid |
| CN104195576A (en) * | 2014-09-10 | 2014-12-10 | 昆山欣谷微电子材料有限公司 | Dry etching cleaning and stripping protective liquid |
| CN107678253A (en) * | 2017-09-26 | 2018-02-09 | 合肥新汇成微电子有限公司 | A kind of cleaning fluid for semiconductor crystal wafer plasma etch residues |
| CN108138334A (en) * | 2015-07-14 | 2018-06-08 | 富士胶片电子材料美国有限公司 | Cleaning compositions and its application method |
| CN108779419A (en) * | 2015-12-25 | 2018-11-09 | 荒川化学工业株式会社 | The cleaning method of cleaning agent for electronic materials composition, cleaning agent stoste and electronic material |
| CN109541897A (en) * | 2018-12-14 | 2019-03-29 | 江苏艾森半导体材料股份有限公司 | A kind of low corrosion aluminum steel cleaning solution |
| CN112424327A (en) * | 2018-07-20 | 2021-02-26 | 恩特格里斯公司 | Cleaning compositions containing corrosion inhibitors |
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| CN101597548A (en) * | 2008-06-06 | 2009-12-09 | 安集微电子科技(上海)有限公司 | A kind of plasma etching residual washing liquid |
| CN101955852A (en) * | 2009-07-13 | 2011-01-26 | 安集微电子（上海）有限公司 | Cleaning solution for plasma etching residues |
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| CN101412950A (en) * | 2007-10-19 | 2009-04-22 | 安集微电子（上海）有限公司 | Cleaning liquid for plasma etching residue |
| CN101597548A (en) * | 2008-06-06 | 2009-12-09 | 安集微电子科技(上海)有限公司 | A kind of plasma etching residual washing liquid |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103695190A (en) * | 2013-12-31 | 2014-04-02 | 镇江市港南电子有限公司 | Novel silicon wafer cleaning liquid |
| CN103695190B (en) * | 2013-12-31 | 2016-06-08 | 江苏美科硅能源有限公司 | Silicon chip cleaning liquid |
| CN104195576A (en) * | 2014-09-10 | 2014-12-10 | 昆山欣谷微电子材料有限公司 | Dry etching cleaning and stripping protective liquid |
| CN108138334A (en) * | 2015-07-14 | 2018-06-08 | 富士胶片电子材料美国有限公司 | Cleaning compositions and its application method |
| JP2018528284A (en) * | 2015-07-14 | 2018-09-27 | フジフイルム エレクトロニック マテリアルズ ユー．エス．エー．， インコーポレイテッド | Cleaning composition and method of use thereof |
| US10619126B2 (en) | 2015-07-14 | 2020-04-14 | Fujifilm Electronic Materials U.S.A., Inc. | Cleaning compositions and methods of use therefor |
| CN108779419A (en) * | 2015-12-25 | 2018-11-09 | 荒川化学工业株式会社 | The cleaning method of cleaning agent for electronic materials composition, cleaning agent stoste and electronic material |
| CN107678253A (en) * | 2017-09-26 | 2018-02-09 | 合肥新汇成微电子有限公司 | A kind of cleaning fluid for semiconductor crystal wafer plasma etch residues |
| CN112424327A (en) * | 2018-07-20 | 2021-02-26 | 恩特格里斯公司 | Cleaning compositions containing corrosion inhibitors |
| US11149235B2 (en) | 2018-07-20 | 2021-10-19 | Entegris, Inc. | Cleaning composition with corrosion inhibitor |
| CN109541897A (en) * | 2018-12-14 | 2019-03-29 | 江苏艾森半导体材料股份有限公司 | A kind of low corrosion aluminum steel cleaning solution |
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Application publication date: 20121219 |