WO2005091347A1 - SOLUTION DE GRAVURE SELECTIVE DE FILM SiN ET METHODE DE GRAVURE - Google Patents

SOLUTION DE GRAVURE SELECTIVE DE FILM SiN ET METHODE DE GRAVURE Download PDF

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Publication number
WO2005091347A1
WO2005091347A1 PCT/JP2005/004494 JP2005004494W WO2005091347A1 WO 2005091347 A1 WO2005091347 A1 WO 2005091347A1 JP 2005004494 W JP2005004494 W JP 2005004494W WO 2005091347 A1 WO2005091347 A1 WO 2005091347A1
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Prior art keywords
ether
solvent
etching solution
etching
mass
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PCT/JP2005/004494
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English (en)
Japanese (ja)
Inventor
Mitsushi Itano
Daisuke Watanabe
Original Assignee
Daikin Industries, Ltd.
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Application filed by Daikin Industries, Ltd. filed Critical Daikin Industries, Ltd.
Publication of WO2005091347A1 publication Critical patent/WO2005091347A1/fr

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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 at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System 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
    • H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
    • H01L21/3105—After-treatment
    • H01L21/311—Etching the insulating layers by chemical or physical means
    • H01L21/31105—Etching inorganic layers
    • H01L21/31111—Etching inorganic layers by chemical means
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K13/00—Etching, surface-brightening or pickling compositions
    • C09K13/04—Etching, surface-brightening or pickling compositions containing an inorganic acid
    • C09K13/08—Etching, surface-brightening or pickling compositions containing an inorganic acid containing a fluorine compound

Definitions

  • the present invention relates to a technique for selectively etching a SiN film formed on a Si substrate, a compound semiconductor substrate, or a glass substrate for a liquid crystal display, and more particularly, to a substrate including a SiON film together with a SiN film. And technology for selectively etching a SiN film.
  • a semiconductor processing process includes a step of selectively removing a certain material with respect to another material.
  • SiN films formed by various CVD methods and SiO films formed by various CVD methods and thermal oxidation methods are generally used as insulating films in various applications.
  • it may be required to selectively etch the SiN film.
  • As an etching method there are wet etching and dry etching. To remove other films without damaging them, a wet etching method is used.
  • a method of wet etching a SiN film generally uses hot phosphoric acid! (Patent Documents 1 and 2).
  • the SiN film can be etched at an etching rate of 100 A / min and the etching rate selectivity of the SiN film and the SiO film can be as high as 100: 1.
  • hot phosphoric acid requires treatment at a high temperature of 140 ° C-180 ° C. At low temperatures below 100 ° C, the SiN film is hardly etched.
  • P (phosphorus) may contaminate the clean room atmosphere, and an alternative process is desired.
  • Patent Document 3 a method of removing a SiN film by using a mixed solution of V or any one of ethylene glycol, glycerol, and diethylene glycol dimethyl ether and dilute hydrofluoric acid is known (Patent Document 3). Using this liquid mixture enables etching at a low temperature (100 ° C. or lower). However, ethylene glycol and water used in Patent Document 3 are not applied as a highly selective etching solution having a very low etching selectivity as shown in Comparative Examples described later (Patent Document 4).
  • Patent Document 1 JP-A-9 45660
  • Patent Document 2 Japanese Patent Application Laid-Open No. 2002-246378
  • Patent Document 3 US Patent 4,269,654
  • Patent Document 4 US Patent No. 3607480
  • An object of the present invention is to achieve etching at a low temperature (100 ° C. or lower) and to etch a SiN film without etching an SiO film! “Highly selective etching chemical for SiN film” and “SiN film” To provide a high selective etching method.
  • the present invention provides a method of forming a SiN film formed on a substrate at a low temperature of 100 ° C or lower using a mixed solution containing hydrogen fluoride, an ether-based solvent, and, if necessary, water. Can be selectively etched with respect to a SiO film, a Si film or a Si substrate, particularly a SiO film.
  • the present invention specifically provides the following etching solution and etching method.
  • An etchant for selectively etching a SiN film containing hydrogen fluoride, an ether-based solvent and a Z or fluorinated ether-based solvent, and if necessary, water.
  • the content of ether solvents and Z or fluorinated ether solvents is 99.9-160% by mass, the content of hydrogen fluoride (HF) is 0.1-30% by mass, and the content of water is 10% by mass or less.
  • Item 4 The etching solution according to any one of Items 1 to 3.
  • the content of ether solvent and / or fluorinated ether solvent is 90-70% by mass, hydrogen fluoride (HF) content is 10-30% by mass, and water content is 10% by mass or less.
  • HF hydrogen fluoride
  • the content of ether solvent and Z or fluorinated ether solvent is 99.9-90% by mass, hydrogen fluoride (HF) content is 0.1-10% by mass, and water content is 3% by mass or less.
  • Item 4. The etching solution according to any one of Items 1 to 3.
  • a substrate including a SiON film together with a SiN film is etched at a temperature of 100 ° C. or less using the etching solution described in any one of Items 1 to 13 above. How to ching.
  • a SiN film formed on a SiO film can be selectively etched at a low temperature of 100 ° C. or less on a substrate such as a semiconductor substrate or a glass substrate.
  • ether solvent and Z or a fluorinated ether solvent may be simply referred to as an ether solvent.
  • ether solvents examples include ethylene glycol dimethyl ether (monoglyme), diethylene glycol dimethyl ether (diglyme), triethylene glycol dimethyl enoate ether (triglyme), 1,2-diethoxyxetane, 1,2-dipropoxyxetane, and dioxo.
  • Sun tetrahydrofuran and the like.
  • formula (1) or (2) the following formula (1) or (2)
  • R and R are the same or different and each have a C 1 -C linear or branched lower alkyl group m 14
  • n an integer of 0-4.
  • Examples of the lower alkyl group having the following include methyl, ethyl, n-propyl, isopropyl, n-butyl, isobutyl, sec-butyl and tert-butyl, preferably methyl, ethyl, n-propyl, isopropyl, and more preferably Is methyl or ethyl, especially methyl.
  • n is an integer of 0-4, preferably an integer of 1-3.
  • ether solvents include (mono-, di-, tri-, tetra-) ethylene glycol dimethyl ether, (mono-, di-, tri-, tetra-) ethylene glycol getyl ether, (mono-, di, tri, tetra-) ethylene glycol di-n- Propyl ether, (mono, di, tri, tetra) ethylene glycol diisopropyl ether, (mono, di, tri, tetra) ethylene glycol di-n-butyl ether, (mono, di, tri, tetra) ethylene glycol diisobutyl ether , (Mono, di, tri, tetra) ethylene glycol di sec-butyl ether, (mono, di, tri, tetra) ethylene glycol ditert-butyl ether, etc., ethylene glycol ether solvents, (mono, di, etc.) , Tri, tetra) propylene
  • the fluorinated ether-based solvent means a solvent obtained by substituting one or more hydrogen atoms and S fluorine atoms in the above-mentioned ether-based solvents, and the fluorine atom is a difference between the alkylene glycol portion and the alkyl ether portion. , Have been introduced, may be.
  • the fluorinated ether solvent is represented by the general formula (If) or (2f):
  • Rf and Rf are the same or different
  • nl represents an integer of 0-4.
  • Rf and Rf contains a fluorine atom
  • nl is an integer of 0-4, preferably an integer of 0-3.
  • n2 is an integer of 0-4, preferably an integer of 0-3.
  • the fluorinated ether solvent has a low toxicity ⁇ C F OCH (trade name "HE-7100”)
  • ethylene daryl glycol dimethyl ether (monoglyme)
  • a high molecular ether solvent such as triethylene glycol dimethyl ether (triglyme) has a high flash point (100 ° C. or higher), and is therefore a preferred solvent from the viewpoint of safety.
  • Patent Document 3 A method of selectively etching a SiN film using a mixed solution of an organic solvent and hydrofluoric acid has been reported (Patent Document 3).
  • This organic solvent has a hydroxyl group.
  • Solvent On the other hand, the raw material organic solvent used in the present invention is characterized in that all the oxygen atoms are esterified, there is no alcoholic or phenolic hydroxyl group, and the ether solvent is a fluorinated ether solvent. Different in that. As shown in the comparative examples of the present specification, the presence of a hydroxyl group has a drawback that the selectivity of the SiN film is reduced.
  • the fluorinated ether-based solvent may be fluorinated to form an alkyl group (Rf m
  • Rf may be a perfluoroalkyl group.
  • the organic solvent containing the compound is not flammable irrespective of whether the alkylene glycol moiety is fluorinated or not, and is therefore preferred from the viewpoint of safety.
  • the etching solution is a solvent in which the ether solvents mentioned above are mixed, and hydrogen fluoride (
  • fluorinated ether-based solvent is mixed with hydrofluoric acid containing water in the composition, it is preferable to use the fluorinated ether-based solvent by mixing with another ether-based solvent from the viewpoint of compatibility with water.
  • the content of the ether solvent and Z or fluorinated ether solvent etching solution of the present invention is usually 99.9 one 60.0 wt%, preferably 99.9 one 70.0% by weight, more preferably 99.9 one 80.0 mass 0/0 It is.
  • the concentration of hydrogen fluoride (HF) contained in the mixed solution is preferably high (for example, 10 to 30% by mass, more preferably 10 to 20% by mass) when the SiN film is etched at a high speed.
  • a low concentration for example, 0.1 to 10% by mass, more preferably 0.1 to 5% by mass is preferable.
  • water is an optional component and may be contained, but may not be contained at all.
  • the water content is usually 10% by mass or less, preferably 5% by mass or less, more preferably 3% by mass or less, further preferably 2% by mass, still more preferably 1% by mass or less, and most preferably 0.5% by mass or less. % Or less. Further, the content of water may be 0% by mass.
  • the concentration of water contained in the etching solution is preferably low when the SiN film is highly selectively etched, and more preferably there is no water at all. Also, when the moisture concentration increases, the etching rate of the SiN film and the SiO film increases, and when the moisture concentration increases too much, the etching rate of the SiO film may be faster than the etching rate of the SiN film. Therefore, the moisture concentration It is possible to adjust the selectivity by adjusting.
  • etching temperature increases the etching rate.
  • the etching selectivity of the SiN film tends to be improved. Therefore, it is preferable to increase the etching temperature in order to increase the etching rate and the selectivity of the SiN film to the SiO film.
  • the temperature is too high, single-wafer processing becomes difficult, and HF gas is released.
  • the required etching rate ratio and etching rate can be adjusted by temperature.
  • a preferred etching temperature is 100 ° C or lower, preferably 20 to 80 ° C, more preferably 20 to 50 ° C, and still more preferably 20 to 30 ° C.
  • the temperature is preferably 100 ° C. or lower.
  • the time required to raise the temperature of the chemical can be shortened, and the temperature control and management are easy.
  • the etching time is generally 0.05-5 minutes, preferably 0.1-2 minutes.
  • the etching method of the present invention includes a method of applying and spraying an etching solution on a substrate to be processed, a method of dipping the substrate in the etching solution, and the like.
  • the above-mentioned SiN film can be formed by various CVD methods of plasma, heat, light, laser, and ion beam. Commonly used methods are the low pressure CVD (LP-CVD) method of the plasma CVD method and the thermal CVD method.
  • LP-CVD low pressure CVD
  • the SiO film described above includes a Si substrate, a thermally oxidized SiO film obtained by thermally oxidizing a Si film,
  • SiO films includes SiO films, chemical SiO films chemically reacted with nitric acid, sulfuric acid, etc., Si substrates, natural oxide films of Si films, and TEOS films formed by various CVD methods of plasma, heat, light, laser, and ion beam.
  • the SiO film does not include a film doped with impurities of BPSG, BSG and AsSG containing boron (B), phosphorus (P) and arsenic (As).
  • the etching solution of the present invention usually has an etching selection ratio of ⁇ SiN film etching speed Z (SiO film etching speed) ⁇ of SiN film of LP-CVD method and SiO film of thermal oxidation method. It is 3 or more, preferably 1.5 or more, more preferably 2.0 or more, still more preferably 2.5 or more, and especially 3 or more.
  • the etchant of the present invention not only selectively etches the SiN film with respect to the SiO film, but also
  • the silicon film or the Si substrate is also selectively etched.
  • the selectivity of the etching solution of the present invention to a Si film or a Si substrate is as follows.
  • the etching selectivity of the SiN film and the Si film ⁇ (etching speed of the SiN film) Z (etching speed of the Si film) ⁇ is usually 10 or more, preferably 100 or more, and more preferably the Si film is completely etched. Preferably not.
  • the etching selectivity of the SiN film and the Si substrate ⁇ (etching rate of the SiN film) / (etching rate of the Si substrate) ⁇ is usually 10 or more, preferably 100 or more, and more preferably the Si substrate is completely etched. What is preferred.
  • examples of the SiN film and the SiO film include a semiconductor substrate, a glass substrate for a display such as a liquid crystal display, a Si substrate, a SiC substrate, and a compound semiconductor substrate such as GaAs, InP, and GaP.
  • a method for preparing an anhydrous etching solution comprising hydrogen fluoride and an ether solvent and Z or a fluorinated ether solvent is as follows. There are a method of absorbing hydrogen fluoride gas into the above ether solvent and Z or a fluorinated ether solvent, and a method of mixing hydrogen fluoride at a temperature of 20 ° C or less and mixing with a liquid. Either method may be used.
  • the hydrous etching solution is prepared by mixing hydrofluoric acid with an ether-based solvent and Z or a fluorinated ether-based solvent to form an etching solution, and forming the hydrogen fluoride and the ether-based solvent and Z or fluorinated ether as described above. Water may be added to the mixture of the system solvents.
  • an etching solution of the present invention is prepared by mixing hydrofluoric acid and an ether-based solvent.
  • the etching solution may be a mixture of hydrogen fluoride or hydrofluoric acid and an ether-based solvent and a solvent containing Z or a fluorinated ether-based solvent.
  • Other surfactants, chelating agents, and anticorrosives may be mixed. .
  • the compounding amount of other components is suppressed to less than 10% by mass.
  • Table 1 shows the etching rates of the etching solution of the present invention, which also has hydrogen fluoride and ether-based solvent power, and the mixed solution composed of a solvent having a hydroxyl group described in Patent Document 3 and hydrogen fluoride. Is shown. The etching characteristics under the same hydrogen fluoride concentration (ma SS %) and the same temperature conditions are shown. As shown in Table 1, as the number of hydroxyl groups becomes 2 ⁇ 1 ⁇ 0 (ethylene glycol ⁇ ethylene glycol monobutyl ether ⁇ ethylene glycol dimethyl ether / comparative example 2 ⁇ comparative example 1 ⁇ example 4), the etching rate selectivity increases. This shows that the mixture is higher, indicating that the mixture of ether-based solvent and HF is superior to the mixture of organic solvent and hydrogen fluoride reported in the literature.
  • Table 2 shows that hydrogen fluoride and ethylene glycol dimethyl ether
  • the etching rate and selectivity of the SiN film by the LP-CVD method and the SiO film by the thermal oxidation method are shown with respect to the partial concentration. As the water concentration increases, the etching rates of the SiN film and the SiO film tend to increase, and the selective etching property of the SiN film tends to decrease.
  • dilute hydrofluoric acid in which water is contained in hydrogen fluoride may be used.
  • water is contained, and only anhydrous hydrogen fluoride is used.
  • the effect of increasing the etching rate due to the increase in the water concentration in the chemical solution is greater than that of the iN film formed by the SiO film. Therefore, it is possible to etch the SiO film and SiN at a constant speed by adjusting the moisture concentration.
  • Table 2 shows the dependence of the water concentration in a mixed solution of hydrogen fluoride and ethylene glycol dimethyl ether at 60 ° C. on the etching rate and the rate selectivity of the SiN film of the LP-CVD method and the SiO of the thermal oxidation method. Show.
  • Table 3 shows the ratio of the etching rate to the etching rate when the concentration of hydrogen fluoride contained in the mixture was changed.
  • a high concentration is preferable.
  • a low concentration is preferable.
  • Table 3 shows the dependence of the etching rate and the etching rate selectivity on the etching temperature.
  • the temperature of the mixed solution of hydrogen fluoride and ethylene glycol dimethyl ether increases, the etching rate of the SiN film and the SiO film increases.
  • the etching rate ratio tends to increase. Therefore, the etching rate and the selectivity can be adjusted by the etching temperature.
  • the etching rate of the SiN film is 71 A / min, and the selectivity is 23. Is obtained. It has become clear that SiN films can be etched with a higher selectivity than conventional etchants.

Abstract

Il est prévu une méthode de réalisation de gravure humide à faible température sélective d'un film SiN contre un film SiO et Si. En outre, il est prévu une solution pour gravure sélective d'un film SiN, comprenant du fluoride d'hydrogène, un solvant d'éther et/ou un solvant d'éther fluoré optionnellement avec de l'eau.
PCT/JP2005/004494 2004-03-19 2005-03-15 SOLUTION DE GRAVURE SELECTIVE DE FILM SiN ET METHODE DE GRAVURE WO2005091347A1 (fr)

Applications Claiming Priority (2)

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JP2004080567A JP2005268605A (ja) 2004-03-19 2004-03-19 ＳｉＮ膜の選択エッチング液及びエッチング方法
JP2004-080567 2004-03-19

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2009542022A (ja) * 2006-07-03 2009-11-26 フラウンホッファー−ゲゼルシャフト・ツァー・フォデラング・デル・アンゲワンテン・フォーシュング・エー．ファウ． 固形物から物質を除去するための液体ジェットガイド式エッチング法およびその使用

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2006126583A1 (fr) * 2005-05-25 2006-11-30 Daikin Industries, Ltd. Agent de gravure pour substrats ayant des couches bpsg et sod
TWI562234B (en) 2006-12-21 2016-12-11 Entegris Inc Compositions and methods for the selective removal of silicon nitride
JP5782279B2 (ja) * 2011-01-20 2015-09-24 株式会社Ｓｃｒｅｅｎホールディングス 基板処理方法および基板処理装置
JP7246990B2 (ja) 2019-03-26 2023-03-28 株式会社東芝 エッチング液、及びエッチング方法

Citations (7)

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JPS4941716B1 (fr) * 1968-12-28 1974-11-11
JPS60137024A (ja) * 1983-12-26 1985-07-20 Matsushita Electronics Corp 窒化珪素膜のエツチング方法
JPH03268327A (ja) * 1990-03-16 1991-11-29 Sony Corp 窒化シリコン膜のエッチング方法
JPH06295898A (ja) * 1993-02-24 1994-10-21 Advanced Chem Syst Internatl Inc 有機金属化合物および有機ケイ素化合物の残留物と損傷酸化物を選択的に除去するための方法
JPH11121442A (ja) * 1997-09-18 1999-04-30 Internatl Business Mach Corp <Ibm> 窒化ケイ素のエッチング方法およびそれに適したエッチング組成物
JP2001100436A (ja) * 1999-09-28 2001-04-13 Mitsubishi Gas Chem Co Inc レジスト剥離液組成物
JP2004140197A (ja) * 2002-10-17 2004-05-13 Nec Electronics Corp 半導体装置の製造方法および半導体装置

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS4941716B1 (fr) * 1968-12-28 1974-11-11
JPS60137024A (ja) * 1983-12-26 1985-07-20 Matsushita Electronics Corp 窒化珪素膜のエツチング方法
JPH03268327A (ja) * 1990-03-16 1991-11-29 Sony Corp 窒化シリコン膜のエッチング方法
JPH06295898A (ja) * 1993-02-24 1994-10-21 Advanced Chem Syst Internatl Inc 有機金属化合物および有機ケイ素化合物の残留物と損傷酸化物を選択的に除去するための方法
JPH11121442A (ja) * 1997-09-18 1999-04-30 Internatl Business Mach Corp <Ibm> 窒化ケイ素のエッチング方法およびそれに適したエッチング組成物
JP2001100436A (ja) * 1999-09-28 2001-04-13 Mitsubishi Gas Chem Co Inc レジスト剥離液組成物
JP2004140197A (ja) * 2002-10-17 2004-05-13 Nec Electronics Corp 半導体装置の製造方法および半導体装置

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2009542022A (ja) * 2006-07-03 2009-11-26 フラウンホッファー−ゲゼルシャフト・ツァー・フォデラング・デル・アンゲワンテン・フォーシュング・エー．ファウ． 固形物から物質を除去するための液体ジェットガイド式エッチング法およびその使用

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