WO2022035111A1 - Verre résistant au plasma et procédé de fabrication de celui-ci - Google Patents

Verre résistant au plasma et procédé de fabrication de celui-ci Download PDF

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Publication number
WO2022035111A1
WO2022035111A1 PCT/KR2021/010136 KR2021010136W WO2022035111A1 WO 2022035111 A1 WO2022035111 A1 WO 2022035111A1 KR 2021010136 W KR2021010136 W KR 2021010136W WO 2022035111 A1 WO2022035111 A1 WO 2022035111A1
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WO
WIPO (PCT)
Prior art keywords
plasma
glass
resistant
mol
fluorine
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PCT/KR2021/010136
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English (en)
Korean (ko)
Inventor
김대근
석혜원
나혜인
이문기
이경민
Original Assignee
아이원스 주식회사
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Priority claimed from KR1020210098388A external-priority patent/KR102608654B1/ko
Application filed by 아이원스 주식회사 filed Critical 아이원스 주식회사
Publication of WO2022035111A1 publication Critical patent/WO2022035111A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B5/00—Melting in furnaces; Furnaces so far as specially adapted for glass manufacture
    • C03B5/16—Special features of the melting process; Auxiliary means specially adapted for glass-melting furnaces
    • C03B5/18—Stirring devices; Homogenisation
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/083—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound
    • C03C3/085—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound containing an oxide of a divalent metal
    • C03C3/087—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound containing an oxide of a divalent metal containing calcium oxide, e.g. common sheet or container glass
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C4/00—Compositions for glass with special properties
    • C03C4/20—Compositions for glass with special properties for chemical resistant glass

Definitions

  • An embodiment of the present invention relates to a plasma-resistant glass and a method for manufacturing the same.
  • a plasma etching process is being applied in the manufacture of semiconductors and/or displays. Recently, as the nano process is applied, the difficulty of etching is increased and the internal parts of the process chamber exposed to the high-density plasma environment have corrosion resistance oxide-based ceramics such as alumina (Al 2 O 3 ) and yttria (Y 2 O 3 ). It is mainly used.
  • An object to be solved according to an embodiment of the present invention is to provide a plasma glass having improved plasma resistance and a method for manufacturing the same.
  • the method of manufacturing a plasma glass comprises the steps of preparing a plasma glass raw material by mixing SiO 2 powder, Al 2 O 3 precursor, CaO precursor and Y-based compound powder; melting the plasma glass raw material in an oxidizing atmosphere; Rapid cooling of the molten plasma-resistant glass material; and heat-treating and annealing the rapidly cooled resultant at a temperature higher than the glass transition temperature (Tg) to obtain a plasma-resistant glass, wherein the obtained plasma-resistant glass is SiO 2 40 to 75 mol%, Al 2 O 3 5 to 20 mol%, CaO 5 to 30 mol%, and a plasma-resistant Y-based compound may contain 0.01 to 10 mol%.
  • the Al 2 O 3 precursor may include Al(OH) 3 powder, and the CaO precursor may include a CaCO 3 powder.
  • the Y-based compound may include YF 3 , YOF or Y(NO 3 ) 3 ⁇ 6H 2 O.
  • the obtained plasma glass may contain 4 to 6 At% of fluorine (F).
  • the obtained plasma glass may contain 1-3 At% of nitrogen (N).
  • the obtained plasma-resistant glass is a glass used in a mixed plasma environment of fluorine and argon (Ar), and the obtained plasma-resistant glass has an etching rate of 5 nm/min to 10 nm with respect to a mixed plasma of fluorine and argon It can have a plasma resistance of /min.
  • the melting step may be performed at a temperature of 1300 °C to 1800 °C.
  • Annealing at a temperature of 700°C to 1000°C may be further included between the melting step and the rapid cooling step.
  • the glass transition temperature (Tg) of the obtained plasma-resistant glass may be 700 °C ⁇ 900 °C.
  • the softening point (Tdsp) of the obtained plasma glass may be 800 °C ⁇ 1000 °C.
  • Plasma glass according to an embodiment of the present invention contains SiO 2 40 to 75 mol%, Al 2 O 3 5 to 20 mol%, CaO 5 to 30 mol% and plasma-resistant Y-based compound 0.01 to 10 mol% can do.
  • the Y-based compound may include YF 3 , YOF or YN.
  • An embodiment of the present invention provides a plasma-resistant glass with improved plasma resistance and a method for manufacturing the same.
  • an embodiment of the present invention provides a plasma glass having a plasma resistance with an etching rate of 5 nm/min to 10 nm/min with respect to a mixed plasma of fluorine and argon, and a method for manufacturing the same.
  • FIG. 1 is a flowchart illustrating a method of manufacturing a plasma-resistant glass according to an embodiment of the present invention.
  • Figures 2a and 2b is a table showing the composition ratio for the manufacture of plasma-resistant glass according to an embodiment of the present invention.
  • Figures 3a to 3d is a photograph showing a plasma-resistant glass according to an embodiment of the present invention.
  • Figure 4 is a table showing the atomic % in the mixture of plasma-resistant glass raw material and plasma-resistant glass according to an embodiment of the present invention.
  • FIG. 5 is a table showing the thermal properties of the plasma glass according to an embodiment of the present invention.
  • Figure 6 is a photograph showing the plasma characteristics of the plasma-resistant glass according to an embodiment of the present invention.
  • the term “and/or” includes any one and all combinations of one or more of those listed items.
  • the terminology used in this specification is used to describe specific embodiments, and is not intended to limit the present invention.
  • the singular form may include the plural form unless the context clearly dictates otherwise.
  • “comprise, include” and/or “comprising, including” refer to the referenced shapes, numbers, steps, actions, members, elements, and/or groups thereof. It specifies the presence and does not exclude the presence or addition of one or more other shapes, numbers, movements, members, elements and/or groups.
  • first, second, etc. are used herein to describe various members, parts, regions, layers and/or parts, these members, parts, regions, layers, and/or parts are limited by these terms so that they It is self-evident that These terms are used only to distinguish one member, component, region, layer or portion from another region, layer or portion. Accordingly, a first member, component, region, layer, or portion described below may refer to a second member, component, region, layer or portion without departing from the teachings of the present invention.
  • FIG. 1 there is shown a flowchart for a method of manufacturing a plasma-resistant glass according to an embodiment of the present invention.
  • the plasma glass manufacturing method is a plasma glass raw material preparation step (S1), melting step (S2), annealing step (S3), cooling step (S4) and It may include a plasma glass obtaining step (S5).
  • SiO 2 powder, Al 2 O 3 precursor powder, CaO precursor powder and Y-based compound powder may be mixed to prepare a plasma glass raw material.
  • the Al 2 O 3 precursor powder may include Al(OH) 3 powder
  • the CaO precursor powder may include CaCO 3 powder
  • the Y-based compound powder may include YF 3 powder, YOF powder, or Y(NO 3 ) 3 .6H 2 O powder.
  • the plasma glass raw material may be melted in an oxidizing atmosphere.
  • the melting step may be performed at a temperature of about 1300° C. to about 1800° C. in an oxidizing atmosphere.
  • the molten plasma-resistant glass material may be annealed in an oxidizing atmosphere (optional).
  • the annealing step may be performed at a temperature of about 700° C. to about 1000° C. in an oxidizing atmosphere.
  • the annealed plasma-resistant glass material may be rapidly cooled.
  • a plasma glass can be obtained by heat-treating and annealing the rapidly cooled product at a temperature higher than the glass transition temperature (Tg).
  • the glass transition temperature (Tg) of the obtained plasma glass may be about 700 °C ⁇ about 900 °C.
  • the obtained plasma glass may have a softening point (Tdsp) of approximately 800°C to approximately 1000°C.
  • the plasma-resistant glass obtained is from about 40 mol% to about 75 mol% of SiO 2 , about 5 mol% to about 20 mol% of Al 2 O 3 , about 5 mol% to about 30 mol% of CaO and plasma resistance It may contain about 0.01 mol% to about 10 mol% of the Y-based compound.
  • the obtained plasma glass may contain about 4 At% to about 6 At% of fluorine (F).
  • the obtained plasma glass may contain about 1 to about 3 At% nitrogen (N).
  • the obtained plasma-resistant glass is a glass used in a mixed plasma environment of fluorine and argon (Ar), and the obtained plasma-resistant glass has an etching rate of about 5 nm/min with respect to a mixed plasma of fluorine and argon ⁇ 10 nm/min. More specifically, the obtained plasma-resistant glass may have an etching rate of about 8.0 nm/min to about 8.3 nm/min with respect to a mixed plasma of fluorine and argon.
  • the plasma glass raw material was mixed using a dry mixing method.
  • the total amount of chemical components was placed in a weight of 100 g, and the plasma glass raw material was mixed for about 1 hour by a zirconia ball milling method.
  • 100 g of raw material: 300 g of zirconia balls (weight ratio 1:3) was dry-mixed with the plasma glass raw material, and then dried for 24 hours.
  • the temperature was increased at a rate of 10°C/min until the plasma glass raw material mixed in the dry mixing manner reached a temperature of 1500°C, and the temperature was maintained at 1500°C for approximately 2 hours. . Then, by performing the annealing step (S3), cooling step (S4) and plasma glass obtaining step (S5) in the same manner as described above, to obtain a plasma glass containing a YOF compound.
  • the plasma glass raw material preparation step (S1) is the same as or similar to Example 1 described above (see FIG. 2A).
  • the plasma glass raw material was mixed using a wet mixing method.
  • the total amount of chemical components was placed in a weight of 100 g, and the plasma glass raw material was mixed for about 1 hour by a zirconia ball milling method.
  • the plasma glass raw material was wet-mixed with 100 g of raw material: 400 g of ethanol: 900 g of zirconia balls (weight ratio 1:4:9), and then dried for 24 hours.
  • the Naplesma glass raw material mixed by the wet mixing method was increased in temperature at a rate of 10°C/min until it reached a temperature of 1500°C, and was maintained at a temperature of 1500°C for approximately 2 hours. . Then, by performing the annealing step (S3), cooling step (S4) and plasma glass obtaining step (S5) in the same manner as described above, to obtain a plasma glass containing a YOF compound.
  • the plasma glass raw material was mixed using a dry mixing method.
  • the total amount of chemical components was placed in a weight of 100 g, and the plasma glass raw material was mixed for about 1 hour by a zirconia ball milling method.
  • 100 g of raw material: 300 g of zirconia balls (weight ratio 1:3) was dry-mixed with the plasma glass raw material, and then dried for 24 hours.
  • the temperature was increased at a rate of 10°C/min until the plasma glass raw material mixed in the dry mixing manner reached a temperature of 1500°C, and the temperature was maintained at 1500°C for approximately 2 hours. . Then, by performing the annealing step (S3), cooling step (S4) and plasma glass obtaining step (S5) in the same manner as described above, to obtain a plasma glass containing a YN compound.
  • the photograph of Figure 3a is the plasma-resistant glass prepared by Example 1
  • the photograph of Figure 3b is the plasma-resistant glass prepared by Example 2
  • the photograph of Figure 3c is the plasma-resistant glass prepared by Example 3 It is glass
  • the photograph of FIG. 3d is a plasma-resistant glass prepared in Example 4.
  • the plasma-resistant glass prepared in Example 1 was generally transparent in appearance, but a large amount of air bubbles and unmelted particles were observed.
  • EDS Electronic Dispersive X-ray Spectroscopy
  • each element of the plasma glass was observed to be in a homogeneous mixed state, and fluorine (F) element was also detected.
  • the plasma-resistant glass prepared in Example 2 was also substantially transparent in appearance, but a large amount of air bubbles was observed. However, unmelted particles were not observed. As a result of EDS analysis, each element of the plasma glass was observed to be in a homogeneous mixed state, and elemental fluorine (F) was also detected.
  • the plasma-resistant glass prepared in Example 3 was also substantially transparent in appearance, but a large amount of air bubbles were observed. However, unmelted particles were not observed.
  • each element of the plasma glass was observed to be in a homogeneous mixed state, and elemental fluorine (F) was also detected.
  • F elemental fluorine
  • the plasma-resistant glass prepared in Example 4 was generally opaque (ivory color), and a large amount of air bubbles were observed. As a result of EDS analysis, each element of the plasma glass was observed to be in a homogeneous mixed state.
  • FIG. 4 a table for atomic (At)% in the plasma glass raw material mixture and the plasma glass according to an embodiment of the present invention is shown.
  • the plasma glass raw material mixture refers to the mixture before performing the melting step, Example 1 (plasma-resistant glass by dry mixing method) and Example 2 (plasma-resistant glass by wet mixing method) after the melting step It means commercialized plasma-resistant glass.
  • yttrium (Y) element and fluorine (F) element were detected in common in the plasma glass raw material mixture and the plasma glass manufactured by Examples 1 and 2 . That is, the yttrium (Y) element was detected at 1.61 At% in the plasma glass raw material mixture, 2.23 At% in Example 1, and 2.94 At% in Example 2, respectively. In addition, the element fluorine (F) was detected at 5.47 At% in the plasma glass raw material mixture, 5.98 At% in Example 1, and 4.71 At% in Example 2, respectively.
  • the yttrium (Y) element and the fluorine (F) element are detected in the plasma-resistant glass raw material mixture before the melting step and the plasma-resistant glass after the melting step, respectively, so that the yttrium (Y) element and the fluorine (F) element during the manufacturing process It can be confirmed that is not lost.
  • the element fluorine (F) affects plasma resistance (eg, etch rate), it is preferable to remain in the commercialized plasma glass.
  • the plasma-resistant glass to which YOF was added according to Example 1 had a CTE of 4.75 * 10 -6 m/(m ° C.), a glass transition temperature of 763.7 ° C., and a softening point of 845.2 ° C.
  • the plasma glass to which YOF according to Example 2 was added had a CTE of 4.92*10 -6 m/(m°C), a glass transition temperature of 769.9°C, and a softening point of 830.9°C, and YN according to Example 4 was added.
  • the plasma-resistant glass was measured to have a CTE of 4.83*10 -6 m/(m°C), a glass transition temperature of 824.3°C, and a softening point of 936.2°C.
  • the plasma glass contains a fluorine (F) element rather than a nitrogen (N) element, it can be seen that the glass transition temperature and softening point are lowered. Therefore, since the plasma glass containing YOF reduces the viscosity and melting point, it provides a low melting point plasma glass that is easy to process in the end.
  • F fluorine
  • N nitrogen
  • the plasma glass contains a fluorine (F) element rather than a nitrogen (N) element
  • plasma resistance is improved.
  • a fluorine compound layer is formed on the plasma glass by reacting with each other. Such a fluorine compound layer reduces the etching rate.
  • the fluorine (F) element is already contained in the plasma-resistant glass, the fluorine compound layer on the surface of the plasma-resistant glass becomes faster and thicker when the plasma glass is exposed to a CF 4 -based plasma environment. formed, and thus plasma resistance can be further improved.
  • FIG. 6 is a photograph showing the plasma characteristics of the plasma-resistant glass according to an embodiment of the present invention.
  • CAS means Ca, Al and Si
  • YO means Y 2 O 3 (see photo 1)
  • YOF literally means YOF (see photo 2)
  • YN is Y (NO 3 ) It means 3 ⁇ 6H 2 O (refer to the 3rd picture).
  • photos 1, 2, and 3 in FIG. 6 show the etch depth before and after etching and the surface roughness before and after etching.
  • ICP Inductively Coupled Plasma
  • Thickness [um] (1) CAS+YO (2) CAS+YOF (3) CAS+YN etch depth (Etching Depth) 0.83 0.482 0.5 Ra @ Before 0.036 0.028 0.032 Ra @ After 0.069 0.031 0.036
  • the etch rate of the plasma glass containing YOF and/or YN is lower than that of the plasma glass containing YO. That is, in the case of plasma-resistant glass containing YO, the etching rate is 830 nm/60 min (ie, 13.8 nm/min), whereas in the case of plasma-resistant glass containing YOF, the etching rate is 8.0 nm/min, and plasma resistance containing YN In the case of glass, the etching rate is 8.3 nm/min.
  • the roughness of the plasma-resistant glass containing YOF and/or YN is lower than the surface roughness of the plasma-resistant glass containing YO. That is, in the case of plasma-resistant glass containing YO, the roughness after etching increased by 60 nm-36 nm (ie, 33 nm), whereas the post-etch roughness of plasma-resistant glass containing YOF increased by 3 nm, and plasma glass containing YN In the case of , the roughness increased by 4 nm after etching.
  • an embodiment of the present invention can provide a plasma glass with improved plasma resistance and a method for manufacturing the same.
  • an embodiment of the present invention may provide a plasma glass having a plasma resistance of about 5 nm/min to about 10 nm/min with respect to a mixed plasma of fluorine and argon and a method for manufacturing the same.

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  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Glass Compositions (AREA)

Abstract

Un mode de réalisation de la présente invention concerne un verre résistant au plasma et un procédé de fabrication de celui-ci. La présente invention vise à résoudre le problème technique de la fourniture d'un verre résistant au plasma présentant une résistance au plasma améliorée, et un procédé de fabrication de celui-ci. A cet effet, la présente invention concerne : un verre plasma comprenant 40 à 75 % en moles de SiO2, 5 à 20 % en moles d'Al2O3, 5 à 30 % en moles de CaO et 0,01 à 10 % en moles d'un composé à base de Y résistant au plasma ; et un procédé de fabrication de celui-ci.
PCT/KR2021/010136 2020-08-11 2021-08-03 Verre résistant au plasma et procédé de fabrication de celui-ci WO2022035111A1 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
KR10-2020-0100546 2020-08-11
KR20200100546 2020-08-11
KR1020210098388A KR102608654B1 (ko) 2020-08-11 2021-07-27 내플라즈마 유리 및 그 제조 방법
KR10-2021-0098388 2021-07-27

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2023189779A1 (fr) * 2022-03-31 2023-10-05 Ａｇｃ株式会社 Bloc de verre, procédé de production d'un tel bloc de verre et élément résistant au plasma

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002356345A (ja) * 2001-06-01 2002-12-13 Tosoh Corp 耐食性石英ガラスの製造方法、これを用いた部材及び装置
KR20110118939A (ko) * 2010-04-26 2011-11-02 한국세라믹기술원 내플라즈마 결정질 세라믹 코팅막 및 그 제조방법
KR20120057272A (ko) * 2010-11-26 2012-06-05 인하대학교 산학협력단 비정질 내플라즈마 유리조성물 및 이를 이용한 내플라즈마 부재
KR20180080429A (ko) * 2017-01-04 2018-07-12 한국세라믹기술원 세라믹 부재의 재사용을 위한 내플라즈마 하드코팅 조성물 및 이를 이용한 세라믹 부재의 재생방법
KR20180092900A (ko) * 2017-02-10 2018-08-20 아이원스 주식회사 글래스 코팅 구조물 및 이의 형성 방법

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002356345A (ja) * 2001-06-01 2002-12-13 Tosoh Corp 耐食性石英ガラスの製造方法、これを用いた部材及び装置
KR20110118939A (ko) * 2010-04-26 2011-11-02 한국세라믹기술원 내플라즈마 결정질 세라믹 코팅막 및 그 제조방법
KR20120057272A (ko) * 2010-11-26 2012-06-05 인하대학교 산학협력단 비정질 내플라즈마 유리조성물 및 이를 이용한 내플라즈마 부재
KR20180080429A (ko) * 2017-01-04 2018-07-12 한국세라믹기술원 세라믹 부재의 재사용을 위한 내플라즈마 하드코팅 조성물 및 이를 이용한 세라믹 부재의 재생방법
KR20180092900A (ko) * 2017-02-10 2018-08-20 아이원스 주식회사 글래스 코팅 구조물 및 이의 형성 방법

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2023189779A1 (fr) * 2022-03-31 2023-10-05 Ａｇｃ株式会社 Bloc de verre, procédé de production d'un tel bloc de verre et élément résistant au plasma

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