TWI444331B - Corrosion resistance components - Google Patents
Corrosion resistance components Download PDFInfo
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- TWI444331B TWI444331B TW097145508A TW97145508A TWI444331B TW I444331 B TWI444331 B TW I444331B TW 097145508 A TW097145508 A TW 097145508A TW 97145508 A TW97145508 A TW 97145508A TW I444331 B TWI444331 B TW I444331B
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C24/00—Coating starting from inorganic powder
- C23C24/02—Coating starting from inorganic powder by application of pressure only
- C23C24/04—Impact or kinetic deposition of particles
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/4401—Means for minimising impurities, e.g. dust, moisture or residual gas, in the reaction chamber
- C23C16/4404—Coatings or surface treatment on the inside of the reaction chamber or on parts thereof
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
- C23C4/10—Oxides, borides, carbides, nitrides or silicides; Mixtures thereof
- C23C4/11—Oxides
Description
本發明係有關耐蝕性構件，有關具有適用於如：半導體製造裝置內、平面顯示器製造裝置內、太陽電池製造裝置內之氧化物被膜之耐蝕性構件的發明。The present invention relates to a corrosion-resistant member, and relates to an invention having a corrosion-resistant member suitable for use in, for example, a semiconductor manufacturing apparatus, a flat display manufacturing apparatus, and an oxide film in a solar cell manufacturing apparatus.
於半導體製造裝置內、平面顯示器製造裝置內、太陽電池製造裝置內時，為於鹵素系腐蝕氣體或鹵素系氣體電漿等之環境下，進行製造，而使用具耐蝕性之構件。近年來，稀土類化合物之耐蝕性被確定，特別以Y2 O3 受矚目，如：特開2001-164354號公報所載之基材表面上施予含有Y2 O3 之耐蝕性被膜之構件被使用之。In the case of a semiconductor manufacturing apparatus, a flat display manufacturing apparatus, or a solar cell manufacturing apparatus, it is manufactured in an environment of a halogen-based etching gas or a halogen-based gas plasma, and a member having corrosion resistance is used. In recent years, the corrosion resistance of the rare earth compound has been determined, and in particular, Y 2 O 3 has been attracting attention. For example, a member for imparting a corrosion resistant film containing Y 2 O 3 on the surface of the substrate as disclosed in JP-A-2001-164354 Used.
惟，Y3 O3 為高熔點者，因此不易熔融，於半熔融狀態下形成氧化物被膜。因此，半導體製造裝置內、平面顯示器製造裝置內、太陽電池製造裝置內，若曝露於鹵素系腐蝕氣體或鹵素系氣體電漿等則將藉由蝕刻由被膜表面使結晶粒子脫粒，產生微粒。而且所產生之微粒附著於晶圓上，導致降低收率之間題存在。However, since Y 3 O 3 is a high melting point, it is not easily melted, and an oxide film is formed in a semi-molten state. Therefore, in the semiconductor manufacturing apparatus, the flat display manufacturing apparatus, and the solar cell manufacturing apparatus, when exposed to a halogen-based etching gas or a halogen-based gas plasma, the crystal particles are degranulated by etching on the surface of the coating film to generate fine particles. Moreover, the generated particles adhere to the wafer, resulting in a problem of reducing the yield.
本發明之目的係為提供一種對於鹵素系腐蝕氣體或鹵素系氣體電漿等，具有良好的耐蝕性之氧化物被膜所形成之耐蝕性構件。An object of the present invention is to provide a corrosion-resistant member formed of an oxide film having good corrosion resistance to a halogen-based etching gas or a halogen-based gas plasma.
本發明鑑於上述現狀，為解決上述課題，而提供一種可充份確保對於鹵素系腐蝕氣體或鹵素系氣體電漿等之耐蝕性之耐蝕性構件者為其目的，因此為達成該目的，而具備如以下之構成。In order to achieve the above object, the present invention has been made in view of the above-mentioned problems, and it is an object of the present invention to provide a corrosion-resistant member capable of sufficiently ensuring corrosion resistance to a halogen-based corrosive gas or a halogen-based gas plasma. As the following composition.
亦即，以基材上形成含有Gd之氧化物被膜所成者為其特徵之耐蝕性構件，或以基材上形成含有Yb之氧化物被膜所成者為其特徵之耐蝕性構件。如：該氧化物被膜中，鐵族金屬化合物以氧化物換算下含有多於5ppm者為其特徵。或該氧化物被膜中，鐵族金屬化合物以氧化物換算下含有少於50ppm者為其特徵。而且，如：該氧化物被膜藉由噴塗法所形成者為其特徵。本發明之耐蝕性構件更以於半導體製造裝置內、平面顯示器製造裝置內、太陽電池製造裝置內所使用之構件者為其特徵。具體而言，可適用於為靜電吸盤、加熱器、氣體擴散板、擋板、擋環、簇射極板、以及棚室、鐘罩、圓頂及其內壁材料、以及高頻透窗、透紅外線窗、監視窗、基座、鎖緊圈、焦距環、shadow ring、絕緣環、仿真晶圓、半導體晶圓之升降針、伸縮護蓋、冷卻板、上部電極、下部電極。In other words, a corrosion-resistant member characterized by forming an oxide film containing Gd on a substrate, or a corrosion-resistant member characterized by forming an oxide film containing Yb on a substrate. For example, in the oxide film, the iron group metal compound is characterized in that it contains more than 5 ppm in terms of oxide. Or in the oxide film, the iron group metal compound is characterized by containing less than 50 ppm in terms of oxide. Further, for example, the oxide film is characterized by being formed by a spray coating method. The corrosion-resistant member of the present invention is further characterized by a member used in a semiconductor manufacturing apparatus, a flat display manufacturing apparatus, or a solar cell manufacturing apparatus. Specifically, it can be applied to an electrostatic chuck, a heater, a gas diffusion plate, a baffle, a retaining ring, a shower plate, and a shed, a bell jar, a dome and an inner wall material thereof, and a high-frequency window, Through infrared window, monitoring window, base, locking ring, focal length ring, shadow ring, insulating ring, dummy wafer, lifting pin of semiconductor wafer, telescopic cover, cooling plate, upper electrode, lower electrode.
本發明可提供一種可適用於利用鹵素系腐蝕氣體或鹵素系氣體電漿等之半導體製造裝置內、平面顯示器製造裝置內、太陽電池製造裝置內之良好耐蝕性之耐蝕性構件，可減少微粒的產生。The present invention can provide a corrosion-resistant member which can be suitably used in a semiconductor manufacturing apparatus using a halogen-based etching gas or a halogen-based gas plasma, in a flat-panel display manufacturing apparatus, or in a solar cell manufacturing apparatus, and can reduce particulates. produce.
又，本發明係藉由，於氧化物被膜中含有以氧化物換算下為多於5ppm之鐵族金屬化合物，可形成良好耐蝕性之氧化物被膜。Moreover, in the present invention, an oxide film having a good corrosion resistance can be formed by containing an iron group metal compound in an oxide film of more than 5 ppm in terms of an oxide.
本發明者為達成該目的，進行精密研討後結果，發現，含有Gd或Yb之氧化物被膜即使曝露於鹵素系腐蝕氣體或鹵素系氣體電漿等仍具良好耐蝕性，極少出現微粒產生。且發現，該氧化物被膜中藉由以氧化物換算下含有多於5ppm之鐵族金屬化合物，可降低Gd或Yb之熔點，形成良好耐蝕性之氧化物被膜。In order to achieve the object, the present inventors have found that the oxide film containing Gd or Yb has good corrosion resistance even when exposed to a halogen-based corrosive gas or a halogen-based gas plasma, and fine particles are rarely generated. Further, it has been found that the oxide film contains more than 5 ppm of the iron group metal compound in terms of oxide, and the melting point of Gd or Yb can be lowered to form an oxide film having good corrosion resistance.
以下，參考圖面等，詳細說明本發明實施之形態例。以下說明之本實施之形態例的耐蝕性構件係形成一種含有Gd(釓：Gadolinium)或Yb(鐿：Ytterbium)，且以氧化物換算下含有多於5ppm之鐵族金屬化合物之氧化物被膜所成。Hereinafter, a form of embodiment of the present invention will be described in detail with reference to the drawings and the like. The corrosion-resistant member of the embodiment of the present embodiment described below is formed of an oxide film containing Gd (Gadolinium) or Yb (Ytterbium) and containing more than 5 ppm of an iron group metal compound in terms of oxide. to make.
本實施之形態例之耐蝕性構件係適用於半導體製造裝置內、平面顯示器製造裝置內、太陽電池製造裝置內之構件、至少於表面對於鹵素系腐蝕氣體或鹵素系氣體電漿等，具有具耐蝕性之氧化物被膜。耐蝕性構件之基材材質並未特別限定，一般可使用如：玻璃、石英、鋁、不鏽鋼等之金屬、氧化鋁等之陶瓷等。又，必要時，亦可進行噴鍍處理，使基材表面變粗後，形成氧化物被膜。The corrosion-resistant member according to the embodiment of the present invention is suitably used in a semiconductor manufacturing apparatus, a flat display manufacturing apparatus, a member in a solar cell manufacturing apparatus, and at least a surface having a corrosion resistance to a halogen-based corrosive gas or a halogen-based gas plasma. Oxide film. The material of the base material of the corrosion-resistant member is not particularly limited, and generally, a metal such as glass, quartz, aluminum, or stainless steel, or a ceramic such as alumina can be used. Further, if necessary, a thermal spraying treatment may be performed to form an oxide film after the surface of the substrate is coarsened.
本實施之形態例之氧化物被膜之純度為99.9%以上者宜。藉由使純度作成99.9%以上，即使曝露於鹵素系腐蝕氣體或鹵素系氣體電漿等，仍可抑制氧化物被膜腐蝕之進行。含於本實施形態例之耐蝕性構件表面所形成之氧化物被膜中之鐵族金屬化合物係為用於Fe、Co、Ni等者宜，更為降低Gd或Yb之熔點之使用。而且，使作為原料之Gd或Yb進行氧化作成粉末化之同時，氧化鐵族金屬化合物，粉末化後，混合此等後，於基材表面以後述之方法形成氧化物被膜。鐵族金屬化合物之混合比例係以氧化物換算下含有多於5ppm者即可。當鐵族金屬化合物以氧化物換算下含有少於5ppm時，則將減少降低Gd或Yb之熔點效果。又，當鐵族金屬化合物以氧化物換算下含有多於50ppm時，則含有Gd或Yb之氧化物被膜曝露於鹵素系腐蝕氣體或鹵素系氣體電漿等時，將活化蝕刻，產生過剩之微粒。因此，以氧化物換算下含有鐵族金屬化合物為多於5ppm、少於50ppm者宜。The purity of the oxide film of the embodiment of the present embodiment is preferably 99.9% or more. When the purity is 99.9% or more, even if it is exposed to a halogen-based corrosive gas or a halogen-based gas plasma, the progress of the oxide film corrosion can be suppressed. The iron group metal compound contained in the oxide film formed on the surface of the corrosion-resistant member of the present embodiment is preferably used for Fe, Co, Ni, etc., and further reduces the melting point of Gd or Yb. In addition, Gd or Yb as a raw material is oxidized and pulverized, and the iron oxide group metal compound is powdered, and after mixing, the oxide film is formed on the surface of the substrate to be described later. The mixing ratio of the iron group metal compound may be more than 5 ppm in terms of oxide. When the iron group metal compound contains less than 5 ppm in terms of oxide, the effect of lowering the melting point of Gd or Yb will be reduced. In addition, when the iron group metal compound contains more than 50 ppm in terms of oxide, when the oxide film containing Gd or Yb is exposed to a halogen-based etching gas or a halogen-based gas plasma, it is activated and etched to generate excess particles. . Therefore, it is preferred that the iron group-containing metal compound is contained in an amount of more than 5 ppm and less than 50 ppm in terms of oxide.
本實施之形態例中氧化物被膜之形成方法並未特別限定，一般可以如：火焰噴塗、高速火焰噴塗(HVOF)、電漿噴塗、***火焰噴塗、冷噴霧、氣熔膠法等形成之。其中又以噴塗輸出功率高、適於高熔點材料之噴塗之電漿噴塗所形成者較佳。The method for forming the oxide film in the embodiment of the present embodiment is not particularly limited, and may be generally formed by flame spraying, high-speed flame spraying (HVOF), plasma spraying, explosion flame spraying, cold spraying, gas melting, or the like. Among them, it is preferably formed by plasma spraying with high spray output power and suitable for spraying of high melting point materials.
電漿噴塗時之電漿產生時所使用之氣體並未特別限定，一般可使用如：氬氣、氦氣、氮氣、氫氣、氧氣等。The gas used in the plasma generation during plasma spraying is not particularly limited, and generally, for example, argon gas, helium gas, nitrogen gas, hydrogen gas, oxygen gas or the like can be used.
本實施形態例中氧化物被膜之氣孔率為5%～15%者宜。5%以上之氧化物被膜於被膜步驟中不易產生龜裂。又，15%以下之氧化物被膜即使曝露於鹵素系腐蝕氣體或鹵素系氣體電漿等時，仍可維持氧化物被膜之強度，可防止缺陷、剝離。更於未透過氧化物被膜之基材上使鹵素系腐蝕氣體或鹵素系氣體電漿等不易受損。In the present embodiment, the porosity of the oxide film is preferably 5% to 15%. More than 5% of the oxide film is less likely to be cracked in the film step. In addition, when the oxide film of 15% or less is exposed to a halogen-based corrosive gas or a halogen-based gas plasma, the strength of the oxide film can be maintained, and defects and peeling can be prevented. Further, the halogen-based corrosive gas or the halogen-based gas plasma is less likely to be damaged on the substrate that does not pass through the oxide film.
為形成本實施形態例之氧化物被膜所使用之噴塗粉末藉由使平均粒徑為20μm～60μm、較佳者為30μm～50μm後，可於電漿火焰上流動、於熔融狀態下附著於構件。平均粒徑為20μm以上，使噴塗粉末投入電漿火焰時，噴塗粉末不會飛散，可流動於電漿火焰，於熔融狀態下附著於構件。又，平均粒徑為60μm以下，使噴塗粉末投入電漿火焰時，噴塗粉末不會經電漿火焰脫落，可流動於電漿火焰，於熔融狀態下，附著於構件。The spray powder used for forming the oxide film of the present embodiment can be adhered to the member in a molten state by having an average particle diameter of 20 μm to 60 μm, preferably 30 μm to 50 μm. . When the average particle diameter is 20 μm or more, when the spray powder is put into the plasma flame, the spray powder does not scatter, and it can flow to the plasma flame and adhere to the member in a molten state. Further, when the average particle diameter is 60 μm or less, when the spray powder is introduced into the plasma flame, the spray powder does not fall off by the plasma flame, and can flow to the plasma flame and adhere to the member in a molten state.
本實施形態例之氧化物被膜厚度為100μm～1000μm者宜。作成100μm以上則即使曝露於鹵素系腐蝕氣體或鹵素系氣體電漿等時，仍可預見耐蝕性之效果，甚至鹵素系腐蝕氣體、或鹵素系氣體電漿等不易透過至基材為止。又，作成1000μm以下，則不易產生經由耐蝕性構件之基材與氧化物被膜之熱膨脹差的剝離。The thickness of the oxide film of the present embodiment is preferably from 100 μm to 1000 μm. When it is 100 μm or more, even when it is exposed to a halogen-based corrosive gas or a halogen-based gas plasma, the effect of corrosion resistance can be expected, and even a halogen-based corrosive gas or a halogen-based gas plasma is hardly transmitted to the substrate. Moreover, when it is 1000 micrometers or less, peeling of the difference of the thermal expansion of the base material of the corrosion-resistant member and an oxide film is hard to arise.
本實施形態例之氧化物被膜之密合強度係以20MPa以上形成於基材者宜。氧化物被膜與基材之密合強度作成20MPa以上，可防止使用中、洗淨中之氧化物被膜之剝離。氧化物被膜經剝離後則易由基材之露出部產生微粒，而作成上述之密合強度則可防止。The adhesion strength of the oxide film of the present embodiment is preferably 20 MPa or more. The adhesion strength between the oxide film and the substrate is 20 MPa or more, and peeling of the oxide film during use and during cleaning can be prevented. When the oxide film is peeled off, particles are easily generated from the exposed portion of the substrate, and the above-described adhesion strength can be prevented.
以下，詳細說明本發明之一實施例。另外，本發明並未受限於以下所說明之實施例。Hereinafter, an embodiment of the present invention will be described in detail. Further, the invention is not limited to the embodiments described below.
實施例中Fe2 O3 值係使用ICP發光分析裝置所測定。實施例中噴塗粉末之平均粒徑係使用雷射衍射‧散射式之粒度測定機所測定。The Fe 2 O 3 value in the examples was measured using an ICP emission spectrometer. The average particle diameter of the sprayed powder in the examples was measured using a laser diffraction/scattering type particle size measuring machine.
實施例中蝕刻率係使部份氧化物被膜以聚醯亞胺膠帶進行標識，利用RIE裝置，於CF4電漿中進行照射10小時，測定標識有無之個處的段差後求取之。In the examples, the etching rate was such that a part of the oxide film was marked with a polyimide film, and the film was irradiated for 10 hours in a CF4 plasma by an RIE apparatus, and the difference in the presence or absence of the mark was measured.
實施例中氣孔率係測定氧化物被膜之乾燥重量W1、水中重量W2、飽水重量W3，利用以下之阿基米德法求取之。In the examples, the porosity was determined by measuring the dry weight W1 of the oxide film, the weight W2 of the water, and the weight W3 of the water, using the following Archimedes method.
使平均粒徑為30μm～40μm之分別含有8ppm、10ppm、20ppm、30ppm、40ppm Fe2 O3 之Gd氧化物的Gd2 O3 之噴塗粉末利用空氣電漿公司製ASP 7100電漿噴塗機，於電壓275V、電流110A、氬氣流量25L/min、氧氣流量40L/min之噴塗條件下，於噴鍍處理之100×100×5t(mm)之鋁基材上進行噴塗，形成200μm～300μm之氧化物被膜。接著進行所形成氧化物被膜之蝕刻率及氣孔率之評定。A spray powder of Gd 2 O 3 containing an average particle diameter of 30 μm to 40 μm containing 8 ppm, 10 ppm, 20 ppm, 30 ppm, and 40 ppm of Fe 2 O 3 Gd oxide was used in an ASP 7100 plasma sprayer manufactured by Air Plasma Co., Ltd. Spraying on a 100×100×5t (mm) aluminum substrate under spray coating with a voltage of 275V, a current of 110A, an argon flow rate of 25L/min, and an oxygen flow rate of 40L/min to form an oxidation of 200μm to 300μm. The film is covered. Next, the etching rate and the porosity of the formed oxide film were evaluated.
使平均粒徑為30μm～40μm之分別含有8ppm、10ppm、20ppm、30ppm、40ppm Fe2 O3 之Yb氧化物的Yb2 O3 之噴塗粉末利用空氣電漿公司製ASP 7100電漿噴塗機，於電壓275V、電流110A、氬氣流量25L/min、氧氣流量40L/min之噴塗條件下，於噴鍍處理之100×100×5t(mm)之鋁基材上進行噴塗，形成200μm～300μm之氧化物被膜。接著，進行所形成氧化物被膜之蝕刻率及氣孔率之評定。A spray powder of Yb 2 O 3 containing an Yb oxide of 8 ppm, 10 ppm, 20 ppm, 30 ppm, and 40 ppm of Fe 2 O 3 having an average particle diameter of 30 μm to 40 μm was used in an ASP 7100 plasma sprayer manufactured by Air Plasma Co., Ltd. Spraying on a 100×100×5t (mm) aluminum substrate under spray coating with a voltage of 275V, a current of 110A, an argon flow rate of 25L/min, and an oxygen flow rate of 40L/min to form an oxidation of 200μm to 300μm. The film is covered. Next, the etching rate and the porosity of the formed oxide film were evaluated.
使平均粒徑為30μm～40μm之分別含有1ppm、3ppm、4ppm、70ppm、80ppm Fe2 O3 之Gd氧化物的Gd2 O3 噴塗粉末，利用空氣電漿公司製ASP 7100電漿噴塗機，於電壓275V、電流110A、氬氣流量25L/min、氧氣流量40L/min之噴塗條件下，於噴鍍處理之100×100×5t(mm)之鋁基材上進行噴塗，形成200μm～300μm之氧化物被膜。接著，進行所形成之氧化物被膜之蝕刻率及氣孔率之評定。A Gd 2 O 3 spray powder containing an average particle diameter of 30 μm to 40 μm containing 1 ppm, 3 ppm, 4 ppm, 70 ppm, and 80 ppm of Fe 2 O 3 Gd oxide was used by an air plasma company ASP 7100 plasma sprayer. Spraying on a 100×100×5t (mm) aluminum substrate under spray coating with a voltage of 275V, a current of 110A, an argon flow rate of 25L/min, and an oxygen flow rate of 40L/min to form an oxidation of 200μm to 300μm. The film is covered. Next, the etching rate and the porosity of the formed oxide film were evaluated.
使平均粒徑為30μm～40μm之分別含有1ppm、3ppm、4ppm、70ppm、80ppm Fe2 O3 之Yb氧化物的Yb2 O3 噴塗粉末，使用空氣電漿公司製ASP 7100電漿噴塗機，於電壓275V、電流110A、氬氣流量25L/min、氧氣流量40L/min之噴塗條件下，於噴鍍處理之100×100×5t(mm)之鋁基材上進行噴塗，形成200μm～300μm之氧化物被膜。接著，進行評定所形成氧化物被膜之蝕刻率及氣孔率。Yb 2 O 3 spray powder containing Yb oxides of 1 ppm, 3 ppm, 4 ppm, 70 ppm, and 80 ppm Fe 2 O 3 having an average particle diameter of 30 μm to 40 μm was used, and an ASP 7100 plasma sprayer manufactured by Air Plasma Co., Ltd. was used. Spraying on a 100×100×5t (mm) aluminum substrate under spray coating with a voltage of 275V, a current of 110A, an argon flow rate of 25L/min, and an oxygen flow rate of 40L/min to form an oxidation of 200μm to 300μm. The film is covered. Next, the etching rate and the porosity of the oxide film formed were evaluated.
使平均粒徑為30μm～40μm之含有10ppm Fe2 O3 之Y的氧化物之Y2 O3 噴塗粉末，利用空氣電漿公司製ASP7100電漿噴塗機，以電壓275V、電流110A、氬氣流量25L/min、氧氣流量40L/min之噴塗條件下，於噴鍍處理之100×100×5t(mm)之鋁基材上進行噴塗、形成200μm～300μm之氧化物被膜。接著，進行評定所形成氧化物被膜之蝕刻率及氣孔率。Y 2 O 3 spray powder containing an oxide of Y of 10 ppm Fe 2 O 3 having an average particle diameter of 30 μm to 40 μm, using an ASP7100 plasma sprayer manufactured by Air Plasma Co., Ltd., with a voltage of 275 V, a current of 110 A, and an argon flow rate Under a spray condition of 25 L/min and an oxygen flow rate of 40 L/min, an aluminum oxide substrate of 100 × 100 × 5 t (mm) was spray-sprayed to form an oxide film of 200 μm to 300 μm. Next, the etching rate and the porosity of the oxide film formed were evaluated.
表1顯示，針對實施例與比較例所測定之蝕刻率及氣孔率之結果。另外，比較例5、10被確定局部性蝕刻，故於表1顯示其部份蝕刻率。Table 1 shows the results of the etching rate and the porosity measured for the examples and the comparative examples. Further, in Comparative Examples 5 and 10, local etching was determined, so that the partial etching rate is shown in Table 1.
由表1得知，Fe2 O3 為少於5ppm之Gd2 O3 及Yb2 O3 其氣孔率為15%以上，因此氧化物被膜曝露於鹵素系腐蝕氣體或鹵素系氣體電漿等，則氧化物被膜因強度不足容易被蝕刻，進而產生微粒。故不適於作為利用鹵素系腐蝕氣體或鹵素系氣體電漿等之半導體製造裝置內、平面顯示器裝置內、太陽電池製造裝置內之耐蝕性構件。反之，Fe2 O3 為多於50ppm之Gd2 O3 及Yb2 O3 其氧化物被膜局部被蝕刻，產生過剩之微粒。因此，不適於作為利用鹵素系腐蝕氣體或鹵素系氣體電漿等之半導體製造裝置內、平面顯示器製造裝置內、太陽電池製造裝置內之耐蝕性構件。As is clear from Table 1, since Fe 2 O 3 is less than 5 ppm of Gd 2 O 3 and Yb 2 O 3 and the porosity is 15% or more, the oxide film is exposed to a halogen-based corrosive gas or a halogen-based gas plasma. Then, the oxide film is easily etched due to insufficient strength, and fine particles are generated. Therefore, it is not suitable as a corrosion-resistant member in a semiconductor manufacturing apparatus using a halogen-based etching gas or a halogen-based gas plasma, in a flat display device, or in a solar cell manufacturing apparatus. On the other hand, Fe 2 O 3 is more than 50 ppm of Gd 2 O 3 and Yb 2 O 3 , and the oxide film is partially etched to generate excess particles. Therefore, it is not suitable as a corrosion-resistant member in a semiconductor manufacturing apparatus using a halogen-based etching gas or a halogen-based gas plasma, in a flat-panel manufacturing apparatus, or in a solar cell manufacturing apparatus.
由表1得知，Fe2 O3 為多於5ppm之Gd2 O3 及Yb2 O3 ，對於Y2 O3 而言，其蝕刻率為1/2～1/3因此極少產生微粒。故適於作為利用鹵素系腐蝕氣體或鹵素系氣體電漿等之半導體製造裝置內、平面顯示器製造裝置內、太陽電池製造裝置內之耐蝕性構件。As is clear from Table 1, Fe 2 O 3 is more than 5 ppm of Gd 2 O 3 and Yb 2 O 3 , and for Y 2 O 3 , the etching rate is 1/2 to 1/3, so that fine particles are rarely generated. Therefore, it is suitable as a corrosion-resistant member in a semiconductor manufacturing apparatus using a halogen-based etching gas or a halogen-based gas plasma, in a flat-panel manufacturing apparatus, and in a solar cell manufacturing apparatus.
由上述顯示，含有Gd或Yb之氧化物，且以氧化物換算下含有多於5ppm鐵族金屬化合物之氧化物被膜所形成之耐蝕性構件對於鹵素系腐蝕氣體或鹵素系氣體電漿等具良好耐蝕性。因此，適於曝露於鹵素系腐蝕氣體或鹵素系氣體電漿等之半導體製造裝置內、平面顯示器製造裝置內、太陽電池製造裝置內之使用。As described above, the corrosion-resistant member containing an oxide film of Gd or Yb and containing more than 5 ppm of an iron group metal compound in terms of oxide has good properties for a halogen-based corrosive gas or a halogen-based gas plasma. Corrosion resistance. Therefore, it is suitable for use in a semiconductor manufacturing apparatus exposed to a halogen-based corrosive gas or a halogen-based gas plasma, in a flat-panel display manufacturing apparatus, or in a solar cell manufacturing apparatus.
使平均粒徑為30μm～40μm之含有8ppm Fe2 O3 之Gd及Yb氧化物之Gd2 O3 及Yb2 O3 噴塗粉末，利用空氣電漿公司製ASP 7100電漿噴塗機，以電壓275V、電流110A、氬氣流量25L/min、氧氣流量40L/min之噴塗條件下，於噴鍍處理之棒狀鋁基材上(表面粗度Ra 5.11μm)進行噴塗，形成200μm～300μm之氧化物被膜。之後，以黏著劑黏接形成該氧化物被膜之基材與另一棒狀鋁基材，測定藉由拉延之剝離強度，亦即密合強度。(JISH 8666為基準之試驗方法)。A Gd 2 O 3 and Yb 2 O 3 spray powder containing 8 ppm of Fe 2 O 3 Gd and Yb oxide having an average particle diameter of 30 μm to 40 μm was used, and an ASP 7100 plasma sprayer manufactured by Air Plasma Co., Ltd. was used at a voltage of 275V. Spraying on a rod-shaped aluminum substrate (surface roughness Ra 5.11 μm) sprayed to form an oxide of 200 μm to 300 μm under spraying conditions of a current of 110 A, an argon flow rate of 25 L/min, and an oxygen flow rate of 40 L/min. Membrane. Thereafter, the base material of the oxide film and the other rod-shaped aluminum substrate were bonded by an adhesive, and the peel strength by drawing, that is, the adhesion strength was measured. (JISH 8666 is the benchmark test method).
使平均粒徑為30μm～40μm之含有8ppm Fe2 O3 之Y氧化物的Y2 O3 噴塗粉末，利用空氣電漿公司製ASP 7100電漿噴塗機，以電壓275V、電流110A、氬氣流量25L/min、氧氣流量40L/min之噴塗條件下，於噴鍍處理之棒狀鋁基材上(表面粗度Ra 5.02μm)進行噴塗，形成200μm～300μm之氧化物被膜。之後，以黏著劑黏接形成該氧化物被膜之基材與另一棒狀之鋁基材，測定藉由拉延之剝離強度，亦即密合強度。(依JISH 8666為基準之試驗方法)。Y 2 O 3 spray powder containing 8 ppm of Fe 2 O 3 Y oxide having an average particle diameter of 30 μm to 40 μm was used by an air plasma company ASP 7100 plasma sprayer at a voltage of 275 V, a current of 110 A, and an argon flow rate. Under a spray condition of 25 L/min and an oxygen flow rate of 40 L/min, a spray-treated bar-shaped aluminum substrate (surface roughness Ra 5.02 μm) was sprayed to form an oxide film of 200 μm to 300 μm. Thereafter, the base material of the oxide film and the other aluminum base material were bonded by an adhesive, and the peel strength by drawing, that is, the adhesion strength was measured. (Test method based on JISH 8666).
表2顯示針對該試料1、2、3所測定之密合強度之結果。Table 2 shows the results of the adhesion strength measured for the samples 1, 2, and 3.
依據表2，同等條件下，相較於Y2 O3 與基材之密合強度14MPa、Gd2 O3 及Yb2 O3 與基材之密合強度分別為22MPa、21MPa。因此，Gd2 O3 與Yb2 O3 比Y2 O3 較易密合於基材，較不易產生剝離。According to Table 2, the adhesion strength between the Y 2 O 3 and the substrate was 14 MPa, and the adhesion strength between the Gd 2 O 3 and Yb 2 O 3 and the substrate was 22 MPa and 21 MPa, respectively. Therefore, Gd 2 O 3 and Yb 2 O 3 are more easily adhered to the substrate than Y 2 O 3 , and are less likely to cause peeling.
由以上顯示，Gd及Yb之氧化物的Gd2 O3 及Yb2 O3 所形成之耐蝕性構件適於半導體製造裝置內、平面顯示器製造裝置內、太陽電池製造裝置內之使用、洗淨環境之使用。As described above, the corrosion-resistant members formed of Gd 2 O 3 and Yb 2 O 3 of the oxides of Gd and Yb are suitable for use in a semiconductor manufacturing apparatus, a flat display manufacturing apparatus, a solar cell manufacturing apparatus, and a cleaning environment. Use.
另外，作為半導體製造裝置內、平面顯示器製造裝置內、太陽電池製造裝置內所使用之構件者，可使用如：靜電吸盤、加熱器等、內部具有靜電電極、電阻發熱體者。靜電電極多半使用耐蝕性低的金屬，因此，以本發明耐蝕性構件被覆此等後，可大幅提昇耐蝕性，亦可長時間使用之。In addition, as a member used in the semiconductor manufacturing apparatus, the flat display manufacturing apparatus, or the solar cell manufacturing apparatus, for example, an electrostatic chuck, a heater, or the like, and an electrostatic electrode or a resistance heating body may be used. Since most of the electrostatic electrodes use a metal having low corrosion resistance, the corrosion-resistant member of the present invention can be used to improve the corrosion resistance and can be used for a long period of time.
本發明之耐蝕性構件可採用為使鹵素系腐蝕氣體導入裝置內之氣體擴散板、擋板、擋環、簇射極板等。更亦可適用導入氣體之處理容器的棚室、鐘罩、圓頂及其內壁材料、以及高頻透窗、透紅外線窗、監視窗。進一步可適用於為支撐容器內所使用之基座、鎖緊圈、焦距環、shadow ring、絕緣環、仿真晶圓、半導體晶圓之升降針、伸縮護蓋、冷卻板、上部電極、下部電極等、電漿雰圍下被曝露，需要耐蝕性之各種構件。The corrosion-resistant member of the present invention may be a gas diffusion plate, a baffle plate, a baffle ring, a shower plate or the like for introducing a halogen-based corrosive gas into the device. It is also possible to use a shed, a bell jar, a dome and its inner wall material for introducing a gas processing container, and a high-frequency window, an infrared ray window, and a monitoring window. Further applicable to the base, the locking ring, the focal length ring, the shadow ring, the insulating ring, the dummy wafer, the lifting needle of the semiconductor wafer, the telescopic cover, the cooling plate, the upper electrode, the lower electrode used for supporting the container Etc., exposed to the plasma atmosphere, requires various components of corrosion resistance.
[圖1]圖1代表於實施例及比較例所得之蝕刻率及氣孔率之圖。Fig. 1 is a graph showing etching rates and porosity obtained in Examples and Comparative Examples.
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