JP4999721B2 - Thermal spray coating coated member having excellent appearance and method for producing the same - Google Patents
Thermal spray coating coated member having excellent appearance and method for producing the same Download PDFInfo
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- 238000005507 spraying Methods 0.000 title claims description 76
- 238000004519 manufacturing process Methods 0.000 title claims description 12
- 238000000576 coating method Methods 0.000 claims description 39
- 239000011248 coating agent Substances 0.000 claims description 37
- 239000000463 material Substances 0.000 claims description 16
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 14
- 239000001301 oxygen Substances 0.000 claims description 14
- 229910052760 oxygen Inorganic materials 0.000 claims description 14
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 10
- 239000000758 substrate Substances 0.000 claims description 10
- 230000001678 irradiating effect Effects 0.000 claims description 7
- 238000007751 thermal spraying Methods 0.000 claims description 4
- 230000003746 surface roughness Effects 0.000 claims description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 21
- 239000000843 powder Substances 0.000 description 12
- 239000007921 spray Substances 0.000 description 10
- 238000000034 method Methods 0.000 description 9
- 238000010894 electron beam technology Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 229910001882 dioxygen Inorganic materials 0.000 description 6
- 239000002344 surface layer Substances 0.000 description 6
- 235000019646 color tone Nutrition 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 230000009467 reduction Effects 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000002845 discoloration Methods 0.000 description 3
- 238000009499 grossing Methods 0.000 description 3
- 230000035939 shock Effects 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000001771 impaired effect Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000011195 cermet Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 238000007750 plasma spraying Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
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Description
本発明は、基材の表面を希土類元素（以下、ＲＥＭという）の酸化物の溶射皮膜で被覆した溶射皮膜被覆部材とその製造方法に関し、特に半導体加工装置の反応容器等に好適な優れた外観を有する溶射皮膜被覆部材およびその製造方法に関するものである。 The present invention relates to a thermal spray coating member in which the surface of a base material is coated with a thermal spray coating of an oxide of a rare earth element (hereinafter referred to as REM) and a method for manufacturing the same, and particularly, an excellent appearance suitable for a reaction vessel of a semiconductor processing apparatus. TECHNICAL FIELD The present invention relates to a thermal spray coating member having the above and a manufacturing method thereof.
溶射技術は、金属，セラミックス，サーメット等の粉末（以下、溶射材粉末という）をプラズマや燃焼炎で溶融し、基材の表面に吹き付けて皮膜を形成するものであり、様々な機械部品や容器等の表面処理に広く採用されている。しかしながら、溶射によって基材の表面に形成された皮膜（以下、溶射皮膜という）は、
(a)溶射材粉末の溶滴が基材の表面に衝突して飛沫となり、溶射位置の周辺に飛散する、
(b)溶射材粉末は必ずしも均一に溶融せず、未溶融の固形物（すなわち溶射材粉末）のまま基材の表面に吹き付けられる
等の理由で、表面に凹凸が生じる。
Thermal spraying technology involves melting powder of metal, ceramics, cermet, etc. (hereinafter referred to as thermal spray powder) with plasma or combustion flame, and spraying it on the surface of the substrate to form a coating. It is widely used for surface treatment. However, the coating formed on the surface of the substrate by thermal spraying (hereinafter referred to as thermal spray coating)
(a) The droplets of the thermal spray powder collide with the surface of the base material and become splashes, which are scattered around the spraying position.
(b) The spray material powder does not necessarily melt uniformly, and irregularities are generated on the surface, for example, because it is sprayed on the surface of the base material as an unmelted solid (that is, spray material powder).
溶射皮膜の外表面に凹凸が生じると、基材の表面を溶射皮膜で被覆した部材（以下、溶射皮膜被覆部材という）の外観が損なわれるばかりでなく、凹凸を起点として亀裂が発生し易くなるので耐熱衝撃性に悪影響を及ぼす。そこで溶射皮膜の外表面を平滑にする技術が種々検討されている。
たとえば特許文献１には、溶射皮膜に電子ビームを照射して、溶射皮膜の外表面を平滑にする技術が開示されている。また、特許文献２には、溶射皮膜にレーザービームを照射して、溶射皮膜の外表面を平滑にする技術が開示されている。これらの技術は、電子ビームやレーザービームを用いて溶射皮膜の表層部を再度溶融させることによって、溶射皮膜の外表面を平滑にするものである。
If irregularities occur on the outer surface of the thermal spray coating, not only the appearance of the member whose surface of the substrate is coated with the thermal spray coating (hereinafter referred to as the thermal spray coating member) is impaired, but cracks are likely to occur starting from the irregularities. So it has an adverse effect on thermal shock resistance. Various techniques for smoothing the outer surface of the thermal spray coating have been studied.
For example,
ところが溶射皮膜に電子ビームやレーザービームを照射すると、溶射皮膜の外表面が変色するという問題がある。たとえば、溶射材粉末としてＲＥＭ酸化物を用いて基材の表面に形成された溶射皮膜は白色であるが、電子ビームやレーザービームを照射することによって黒色に変化する。
電子ビームやレーザービームの発生装置は比較的大型であるから、溶射皮膜被覆部材の全面に電子ビームやレーザービームを照射することは困難である。つまり、機械部品や容器等に用いられる溶射皮膜被覆部材の複雑な形状の部位には照射できないので溶射皮膜が白色を呈し、その他の照射した部位では溶射皮膜が黒色を呈する。その結果、単一の溶射皮膜被覆部材であるにも関わらず白色の部位と黒色の部位が混在することになり、外観が損なわれる。
However, when the sprayed coating is irradiated with an electron beam or a laser beam, there is a problem that the outer surface of the sprayed coating is discolored. For example, a sprayed coating formed on the surface of a substrate using REM oxide as a spraying material powder is white, but turns black when irradiated with an electron beam or a laser beam.
Since the electron beam or laser beam generator is relatively large, it is difficult to irradiate the entire surface of the sprayed coating member with the electron beam or laser beam. That is, since it cannot irradiate the site | part of the complicated shape of the thermal spray coating coating | coated member used for a machine part, a container, etc., a thermal spray coating exhibits white, and the thermal spray coating exhibits black in the other irradiated part. As a result, although it is a single sprayed coating member, a white part and a black part are mixed, and the appearance is impaired.
つまり特許文献１，２に開示された技術は、溶射皮膜被覆部材の外観を向上するという観点から改善の余地が残されていた。
本発明は、半導体加工装置の反応容器等に好適な優れた外観を有する溶射皮膜被覆部材、およびその製造方法を提供することを目的とする。 An object of the present invention is to provide a thermal spray coating covering member having an excellent appearance suitable for a reaction vessel or the like of a semiconductor processing apparatus, and a manufacturing method thereof.
発明者は、溶射材粉末としてＲＥＭ酸化物を用いて形成した溶射皮膜の変色について調査検討した。その検討結果を、ＲＥＭ酸化物としてＹ2Ｏ3を溶射材粉末とした例について以下に説明する。
発明者の研究によれば、Ｙ2Ｏ3を溶射材粉末として基材の表面に形成した溶射皮膜は、Ｙ2Ｏ3を主成分とし、白色を呈する。この溶射皮膜に電子ビームやレーザービームを照射すると、Ｙ2Ｏ3の一部が還元されて、Ｙ2Ｏ2あるいはＹ2Ｏ2.5が生成して黒色に変化する。したがって照射位置に酸素ガスを供給してＹ2Ｏ3の還元を防止すれば、溶射皮膜の変色を防止できる。ただし、酸素ガスによるＹ2Ｏ3の還元防止の効果は、レーザービームの照射において顕著に発揮される。
The inventor investigated and examined the discoloration of the thermal spray coating formed using REM oxide as the thermal spray powder. The result of the examination will be described below with respect to an example in which Y 2 O 3 is used as the spray material powder as the REM oxide.
According to the inventor's research, the thermal spray coating formed on the surface of the base material using Y 2 O 3 as the thermal spray material powder has Y 2 O 3 as a main component and exhibits a white color. When this sprayed coating is irradiated with an electron beam or a laser beam, a part of Y 2 O 3 is reduced and Y 2 O 2 or Y 2 O 2.5 is generated and turns black. Therefore, if oxygen gas is supplied to the irradiation position to prevent the reduction of Y 2 O 3 , discoloration of the sprayed coating can be prevented. However, the effect of preventing reduction of Y 2 O 3 by oxygen gas is remarkably exhibited in laser beam irradiation.
また、Ｙ2Ｏ3の溶射皮膜にレーザービームを照射しつつ、その照射位置に酸素ガスを供給することによって溶射皮膜の表層部が緻密になり、溶射皮膜の外表面に存在する亀裂の長さと幅が著しく縮小されることが分かった。溶射皮膜の外表面の亀裂が縮小されることによって、溶射皮膜被覆部材の外観が改善される。
本発明は、これらの知見に基づいてなされたものである。
In addition, by irradiating the Y 2 O 3 sprayed coating with a laser beam and supplying oxygen gas to the irradiated position, the surface layer of the sprayed coating becomes dense, and the length of cracks existing on the outer surface of the sprayed coating It was found that the width was significantly reduced. The appearance of the thermal spray coating member is improved by reducing cracks on the outer surface of the thermal spray coating.
The present invention has been made based on these findings.
すなわち本発明は、基材の表面がＲＥＭ酸化物の溶射皮膜で被覆され、溶射皮膜の外表面から深さ50μｍ以下の領域に形成される緻密な組織の気孔率が１％未満であり、かつ緻密な組織が透明または白色を呈するとともに、溶射皮膜の外表面の粗さがＲa１〜３μｍの範囲内を満足する優れた外観を有する溶射皮膜被覆部材である。
本発明の溶射皮膜被覆部材においては、ＲＥＭ酸化物がＹ2Ｏ3であることが好ましい。
That is, according to the present invention, the surface of the substrate is coated with a sprayed coating of REM oxide, and the porosity of the dense tissue formed in a region having a depth of 50 μm or less from the outer surface of the sprayed coating is less than 1%, and This is a thermal spray coating member having an excellent appearance in which a dense structure is transparent or white and the outer surface roughness of the thermal spray coating satisfies the range of
In the thermal spray coating member of the present invention, the REM oxide is preferably Y 2 O 3 .
また本発明は、基材の表面にＲＥＭ酸化物の溶射皮膜を形成し、次いで溶射皮膜の外表面にレーザービームを照射しつつ、レーザービームの照射面における酸素濃度80体積％以上となるように純酸素を吹き付ける優れた外観を有する溶射皮膜被覆部材の製造方法である。
あるいは本発明は、基材の表面にＲＥＭ酸化物の溶射皮膜を形成し、次いで酸素濃度80体積％以上となる雰囲気中で溶射皮膜の外表面にレーザービームを照射する優れた外観を有する溶射皮膜被覆部材の製造方法である。
Further, in the present invention, a thermal spray coating of REM oxide is formed on the surface of the substrate, and then the outer surface of the thermal spray coating is irradiated with a laser beam so that the oxygen concentration on the laser beam irradiation surface is 80% by volume or more. It is a manufacturing method of a thermal spray coating covering member which has the outstanding appearance which sprays pure oxygen.
Alternatively, the present invention provides a thermal spray coating having an excellent appearance in which a thermal spray coating of REM oxide is formed on the surface of a substrate and then the outer surface of the thermal spray coating is irradiated with a laser beam in an atmosphere having an oxygen concentration of 80% by volume or more. It is a manufacturing method of a covering member.
本発明の溶射皮膜被覆部材の製造方法においては、ＲＥＭ酸化物がＹ2Ｏ3であることが好ましい。 In the method for producing a thermal spray coating member according to the present invention, the REM oxide is preferably Y 2 O 3 .
本発明によれば、半導体加工装置の反応容器等に好適な優れた耐熱衝撃性を有するとともに、良好な外観を有する溶射皮膜被覆部材を得ることができる。 ADVANTAGE OF THE INVENTION According to this invention, while having the outstanding thermal shock resistance suitable for the reaction container etc. of a semiconductor processing apparatus, the thermal spray coating coating | coated member which has a favorable external appearance can be obtained.
本発明の溶射皮膜被覆部材とその製造方法について、製造手順に沿って説明する。
所定の形状に加工成形した基材の表面にＲＥＭ酸化物の溶射皮膜を形成する。その例を図２に示す。溶射皮膜２を形成するにあたって、溶射材粉末としてＲＥＭ酸化物の粉末を用いる。この溶射皮膜２は、Ｙ2Ｏ3の場合、透明または白色を呈する。ここでＲＥＭは、周期表の３族に属する元素を指す。ただしＲＥＭに分類される元素のうちのＹが、溶射皮膜被覆部材の外観を改善する効果を最も顕著に発揮する。
The thermal spray coating member of the present invention and the manufacturing method thereof will be described along the manufacturing procedure.
A thermal spray coating of REM oxide is formed on the surface of the base material processed and molded into a predetermined shape. An example is shown in FIG. In forming the thermal spray coating 2, REM oxide powder is used as the thermal spray powder. In the case of Y 2 O 3 , the sprayed coating 2 is transparent or white. Here, REM refers to an element belonging to Group 3 of the periodic table. However, Y among the elements classified as REM exhibits the effect of improving the appearance of the thermal spray coating member most significantly.
溶射皮膜２の厚みＬ1は300μｍ以下が好ましい。その理由は、厚みＬ1が300μｍを超えると、後述するレーザービームの照射によって、溶射皮膜が剥離し易いからである。なお、溶射皮膜の厚みＬ1は200μｍ以下が一層好ましい。溶射皮膜被覆部材として複数の溶射皮膜（たとえばアンダーコート，トップコート等）を形成する場合は、それらの溶射皮膜の厚みを合計300μｍ以下（より好ましくは合計200μｍ以下）とすることが好ましい。 The thickness L 1 of the thermal spray coating 2 is preferably 300 μm or less. The reason is that when the thickness L 1 exceeds 300 μm, the thermal spray coating is easily peeled off by laser beam irradiation described later. The thickness L 1 of the thermal spray coating is more preferably 200 μm or less. When a plurality of sprayed coatings (for example, undercoat, topcoat, etc.) are formed as the sprayed coating covering member, it is preferable that the thickness of these sprayed coatings is 300 μm or less in total (more preferably 200 μm or less in total).
この溶射皮膜２にレーザービームを照射する。ただし、溶射皮膜２の全面にレーザービームを同時に照射することは困難であるから、照射点を移動させながらレーザービームを照射する。その結果、レーザービームによって溶射皮膜２の表層部が溶融して再凝固するので、緻密な組織が得られ、かつその外表面が平滑になる。その例を図１に示す。
この緻密な組織３は、溶射皮膜の外表面から深さ（すなわち緻密な組織３の厚みＬ2）50μｍ以下の領域に形成され、気孔率は１％未満である。気孔率は、溶射皮膜の表層部に形成される緻密な組織３の断面を電子顕微鏡（1000倍）で観察し、クラックを除いた空隙の合計面積を測定し、その視野に占める空隙の比率を百分率で示す値である。緻密な組織３の外表面（すなわち溶射皮膜の外表面）の粗さはＲa１〜３μｍである。なお、緻密な組織３の下方に位置する溶射皮膜（すなわち溶融，再凝固を生じていないＲＥＭ酸化物）の気孔率は１〜５％であり、その粗さはＲa４〜６μｍである。
This thermal spray coating 2 is irradiated with a laser beam. However, since it is difficult to simultaneously irradiate the entire surface of the thermal spray coating 2 with a laser beam, the laser beam is irradiated while moving the irradiation point. As a result, the surface layer portion of the thermal spray coating 2 is melted and re-solidified by the laser beam, so that a dense structure is obtained and the outer surface thereof becomes smooth. An example is shown in FIG.
The dense structure 3 is formed in a region having a depth of 50 μm or less from the outer surface of the thermal spray coating (that is, the thickness L 2 of the dense structure 3), and the porosity is less than 1%. The porosity is determined by observing the cross section of the dense structure 3 formed on the surface layer of the sprayed coating with an electron microscope (1000 times), measuring the total area of voids excluding cracks, and determining the ratio of voids in the field of view. It is a value expressed as a percentage. The roughness of the outer surface of the dense structure 3 (that is, the outer surface of the sprayed coating) is Ra 1 to 3 μm. In addition, the porosity of the thermal spray coating (namely, REM oxide which has not melted and re-solidified) located below the dense structure 3 is 1 to 5%, and its roughness is Ra 4 to 6 μm.
照射するレーザービームは、特定の種類に限定しない。ただし、ＹＡＧレーザービーム，ＣＯ2レーザービーム，半導体レーザービーム等を使用すれば、溶射皮膜被覆部材の外観を改善する効果が顕著に発揮されるので好ましい。
本発明ではレーザービームを照射しながら、その照射点に純酸素を吹き付ける。その際、レーザービームを照射する面における酸素濃度を80体積％以上とする。レーザービームの照射面における酸素濃度は、純酸素の流量あるいはノズルと照射面との距離等に応じて変化するので、酸素濃度が80体積％以上となるように設定条件を適宜調整する。レーザービームの照射面における酸素濃度が80体積％未満では、レーザービームの照射によるＲＥＭ酸化物の還元を防止できず、溶射皮膜の変色を防止できない。
The laser beam to be irradiated is not limited to a specific type. However, it is preferable to use a YAG laser beam, a CO 2 laser beam, a semiconductor laser beam or the like because the effect of improving the appearance of the thermal spray coating member is remarkably exhibited.
In the present invention, pure oxygen is sprayed to the irradiation point while irradiating the laser beam. At that time, the oxygen concentration on the surface irradiated with the laser beam is set to 80% by volume or more. Since the oxygen concentration on the laser beam irradiation surface changes according to the flow rate of pure oxygen or the distance between the nozzle and the irradiation surface, the setting conditions are adjusted as appropriate so that the oxygen concentration is 80% by volume or more. When the oxygen concentration on the laser beam irradiation surface is less than 80% by volume, reduction of the REM oxide due to laser beam irradiation cannot be prevented, and discoloration of the sprayed coating cannot be prevented.
あるいは酸素濃度が80体積％以上となる雰囲気中でレーザービームを照射する。
レーザービームの照射面における雰囲気ガスの酸素以外の残部は、特定の成分に限定しない。ただし酸素以外の残部が不活性ガス（たとえば窒素，アルゴン等）であれば、レーザービームの照射によってＲＥＭ酸化物が還元されるのを防止する効果が高められる。
このようにしてレーザービームを照射しつつその照射点面に酸素を吹き付ける、あるいは酸素雰囲気中でレーザービームを照射することによって、ＲＥＭ酸化物の還元を防止できる。
Alternatively, the laser beam is irradiated in an atmosphere where the oxygen concentration is 80% by volume or more.
The remainder of the atmosphere gas other than oxygen on the laser beam irradiation surface is not limited to a specific component. However, if the balance other than oxygen is an inert gas (for example, nitrogen, argon, etc.), the effect of preventing the REM oxide from being reduced by laser beam irradiation is enhanced.
Thus, reduction of the REM oxide can be prevented by irradiating a laser beam while spraying oxygen on the irradiation point surface or irradiating the laser beam in an oxygen atmosphere.
たとえばＹ2Ｏ3の溶射皮膜の場合は、照射した後も溶射皮膜は透明または白色を呈する。その結果、溶射皮膜のレーザービームを照射した部位と照射しなかった部位が、ともに透明または白色を呈するようになり、外表面の平滑化と相まって良好な外観が得られる。
ここではＲＥＭ酸化物の一例としてＹ2Ｏ3を挙げたが、本発明はＲＥＭ酸化物をＹ2Ｏ3に限定するものではない。Ｙ2Ｏ3以外のＲＥＭ酸化物の溶射皮膜は、必ずしも白色ではなく、青色，桃色，淡黄色等を呈するものもある。このような溶射皮膜に酸素を供給しながらレーザービームを照射すると、溶射皮膜の表層部に形成される緻密な組織は必ずしも白色にはならない。そのような溶射皮膜であっても、緻密な組織は透明になるので、色調の変化は認められず、良好な外観が得られる。あるいは、緻密な組織が透明にならない場合は、溶射皮膜と同様の色調を有する緻密な組織が得られるので、良好な外観が得られる。
For example, in the case of a Y 2 O 3 sprayed coating, the sprayed coating is transparent or white even after irradiation. As a result, the portion of the sprayed coating that has been irradiated with the laser beam and the portion that has not been irradiated are both transparent or white, and a good appearance is obtained in combination with the smoothing of the outer surface.
Here, Y 2 O 3 is cited as an example of a REM oxide, but the present invention does not limit the REM oxide to Y 2 O 3 . A sprayed coating of REM oxide other than Y 2 O 3 is not necessarily white, but may exhibit blue, pink, light yellow, and the like. When a laser beam is irradiated while supplying oxygen to such a thermal spray coating, the dense structure formed in the surface layer portion of the thermal spray coating does not necessarily become white. Even with such a thermal spray coating, the dense structure becomes transparent, so no change in color tone is observed and a good appearance is obtained. Alternatively, when the dense structure does not become transparent, a dense structure having the same color tone as that of the sprayed coating can be obtained, so that a good appearance can be obtained.
また、溶射皮膜を形成する過程で、色調の異なる部位が分散する場合がある。たとえばＹ2Ｏ3の溶射皮膜の場合は、時として、透明または白色の表面に黒色の部位が分散する。このような場合でも本発明を適用して溶射皮膜の表層部に緻密な組織を形成すると、黒色の部位が透明または白色に変化し、全面が透明または白色を呈するようになる。 Further, in the process of forming the thermal spray coating, parts having different color tones may be dispersed. For example, in the case of a sprayed coating of Y 2 O 3 , sometimes black portions are dispersed on a transparent or white surface. Even in such a case, when the present invention is applied to form a dense structure in the surface layer portion of the thermal spray coating, the black portion changes to transparent or white, and the entire surface becomes transparent or white.
一辺50mmの正方形のSUS304鋼（厚み３mm）を基材試験片とし、その基材試験片の片面にショットブラストを施して粗化表面とした。次いで、基材試験片の粗化表面に大気プラズマ溶射法によって50質量％Al2Ｏ3−50質量％Ｙ2Ｏ3-の溶射皮膜（厚み150μｍ）をアンダーコートとして施工した後、溶射材粉末としてＹ2Ｏ3-を用いて大気プラズマ溶射を行ない、アンダーコートの表面にＹ2Ｏ3-の溶射皮膜（厚み150μｍ）をトップコートとして形成した。この溶射皮膜（すなわちトップコート）の外観は白色であった。 A square SUS304 steel (thickness 3 mm) with a side of 50 mm was used as a base material test piece, and a shot blast was applied to one side of the base material test piece to obtain a roughened surface. Then, after construction 50 wt% Al 2 O 3 -50 wt% Y 2 O 3- of the thermal spray coating (thickness 150 [mu] m) as an undercoat by atmospheric plasma spraying method roughened surface of the substrate specimens, the thermal spraying material powder as Y 2 O 3- performs air plasma spray was used to form Y 2 O 3- of the thermal spray coating (thickness 150 [mu] m) as a top coat on the surface of the undercoat. The appearance of this sprayed coating (ie, top coat) was white.
次に、トップコートの表面にＹＡＧレーザービームを照射して、溶射皮膜被覆試験片とした。その際、照射点に純酸素ガスを供給した。これを発明例とする。ＹＡＧレーザービームの照射条件と酸素ガスの供給条件は表１に示す通りである。 Next, the surface of the top coat was irradiated with a YAG laser beam to obtain a sprayed coating-coated test piece. At that time, pure oxygen gas was supplied to the irradiation point. This is an invention example. Table 1 shows the YAG laser beam irradiation conditions and oxygen gas supply conditions.
一方、比較例として、酸素ガスを供給せず、トップコートの表面にＹＡＧレーザービームを照射して、溶射皮膜被覆試験片とした。ＹＡＧレーザービームの照射条件を表１に併せて示す。基材試験片やアンダーコート，トップコートの作製の手順は、発明例と同じであるから説明を省略する。
発明例と比較例の溶射皮膜被覆試験片について、外観の色調を調査したところ、発明例の外観は白色であったのに対して、比較例の外観は黒色であった。発明例の溶射皮膜被覆試験片の外観は、ＹＡＧレーザービームを照射する前の外観と同等の色調であり、比較例に比べて優れた外観を有していた。
On the other hand, as a comparative example, oxygen gas was not supplied, and the surface of the top coat was irradiated with a YAG laser beam to obtain a sprayed coating-coated test piece. Table 1 also shows the irradiation conditions of the YAG laser beam. The procedure for producing the base material test piece, the undercoat, and the topcoat is the same as that of the invention example, and thus the description thereof is omitted.
When the color tone of the appearance of the thermal spray coating coated test pieces of the inventive example and the comparative example was examined, the appearance of the inventive example was white, whereas the appearance of the comparative example was black. The appearance of the sprayed coating-coated test piece of the inventive example had the same color tone as that of the appearance before irradiation with the YAG laser beam, and had an excellent appearance as compared with the comparative example.
さらに、それぞれの溶射皮膜被覆試験片を300℃に加熱しさらに常温まで空冷する熱サイクルを10回繰り返した後、溶射皮膜を目視で観察し、剥離の有無を調査した。その結果、いずれも溶射皮膜の剥離は認められなかった。
したがって、発明例の溶射皮膜被覆試験片の耐熱衝撃性は比較例と同等であり、外観は比較例に比べて良好であることが確かめられた。
Furthermore, after each thermal spray coating test piece was heated to 300 ° C. and further air-cooled to room temperature for 10 times, the thermal spray coating was visually observed to investigate the presence or absence of peeling. As a result, no thermal spray coating was observed.
Therefore, it was confirmed that the thermal shock resistance of the thermal spray coating-coated test piece of the inventive example was equivalent to that of the comparative example, and the appearance was better than that of the comparative example.
１ 基材
２ 溶射皮膜
３ 緻密な組織
DESCRIPTION OF
Claims (5)
The method for producing a thermal spray coating member having an excellent appearance according to claim 3 or 4, wherein the REM oxide is Y 2 O 3 .
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| JP5001323B2 (en) * | 2009-03-27 | 2012-08-15 | トーカロ株式会社 | White yttrium oxide spray coating surface modification method and yttrium oxide spray coating coating member |
| JP5167491B2 (en) * | 2010-09-24 | 2013-03-21 | トーカロ株式会社 | Thermal spray coating coated member with excellent corrosion resistance and plasma erosion resistance and crack prevention method for thermal spray coating treated with high energy irradiation |
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