JP2014173106A - Deposition preventive plate for vacuum film deposition apparatus, vacuum film deposition apparatus, and vacuum film deposition method - Google Patents
Deposition preventive plate for vacuum film deposition apparatus, vacuum film deposition apparatus, and vacuum film deposition method Download PDFInfo
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- JP2014173106A JP2014173106A JP2013044908A JP2013044908A JP2014173106A JP 2014173106 A JP2014173106 A JP 2014173106A JP 2013044908 A JP2013044908 A JP 2013044908A JP 2013044908 A JP2013044908 A JP 2013044908A JP 2014173106 A JP2014173106 A JP 2014173106A
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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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/56—Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks
- C23C14/564—Means for minimising impurities in the coating chamber such as dust, moisture, residual gases
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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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
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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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
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Abstract
Description
本発明は、真空蒸着装置やスパッタリング装置等の真空成膜装置に用いられる防着板に関し、詳しくは、付着した成膜材料の剥離を防止することができる真空成膜装置用防着板に関する。 The present invention relates to an adhesion-preventing plate used in a vacuum film-forming apparatus such as a vacuum vapor deposition apparatus or a sputtering apparatus, and more particularly to an adhesion-preventing plate for a vacuum film-forming apparatus that can prevent peeling of attached film-forming material.
スパッタリング装置等の真空成膜装置は、真空チャンバの内壁や各種構成部品への成膜材料の付着による汚染を防止するため、被成膜基材の周囲に防着板（防着シート）を備えている。
このような防着板の表面には、付着した成膜材料の剥離を防ぎ、成膜材料の剥離に起因するパーティクルの発生を抑える観点から、凹凸を形成することが知られている。
Vacuum deposition equipment such as sputtering equipment is equipped with a deposition plate (a deposition sheet) around the substrate to be deposited in order to prevent contamination due to deposition of deposition materials on the inner wall of the vacuum chamber and various components. ing.
It is known to form irregularities on the surface of such a deposition preventing plate from the viewpoint of preventing the peeling of the deposited film forming material and suppressing the generation of particles due to the peeling of the film forming material.
例えば、特許文献１には、「第１の面を有し、任意の形状に折り曲げ可能な金属製のシート基材と、前記第１の面に形成され、前記第１の面内に島状に分布する複数の突出部と、前記第１の面及び前記突出部の表面に形成された凹凸部とを具備する成膜装置用シート。」が記載されており（［請求項１］）、また、突出部がエンボス加工により形成され、凹凸部がブラスト加工により形成されることが記載されている（［請求項２］［請求項３］）。 For example, Patent Document 1 states that “a metal sheet base material that has a first surface and can be bent into an arbitrary shape, and is formed on the first surface and has an island shape in the first surface. A film forming apparatus sheet comprising a plurality of protrusions distributed on the surface, and uneven portions formed on the first surface and the surface of the protrusions ([Claim 1]). Further, it is described that the protruding portion is formed by embossing and the uneven portion is formed by blasting ([Claim 2] [Claim 3]).
しかしながら、特許文献１に記載の成膜装置用シート（防着板）では、蒸着を繰り返した際に、成膜材料の剥離防止効果が十分ではない場合があることが明らかとなった。 However, it has been clarified that the film forming apparatus sheet (protection plate) described in Patent Document 1 may not have a sufficient effect of preventing the film forming material from being peeled off when repeated deposition is performed.
そこで、本発明は、蒸着を繰り返した場合にも成膜材料の剥離防止効果に優れる真空成膜装置用防着板およびその製造方法、ならびに、この防着板を用いる真空成膜装置および真空成膜方法を提供することを目的とする。 Accordingly, the present invention provides an adhesion preventing plate for a vacuum film forming apparatus that is excellent in the effect of preventing the peeling of the film forming material even when deposition is repeated, a manufacturing method thereof, a vacuum film forming apparatus using the adhesion preventing plate, and a vacuum forming apparatus. An object is to provide a membrane method.
本発明者は、上記目的を達成すべく鋭意研究した結果、特定の平均開口径の凹部を含む凹凸構造が形成された表面を有し、この表面に特定の平均高さの複数の突出部を所定の割合で配列させることにより、蒸着を繰り返した場合にも成膜材料の剥離防止効果が高くなることを見出し、本発明を完成させた。
すなわち、以下の構成により上記目的を達成することができることを見出した。
As a result of earnest research to achieve the above object, the inventor has a surface on which an uneven structure including a recess having a specific average opening diameter is formed, and a plurality of protrusions having a specific average height are formed on the surface. By arranging at a predetermined ratio, it was found that the effect of preventing the film-forming material from peeling off was increased even when deposition was repeated, and the present invention was completed.
That is, it has been found that the above object can be achieved by the following configuration.
（１） 真空成膜装置において、不要な位置への成膜材料の付着を防止するための真空成膜装置用防着板であって、
アルミニウム製であり、
平均開口径０．０１〜９μｍの凹部を含む凹凸構造が形成された表面を有し、
表面に、平均高さ３０〜１０００μｍの複数の突出部が配列されており、
突出部の平均密度が、１０個／１０ｍｍ角以上であり、
突出部の底部面積の比率が、１０ｍｍ角の領域において９０％超である真空成膜装置用防着板。
（２） 突出部の垂直方向上方から見た時の外形が、菱形、矩形または円形である（１）に記載の真空成膜装置用防着板。
（３） 凹凸構造が、平均開口径０．５〜９μｍの凹部を含む凹凸構造、または、平均開口径０．０１〜０．３μｍの凹部を含む凹凸構造である、（１）または（２）に記載の真空成膜装置用防着板。
（４） 凹凸構造が、平均開口径０．５〜９μｍの凹部を含む凹凸構造に、平均開口径０．０１〜０．３μｍの凹部を含む凹凸構造が重畳された凹凸構造である、（１）〜（３）のいずれかに記載の真空成膜装置用防着板。
（５） 表面が、アルミニウムの陽極酸化皮膜で構成される（１）〜（４）のいずれかに記載の真空成膜装置用防着板。
（６） 表面に、クラックを有する（１）〜（５）のいずれかに記載の真空成膜装置用防着板。
（７） 突出部が、エンボス加工により形成される（１）〜（６）のいずれかに記載の真空成膜装置用防着板。
（８） 平均開口径０．０１〜９μｍの凹部を含む凹凸構造が、電気化学的粗面化処理により形成される（１）〜（７）のいずれかに記載の真空成膜装置用防着板。
(1) In a vacuum film forming apparatus, a deposition plate for a vacuum film forming apparatus for preventing adhesion of a film forming material to an unnecessary position,
Made of aluminum,
It has a surface on which a concavo-convex structure including recesses having an average opening diameter of 0.01 to 9 μm is formed,
A plurality of protrusions having an average height of 30 to 1000 μm are arranged on the surface,
The average density of the protrusions is 10 pieces / 10 mm square or more,
A deposition preventing plate for a vacuum film-forming apparatus, wherein the ratio of the bottom area of the protruding portion is more than 90% in a 10 mm square region.
(2) The deposition plate for a vacuum film forming apparatus according to (1), wherein the outer shape of the protruding portion when viewed from above in the vertical direction is a rhombus, a rectangle, or a circle.
(3) The concavo-convex structure is a concavo-convex structure including a concave portion having an average opening diameter of 0.5 to 9 μm, or a concavo-convex structure including a concave portion having an average opening diameter of 0.01 to 0.3 μm (1) or (2) 2. An adhesion-preventing plate for a vacuum film-forming apparatus as described in 1.
(4) The concavo-convex structure is a concavo-convex structure in which a concavo-convex structure including concave portions having an average opening diameter of 0.01 to 0.3 μm is superimposed on a concavo-convex structure including concave portions having an average opening diameter of 0.5 to 9 μm. The deposition preventing plate for a vacuum film-forming apparatus according to any one of (1) to (3).
(5) The deposition preventing plate for a vacuum film forming apparatus according to any one of (1) to (4), wherein the surface is composed of an anodized film of aluminum.
(6) The deposition preventing plate for a vacuum film forming apparatus according to any one of (1) to (5), wherein the surface has a crack.
(7) The deposition preventing plate for a vacuum film forming apparatus according to any one of (1) to (6), wherein the protrusion is formed by embossing.
(8) The deposition structure for a vacuum film forming apparatus according to any one of (1) to (7), wherein a concavo-convex structure including a concave portion having an average opening diameter of 0.01 to 9 μm is formed by an electrochemical roughening treatment. Board.
（９） 真空成膜装置において、不要な位置への成膜材料の付着を防止するための真空成膜装置用防着板を製造する製造方法であって、
アルミニウム板の表面に電気化学的粗面化処理を施し、表面に平均開口径０．０１〜９μｍの凹部を含む凹凸構造を形成する凹凸形成工程と、
アルミニウム板の表面にエンボス加工を施し、表面の一部に平均高さ３０〜１０００μｍの複数の突出部を形成する突出部形成工程とを有する製造方法。
（１０） 凹凸形成工程の後に、陽極酸化処理を施し、表面にアルミニウムの陽極酸化皮膜を形成する陽極酸化処理工程を有する（９）に記載の真空成膜装置用防着板の製造方法。
（１１） 突出部形成工程の後に、焼鈍処理を施す焼鈍処理工程を有する（９）または（１０）に記載の真空成膜装置用防着板の製造方法。
(9) In a vacuum film forming apparatus, a manufacturing method for manufacturing a deposition plate for a vacuum film forming apparatus for preventing adhesion of a film forming material to an unnecessary position,
An uneven surface forming step of performing an electrochemical surface roughening treatment on the surface of the aluminum plate and forming an uneven structure including recesses having an average opening diameter of 0.01 to 9 μm on the surface;
The manufacturing method which has a protrusion part formation process which gives the embossing to the surface of an aluminum plate, and forms several protrusion part with an average height of 30-1000 micrometers in a part of surface.
(10) The method for producing a deposition-preventing plate for a vacuum film-forming apparatus according to (9), further comprising an anodizing treatment step of forming an aluminum anodized film on the surface after an unevenness forming step.
(11) The manufacturing method of the deposition prevention board for vacuum film-forming apparatuses as described in (9) or (10) which has an annealing treatment process which performs an annealing process after a protrusion part formation process.
（１２） （１）〜（８）のいずれかに記載の真空成膜装置用防着板を有する真空成膜装置。 (12) A vacuum film forming apparatus having the deposition preventive plate for a vacuum film forming apparatus according to any one of (1) to (8).
（１３） （１）〜（８）のいずれかに記載の真空成膜装置用防着板を有する真空成膜装置を用いて、被成膜基板の表面に、Ｔｉ、Ｚｒ、Ｎｂ、Ｔａ、Ｃｒ、Ｍｏ、Ｗ、Ｐｔ、Ａｕ、Ａｇ、Ｆｅ、Ｎｉ、Ｍｎ、Ｓｎ、Ｚｎ、Ｃｏ、Ａｌ、ＣｕおよびＳｉから選択された１種の元素、または、その合金、窒化物もしくは酸化物を成膜する真空成膜方法。 (13) Using the vacuum film-forming apparatus having the vacuum film-forming apparatus deposition plate according to any one of (1) to (8), Ti, Zr, Nb, Ta, One element selected from Cr, Mo, W, Pt, Au, Ag, Fe, Ni, Mn, Sn, Zn, Co, Al, Cu and Si, or an alloy, nitride or oxide thereof is formed. Vacuum film forming method for film formation.
本発明によれば、蒸着を繰り返した場合にも成膜材料の剥離防止効果に優れる真空成膜装置用防着板およびその製造方法、ならびに、この防着板を用いる真空成膜装置および真空成膜方法を提供することができる。 According to the present invention, the deposition preventing plate for a vacuum film forming apparatus that is excellent in the effect of preventing the peeling of the film forming material even when deposition is repeated, the manufacturing method thereof, the vacuum film forming apparatus using this deposition preventing plate, and the vacuum deposition A membrane method can be provided.
以下に、本発明の真空成膜装置用防着板およびその製造方法、ならびに、この防着板を用いる真空成膜装置および真空成膜方法の好適態様について詳述する。
まず、本発明の従来技術と比較した特徴点について詳述する。
上述したように、本発明の特徴点の１つは、特定の平均開口径の凹部を含む凹凸構造が形成された表面を有し、この表面に特定の平均高さの複数の突出部が所定の割合で配列している点である。本発明者は、本発明の効果が得られる理由を以下のように推測する。なお、この推測によって本発明の範囲が限定的に解釈されるものではない。
すなわち、凹凸構造に含まれる平均開口径が０．０１〜９μｍの凹部が、防着板に付着した成膜材料を非常に強く保持するため、特に付着した材料が薄い場合であっても、剥離によるパーティクルの発生を抑制することができると考えられる。
また、平均高さが３０〜１０００μｍの突出部が、防着板に付着した成膜材料の残留応力、特に繰り返し蒸着による温度変化（熱サイクル）により防着板の基材および成膜材料に生じる熱膨張に起因する応力を緩和することができるため、蒸着を繰り返した場合にも剥離によるパーティクルの発生を抑制することができると考えられる。具体的には、この突出部を表面の大部分に存在させることにより、等方位的な伸縮（等方性）を可能とし、その結果、防着板の基材および防着板に付着した成膜材料の残留応力（内部応力）に起因する成膜材料の反りなどによる変形や剥離を防止することができると考えられる。
このような特徴を有する本発明によれば、防着板から剥離したパーティクルが基板に付着することに起因する製品不良や品質低下が無い、高品質な製品を安定して作製することができる。
そのため、本発明によれば、真空成膜法を利用する半導体装置の製造や電子部品材料の製造において、防着板から剥離したパーティクルに起因する製品の不良等の発生を防止して、製品歩留りの向上、生産性の向上、生産コストの低減等を図ることができる。
In the following, preferred embodiments of the vacuum deposition apparatus for vacuum film-forming apparatus and the method for producing the same, and the vacuum film-forming apparatus and vacuum film-forming method using this deposition board will be described in detail.
First, the feature point compared with the prior art of this invention is explained in full detail.
As described above, one of the features of the present invention has a surface on which a concavo-convex structure including a concave portion having a specific average opening diameter is formed, and a plurality of protrusions having a specific average height are predetermined on the surface. It is the point which is arranged in the ratio of. The inventor presumes the reason why the effect of the present invention is obtained as follows. Note that the scope of the present invention is not limitedly interpreted by this estimation.
That is, since the concave portion having an average opening diameter of 0.01 to 9 μm included in the concavo-convex structure holds the film forming material adhering to the adhesion preventing plate very strongly, even if the adhering material is thin, it is peeled off. It is considered that the generation of particles due to the can be suppressed.
Further, protrusions having an average height of 30 to 1000 μm are generated in the base material and the film forming material of the deposition plate due to the residual stress of the film deposition material adhering to the deposition plate, particularly the temperature change (thermal cycle) due to repeated vapor deposition. Since stress due to thermal expansion can be relieved, it is considered that generation of particles due to peeling can be suppressed even when deposition is repeated. Specifically, by allowing this protrusion to exist over most of the surface, it is possible to expand and contract in an isotropic direction (isotropic property), and as a result, the component adhered to the base material and the anti-adhesion plate of the anti-adhesion plate. It is considered that deformation and peeling due to the warp of the film forming material due to the residual stress (internal stress) of the film material can be prevented.
According to the present invention having such characteristics, it is possible to stably produce a high-quality product that is free from product defects and quality degradation caused by particles peeled off from the deposition preventing plate adhering to the substrate.
Therefore, according to the present invention, in the manufacture of semiconductor devices and electronic component materials using the vacuum film formation method, the product yield is prevented by preventing the occurrence of product defects due to the particles peeled off from the deposition preventive plate. Improvement of productivity, improvement of productivity, reduction of production cost, etc. can be aimed at.
以下では、まず、本発明の真空成膜方法および真空成膜装置について説明し、その後、本発明の真空成膜装置用防着板（以下、本発明の「防着板」と略す。）およびその製造方法について詳述する。 In the following, first, the vacuum film forming method and the vacuum film forming apparatus of the present invention will be described, and thereafter, the deposition preventing plate for the vacuum deposition apparatus of the present invention (hereinafter abbreviated as “an adhesion preventing plate” of the present invention) and. The manufacturing method will be described in detail.
〔真空成膜方法および真空成膜装置〕
図１に、本発明の真空成膜方法の一例を実施する、本発明の真空成膜装置の一例を概念的に示す。
[Vacuum film forming method and vacuum film forming apparatus]
FIG. 1 conceptually shows an example of a vacuum film forming apparatus of the present invention, which implements an example of the vacuum film forming method of the present invention.
図１に示す本発明の真空成膜装置１０は、真空蒸着によって被成膜部材である基板Ｚの表面に成膜を行う装置であり、後述する本発明の防着板１２を有するものである。
また、本発明の真空成膜方法は、本発明の防着板１２を有する本発明の真空成膜装置１０を用いて、基板Ｚの表面に、Ｔｉ、Ｚｒ、Ｎｂ、Ｔａ、Ｃｒ、Ｍｏ、Ｗ、Ｐｔ、Ａｕ、Ａｇ、Ｆｅ、Ｎｉ、Ｍｎ、Ｓｎ、Ｚｎ、Ｃｏ、Ａｌ、ＣｕおよびＳｉから選択される１種の元素、または、その合金、窒化物もしくは酸化物を成膜する成膜方法である。
A vacuum film forming apparatus 10 of the present invention shown in FIG. 1 is an apparatus for forming a film on the surface of a substrate Z as a film forming member by vacuum vapor deposition, and has a deposition plate 12 of the present invention to be described later. .
Moreover, the vacuum film-forming method of the present invention uses the vacuum film-forming apparatus 10 of the present invention having the adhesion-preventing plate 12 of the present invention to form Ti, Zr, Nb, Ta, Cr, Mo, Film formation for forming one element selected from W, Pt, Au, Ag, Fe, Ni, Mn, Sn, Zn, Co, Al, Cu and Si, or an alloy, nitride or oxide thereof. Is the method.
ここで、本発明の真空成膜方法および真空成膜装置は、図示例のような真空蒸着によって基板Ｚの表面に成膜を行うものに限定されない。
すなわち、本発明の真空成膜方法および真空成膜装置は、スパッタリング、ＣＶＤ、プラズマＣＶＤ、イオンプレーティングなど、公知の各種のＣＶＤ(chemical vapor deposition 化学的気相成膜法）およびＰＶＤ(physical vapor deposition 物理的気相成膜法)による真空成膜に適用することができる。
同様に、本発明の真空成膜方法および真空成膜装置においては、成膜条件も特に限定されず、成膜方法、成膜する膜、成膜レート、成膜する膜の膜厚等に応じて、適宜、設定すればよい。
Here, the vacuum film forming method and the vacuum film forming apparatus of the present invention are not limited to those which form a film on the surface of the substrate Z by vacuum vapor deposition as shown in the illustrated example.
That is, the vacuum film forming method and the vacuum film forming apparatus of the present invention include various known CVD (chemical vapor deposition) and PVD (physical vapor) methods such as sputtering, CVD, plasma CVD, and ion plating. Deposition can be applied to vacuum deposition by physical vapor deposition.
Similarly, in the vacuum film forming method and the vacuum film forming apparatus of the present invention, the film forming conditions are not particularly limited, depending on the film forming method, the film to be formed, the film forming rate, the film thickness of the film to be formed, and the like. And may be set as appropriate.
図１に示すように、本発明の真空成膜装置１０は、公知の真空蒸着装置と同様、真空チャンバ１４と、真空チャンバ１４の内に配置される蒸着源１６および基板ホルダ１８と、真空ポンプ２０とを有する。
そして、本発明の真空成膜装置１０は、真空チャンバ１４の内壁面を覆って、本発明の防着板１２が設けられる。
As shown in FIG. 1, a vacuum film forming apparatus 10 according to the present invention includes a vacuum chamber 14, a vapor deposition source 16 and a substrate holder 18 disposed in the vacuum chamber 14, and a vacuum pump, as in a known vacuum vapor deposition apparatus. And 20.
And the vacuum film-forming apparatus 10 of this invention covers the inner wall face of the vacuum chamber 14, and the adhesion prevention board 12 of this invention is provided.
ここで、本発明の真空成膜装置１０は、本発明の防着板１２を用いる以外は、基本的に、公知の真空蒸着装置と同様である。この点に関しては、スパッタリング装置やプラズマＣＶＤ装置等の他の真空成膜装置（方法）に適用した場合でも、同様である。
そのため、本発明の真空成膜装置１０においては、蒸着源１６は、成膜材料が充填され、溶融、蒸発する公知の蒸着源（蒸発源）である。また、基板ホルダ１８も、公知の手段で基板Ｚを保持する公知の基板ホルダである。さらに、真空ポンプ２０も、真空チャンバ１４内を排気して、所定の成膜圧力に保つための、公知の真空ポンプである。
また、本発明の真空成膜装置１０は、必要に応じて、基板ホルダ１８（基板Ｚ）を回転（自転、公転、自公転）する回転手段を有してもよい。
Here, the vacuum film forming apparatus 10 of the present invention is basically the same as a known vacuum deposition apparatus except that the deposition preventing plate 12 of the present invention is used. This is the same even when applied to other vacuum film forming apparatuses (methods) such as a sputtering apparatus and a plasma CVD apparatus.
Therefore, in the vacuum film forming apparatus 10 of the present invention, the vapor deposition source 16 is a known vapor deposition source (evaporation source) that is filled with a film forming material and melts and evaporates. The substrate holder 18 is also a known substrate holder that holds the substrate Z by a known means. Further, the vacuum pump 20 is also a known vacuum pump for evacuating the vacuum chamber 14 and maintaining a predetermined film forming pressure.
Moreover, the vacuum film-forming apparatus 10 of this invention may have a rotation means which rotates the substrate holder 18 (substrate | substrate Z) as needed (rotation, revolution, self-revolution).
上述したように、本発明の真空成膜装置１０は、真空チャンバ１４の内壁面を覆って、本発明の防着板１２が設けられる。
図示例においては、防着板１２として、真空チャンバ１４内の上面（天井面）を覆う上面防着板１２ａ、同側面を覆う側面防着板１２ｂ、および、同下面（床面）を覆う下面防着板１２ｃが、設けられている。
As described above, the vacuum film forming apparatus 10 of the present invention covers the inner wall surface of the vacuum chamber 14 and is provided with the deposition preventing plate 12 of the present invention.
In the illustrated example, as the adhesion preventing plate 12, an upper surface adhesion preventing plate 12a covering the upper surface (ceiling surface) in the vacuum chamber 14, a side adhesion preventing plate 12b covering the same side surface, and a lower surface covering the same lower surface (floor surface). A protection plate 12c is provided.
図示例の真空成膜装置１０は、好ましい態様として、基板ホルダ１８および蒸着源１６に対応する領域以外において、真空チャンバ１４の内壁面のほぼ全面を、本発明の防着板１２で覆っている。
本発明は、これに限定はされず、例えば、側面防着板１２ｂのみを設けてもよく、あるいは、上面防着板１２ａのみを設けてもよい。
しかしながら、成膜材料の付着および堆積を、より好適に防止するためには、少なくとも真空チャンバ１４内の蒸着源１６（成膜材料が存在する空間）と対向する面、すなわち、上面防着板１２ａを設けるのが好ましく、真空チャンバ１４の内壁面を可能な限り本発明の防着板１２で覆うのがより好ましい。
また、本発明の防着板１２は、アルミニウム製であるので、基板ＺにＡｕやＰｔ等の金属膜や合金膜を成膜した際には、防着板１２に付着した成膜材料を分離して回収できる。そのため、基板Ｚに成膜されなかった成膜材料の回収率の点でも、真空チャンバ１４の内壁面を可能な限り防着板で覆った方が、有利である。
In a preferred embodiment, the vacuum film forming apparatus 10 in the illustrated example covers almost the entire inner wall surface of the vacuum chamber 14 with the deposition preventing plate 12 of the present invention, except for the region corresponding to the substrate holder 18 and the vapor deposition source 16. .
The present invention is not limited to this. For example, only the side surface protection plate 12b may be provided, or only the top surface protection plate 12a may be provided.
However, in order to more suitably prevent the deposition and deposition of the film forming material, at least the surface facing the vapor deposition source 16 (the space where the film forming material exists) in the vacuum chamber 14, that is, the upper surface protection plate 12a. It is preferable to cover the inner wall surface of the vacuum chamber 14 with the deposition preventing plate 12 of the present invention as much as possible.
Further, since the deposition preventive plate 12 of the present invention is made of aluminum, when a metal film such as Au or Pt or an alloy film is formed on the substrate Z, the deposition material attached to the deposition preventive plate 12 is separated. And can be recovered. For this reason, it is advantageous to cover the inner wall surface of the vacuum chamber 14 with an anti-adhesion plate as much as possible in terms of the recovery rate of the film forming material that has not been formed on the substrate Z.
また、本発明の真空成膜方法および真空成膜装置においては、必要に応じて、基板ホルダ１８の裏面など、真空チャンバ１４の内壁面以外の成膜材料が付着して堆積する可能性を有する部位を、本発明の防着板１２で覆ってもよい。 Moreover, in the vacuum film-forming method and the vacuum film-forming apparatus of the present invention, there is a possibility that film-forming materials other than the inner wall surface of the vacuum chamber 14 such as the back surface of the substrate holder 18 adhere and deposit as necessary. The part may be covered with the deposition preventing plate 12 of the present invention.
本発明の真空成膜装置１０において、防着板１２の取付方法には、特に限定はなく、真空成膜装置において防着板の取付方法として利用されている、公知の板状物やシート状物の取付方法が、各種、利用可能である。
一例として、カプトンテープ等の十分な耐熱性を有する接着テープを用いて、真空チャンバ１４内に防着板１２を貼着する方法が例示される。また、ビスや取付治具を用いる方法、フック等を用いて吊り下げる方法等の公知の機械的な板状物やシート状物の取付方法も利用可能である。さらに、防着板１２が十分な剛性を有する筒状物である場合には、蒸発源を囲んで真空チャンバ１４の下面に載置することで、真空チャンバ１４内に防着板１２を取り付けてもよい。
In the vacuum film forming apparatus 10 of the present invention, there is no particular limitation on the method of attaching the deposition plate 12, and a known plate-like object or sheet shape that is used as a method of attaching the deposition plate in the vacuum deposition apparatus. Various attachment methods can be used.
As an example, a method of adhering the deposition preventing plate 12 in the vacuum chamber 14 using an adhesive tape having sufficient heat resistance such as Kapton tape is exemplified. In addition, a known mechanical plate-like or sheet-like attachment method such as a method using a screw or an attachment jig or a method using a hook or the like can be used. Further, when the deposition preventing plate 12 is a cylindrical object having sufficient rigidity, the deposition preventing plate 12 is attached in the vacuum chamber 14 by surrounding the evaporation source and placing it on the lower surface of the vacuum chamber 14. Also good.
〔防着板〕
本発明の防着板は、真空成膜装置において不要な位置への成膜材料の付着を防止するための真空成膜装置用の防着板であって、アルミニウム製であり、平均開口径０．０１〜９μｍの凹部を含む凹凸構造が形成された表面を有し、かつ、この表面に平均高さ３０〜１０００μｍの複数の突出部が配列された防着板である。
次に、本発明の防着板について図２〜図７を用いて説明する。
[Protection plate]
The adhesion-preventing plate of the present invention is an adhesion-preventing plate for a vacuum film forming apparatus for preventing adhesion of a film forming material to an unnecessary position in the vacuum film forming apparatus, and is made of aluminum and has an average opening diameter of 0. This is an adhesion-preventing plate having a surface on which a concavo-convex structure including recesses of 0.01 to 9 μm is formed, and a plurality of protrusions having an average height of 30 to 1000 μm arranged on the surface.
Next, the adhesion prevention board of this invention is demonstrated using FIGS.
＜全体構成＞
図２および図４に示す通り、本発明の防着板１２は、平均開口径０．０１〜９μｍの凹部を含む凹凸構造３０が形成された表面を有し、かつ、この表面に平均高さ３０〜１０００μｍの複数の突出部４０が所定の割合で配列されている。
<Overall configuration>
As shown in FIGS. 2 and 4, the deposition preventing plate 12 of the present invention has a surface on which an uneven structure 30 including recesses having an average opening diameter of 0.01 to 9 μm is formed, and an average height on this surface. A plurality of protrusions 40 of 30 to 1000 μm are arranged at a predetermined ratio.
＜基材＞
本発明の防着板１２は、純アルミニウムやアルミニウム合金からなるアルミニウム製であれば特に限定されず、その形状は、図２に示す通り、板状ないしシート状であるのが好ましい。
ここで、アルミニウム製の基材としては、真空成膜装置用の防着板として市販されているアルミニウム箔など、各種のアルミニウム製の板状物やシート状物が利用可能である。
また、基材を構成するアルミニウムは、付着物を回収する際にアルミニウム中の不純物が回収物に混入し、回収物の純度が低下するのを抑止するため、その純度が９７％以上であるのが好ましく、９８％以上がより好ましく、９９％以上が更に好ましく、９９．５％以上が特に好ましい。
<Base material>
The adhesion-preventing plate 12 of the present invention is not particularly limited as long as it is made of aluminum made of pure aluminum or an aluminum alloy, and the shape thereof is preferably plate-shaped or sheet-shaped as shown in FIG.
Here, as an aluminum base material, various aluminum plate-like materials and sheet-like materials such as an aluminum foil commercially available as a deposition preventing plate for a vacuum film forming apparatus can be used.
In addition, the aluminum constituting the base material has a purity of 97% or more in order to prevent impurities in the aluminum from being mixed into the recovered material and reducing the purity of the recovered material when recovering the deposit. Is preferable, 98% or more is more preferable, 99% or more is further preferable, and 99.5% or more is particularly preferable.
本発明の防着板１２の厚さは特に限定されず、装着される真空成膜装置の構成、防着板の利用方法（使い捨てタイプか、洗浄して再利用するタイプか）、防着板１２のサイズ、成膜方法、成膜条件等に応じて、十分な機械的強度および熱的強度を確保でき、また、真空チャンバ１４内への取付などの際に扱い易い厚さを、適宜、設定すればよい。
このような取り扱いの容易性や作業性や、成膜材料の回収処理のし易さなどを考慮すると、本発明の防着板１２の厚さは、３０〜３００μｍ程度とするのが好ましい。
The thickness of the deposition preventing plate 12 of the present invention is not particularly limited, and the configuration of the vacuum film forming apparatus to be mounted, the method of using the deposition preventing plate (disposable type or the type to be reused after washing), the deposition preventing plate. According to the size, film forming method, film forming conditions, etc., sufficient mechanical strength and thermal strength can be secured, and a thickness that is easy to handle when mounting in the vacuum chamber 14 is appropriately set. You only have to set it.
Considering the ease of handling and workability, the ease of collecting the film forming material, etc., the thickness of the deposition preventing plate 12 of the present invention is preferably about 30 to 300 μm.
＜凹凸構造＞
平均開口径０．０１〜９μｍの凹部（後述する陽極酸化皮膜に形成されるマイクロポアに起因する凹部を除く。）を含む凹凸構造３０は、本発明の防着板１２の表面を構成するものである。
ここで、図５に示す通り、凹部３０ａの開口径は、凹部３０ａ（凹部３０ａを形成する環状に連なる周囲）の直径であり、平均開口径とは、その平均である。
具体的には、電子顕微鏡を用いて、防着板１２の表面を真上から倍率２０００〜３００００倍で撮影し、得られた電子顕微鏡写真において、周囲が環状に連なっている凹部３０ａを少なくとも５０個抽出し、その直径（あるいは、凹部３０ａを内接する円の直径）を読み取って開口径とし、平均開口径を算出する。
また、凹部を含む凹凸構造とは、図５（Ａ）に示すように波型の構造のものであってもよく、図５（Ｂ）に示すように凸部が表面の平坦部分で構成される凹部の繰り返し構造であってもよい。
<Uneven structure>
The concavo-convex structure 30 including a recess having an average opening diameter of 0.01 to 9 μm (excluding a recess due to a micropore formed in an anodic oxide film described later) constitutes the surface of the deposition preventing plate 12 of the present invention. It is.
Here, as shown in FIG. 5, the opening diameter of the recessed part 30a is the diameter of the recessed part 30a (circumferential continuous circumference forming the recessed part 30a), and the average opening diameter is an average thereof.
Specifically, using an electron microscope, the surface of the deposition preventing plate 12 was photographed from directly above at a magnification of 2000 to 30000 times, and in the obtained electron micrograph, at least 50 concave portions 30a that are connected in a ring shape are provided. The diameter is extracted, the diameter (or the diameter of a circle inscribed in the concave portion 30a) is read and set as the opening diameter, and the average opening diameter is calculated.
Further, the concavo-convex structure including the concave portion may be a corrugated structure as shown in FIG. 5 (A), and the convex portion is constituted by a flat portion on the surface as shown in FIG. 5 (B). The concave structure may be a repeated structure.
本発明の防着板１２は、平均開口径０．０１〜９μｍの凹部３０ａを含む凹凸構造３０が形成された表面に有することにより、上述した通り、防着板に付着した成膜材料を非常に強く保持するため、剥離によるパーティクルの発生を抑制することができる。 The deposition preventive plate 12 of the present invention has a film-forming material attached to the deposition preventive plate as described above by having the concave / convex structure 30 including the concave portions 30a having an average opening diameter of 0.01 to 9 μm on the surface. Therefore, the generation of particles due to peeling can be suppressed.
本発明においては、成膜材料の剥離防止効果がより向上する理由から、平均開口径０．０１〜９μｍの凹部３０ａを含む凹凸構造３０は、平均開口径０．５〜９μｍの凹部を含む凹凸構造（以下、「中波構造」ともいう。）、もしくは、平均開口径０．０１〜０．３μｍの凹部を含む凹凸構造（以下、「小波構造」ともいう。）、または、これらが重畳している構造であるのが好ましい。
これらのうち、中波構造および小波構造が重畳している構造であるのが好ましく、具体的には、図６に示す通り、平均開口径０．５〜９μｍの凹部３２ａを含む中波構造３２に、さらに、平均開口径０．０１〜０．３μｍの凹部３４ａを含む小波構造３４が重畳している態様が好適に挙げられる。
ここで、中波構造３２における凹部３２ａの平均開口径は、電子顕微鏡を用いて、防着板の表面を真上から倍率２０００倍で撮影し、得られた電子顕微鏡写真において、周囲が環状に連なっている凹部３２ａ（重畳する小波構造３４における凹部３４ａは除く）を少なくとも５０個抽出し、その直径（あるいは、凹部３２ａを内接する円の直径）を読み取って開口径とし、平均開口径を算出する。
同様に、小波構造３４における凹部３４ａの平均開口径は、電子顕微鏡を用いて、防着板の表面を真上から倍率１００００〜３００００倍で撮影し、得られた電子顕微鏡写真において、周囲が環状に連なっている凹部３４ａ（重畳する中波構造３２における凹部３２ａは除く）を少なくとも５０個抽出し、その直径（あるいは、凹部３４ａを内接する円の直径）を読み取って開口径とし、平均開口径を算出する。
In the present invention, the uneven structure 30 including the recesses 30a having the average opening diameter of 0.01 to 9 μm is the unevenness including the recesses having the average opening diameter of 0.5 to 9 μm because the effect of preventing the peeling of the film forming material is further improved. A structure (hereinafter also referred to as “medium wave structure”), a concavo-convex structure including recesses having an average opening diameter of 0.01 to 0.3 μm (hereinafter also referred to as “small wave structure”), or a combination thereof. It is preferable that it is a structure.
Of these, a structure in which a medium wave structure and a small wave structure are overlapped is preferable. Specifically, as shown in FIG. 6, the medium wave structure 32 including the recesses 32 a having an average opening diameter of 0.5 to 9 μm. Furthermore, a mode in which a small wave structure 34 including a concave portion 34a having an average opening diameter of 0.01 to 0.3 μm is preferably mentioned.
Here, the average opening diameter of the recesses 32a in the medium wave structure 32 is obtained by photographing the surface of the deposition preventing plate from directly above at a magnification of 2000 using an electron microscope. In the obtained electron micrograph, the periphery is circular. At least 50 consecutive recesses 32a (excluding the recesses 34a in the overlapping small wave structure 34) are extracted, and the diameter (or the diameter of a circle inscribed in the recess 32a) is read as an opening diameter to calculate an average opening diameter. To do.
Similarly, the average opening diameter of the concave portion 34a in the small wave structure 34 is obtained by photographing the surface of the deposition preventing plate from directly above at a magnification of 10,000 to 30,000 times using an electron microscope. At least 50 recesses 34a (excluding the recesses 32a in the overlapping medium wave structure 32) are extracted, and the diameter (or the diameter of a circle inscribed in the recess 34a) is read as the opening diameter, and the average opening diameter Is calculated.
（中波構造）
本発明においては、中波構造３２を構成する凹部３２ａの平均開口径は、成膜材料の剥離防止効果が更に向上する理由から、０．５〜５μｍが好ましく、１〜５μｍがより好ましく、１．５〜３μｍが更に好ましい。
また、中波構造３２を構成する凹部３２ａの深さは特に限定されない。なお、本発明の防着板は、後述する防着板の製造方法に示すように、アルミニウム板に電気化学的粗面化処理を施すことで凹凸構造を形成しているため、凹部３２ａの深さは、ほぼ、凹部３２ａの開口径に等しいと考えられる。
(Medium wave structure)
In the present invention, the average opening diameter of the recesses 32a constituting the medium wave structure 32 is preferably 0.5 to 5 μm, more preferably 1 to 5 μm, because the effect of preventing the film-forming material from peeling off is further improved. More preferably, it is 5-3 micrometers.
Further, the depth of the concave portion 32a constituting the medium wave structure 32 is not particularly limited. In addition, since the deposition preventing plate of the present invention forms an uneven structure by subjecting the aluminum plate to an electrochemical roughening treatment, as shown in a manufacturing method of the deposition preventing plate described later, the depth of the recess 32a is reduced. This is considered to be substantially equal to the opening diameter of the recess 32a.
（小波構造）
本発明においては、小波構造３４を構成する凹部３４ａの平均開口径は、成膜材料の剥離防止効果が更に向上する理由から、０．１〜０．２μｍが好ましい。
また、同様の理由から、小波構造３４を構成する凹部３４ａの開口径に対する深さの比の平均は、０．２〜０．５であるのが好ましい。
ここで、凹部３４ａにおける開口径に対する深さの比の平均は、高分解能走査型電子顕微鏡（ＳＥＭ）を用いて防着板の破断面を倍率５００００倍で撮影し、得られたＳＥＭ写真において微細凹部を少なくとも２０個抽出し、開口径と深さとを読み取って比を求めて平均値を算出する。
(Small wave structure)
In the present invention, the average opening diameter of the recesses 34a constituting the small wave structure 34 is preferably 0.1 to 0.2 μm because the effect of preventing the film-forming material from peeling off is further improved.
For the same reason, the average of the ratio of the depth to the opening diameter of the recesses 34a constituting the small wave structure 34 is preferably 0.2 to 0.5.
Here, the average of the ratio of the depth to the opening diameter in the recess 34a is obtained by photographing the fractured surface of the adhesion-preventing plate at a magnification of 50000 times using a high-resolution scanning electron microscope (SEM). At least 20 recesses are extracted, the aperture diameter and depth are read, the ratio is obtained, and the average value is calculated.
本発明の防着板１２の表面（凹凸構造３０）の算術平均粗さＲａは特に限定されず、０．２５〜０．６０μｍであるのが好ましく、０．３０〜０．６０μｍであるのがより好ましく、０．３０〜０．５５μｍであるのが更に好ましい。
ここで、表面粗さＲａは、触針式の表面粗さ計（例えば、ミツトヨ社製の表面粗さ測定機ＳＪ−４０１など）を用いて測定した、ＪＩＳ Ｂ０６０１：２００１に準拠する算術平均粗さである。
The arithmetic average roughness Ra of the surface (uneven structure 30) of the deposition preventing plate 12 of the present invention is not particularly limited, and is preferably 0.25 to 0.60 μm, and preferably 0.30 to 0.60 μm. More preferably, it is 0.30 to 0.55 μm.
Here, the surface roughness Ra is an arithmetic average roughness based on JIS B0601: 2001, measured using a stylus type surface roughness meter (for example, a surface roughness measuring machine SJ-401 manufactured by Mitutoyo Corporation). That's it.
＜突出部＞
平均高さ３０〜１０００μｍの複数の突出部４０は、本発明の防着板１２の表面に所定の割合で配列されるものである。
ここで、図４に示す通り、突出部４０の高さは、突出部４０の底面４０ａから頂辺（頂点４０ｂ）までの距離であり、平均高さとは、その平均である。なお、突出部４０は、図２（Ａ）、図４、図７および図８に示す通り、傾斜構造、すなわち、稜線（図４および図７においては符号４０ｃ）を有する山状の構造であってもよく、その場合の高さは、底面から頂点までの距離をいう。
具体的には、高分解能走査型電子顕微鏡（ＳＥＭ）を用いて、防着板１２の断面を倍率５０〜１００倍で撮影し、得られた電子顕微鏡写真において、突出部４０を少なくとも２０個抽出し、その高さの平均値を算出する。
本発明においては、成膜材料の剥離防止効果がより向上する理由から、突出部４０の平均高さは、１００〜５００μｍであるのが好ましい。
<Projection>
The plurality of protrusions 40 having an average height of 30 to 1000 μm are arranged at a predetermined ratio on the surface of the deposition preventing plate 12 of the present invention.
Here, as shown in FIG. 4, the height of the protrusion 40 is a distance from the bottom surface 40a of the protrusion 40 to the top side (vertex 40b), and the average height is an average thereof. As shown in FIGS. 2A, 4, 7, and 8, the protrusion 40 has an inclined structure, that is, a mountain-like structure having a ridge line (reference numeral 40 c in FIGS. 4 and 7). The height in that case refers to the distance from the bottom to the apex.
Specifically, using a high-resolution scanning electron microscope (SEM), the cross section of the deposition preventing plate 12 was photographed at a magnification of 50 to 100 times, and at least 20 protrusions 40 were extracted from the obtained electron micrograph. And the average value of the height is calculated.
In the present invention, the average height of the protrusions 40 is preferably 100 to 500 μm because the effect of preventing the film-forming material from peeling off is further improved.
突出部４０の垂直方向上方から見た時の外形は、成膜材料の剥離防止効果がより向上する理由から、不定形ではなく、菱形（図３および図８参照）、矩形または円形であるのが好ましく、なかでも、菱形であるのがより好ましい。
ここで、突出部の外形が定形であると、防着板に付着する成膜材料の残留応力の緩和効果が均一となり、成膜材料の剥離防止効果が良化する傾向がある。
The outer shape of the protrusion 40 as viewed from above in the vertical direction is not an indeterminate shape but a rhombus (see FIGS. 3 and 8), a rectangle, or a circle because the effect of preventing the peeling of the film forming material is further improved. Among them, a rhombus is more preferable.
Here, if the outer shape of the protruding portion is a fixed shape, the effect of reducing the residual stress of the film forming material adhering to the deposition preventing plate becomes uniform, and the effect of preventing the film forming material from peeling off tends to be improved.
また、突出部４０の平均密度は、１０個／１０ｍｍ角以上であり、成膜材料の剥離防止効果がより向上する理由から、１０〜１００個／１０ｍｍ角であるのが好ましく、３０〜１００個／１０ｍｍ角であるのがより好ましく、５０〜９０個／１０ｍｍ角であるのが更に好ましい。
ここで、突出部４０の平均密度は、任意の５箇所における１０ｍｍ角（１０ｍｍ×１０ｍｍ）の領域における突出部の数を測定し、これらの合計値を５で除した平均値として算出することができる。
Moreover, the average density of the protrusions 40 is 10 pieces / 10 mm square or more, and it is preferably 10-100 pieces / 10 mm square, for the reason that the peeling prevention effect of the film forming material is further improved, and 30-100 pieces. / 10 mm square is more preferable, and 50 to 90 pieces / 10 mm square is more preferable.
Here, the average density of the protrusions 40 may be calculated as an average value obtained by measuring the number of protrusions in a 10 mm square (10 mm × 10 mm) region at any five locations and dividing the total value by five. it can.
また、突出部４０の底部面積の比率は、１０ｍｍ角の領域において９０％超であり、蒸着を繰り返した場合にも成膜材料の剥離防止効果がより向上する理由から、９５〜１００％であるのが好ましい。
ここで、突出部４０の底部面積とは、図２に示す突出部４０の底部、例えば、図４の波線で示す部分の面積をいい、その比率とは、１０ｍｍ角の領域、すなわち１００ｍｍ2の面積における突出部４０の底部面積の占める割合をいい、本発明においては、任意の５箇所における平均値をいう。
Further, the ratio of the bottom area of the protrusion 40 is more than 90% in a 10 mm square region, and is 95 to 100% because the effect of preventing the peeling of the film forming material is further improved even when the deposition is repeated. Is preferred.
Here, the bottom area of the protrusion 40 refers to the area of the bottom of the protrusion 40 shown in FIG. 2, for example, the portion indicated by the wavy line in FIG. 4, and the ratio is a 10 mm square region, that is, 100 mm 2 . It refers to the proportion of the bottom area of the protrusion 40 in the area, and in the present invention, it refers to the average value at any five locations.
本発明の防着板１２は、平均高さ３０〜１０００μｍの複数の突出部４０を上述した所定の平均密度および底部面積の比率で均一に配列することにより、上述した通り、防着板に付着した成膜材料の残留応力を緩和することができるため、特に蒸着を繰り返した場合であっても、剥離によるパーティクルの発生を抑制することができると考えられる。 As described above, the deposition preventing plate 12 of the present invention adheres to the deposition preventing plate as described above by uniformly arranging the plurality of protrusions 40 having an average height of 30 to 1000 μm at the ratio of the predetermined average density and the bottom area described above. Since it is possible to relieve the residual stress of the deposited material, it is considered that the generation of particles due to peeling can be suppressed even when the deposition is repeated.
＜陽極酸化皮膜＞
本発明の防着板１２は、その表面がアルミニウムの陽極酸化皮膜で構成されているのが好ましい。
陽極酸化皮膜で構成されることで、表面に、マイクロポアと呼ばれる細孔を、多数、保有させることができる。その結果、より高いアンカー効果を得て、密着強度が高くなることで、防着板１２に付着した成膜材料の剥離をより好適に防止できる。
陽極酸化皮膜の厚さには、限定は無いが、０．０５〜３０μｍが好ましく、特に０．２５〜５μｍが好ましい。陽極酸化皮膜の厚さを、上記範囲とすることにより、防着板の表面に陽極酸化皮膜を有することの効果を、更に好適に得ることができ、成膜材料が防着板から剥離してことによりパーティクルの発生を、更に好適に防止することができる。
<Anodized film>
The surface of the deposition preventing plate 12 of the present invention is preferably composed of an anodized aluminum film.
By being composed of an anodized film, a large number of micropores called micropores can be retained on the surface. As a result, a higher anchor effect is obtained, and the adhesion strength is increased, so that the film-forming material attached to the deposition preventing plate 12 can be more suitably prevented from peeling.
Although there is no limitation in the thickness of an anodized film, 0.05-30 micrometers is preferable and especially 0.25-5 micrometers is preferable. By making the thickness of the anodic oxide film within the above range, the effect of having the anodic oxide film on the surface of the deposition preventive plate can be obtained more suitably, and the film forming material is peeled off from the deposition preventive plate. Thus, the generation of particles can be more suitably prevented.
＜クラック＞
本発明の防着板１２は、その表面にクラックを有しているのが好ましい。
表面にクラックを有することにより、防着板１２に付着した成膜材料がクラックに入り込み、密着強度が高くなることで、防着板１２に付着した成膜材料の剥離をより好適に防止できる。
本発明においては、成膜材料の剥離を更に好適に防止することができる理由から、図７に示すように、クラック４２は、上述した突出部４０に有しているのが好ましく、突出部４０の頂点４０ｂ付近や、斜面４０ｄに有しているのがより好ましい。
ここで、クラックは、幅０．０５〜２０μｍの線状の亀裂であることが好ましく、その長さは、０．５μｍ以上であって突出部の周径（例えば、４ｍｍ程度）以下であるのが好ましい。
また、このようなクラックを１本以上有しているのが好ましく、１０本以上有しているのがより好ましい。
<Crack>
The deposition preventing plate 12 of the present invention preferably has a crack on the surface thereof.
By having a crack on the surface, the film forming material attached to the deposition preventing plate 12 enters the crack, and the adhesion strength is increased, so that peeling of the film forming material adhered to the deposition preventing plate 12 can be more suitably prevented.
In the present invention, for the reason that peeling of the film forming material can be more preferably prevented, as shown in FIG. It is more preferable to have in the vicinity of the apex 40b and the inclined surface 40d.
Here, the crack is preferably a linear crack having a width of 0.05 to 20 μm, and the length thereof is 0.5 μm or more and not more than the peripheral diameter (for example, about 4 mm) of the protruding portion. Is preferred.
Moreover, it is preferable to have one or more such cracks, and more preferably ten or more.
［防着板の製造方法］
本発明の防着板の製造方法は、上述した本発明の防着板を製造する製造方法であって、上記凹凸構造を形成する凹凸形成工程および上記突出部を形成する突出部形成工程を有する製造方法である。
なお、本発明においては、凹凸形成工程および突出部形成工程は、その順序を問わないが、凹凸形成工程の後に突出部形成工程を施す態様であるのが好ましい。
[Manufacturing method of deposition prevention plate]
The manufacturing method of the deposition preventing plate of the present invention is a manufacturing method for manufacturing the deposition preventing plate of the present invention described above, and includes a concavo-convex forming step for forming the concavo-convex structure and a protruding portion forming step for forming the protruding portion. It is a manufacturing method.
In addition, in this invention, although the unevenness | corrugation formation process and a protrusion part formation process do not ask | require the order, it is preferable that it is an aspect which performs a protrusion part formation process after an unevenness | corrugation formation process.
＜凹凸形成工程＞
凹凸形成工程は、アルミニウム板の表面に電気化学的粗面化処理を施し、表面に上述した平均開口径０．０１〜９μｍの凹部を含む凹凸構造を形成する工程である。
上記電気化学的粗面化処理としては、例えば、塩酸や硝酸を含む電解液を用いて、交流で電解処理する方法が挙げられる。
<Roughness formation process>
The concavo-convex forming step is a step in which the surface of the aluminum plate is subjected to an electrochemical roughening treatment to form the concavo-convex structure including the concave portions having the average opening diameter of 0.01 to 9 μm on the surface.
Examples of the electrochemical surface roughening treatment include a method of performing an electrolytic treatment with an alternating current using an electrolytic solution containing hydrochloric acid or nitric acid.
具体的には、上述した中波構造の凹凸構造を得るためには、電解反応が終了した時点でのアルミニウム基材のアノード反応にあずかる電気量の総和が、１〜１０００Ｃ／ｄｍ2であるのが好ましく、５０〜３００Ｃ／ｄｍ2であるのがより好ましい。また、電流密度は２０〜１００Ａ／ｄｍ2であるのが好ましい。
より具体的には、例えば、０．１〜５０質量％の塩酸または硝酸を含む電解液中で、２０〜８０℃の温度、時間１秒〜１０分の範囲で処理するのが好ましい。
Specifically, in order to obtain the above-described uneven structure having a medium wave structure, the total amount of electricity involved in the anode reaction of the aluminum substrate at the time when the electrolytic reaction is completed is 1 to 1000 C / dm 2 . Is preferable, and it is more preferable that it is 50-300 C / dm < 2 >. The current density is preferably 20 to 100 A / dm2.
More specifically, for example, the treatment is preferably performed in an electrolyte solution containing 0.1 to 50% by mass of hydrochloric acid or nitric acid at a temperature of 20 to 80 ° C. and a time of 1 second to 10 minutes.
また、上述した小波構造の凹凸構造を得るためには、塩酸を含む電解液を用いて処理するのが好ましく、具体的には、電解反応が終了した時点でのアルミニウム基材のアノード反応にあずかる電気量の総和が、１〜１００Ｃ／ｄｍ2であるのが好ましく、２０〜７０Ｃ／ｄｍ2であるのがより好ましい。この際の電流密度は２０〜５０Ａ／ｄｍ2であるのが好ましい。
より具体的には、例えば、０．１〜１０質量％の塩酸を含む電解液中で、２０〜８０℃の温度、時間１秒〜１０分の範囲で処理するのが好ましい。なお、塩酸を含む電解液で、中波構造に重畳された小波構造を、同一工程中で形成することも可能である。
Further, in order to obtain the above-described concave / convex structure of the small wave structure, it is preferable to perform treatment using an electrolytic solution containing hydrochloric acid, and specifically, to participate in the anodic reaction of the aluminum substrate when the electrolytic reaction is completed. total amount of electricity is, is preferably from 1~100C / dm 2, and more preferably 20~70C / dm 2. The current density at this time is preferably 20 to 50 A / dm 2 .
More specifically, for example, the treatment is preferably performed in an electrolytic solution containing 0.1 to 10% by mass of hydrochloric acid at a temperature of 20 to 80 ° C. and a time of 1 second to 10 minutes. Note that it is also possible to form a small wave structure superimposed on a medium wave structure in the same process with an electrolyte containing hydrochloric acid.
また、塩酸と硫酸との混合液を用いて、アルミニウム製の基材を電解処理する電気化学的粗面化処理を行うことにより、上述した中波構造に小波構造を重畳してなる凹凸構造を形成することができる。 In addition, an uneven surface structure in which a small wave structure is superimposed on the above-described medium wave structure is obtained by performing an electrochemical surface roughening process in which an aluminum base material is electrolytically treated using a mixed solution of hydrochloric acid and sulfuric acid. Can be formed.
＜突出部形成工程＞
突出部形成工程は、アルミニウム板の表面にエンボス加工を施し、表面の一部または全部に上述した平均高さ３０〜１０００μｍの複数の突出部を形成する工程である。
ここで、エンボス加工としては、例えば、プレス加工であってもよいが、本発明においては、特開２００５−２０５４４４号公報の［００１２］〜［００３３］段落に記載するエンボス加工用ロールを用いたロールフォーミングであるのが好ましい。
<Projection formation process>
The protruding portion forming step is a step of embossing the surface of the aluminum plate to form the plurality of protruding portions having the average height of 30 to 1000 μm described above on part or all of the surface.
Here, the embossing may be, for example, press working, but in the present invention, the embossing roll described in paragraphs [0012] to [0033] of JP-A-2005-205444 is used. Roll forming is preferred.
＜陽極酸化処理工程＞
陽極酸化処理工程は、上述した凹凸形成工程の後に、陽極酸化処理を施し、表面の全域にアルミニウムの陽極酸化皮膜を形成する任意の工程である。なお、陽極酸化処理工程は、上述した突出部形成工程の前工程であっても後工程であってもよいが、表面に上述したクラックを形成させる理由から、突出部形成工程の前工程であるのが好ましい。
この工程により、本発明の防着板の任意の構成である陽極酸化皮膜を形成することができる。
<Anodizing process>
The anodizing process is an arbitrary process in which an anodizing process is performed after the above-described unevenness forming process to form an anodized aluminum film over the entire surface. The anodizing process may be a pre-process or a post-process of the protrusion forming process described above, but is a pre-process of the protrusion forming process for the reason of forming the crack described above on the surface. Is preferred.
By this step, an anodic oxide film that is an arbitrary configuration of the deposition-preventing plate of the present invention can be formed.
防着板表面の陽極酸化は、公知の方法で行えばよい。
具体的には、硫酸濃度５０〜３００ｇ／Ｌで、アルミニウム濃度５質量％以下の溶液中で、アルミニウム板を陽極として通電する方法が、好適に例示される。
また、陽極酸化処理に用いられる溶液としては、硫酸のみならず、リン酸、クロム酸、シュウ酸、スルファミン酸、ベンゼンスルホン酸、アミドスルホン酸等を単独でまたは２種以上を組み合わせて用いることができる。
陽極酸化処理の好ましい条件は、使用する電解液によって異なるが、一般的には電解液濃度１〜８０質量％、液温５〜７０℃、電流密度０．５〜６０Ａ／ｄｍ2、電圧１〜１００Ｖ、電解時間１５秒〜５０分程度であり、所望の陽極酸化皮膜量が形成できるように、適宜、調整すればよい。
What is necessary is just to perform the anodic oxidation of the surface of a deposition preventing plate by a well-known method.
Specifically, a method of energizing an aluminum plate as an anode in a solution having a sulfuric acid concentration of 50 to 300 g / L and an aluminum concentration of 5% by mass or less is suitably exemplified.
As the solution used for the anodizing treatment, not only sulfuric acid but also phosphoric acid, chromic acid, oxalic acid, sulfamic acid, benzenesulfonic acid, amidosulfonic acid, etc. may be used alone or in combination of two or more. it can.
The preferred conditions for the anodizing treatment vary depending on the electrolyte used, but in general, the electrolyte concentration is 1 to 80% by mass, the solution temperature is 5 to 70 ° C., the current density is 0.5 to 60 A / dm 2 , and the voltage is 1 What is necessary is just to adjust suitably so that it may be 100V and electrolysis time is 15 second-about 50 minutes, and the desired amount of anodic oxide films can be formed.
＜焼鈍処理工程＞
焼鈍処理工程は、上述した突出部形成工程の後に、真空雰囲気中または大気中において、焼鈍処理（アニーリング処理）を施す任意の工程である。
この工程により、防着板の加工性が向上し、真空チャンバの内壁面に沿った変形や穴開け等が容易となり、その結果、作製される真空成膜装置において蒸着源から生じる異常放電が抑制され、また、真空排気時間が短縮されるという効果も期待することができる。
<Annealing process>
An annealing treatment process is an arbitrary process which performs an annealing treatment (annealing treatment) in a vacuum atmosphere or air after the above-mentioned projection formation process.
This process improves the workability of the deposition plate and facilitates deformation and drilling along the inner wall surface of the vacuum chamber. As a result, abnormal vacuum generated from the deposition source is suppressed in the vacuum film forming apparatus that is produced. In addition, the effect of shortening the evacuation time can be expected.
焼鈍処理の加熱条件は特に限定されず、２００〜５００℃であるのが好ましく、３００℃〜４００℃であるのがより好ましい。なお、焼鈍処理に用いる加熱炉としては、ヒーター式や輻射加熱等の一般的な炉を用いることができる。
また、焼鈍処理の処理時間は特に限定されず、１０〜１２０分が好ましく、１５〜６０分がより好ましい。
The heating conditions for the annealing treatment are not particularly limited, and are preferably 200 to 500 ° C, more preferably 300 to 400 ° C. In addition, as a heating furnace used for an annealing process, general furnaces, such as a heater type and radiation heating, can be used.
Moreover, the processing time of an annealing process is not specifically limited, 10 to 120 minutes are preferable and 15 to 60 minutes are more preferable.
＜他の任意の処理工程＞
（機械的粗面化処理）
本発明においては、上述した電解粗面化処理の前に、アルミニウム板の表面にブラシグレイン等の機械的粗面化処理を施してもよい。
<Other optional processing steps>
(Mechanical roughening treatment)
In the present invention, a mechanical surface roughening treatment such as brush grain may be performed on the surface of the aluminum plate before the electrolytic surface roughening treatment described above.
（封孔処理など）
本発明においては、陽極酸化処理の後に、陽極酸化皮膜に存在するマイクロポアを封じる封孔処理を行ってもよい。封孔処理は、沸騰水処理、熱水処理、蒸気処理、ケイ酸ソーダ処理、亜硝酸塩処理、酢酸アンモニウム処理等の公知の方法に従って行うことができる。
また、陽極酸化処理を施した表面や、この表面に封孔処理を施した表面に対して、シリケート、または、ポリビニルホスホン酸、有機カルボン酸化合物、有機スルホン酸化合物などの酸を付着させる親水化処理を施してもよい。
(Sealing treatment etc.)
In this invention, you may perform the sealing process which seals the micropore which exists in an anodized film after an anodizing process. The sealing treatment can be performed according to a known method such as boiling water treatment, hot water treatment, steam treatment, sodium silicate treatment, nitrite treatment, ammonium acetate treatment and the like.
Hydrophilization that attaches an acid such as silicate or polyvinylphosphonic acid, organic carboxylic acid compound, organic sulfonic acid compound to the surface that has been anodized or the surface that has been sealed. Processing may be performed.
以上、本発明の真空成膜装置用防着板およびその製造方法、ならびに、それを用いた真空成膜装置および真空成膜方法に関して詳細に説明したが、本発明は上述の例に限定はされず、本発明の要旨を逸脱しない範囲において、各種の改良や変更を行ってもよいのは、もちろんである。 As mentioned above, although the deposition board for vacuum film-forming apparatuses of this invention, its manufacturing method, and the vacuum film-forming apparatus and vacuum film-forming method using the same were demonstrated in detail, this invention is limited to the above-mentioned example. Needless to say, various improvements and modifications may be made without departing from the scope of the present invention.
以下、本発明の具体的実施例を挙げ、本発明について、より詳細に説明する。 Hereinafter, the present invention will be described in more detail with reference to specific examples of the present invention.
〔実施例１〜１０および比較例１〜５〕
＜凹凸形成工程（粗面化処理）＞
厚さ１５０μｍのアルミニウム板（ＪＩＳ １０５０材）の表面に、平均粒径３０μｍのパミストンを研磨剤とする、比重１．１２のスラリー液を供給し、回転するローラ状ナイロンブラシを２本にて、アルミニウム板を移動させて、表面処理を行った。使用したナイロンブラシの直径は０．５ｍｍ、毛密度は４５０本／ｃｍ2でブラシ回転数は１５０ｒｐｍとした。
次いで、４０℃に保温した硝酸濃度１０ｇ／Ｌの電解槽に入れて、電気量総和が３００Ｃ／ｄｍ2の条件下で電解処理を行った。なお、交流電源波は、６０Ｈｚ周波数の台形波を使用した。電流密度は１００Ａ／ｄｍ2とした。
次いで、このアルミニウム板を、４５℃に保温した塩酸濃度１０ｇ／Ｌの電解槽に入れて、電気量総和が７０Ｃ／ｄｍ2の条件下で電解処理を行って、図６に示すような防着板を作製した。なお、交流電源波は、６０Ｈｚ周波数の台形波を使用した。電流密度は５０Ａ／ｄｍ2とした。
ここで、粗面化処理後の防着板の表面、すなわち、凹凸構造の算術平均粗さＲａは０．５３μｍであった。
なお、比較例５については、凹凸形成工程は施さなかった。
[Examples 1 to 10 and Comparative Examples 1 to 5]
<Roughness forming step (roughening treatment)>
A slurry liquid having a specific gravity of 1.12 using pumiston with an average particle diameter of 30 μm as an abrasive is supplied to the surface of an aluminum plate (JIS 1050 material) having a thickness of 150 μm, and two rotating roller nylon brushes are used. The aluminum plate was moved to perform surface treatment. The diameter of the nylon brush used was 0.5 mm, the hair density was 450 / cm 2 , and the brush rotation speed was 150 rpm.
Subsequently, it was put into an electrolytic cell having a nitric acid concentration of 10 g / L kept at 40 ° C., and electrolytic treatment was performed under the condition that the total amount of electricity was 300 C / dm 2 . Note that a trapezoidal wave having a frequency of 60 Hz was used as the AC power source wave. Current density was set to 100A / dm 2.
Next, this aluminum plate was placed in an electrolytic cell having a hydrochloric acid concentration of 10 g / L kept at 45 ° C., and subjected to electrolytic treatment under the condition that the total amount of electricity was 70 C / dm 2 , thereby preventing adhesion as shown in FIG. A plate was made. Note that a trapezoidal wave having a frequency of 60 Hz was used as the AC power source wave. Current density was 50A / dm 2.
Here, the surface of the adhesion-preventing plate after the roughening treatment, that is, the arithmetic average roughness Ra of the concavo-convex structure was 0.53 μm.
In Comparative Example 5, the unevenness forming step was not performed.
＜陽極酸化処理＞
作製した防着板に硫酸濃度２５０ｇ／Ｌで、アルミニウム濃度５％以下の溶液を用い、アルミニウム板を陽極として、直流電圧を４５分間印加して、表面に厚さ１．０μｍの陽極酸化皮膜を形成した。電流密度は５０Ａ／ｄｍ2とした。
ここで、陽極酸化処理後の防着板の表面、すなわち、凹凸構造の算術平均粗さＲａは、上述した凹凸形成工程（粗面化処理）後の値と同じであった。
なお、実施例７については、後述する突出部形成工程（エンボス加工）の後に、陽極酸化処理を施した。
<Anodizing treatment>
A solution having a sulfuric acid concentration of 250 g / L and an aluminum concentration of 5% or less was used for the produced deposition preventing plate, and an aluminum plate was used as an anode and a DC voltage was applied for 45 minutes to form a 1.0 μm thick anodic oxide film on the surface. Formed. Current density was 50A / dm 2.
Here, the surface of the adhesion-preventing plate after the anodic oxidation treatment, that is, the arithmetic average roughness Ra of the concavo-convex structure was the same as the value after the concavo-convex formation step (roughening treatment) described above.
In addition, about Example 7, the anodic oxidation process was performed after the protrusion part formation process (embossing) mentioned later.
＜突出部形成工程（エンボス加工）＞
特開２００５−２０５４４４号公報の［００１２］〜［００３３］段落に記載された方法により各種のエンボス加工用ロールを作製し、これを用いて上記凹凸形成工程後のアルミニウム板に対して、下記第１表に示す外形、高さおよび密度の突出部を形成させることにより、防着板を作製した。
ここで、ニップは、型同士が板厚〜板厚＋０．０２ｍｍとなるように、クリアランスを矯正して行った。
なお、比較例１については、突出部形成工程は施さなかった。
<Projection formation process (embossing)>
Various embossing rolls are prepared by the method described in paragraphs [0012] to [0033] of Japanese Patent Application Laid-Open No. 2005-205444, and the following are used for the aluminum plate after the above irregularity forming step using the roll. By forming protrusions having the outer shape, height and density shown in Table 1, a deposition preventing plate was produced.
Here, the nip was performed by correcting the clearance so that the molds had a plate thickness to a plate thickness +0.02 mm.
In addition, about the comparative example 1, the protrusion part formation process was not performed.
＜焼鈍処理工程＞
実施例１０で作製した防着板については、突出部形成工程の後に、更に下記第１表に示す条件で焼鈍処理を施した。なお、焼鈍処理の昇温速度は１５℃／分で行った。
<Annealing process>
About the adhesion prevention board produced in Example 10, the annealing process was given on the conditions shown in the following Table 1 after the protrusion part formation process. In addition, the temperature increase rate of annealing treatment was performed at 15 degrees C / min.
作製した防着板の表面および断面を電子顕微鏡によって倍率２０００倍および倍率３００００倍で観察し、凹凸構造（中波構造および小波構造）における凹部の平均開口径、ならびに、突出部の外形、平均高さ、平均密度および底部面積比率を測定した。これらの結果を陽極酸化皮膜の有無およびクラックの有無とともに下記第１表に示す。なお、下記第１表中、「−」で表される項目は、当該項目が存在していないことを示す。
また、電子顕微鏡による観察により、実施例において作製した防着板の表面は、凹凸構造が形成され、複数の突出部が配列されていることが分かった。なお、実施例１で作製した防着板の表面の倍率５０倍および倍率３５０倍の写真をそれぞれ図８および図９に示し、また、実施例１で作製した防着板の突出部における頂点および斜面の倍率２０００倍の写真をそれぞれ図１０（Ａ）および（Ｂ）に示す。
The surface and cross-section of the prepared protective plate were observed with an electron microscope at a magnification of 2000 times and a magnification of 30000 times, the average opening diameter of the recesses in the concavo-convex structure (medium wave structure and small wave structure), the outer shape of the protrusions, and the average height The average density and the bottom area ratio were measured. These results are shown in Table 1 below together with the presence or absence of an anodized film and the presence or absence of cracks. In Table 1 below, an item represented by “-” indicates that the item does not exist.
Moreover, it was found by observation with an electron microscope that the surface of the deposition preventive plate produced in the example had a concavo-convex structure and a plurality of protrusions arranged. 8 and 9 show photographs of the surface of the adhesion-preventing plate produced in Example 1 at a magnification of 50 times and 350 times, respectively, and the apex at the protrusion of the adhesion-prevention plate produced in Example 1 and FIGS. 10A and 10B show photographs of the slope magnification of 2000 times, respectively.
＜剥離防止性＞
作製した防着板を、真空蒸着装置（昭和真空社製 ＳＧＣ−２２ＳＡ）の内壁面に、カプトンテープを用いて図１に示すように貼着した。
防着板を貼着した成膜装置を用いて、基板Ｚの表面に、真空蒸着によって金を成膜した。具体的には、蒸着１回あたりの成膜量を１μｍとし、成膜圧力を１×１０-3Ｐａとし、サンプル温度を２５０℃とし、蒸着ごとに熱サイクル（室温⇔２５０℃）を繰り返した際に、以下の基準により剥離防止性を評価した。
Ａ１：２００回の蒸着を繰り返して目視による剥離が観測されない。
Ａ２：１８０回以上２００回未満の蒸着で目視による剥離が観察される。
Ｂ：１００回以上１８０回未満の蒸着で目視による剥離が観察される。
Ｃ：５０回以上１００回未満の蒸着で目視による剥離が観察される。
Ｄ：３０回以上５０回未満の蒸着で目視による剥離が観察される。
<Peeling prevention property>
The produced adhesion prevention board was affixed on the inner wall surface of the vacuum evaporation system (Showa Vacuum SGC-22SA) as shown in FIG. 1 using the Kapton tape.
A gold film was formed on the surface of the substrate Z by vacuum vapor deposition using a film forming apparatus to which an adhesion preventing plate was attached. Specifically, the deposition amount per deposition was 1 μm, the deposition pressure was 1 × 10 −3 Pa, the sample temperature was 250 ° C., and the thermal cycle (room temperature to 250 ° C.) was repeated for each deposition. At that time, the anti-peeling property was evaluated according to the following criteria.
A1: Deposition by visual observation is not observed after repeated 200 depositions.
A2: Visual peeling is observed by vapor deposition of 180 times or more and less than 200 times.
B: Peeling by visual observation is observed by vapor deposition of 100 times or more and less than 180 times.
C: Visual peeling is observed by vapor deposition of 50 times or more and less than 100 times.
D: Visual peeling is observed by vapor deposition 30 times or more and less than 50 times.
＜加工性＞
作製した各防着板について、以下に示す方法により加工性を評価した。
すなわち、カプトンテープを用いて、防着板を真空蒸着装置（昭和真空社製 ＳＧＣ−２２ＳＡ）の内壁面に貼着する際に、真空チャンバの内壁面から浮き上がらず、容易に貼着することができたものを加工性に大変優れるものとして「Ａ」と評価し、真空チャンバの内壁面からわずかに浮きあがりが生じたものの、容易に貼着することができたものを加工性に優れるものとして「Ｂ」と評価した。この結果を下記第１表に示す。
<Processability>
About each produced adhesion prevention board, workability was evaluated by the method shown below.
That is, when using a Kapton tape to attach an adhesion-preventing plate to the inner wall surface of a vacuum vapor deposition apparatus (SGC-22SA manufactured by Showa Vacuum Co., Ltd.), it can be easily attached without lifting from the inner wall surface of the vacuum chamber. The product was evaluated as “A” as having excellent workability, and although it was slightly lifted from the inner wall surface of the vacuum chamber, it could be easily pasted and had excellent workability. Rated “B”. The results are shown in Table 1 below.
上記第１表に示す通り、特定の平均開口径の凹部を含む凹凸構造が形成された表面を有し、かつ、この表面に特定の平均高さの複数の突出部が所定の割合で配列された防着板は、蒸着を繰り返した場合にも、剥離防止効果に優れることが分かった（実施例１〜１０）。特に、実施例１と実施例２との対比などからも分かるように、突出部の底部面積比率が高い程、蒸着を繰り返した際の剥離防止効果がより向上することが分かった。また、実施例２と実施例７との対比から、表面にクラックを有する防着板は、蒸着を繰り返した際の剥離防止効果がより向上することが分かった。更に、実施例２と実施例１０との対比から、焼鈍処理を施すことにより、防着板の加工性が良好となることが分かった。
これに対し、表面に突出部または凹凸構造を有さない防着板や、表面に配列される突出部の割合を満たさない防着板は、いずれも、蒸着を繰り返した場合に、剥離防止効果が劣る場合があることが分かった（比較例１〜５）。
As shown in Table 1, the surface has a concavo-convex structure including a recess having a specific average opening diameter, and a plurality of protrusions having a specific average height are arranged on the surface at a predetermined ratio. It was found that the adhesion preventing plate was excellent in the effect of preventing peeling even when the deposition was repeated (Examples 1 to 10). In particular, as can be seen from the comparison between Example 1 and Example 2, it was found that the higher the bottom area ratio of the protrusions, the more improved the anti-peeling effect upon repeated deposition. Moreover, it turned out from the comparison with Example 2 and Example 7 that the peeling prevention effect at the time of repeating vapor deposition improves the adhesion prevention board which has a crack in the surface. Furthermore, it was found from the comparison between Example 2 and Example 10 that the workability of the adhesion-preventing plate is improved by performing the annealing treatment.
On the other hand, the adhesion preventing plate that does not have protrusions or uneven structures on the surface and the adhesion preventing plate that does not satisfy the ratio of the protrusions arranged on the surface are effective in preventing peeling when repeated deposition is performed. Was found to be inferior (Comparative Examples 1 to 5).
半導体装置や電子部品材料の製造等、真空蒸着、スパッタリング、プラズマＣＶＤなどの真空成膜法を利用する各種の製品の製造に、好適に利用可能である。 The present invention can be suitably used for manufacturing various products using vacuum film forming methods such as vacuum deposition, sputtering, and plasma CVD, such as manufacturing semiconductor devices and electronic component materials.
１０ 真空成膜装置
１２ 防着板
１２ａ 上面防着板
１２ｂ 側面防着板
１２ｃ 下面防着板
１４ 真空チャンバ
１６ 蒸着源
１８ 基板ホルダ
２０ 真空ポンプ
３０、３２、３４ 凹凸構造
３０ａ、３２ａ、３４ａ、 凹部
３０ｂ、３２ｂ、３４ｂ 凸部
４０ 突出部
４０ａ 底面
４０ｂ 頂点
４０ｃ 稜線
４０ｄ 斜面
４２ クラック
DESCRIPTION OF SYMBOLS 10 Vacuum film-forming apparatus 12 Adhesion board 12a Upper surface adhesion board 12b Side surface adhesion board 12c Lower surface adhesion board 14 Vacuum chamber 16 Deposition source 18 Substrate holder 20 Vacuum pump 30, 32, 34 Uneven structure 30a, 32a, 34a, Concave part 30b, 32b, 34b Projection 40 Projection 40a Bottom 40b Vertex 40c Ridge 40d Slope 42 Crack
Claims (13)
アルミニウム製であり、
平均開口径０．０１〜９μｍの凹部を含む凹凸構造が形成された表面を有し、
前記表面に、平均高さ３０〜１０００μｍの複数の突出部が配列されており、
前記突出部の平均密度が、１０個／１０ｍｍ角以上であり、
前記突出部の底部面積の比率が、１０ｍｍ角の領域において９０％超である真空成膜装置用防着板。 In a vacuum film forming apparatus, a deposition plate for a vacuum film forming apparatus for preventing adhesion of a film forming material to an unnecessary position,
Made of aluminum,
It has a surface on which a concavo-convex structure including recesses having an average opening diameter of 0.01 to 9 μm is formed,
A plurality of protrusions having an average height of 30 to 1000 μm are arranged on the surface,
The average density of the protrusions is 10 pieces / 10 mm square or more,
An adhesion-preventing plate for a vacuum film-forming apparatus, wherein the ratio of the bottom area of the protrusion is more than 90% in a 10 mm square region.
アルミニウム板の表面に電気化学的粗面化処理を施し、表面に平均開口径０．０１〜９μｍの凹部を含む凹凸構造を形成する凹凸形成工程と、
アルミニウム板の表面にエンボス加工を施し、表面の一部に平均高さ３０〜１０００μｍの複数の突出部を形成する突出部形成工程とを有する製造方法。 In a vacuum film forming apparatus, a manufacturing method for manufacturing a deposition plate for a vacuum film forming apparatus for preventing adhesion of a film forming material to an unnecessary position,
An uneven surface forming step of performing an electrochemical surface roughening treatment on the surface of the aluminum plate and forming an uneven structure including recesses having an average opening diameter of 0.01 to 9 μm on the surface;
The manufacturing method which has a protrusion part formation process which gives the embossing to the surface of an aluminum plate, and forms several protrusion part with an average height of 30-1000 micrometers in a part of surface.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
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| JP2013044908A JP2014173106A (en) | 2013-03-07 | 2013-03-07 | Deposition preventive plate for vacuum film deposition apparatus, vacuum film deposition apparatus, and vacuum film deposition method |
| KR1020140015058A KR20140110729A (en) | 2013-03-07 | 2014-02-10 | Deposition prevention plate for vacuum film forming device, method for manufacturing deposition prevention plate for vacuum film forming device, vacuum film forming device, and vacuum film forming method |
| CN201410072392.2A CN104032259A (en) | 2013-03-07 | 2014-02-28 | Adhesion-prevention Plate Used For Vacuum Film-forming Device And Applications Thereof |
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| JP2013044908A JP2014173106A (en) | 2013-03-07 | 2013-03-07 | Deposition preventive plate for vacuum film deposition apparatus, vacuum film deposition apparatus, and vacuum film deposition method |
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| JP2020507674A (en) * | 2017-01-20 | 2020-03-12 | ハネウェル・インターナショナル・インコーポレーテッドＨｏｎｅｙｗｅｌｌ Ｉｎｔｅｒｎａｔｉｏｎａｌ Ｉｎｃ． | Particle trap for sputtering coil and manufacturing method |
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| CN105900210B (en) * | 2014-12-15 | 2021-06-01 | 应用材料公司 | Method for texturing a chamber component and chamber component with textured surface |
| CN105568224B (en) * | 2016-01-28 | 2018-09-21 | 京东方科技集团股份有限公司 | Vapor deposition radical occlusion device and evaporated device |
| CN107513683A (en) * | 2017-08-31 | 2017-12-26 | 深圳市华星光电技术有限公司 | Plate and preparation method thereof is prevented in one kind vapour deposition |
| JP2019157144A (en) * | 2018-03-07 | 2019-09-19 | シャープ株式会社 | Film deposition apparatus |
| CN108546913B (en) * | 2018-05-03 | 2021-04-27 | 京东方科技集团股份有限公司 | Mask plate and preparation method thereof |
| KR102148072B1 (en) * | 2018-05-14 | 2020-08-26 | 주식회사 야스 | Vacuum deposition chamber with latch screen |
| JP7072999B2 (en) * | 2018-11-30 | 2022-05-23 | 株式会社吉野工業所 | Synthetic resin container and method for manufacturing synthetic resin container |
| CN110453181A (en) * | 2019-08-08 | 2019-11-15 | 深圳市华星光电半导体显示技术有限公司 | Evaporated device and its prevent plate |
| CN113373421B (en) * | 2021-06-08 | 2022-11-18 | 京东方科技集团股份有限公司 | Anti-sticking plate, preparation method thereof and evaporation equipment |
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| JP2020507674A (en) * | 2017-01-20 | 2020-03-12 | ハネウェル・インターナショナル・インコーポレーテッドＨｏｎｅｙｗｅｌｌ Ｉｎｔｅｒｎａｔｉｏｎａｌ Ｉｎｃ． | Particle trap for sputtering coil and manufacturing method |
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| Publication number | Publication date |
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| KR20140110729A (en) | 2014-09-17 |
| CN104032259A (en) | 2014-09-10 |
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