JP5039907B2 - 非平面状基体のためのプラズマ被覆装置 - Google Patents
非平面状基体のためのプラズマ被覆装置 Download PDFInfo
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- JP5039907B2 JP5039907B2 JP2007502917A JP2007502917A JP5039907B2 JP 5039907 B2 JP5039907 B2 JP 5039907B2 JP 2007502917 A JP2007502917 A JP 2007502917A JP 2007502917 A JP2007502917 A JP 2007502917A JP 5039907 B2 JP5039907 B2 JP 5039907B2
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Classifications
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/50—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges
- C23C16/513—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges using plasma jets
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/50—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
- B05D1/62—Plasma-deposition of organic layers
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/31504—Composite [nonstructural laminate]
- Y10T428/31652—Of asbestos
- Y10T428/31663—As siloxane, silicone or silane
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- Organic Chemistry (AREA)
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Description
本願は、2004年3月9日に出願された米国特許仮出願No.60/551,931の利権を主張するものであり、その全内容を参考のためここに組み入れる。
一般に、本発明は、実質的に均一な厚さを有し、平均値の約±0.25の範囲にある△曇り度(%)を有する実質的に均一な摩耗抵抗を有するプラズマ蒸着耐摩耗性被覆を有する非平面状物品に関する。
先ず図1に関し、そこには被覆場所10が示されており、そこでは基体12が、矢印13で示されているように、被覆場所を通って一定の直線経路に従って移動する。基体12は自動車乗り物のための部品でもよい。例えば、基体はプラスチックから作られた後部窓又は屋根のパネルでもよい。基体12はポリカーボネートを含んでいてもよい。
R1 nSiZ(4−n)
(式中、R1は、一価炭化水素ラジカル、又は一価ハロゲン化炭化水素ラジカルを表し、Zは加水分解可能な基を表し、nは0〜2の間で変化させることができる)
により表される化合物である。特にZは、ハロゲン、アルコキシ、アシルオキシ、又はアリールオキシのようなものであるのが典型的である。そのような化合物は、例えば、シュレーテル(Schroeter)その他による米国特許第4,224,378号明細書(それらの全内容は参考のためここに入れてある)に記載されている。
R2Si(OH)3
(式中、R2は、約1〜約3個の炭素原子を有するアルキルラジカル、ビニルラジカル、3,3,3−トリフルオロプロピルラジカル、γ−グリシドキシプロピルラジカル、γ−メタクリロキシプロピルラジカルを含む群から選択される)
を有するシラノールが含まれ、そのシラノールの少なくとも約70重量%はCH3Si(OH)3である。そのような化合物は、米国特許第4,242,381号明細書(これは参考のため全体的にここに入れてある)に記載されている。
この例では、ゼネラル・エレクトリックからのレキサンMR10シートを、プラズマ重合及び酸化D4で被覆した。被覆処理では、二つの静止ETP源14を、それらの中心線が平行に約16cm離れて配置されるように配列した。この構成を用いて、基体の約64in2を被覆した。4つの4in×4in試料39を、図2に示したように、アルミニウム保持器上に取付けた。それら試料を1T(右上)、1B(右下)、2T(左上)、及び2B(左下)として記号を付けた。基体を約2.3cm/秒の走査速度でETP源14に対し垂直に移動させた。四角形40は、珪素チップの典型的な位置を示している。これらのチップの上の被覆厚さを、偏光法により測定した。珪素チップは、被覆厚さのプロファイルを生じさせる実験中、垂直及び水平の両方の直線上で基体に沿って1in毎に配置した。陰影42は、65℃の水に3日間浸漬する前及び後で被覆の接着性を測定した場所である。リング44は、ASTM D1044摩耗試験後のテーバー輪の軌跡を示している。テーバー摩耗試験は、CS10F輪を用い1000サイクル行なわれた。リング44中の90°の角度で4つの場所で△曇り度を測定した。垂直の点線は、基体を移動させた時の夫々のETP源14の中心線の通路を示している。
処理条件は例1の場合と同様であった。但しWDを31cmに増大した。最終被覆厚さは2.1μで、例1と同じであったが、平均テーバー△曇り度は約3%に増大し、二つの実験については約4%に増大した。このように、希望の被覆厚さを得ることは、必ずしも良好な耐摩耗性を有する被覆を確実に与えるものとは限らず、特にWDを大きくして製造した被覆の場合にはそうである。従って、閾値WDを越えるWDを用いた非平面状部品は、被覆厚さが均一であったとしても、均一な耐摩耗性を持たないことがある。
処理条件は例1の場合と同様であった。但し基体保持器を約20°に傾斜させ(図3に示したように)、基体の上端の所でのWDが31cm、下端で24cmであった。約2.1μの均一な被覆厚さが得られたが、テーバー△曇り度は下端(即ち、作用距離が一層短い所)での約4%から上端での10%まで増大した。このように、例1〜3を比較すると、これらの処理条件で被覆したフラットな又は傾斜した部品の両方で、作用距離が比較的長くなるとテーバーは悪くなることを示している。
処理条件は例2のものと同様であったが、基体上に4つの層を蒸着し、全被覆厚さを約4μとした。層2〜4についての条件は、例2の層2の場合と同じであった。従って、耐摩耗性層の組成は同じままであったが、被覆厚さだけが変化した。テーバー△曇り度は、2.4%〜3.1%であった。このように、厚さを増大しただけでは、2%未満のテーバー△曇り度を与える結果にはならなかった。
この例では、耐摩耗性層2〜4についてアルゴン流を2.5slmに増大し、それはイオンフラックスを52.5Aに増大した。予熱温度を約75℃に低下し、第2〜第4層の時の酸素流量は2slmであった。他の条件は例4の場合と同じであった。3つの異なった試料について夫々31、20、及び25cmのWDを用いて3つの異なった実験を行なった。得られた被覆厚さは、例4の場合と同様であり、夫々4.5、4.7、及び5.4μであった。テーバー△曇り度は、夫々1.2%、1.1%、及び1.2%に改善した。
処理条件は例5のものと同様であった。基体の配列は図4に示してある。12aT、12aB、12bT、12bB、12c、及び12dの6つの傾斜した基体、即ち、試料が存在する。4つの基体12aT、12aB、12bT、12bBは20°の角度にしてあり、24〜31cmのWDを有する。他の二つの基体12c及び12dは、基体12aT、12aB、12bT、12bBの両側に立ててある。基体12c、12dは、4in×6inであり、21〜31cmのWDでETP中心線に平行に置かれている。図4Aでは、設定は移動方向に沿って見たものであり、従って、走査方向はその頁を出入るする方向である。図4Bでは、走査方向を上下にしてETP源から見たように基体が示されている。20°に傾斜した基体12aT、12aB、12bT、12bBについては、被覆厚さは約4.6〜4.9μであり、テーバー摩耗は約1.4%〜2.0%であった。ETP中心線に平行な2つの基体12c及び12dは、前面(即ち、基体12aT、12aB、12bT、12bBの方向に向いた側)では、夫々約2.8μm及び2.5%の平均厚さ及びテーバーを有し、後面(即ち、基体12aT、12aB、12bT、12bBから離れる方向を向いた側)では、夫々約3.1μm及び3.5%の平均厚さ及びテーバーを持っていた。
処理条件は例6のものと同様であった。図5に示したように、6つの4in×4in試料、即ち、基体12e、12f、12g、12h、12i、及び12jを、試料保持器50の前面及び後面の上に種々の角度で取付けた。2つの基体、12f、12hは、基体保持器に対し夫々50°及び60°の角度にし、「前面」の上にあるものとして標識を付け、ETP14の方に向けてある。2つの基体12g、12eは夫々120°及び130°の入射角度をもち、「後面」の上にあるものとして標識を付け、プラズマから離れて行く方向に向けてある。2つの基体12i、12jは、夫々前面試料12h、12fの夫々の基底の所にフラットに横たえてある。基体12e〜12jについてのWDは19.8cm〜27.8cmの範囲にあった。走査方向は上下であり、実験は2度行われたことに注意されたい。
この場合には、例1の被覆条件を用いて、ゼネラル・エレクトリックにより製造されたレキサンMR7シート及び石英スライドを、約2μのD4で被覆した。プラズマ被覆したMR7のUV照射前の耐摩耗性は2%より低かった。吸光度(absorbance)を厚さ(μ)で割ったものとして定義されている被覆のUV吸収性(absorbency)は、石英スライドで測定して300nm(UVB)で0.012μm−1、350nm(UVA)で0.007μm−1であった。被覆をQUVA及びQUVB強制耐候試験にかけた。テーバー摩耗を約1000時間毎に測定した。4000時間のQUVB及び2500時間のQUVA試験後に、性能の劣化は観察されなかった。
この例では、例8の条件を用いた。但し、有機珪素はTMDSOであった。被覆厚さは約1.5μであり、初期テーバー摩耗は約4%であった。被覆吸光度は300nmで0.057、350nmで0.031であった。QUVBに露出した後の耐摩耗性は、1000、2000、4000、及び5000時間で、夫々約6%、7%、9%、及び17%であった。
この例では、慣用的PVCVD反応器で適用したTMDSOで被覆した基体を評価した。被覆厚さは約4μであり、初期テーバー摩耗は約2%であった。被覆吸光度は300nmで0.37、350nmで0.1であった。QUVBに露出した後の耐摩耗性は、1000及び2000時間で、夫々約12%及び20%であった。2550時間のQUVA試験後、耐摩耗性は12%へ劣化した。
Claims (10)
- 非平面状基体を被覆する方法であって、該方法が、
一つ以上の静止した膨張熱プラズマ源からプラズマを発生させる工程と、
前記プラズマ中に第一組の気化した試薬を注入して基体上に第一被覆を形成する工程と、
前記プラズマ中に第二組の気化した試薬を注入して前記第一被覆上に一つ以上の被覆を形成する工程とを有しており、
前記プラズマがイオンフラックスを決定するアルゴン流れとアーク電流を有しており、
均一な被覆特性を与えるように前記イオンフラックスを調節する工程をさらに有している、方法。 - 前記均一な被覆特性が被覆の厚さである、請求項1に記載の方法。
- 前記均一な被覆特性が被覆の耐摩耗性である、請求項1に記載の方法。
- 前記耐摩耗性被覆がプラズマ重合した有機珪素である、請求項3に記載の方法。
- 前記有機珪素は、オクタメチルシクロテトラシロキサン、デカメチルシクロペンタシロキサン、ヘキサメチルジシロキサン、テトラメチルジシロキサン、テトラメチルテトラビニルシクロテトラシロキサン、ビニルトリメチルシラン及びジメチルジメトキシシランからなる群から選択される、請求項4に記載の方法。
- 前記耐摩耗性被覆が二つ以上の層として蒸着される、請求項3に記載の方法。
- 第一層が他の層の酸素含有量よりも低い酸素含有量を有する、請求項6に記載の方法。
- 第一層以外の層が同じ組成を有する、請求項7に記載の方法。
- 前記耐摩耗性被覆の層が300nmで約0.02μm−1の有機UV吸収剤を含む、請求項6に記載の方法。
- 前記プラズマを発生させる工程及び気化試薬を注入する工程が、1.65〜2.5slmのアルゴン流、0.3〜2slmの酸素流、0.19slm以下のオクタメチルシクロテトラシロキサン流、70アンペア以下のアーク電流と共に行われる、請求項1に記載の方法。
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US55193104P | 2004-03-09 | 2004-03-09 | |
US60/551,931 | 2004-03-09 | ||
PCT/US2005/007502 WO2005087978A1 (en) | 2004-03-09 | 2005-03-08 | Plasma coating system for non-planar substrates |
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-
2005
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EP1725699A1 (en) | 2006-11-29 |
KR20070010025A (ko) | 2007-01-19 |
US7390573B2 (en) | 2008-06-24 |
CN104746050A (zh) | 2015-07-01 |
CN104746050B (zh) | 2017-05-03 |
KR101246387B1 (ko) | 2013-03-21 |
WO2005087978A1 (en) | 2005-09-22 |
US20050202259A1 (en) | 2005-09-15 |
CN1946874A (zh) | 2007-04-11 |
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