JP5965225B2 - 微小亀裂耐性の向上した積層品及びその製造方法 - Google Patents
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Description
式中、R1は炭素原子数1〜約6のアルキル基又はアルコキシアルキル基であり、R2は炭素原子数1〜約6のアルキレン基であるが、R1及びR2に存在する炭素原子の数の合計が3〜約10であることを条件とする。炭素原子数1〜4のアルカノールには、メタノール、エタノール、プロパノール、イソプロパノール及びtert−ブタノール等がある。
式中、YはH又はメチル基であり、R1はアルキル基であり、好ましくは炭素原子数1〜約20のアルキル基である。
YはH又はOHであり、
ZはH、OH、OQ又はOWであり、
Qは−CH2(CH2)nSi(R2)u(OR1)vであり、
Wは−CmH2m+1であり、
上式中、Uは0、1又は2であり、Vは1、2又は3であり、U+V=3であり、R1は炭素原子数1〜6のアルキル又はアルカノイルであり、R2は炭素原子数1〜6のアルキルであり、好ましくはメチルであり、nは0、1又は2であり、m=1〜18である。
ポリカーボネートを含んでなる自動車用プライバシーグレードの後部ウィンドウに、アクリル系プライマー層を塗工した。アクリル材料は、B.F.Goodrich Companyによって供給されたHycar237及びHycar256の二つの熱硬化性エマルションの重量基準で50/50のブレンドとした。エマルションを2−エチルヘキシル−2−シアノ−3,3−ジフェニルシアノアクリレート(GAF Corp.から販売されているUvinul N−539(商標)として公知のUV吸収剤)、クエン酸及びブトキシエタノール水溶液と併せて、2−ブトキシエタノール25重量%/水75重量%中で固形分がアクリルポリマー2.56重量%、2−エチルヘキシル−2−シアノ−3,3−ジフェニルシアノアクリレート1.44重量%及びクエン酸0.025重量%からなるようにした。
第二の後部ウィンドウを製造した。第二の後部ウィンドウは実施例1のウィンドウと同じであったが、前述のような二つの副層を含んでなる耐摩耗性層でさらに被覆した点が異なる。耐摩耗性層は、テトラメチルジシロキサン(TMDSO)のプラズマ重合によって塗工された。プラズマ重合は、図3に示したPECVD装置で行われた。第一の副層については、試薬はTMDSO及びアルゴンであり、流量比を2:1(TMDSO:アルゴン)とした。パワー密度は7×107J/Kgであった。圧力は3ミリトルであり、持続時間は3分間であった。第二の副層については、試薬はTMDSO及び酸素であり、流量比を1:1(TMDSO:酸素)とした。パワー密度は7×107J/Kgであった。圧力は3ミリトルであり、持続時間は73分間であった。二つの副層の合計厚さは約2.5ミクロンであった。
実施例1と同じポリカーボネート/プライマー/中間層のサンプルを製造したが、中間層のpHが5であった点が異なる。サンプルをASTM G26に従ってAtlas Xenon Arc Weatherometerで6875kJ/m2の輻射線に曝露した。ASTM G26は、光への連続的曝露及び水噴射への間歇的曝露を指定している。サイクルは、102分間の光の後に、18分の光及び水噴射の1サイクルとした。6875KJ/M2の曝露の後に、サンプルはASTM D3359−92a接着性試験に合格したが、極端な微小亀裂を呈していた。
実施例3と同じサンプルを製造したが、前述のような二つの副層を含んでなる耐摩耗性層でさらに被覆した点が異なる。耐摩耗性層は、テトラメチルジシロキサン(TMDSO)のプラズマ重合によって塗工された。プラズマ重合は、図3に示したPECVD装置で行われた。第一の副層については、試薬はTMDSO及びアルゴンであり、流量比を2:1(TMDSO:アルゴン)とした。パワー密度は7×107J/Kgであった。圧力は3ミリトルであり、持続時間は約3分間であった。第二の副層については、試薬はTMDSO及び酸素であり、流量比を1:1(TMDSO:酸素)とした。パワー密度は7×107J/Kgであった。圧力は3ミリトルであり、持続時間は約27分間であった。二つの副層の合計厚さは約1ミクロンであった。
実施例4と同じサンプルを製造したが、耐摩耗性層の厚さが4ミクロンであった点が異なる。サンプルをASTM G26に従ってAtlas XenonArc Weatherometerで6875kJ/m2の輻射線に曝露した。サンプルはASTM D3359−92a接着性試験に合格し、微小亀裂を全く呈さなかった。
15 プライマー層
20 中間層
30 耐摩耗性層
100 プラズマ重合フィルム形成用装置
102 反応容器
103、105、107 マスフローコントローラ
104 有機ケイ素単量体供給源
106 酸素供給源
108 不活性ガス供給源
110 混合器
112 ガス供給線
120、121 電極
122 基材
140 後方プレート
142 前方プレート
144 磁石
146 孔
Claims (8)
- ポリマー基材(10)と、第一の層(20)と、第二の層(30)とを含んでなる多層品を作製する方法であって、
該方法は、
前記第一の層(20)を形成する工程;ならびに
前記第二の層(30)を形成する工程
を含んでおり;
第二の層(30)は、第一の層(20)の上に堆積されており;
第一の層(20)は、
式R2Si(OR’)2のジオルガノジオルガノオキシシラン、式RSi(OR’)3のオルガノトリオルガノオキシシラン又は両者の部分縮合物を含んでなる第一の層(20)(式中、Rは独立に炭素原子数1〜3のアルキル基、炭素原子数6〜13の芳香族基、ビニル基、3,3,3−トリフルオロプロピル基、γ−グリシドキシプロピル基及びγ−メタクリロキシプロピル基からなる群から選択され、R’は独立に炭素原子数1〜8のアルキル基、炭素原子数6〜20の芳香族基及び水素からなる群から選択される。)であり;
第一の層(20)は、硬化処理を施してシルセスキオキサンRSiO 3/2 が形成されており、
第二の層(30)は、最初の副層ならびに、ケイ素、酸素、炭素及び水素を含む第二の副層を含んでなり、
最初の副層は、プラズマ中で重合された有機ケイ素材料を含んでなり、
第二の副層は、過剰の酸素の存在下、106〜108J/Kgのパワーレベルで、プラズマ中で重合及び酸化した有機ケイ素材料を含んでなり、
前記有機ケイ素材料は、シロキサンであり、
第二の副層は、最初の副層の上に堆積されており;
第二の副層の厚さと最初の副層の厚さの比(第二の副層:最初の副層)は、1:1〜30:1の範囲に選択されており、
最初の副層の厚さは、0.05〜1.5ミクロンの範囲に選択されており、第二の副層の厚さは、0.5〜3.0ミクロンの範囲に選択されており、
最初の副層の厚さと、第二の副層の厚さの合計は、1〜4ミクロンの範囲に選択されている
ことを特徴とする、多層品の作製方法。 - 多層品は、ポリマー基材(10)と第一の層(20)の間に、プライマー層(15)をさらに含んでなる
ことを特徴とする、請求項1に記載の方法。 - ポリマー基材(10)と、第一の層(20)と、第二の層(30)とを含んでなる多層品を作製する方法であって、
前記多層品は、ポリマー基材(10)と第一の層(20)の間に、プライマー層(15)をさらに含んでおり、
該方法は、
前記ポリマー基材(10)上に前記プライマー層(15)を形成する工程;
前記第一の層(20)を形成する工程;ならびに
前記第二の層(30)を形成する工程
を含んでおり;
第二の層(30)は、第一の層(20)の上に堆積されており;
第一の層(20)は、
式R2Si(OR’)2のジオルガノジオルガノオキシシラン、式RSi(OR’)3のオルガノトリオルガノオキシシラン又は両者の部分縮合物を含んでなる層(式中、Rは独立に炭素原子数1〜3のアルキル基、炭素原子数6〜13の芳香族基、ビニル基、3,3,3−トリフルオロプロピル基、γ−グリシドキシプロピル基及びγ−メタクリロキシプロピル基からなる群から選択され、R’は独立に炭素原子数1〜8のアルキル基、炭素原子数6〜20の芳香族基及び水素からなる群から選択される。)であり;
第一の層(20)は、硬化処理を施してシルセスキオキサンRSiO 3/2 が形成されており、
第二の層(30)は、最初の副層ならびに、ケイ素、酸素、炭素及び水素を含む第二の副層を含んでなり、
最初の副層は、プラズマ中で重合された有機ケイ素材料を含んでなり、
第二の副層は、過剰の酸素の存在下、106〜108J/Kgのパワーレベルで、プラズマ中で重合及び酸化した有機ケイ素材料を含んでなり、
前記有機ケイ素材料は、シロキサンであり、
最初の副層は、第一の層の上に堆積され、その後、
第二の副層は、最初の副層の上に堆積されており;
第二の副層の厚さと最初の副層の厚さの比(第二の副層:最初の副層)は、1:1〜30:1の範囲に選択されており、
最初の副層の厚さは、0.05〜1.5ミクロンの範囲に選択されており、第二の副層の厚さは、0.5〜3.0ミクロンの範囲に選択されており、
最初の副層の厚さと、第二の副層の厚さの合計は、1〜4ミクロンの範囲に選択されている
ことを特徴とする、多層品の作製方法。 - 第一の層(20)が紫外線吸収剤をさらに含んでなる
ことを特徴とする、請求項1〜3のいずれか一項に記載の方法。 - 第一の層(20)の厚さが1〜15ミクロンである
ことを特徴とする、請求項1〜4のいずれか一項に記載の方法。 - プライマー層(15)は、アクリルプライマー層である
ことを特徴とする、請求項2〜5のいずれか一項に記載の方法。 - アクリルプライマー層の厚さが0.6〜1.0ミクロンである
ことを特徴とする、請求項6に記載の方法。 - 有機ケイ素材料の単量体が、テトラメチルジシロキサン、ヘキサメチルジシロキサン及びオクタメチルシクロテトラシロキサンの1以上を含んでなる
ことを特徴とする、請求項1〜7のいずれか一項に記載の方法。
Applications Claiming Priority (2)
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US46005799A | 1999-12-13 | 1999-12-13 | |
US09/460,057 | 1999-12-13 |
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JP2001542728A Division JP2003515480A (ja) | 1999-12-13 | 2000-11-15 | 微小亀裂耐性の向上した積層品及びその製造方法 |
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JP2012232591A JP2012232591A (ja) | 2012-11-29 |
JP2012232591A5 JP2012232591A5 (ja) | 2013-05-30 |
JP5965225B2 true JP5965225B2 (ja) | 2016-08-03 |
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JP2001542728A Ceased JP2003515480A (ja) | 1999-12-13 | 2000-11-15 | 微小亀裂耐性の向上した積層品及びその製造方法 |
JP2012149041A Expired - Fee Related JP5965225B2 (ja) | 1999-12-13 | 2012-07-03 | 微小亀裂耐性の向上した積層品及びその製造方法 |
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US (1) | US6376064B1 (ja) |
EP (1) | EP1242196A2 (ja) |
JP (2) | JP2003515480A (ja) |
KR (1) | KR100745852B1 (ja) |
CN (1) | CN1329131C (ja) |
AU (1) | AU1610301A (ja) |
BR (1) | BR0016361A (ja) |
CA (1) | CA2394338A1 (ja) |
MX (1) | MXPA02005824A (ja) |
WO (1) | WO2001041541A2 (ja) |
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2000
- 2000-08-07 US US09/633,714 patent/US6376064B1/en not_active Expired - Lifetime
- 2000-11-15 JP JP2001542728A patent/JP2003515480A/ja not_active Ceased
- 2000-11-15 WO PCT/US2000/031331 patent/WO2001041541A2/en not_active Application Discontinuation
- 2000-11-15 MX MXPA02005824A patent/MXPA02005824A/es unknown
- 2000-11-15 EP EP00978664A patent/EP1242196A2/en not_active Ceased
- 2000-11-15 CA CA002394338A patent/CA2394338A1/en not_active Abandoned
- 2000-11-15 KR KR1020027007556A patent/KR100745852B1/ko active IP Right Grant
- 2000-11-15 CN CNB00818965XA patent/CN1329131C/zh not_active Expired - Fee Related
- 2000-11-15 BR BR0016361-9A patent/BR0016361A/pt not_active IP Right Cessation
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CA2394338A1 (en) | 2001-06-14 |
BR0016361A (pt) | 2002-10-01 |
CN1434750A (zh) | 2003-08-06 |
EP1242196A2 (en) | 2002-09-25 |
CN1329131C (zh) | 2007-08-01 |
WO2001041541A2 (en) | 2001-06-14 |
KR100745852B1 (ko) | 2007-08-02 |
KR20020060263A (ko) | 2002-07-16 |
MXPA02005824A (es) | 2002-09-24 |
US6376064B1 (en) | 2002-04-23 |
AU1610301A (en) | 2001-06-18 |
JP2003515480A (ja) | 2003-05-07 |
JP2012232591A (ja) | 2012-11-29 |
WO2001041541A3 (en) | 2002-01-17 |
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