JPS63247351A - Manufacture of silicon compound-coated resin body - Google Patents
Manufacture of silicon compound-coated resin bodyInfo
- Publication number
- JPS63247351A JPS63247351A JP8176187A JP8176187A JPS63247351A JP S63247351 A JPS63247351 A JP S63247351A JP 8176187 A JP8176187 A JP 8176187A JP 8176187 A JP8176187 A JP 8176187A JP S63247351 A JPS63247351 A JP S63247351A
- Authority
- JP
- Japan
- Prior art keywords
- resin body
- silicon
- silicon monoxide
- partial pressure
- torr
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000011347 resin Substances 0.000 title claims abstract description 19
- 229920005989 resin Polymers 0.000 title claims abstract description 19
- 150000003377 silicon compounds Chemical class 0.000 title claims abstract description 12
- 238000004519 manufacturing process Methods 0.000 title claims description 6
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 claims abstract description 32
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910001873 dinitrogen Inorganic materials 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000007733 ion plating Methods 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 239000011248 coating agent Substances 0.000 claims description 2
- 238000000576 coating method Methods 0.000 claims description 2
- 238000001771 vacuum deposition Methods 0.000 claims description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 6
- 229910052802 copper Inorganic materials 0.000 abstract description 6
- 239000010949 copper Substances 0.000 abstract description 6
- 239000000758 substrate Substances 0.000 abstract description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 3
- 238000005336 cracking Methods 0.000 abstract description 2
- 229960005419 nitrogen Drugs 0.000 abstract 2
- 238000000151 deposition Methods 0.000 abstract 1
- 238000010891 electric arc Methods 0.000 abstract 1
- 229910052814 silicon oxide Inorganic materials 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 238000007738 vacuum evaporation Methods 0.000 description 3
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920006393 polyether sulfone Polymers 0.000 description 2
- 239000004695 Polyether sulfone Substances 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 210000002468 fat body Anatomy 0.000 description 1
- 239000005357 flat glass Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000014347 soups Nutrition 0.000 description 1
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明はシリコン化合物被ffl樹脂体の製造方法に関
する5、
〔従来の技術〕
真空蒸着法やイオンプレーティング法によりてシリコン
酸化物の薄膜を形成することは従来公知である、たとえ
ばVACUUM Mo1.14.385〜392 (1
964)やJourmal of Applied P
hysicsVoL 34.347〜351 (196
2)には真空蒸着により一酸化ケイ素被膜を形成するこ
とが記載されている。[Detailed Description of the Invention] [Industrial Application Field] The present invention relates to a method for producing a silicon compound-covered ffl resin body. It is conventionally known to form, for example, VACUUM Mo1.14.385-392 (1
964) and Journal of Applied P
hysicsVoL 34.347~351 (196
2) describes that a silicon monoxide film is formed by vacuum deposition.
一般に樹脂体表面にセラミックスを被覆した場合、セラ
ミックス層の膜厚が厚いほど、表面硬度、耐摩耗性、耐
擦傷性等が侵れているが、一酸化ケイ素の蒸着層は膜厚
を厚くすると残留応力が大きくなり、クラックが発生し
たり、膜剥離が発生し、連続膜が得られないという欠点
があった。Generally, when the surface of a resin body is coated with ceramics, the thicker the ceramic layer, the worse the surface hardness, wear resistance, scratch resistance, etc. This method has the drawback that residual stress becomes large, cracks occur, film peeling occurs, and a continuous film cannot be obtained.
本発明の目的は上記欠点に艦み、厚膜のシリコン化合物
の被膜が、クラックを発生したり、剥離したりすること
なく強固にW!看した樹脂体の製造方法を提供すること
にある。The object of the present invention is to solve the above-mentioned drawbacks, and to make the thick silicon compound coating strong and strong without cracking or peeling! It is an object of the present invention to provide a method for manufacturing a resin body.
以下、本発明のシリコン化合物被覆樹脂体の製造方法を
9面を参照して説明する。Hereinafter, the method for manufacturing a silicon compound-coated resin body of the present invention will be explained with reference to page 9.
第1図は本発明で用いられる装置の一例を示す模式図で
ある。図中1は真空槽であり、排気口2に連結される排
気装置1(図示せず)によって高真空に排気されるよう
になされている。真空槽1内1こは一酸化ケイ素4が供
給された、加熱及び冷却装置付きの銅ハース3が設けら
れでいる。銅ハース3の上方には電極に接続されたイオ
ン化電極5が設置され、蒸発した一酸化ケイ素をイオン
化できるようになされている。又、イオン化電極5のさ
らに上方には樹脂体7を固定するための基板6が設けら
れ、基板6は電極に接続されている。又8はガス導入口
であり、水蒸気や窒素ガスを導入できるようになされて
いる。FIG. 1 is a schematic diagram showing an example of a device used in the present invention. In the figure, reference numeral 1 denotes a vacuum chamber, which is evacuated to a high vacuum by an exhaust device 1 (not shown) connected to an exhaust port 2. Inside the vacuum chamber 1 is provided a copper hearth 3 equipped with a heating and cooling device to which silicon monoxide 4 is supplied. An ionization electrode 5 connected to an electrode is installed above the copper hearth 3 so as to be able to ionize the evaporated silicon monoxide. Furthermore, a substrate 6 for fixing the resin body 7 is provided further above the ionization electrode 5, and the substrate 6 is connected to the electrode. Further, 8 is a gas introduction port, which is designed to allow introduction of water vapor or nitrogen gas.
本発明においては、真空槽lの減圧度が小さいと一酸化
ケイ素を真空蒸着又はイオンプレーティングする際に残
存酸素によって一酸化ケイ素が二酸化ケイ素になり、密
着性が低下するので、最初に1×10−5 )−ル以
下に減圧し、しかる後水蒸気又は窒素ガスを導入する。In the present invention, if the degree of decompression in the vacuum chamber l is low, silicon monoxide turns into silicon dioxide due to residual oxygen during vacuum evaporation or ion plating of silicon monoxide, reducing adhesion. The pressure is reduced to below 10-5) liters, and then steam or nitrogen gas is introduced.
水蒸気又は窒素ガスの導入量は多くなると一酸化ケイ素
と水蒸気又は窒素との反応物の急が多くなり、シリコン
化合物の層の残留応力が大きくなってクラックが発生し
やすくなるので、水蒸気分圧又は窒素分圧が5×lO〜
5xlOトールになるように導入する。If the amount of water vapor or nitrogen gas introduced increases, the reaction product between silicon monoxide and water vapor or nitrogen will increase, and the residual stress in the silicon compound layer will increase, making cracks more likely to occur. Nitrogen partial pressure is 5×1O ~
Introduce the solution to a concentration of 5xlO torr.
本発明においては上記減圧状態で、銅ハース3を加熱し
て、銅ハース3に供給された一酸化ケイ素4を蒸発させ
樹脂体7上にシリコン化合物層を形成する。In the present invention, the copper hearth 3 is heated in the reduced pressure state to evaporate the silicon monoxide 4 supplied to the copper hearth 3 and form a silicon compound layer on the resin body 7.
この際、イオンプレーティング法によって被覆するには
イオン化電極5に直流電圧を印加し、^−り放電を発生
させて蒸発した一酸化ケイ素の一部をイオン化すればよ
く、さらに基板6にも負の直流電圧を印加してもよい。At this time, in order to coat with the ion plating method, it is sufficient to apply a DC voltage to the ionization electrode 5 to generate a back discharge and ionize a part of the evaporated silicon monoxide. You may apply a DC voltage of .
尚、この印加電圧は基板6の温度上昇をまねくので、樹
脂体7の樹脂の耐熱性によって適宜決定される。Note that this applied voltage causes a rise in the temperature of the substrate 6, so it is determined appropriately depending on the heat resistance of the resin of the resin body 7.
又、真空蒸着法によって被覆するにはイオン化電極5及
び基板7をアース状態番こし、それ以外はイオンプレー
ティング法と同様に行なえばよい。Further, in order to coat the film by vacuum evaporation, the ionization electrode 5 and the substrate 7 may be kept in a grounded state, and the other steps may be carried out in the same manner as in the ion plating method.
本発明の構T!tFi上述の通りであり、真空槽内を1
x 10−’ )−ル以下に減圧した後水蒸気又は窒
素ガスを水蒸気分圧又は窒素分圧が5X10’〜5X1
0’)−ルに々るように導入し、その状態で一酸化グイ
素を真空蒸着法又はイオンプレーティング法によって樹
脂体に被覆するのであるから、被覆されたシリコン化合
物の層は大部分の一酸化グイ素と、一部の一酸化ケイ素
と水蒸気又は窒素との反応物によって形成されており、
残留応力が小さく、膜厚を厚くしてもクラックが発生し
たり、膜剥離が発生することがない。従って、膜厚の厚
いシリコン化合物層が強固に密着された樹脂体を得るこ
とができ、得られた樹脂体Fi表面硬度、耐摩耗性、耐
擦傷性等がすぐれており、プラスチックレンズ、窓ガラ
ス、その他表面硬化プラスチック製品として好適に使用
できる。Structure of the present invention! tFi is as described above, and the inside of the vacuum chamber is 1
After reducing the pressure to below x 10-'), the water vapor or nitrogen gas is heated to a water vapor partial pressure or nitrogen partial pressure of 5X10' to 5X1.
Since the resin body is coated with gulyric monoxide by vacuum evaporation or ion plating in that state, most of the coated silicon compound layer is It is formed by a reaction product of guyric monoxide, some silicon monoxide, and water vapor or nitrogen.
Residual stress is small, and even if the film thickness is increased, cracks will not occur or film peeling will occur. Therefore, it is possible to obtain a resin body to which a thick silicon compound layer is firmly adhered, and the resulting resin body Fi has excellent surface hardness, abrasion resistance, scratch resistance, etc., and is suitable for use in plastic lenses, window glasses, etc. , and other surface-hardened plastic products.
次に本発明の詳細な説明する。 Next, the present invention will be explained in detail.
実施例1〜11.比較例1〜6
第1図に示した装置IIこおいて411脂体7としてポ
リエーテルサルフオンフイルムを設置し、8×10 ト
ールまで減圧した後、第1表に示したガスを導入し、導
入ガス分圧を第1表に示す通り維持した。イオン化電極
5に40Vの直流電圧を印加し、基板6はアース状態に
し、銅ハース3を加熱することにより一酸化ケイ素を蒸
発させ、イオンプレーティング法により、シリコン化合
物層が被覆されたポリエーテルサルフオンフイルムを得
た。シリコン化合物層の厚みを測定し第1表に示した。Examples 1-11. Comparative Examples 1 to 6 A polyether sulfon film was installed as the 411 fat body 7 in the apparatus II shown in FIG. 1, and after reducing the pressure to 8×10 Torr, the gases shown in Table 1 were introduced, The inlet gas partial pressure was maintained as shown in Table 1. A DC voltage of 40 V is applied to the ionizing electrode 5, the substrate 6 is grounded, silicon monoxide is evaporated by heating the copper hearth 3, and polyether salt coated with a silicon compound layer is formed by the ion plating method. I got Huon film. The thickness of the silicon compound layer was measured and shown in Table 1.
又、表面硬度試験(ヌープ硬度、荷[25gで測定)及
びヒートサイクルテスト(−20C% 1時間保持と1
00σ1時間保持を100回繰返した後光学顕微鏡で表
面を観察)を行い結果を第1表に示した。尚、ポリエー
テルサルフォンフイルムのスープ硬度−は20KII/
dであった。In addition, surface hardness test (Knoop hardness, measured with a load of 25 g) and heat cycle test (-20C% 1 hour holding and 1
After repeating 00σ for 1 hour 100 times, the surface was observed using an optical microscope, and the results are shown in Table 1. In addition, the soup hardness of polyether sulfone film is 20KII/
It was d.
第 1 表Table 1
eE1図は本発明の製造方法で用いられる装置の一例を
示す模式図である。Figure eE1 is a schematic diagram showing an example of an apparatus used in the manufacturing method of the present invention.
Claims (1)
酸化ケイ素を樹脂体に被覆するに際し、真空槽内を1×
10^−^5トール以下に減圧した後水蒸気又は窒素ガ
スを導入し、水蒸気分圧又は窒素分圧を5×10^−^
5〜5×10^−^4トールに維持しながら一酸化ケイ
素を加熱し、樹脂体に被覆することを特徴とするシリコ
ン化合物被覆樹脂体の製造方法。1. When coating silicon monoxide on a resin body by vacuum evaporation method or ion plating method, the inside of the vacuum chamber is
After reducing the pressure to 10^-^5 torr or less, water vapor or nitrogen gas is introduced to reduce the water vapor partial pressure or nitrogen partial pressure to 5 x 10^-^.
1. A method for producing a silicon compound-coated resin body, which comprises heating silicon monoxide while maintaining the temperature at 5 to 5×10^-^4 Torr to coat the resin body.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP8176187A JPS63247351A (en) | 1987-04-01 | 1987-04-01 | Manufacture of silicon compound-coated resin body |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP8176187A JPS63247351A (en) | 1987-04-01 | 1987-04-01 | Manufacture of silicon compound-coated resin body |
Publications (1)
Publication Number | Publication Date |
---|---|
JPS63247351A true JPS63247351A (en) | 1988-10-14 |
Family
ID=13755435
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP8176187A Pending JPS63247351A (en) | 1987-04-01 | 1987-04-01 | Manufacture of silicon compound-coated resin body |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPS63247351A (en) |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS5334474A (en) * | 1976-09-11 | 1978-03-31 | Nippon Chemical Ind | Method of making colored opaque photomask blank material by ion plating method |
JPS5558230A (en) * | 1978-10-24 | 1980-04-30 | Asahi Glass Co Ltd | Method of forming cured siox coating film |
-
1987
- 1987-04-01 JP JP8176187A patent/JPS63247351A/en active Pending
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS5334474A (en) * | 1976-09-11 | 1978-03-31 | Nippon Chemical Ind | Method of making colored opaque photomask blank material by ion plating method |
JPS5558230A (en) * | 1978-10-24 | 1980-04-30 | Asahi Glass Co Ltd | Method of forming cured siox coating film |
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