JPS63247351A - Manufacture of silicon compound-coated resin body - Google Patents

Manufacture of silicon compound-coated resin body

Info

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
Application number
JP8176187A
Other languages
Japanese (ja)
Inventor
Yoshiyuki Fukumoto
福本 義行
Atsushi Mansei
満生 敦士
Tadahiro Ota
忠宏 太田
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Sekisui Chemical Co Ltd
Original Assignee
Sekisui Chemical Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Sekisui Chemical Co Ltd filed Critical Sekisui Chemical Co Ltd
Priority to JP8176187A priority Critical patent/JPS63247351A/en
Publication of JPS63247351A publication Critical patent/JPS63247351A/en
Pending legal-status Critical Current

Links

Abstract

PURPOSE:To allow a thick silicon-compound film to adhere firmly to a resin body in a superior state, by introducing vapor into a vacuum tank evacuated to a specific pressure so that a specific partial pressure is reached and then heating silicon monoxide at the time of vacuum-depositing silicon oxide on a resin body. CONSTITUTION:The inside of a vacuum tank 1 is evacuated to <=1X10<-5>Torr and then maintained so that vapor partial pressure or nitrogen-gas partial pressure becomes 5X10<-5>-5X10<-4>Torr by introducing vapor or a nitrogen gas. A copper hearth 3 is heated in the above state to evaporate silicon monoxide 4 and DC voltage is impressed on an ionization electrode 5 to ionize a part of the silicon monoxide 4 by means of arc discharge, and then negative DC voltage is impressed on a substrate so as to coat a resin body 7 with the silicon monoxide 4. In this way, the thick film of silicon compound can be formed on the resin body 7 with firm adhesion without causing cracking and peeling.

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.

〔発明が解決しようとする問題点〕[Problem that the invention seeks to solve]

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.

〔問題点を解決するための手段〕[Means for solving problems]

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.

〔発明の効果〕〔Effect of the invention〕

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.

〔実施例〕〔Example〕

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

【図面の簡単な説明】[Brief explanation of drawings]

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)

【特許請求の範囲】[Claims] 1、真空蒸着法又はイオンプレーティング法により、一
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.
JP8176187A 1987-04-01 1987-04-01 Manufacture of silicon compound-coated resin body Pending JPS63247351A (en)

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)

* Cited by examiner, † Cited by third party
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

Patent Citations (2)

* Cited by examiner, † Cited by third party
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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