JPH0733524A - Material coated with glassy carbon - Google Patents
Material coated with glassy carbonInfo
- Publication number
- JPH0733524A JPH0733524A JP4068988A JP6898892A JPH0733524A JP H0733524 A JPH0733524 A JP H0733524A JP 4068988 A JP4068988 A JP 4068988A JP 6898892 A JP6898892 A JP 6898892A JP H0733524 A JPH0733524 A JP H0733524A
- Authority
- JP
- Japan
- Prior art keywords
- glassy carbon
- graphite substrate
- material coated
- graphite
- coating layer
- 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.)
- Granted
Links
Landscapes
- Crucibles And Fluidized-Bed Furnaces (AREA)
- Recrystallisation Techniques (AREA)
- Ceramic Products (AREA)
- Chemically Coating (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、ガラス状炭素被覆物
品、詳しくは半導体などのハーメチックシール、ロー付
け等に用いられる治具、高温で溶融金属や溶融ガラスを
処理する際に用いられるルツボ、ボート、ダイス、鋳型
等の黒鉛材料に関する。BACKGROUND OF THE INVENTION The present invention relates to a glassy carbon-coated article, more specifically, a hermetic seal for semiconductors, jigs used for brazing, crucibles used for treating molten metal or molten glass at high temperatures, The present invention relates to graphite materials such as boats, dies, and molds.
【０００２】[0002]
【従来の技術】黒鉛材料はその優れた熱的性質と易加工
性のために、上記用途の処理容器として利用されてい
る。また、その黒鉛材料にガラス状炭素を被覆したもの
も知られている。（特開昭６２−２０７７８５号公報、
特開昭６２−２５２３９４号公報、特開昭６３−５４７
２９号公報等）。2. Description of the Related Art Graphite materials have been used as a processing container for the above applications because of their excellent thermal properties and easy workability. In addition, a graphite material coated with glassy carbon is also known. (JP-A-62-207785,
JP-A-62-252394, JP-A-63-547
No. 29, etc.).
【０００３】しかしながら、黒鉛基体にガラス状炭素を
被覆した物品は、それを被覆しないものに比べて、黒鉛
ダストの低減効果や、空気中の水分の吸湿又は吸着ガス
の防止効果はあるが、溶融金属や溶融ガラスとの付着性
が大きくなり、組成によっては、冷却後に金属やガラス
が付着してしまうという問題があった。However, an article obtained by coating a graphite substrate with glassy carbon has the effect of reducing graphite dust and the effect of absorbing moisture in the air or preventing adsorbed gas, as compared with the article in which the substrate is not coated, but it melts. There is a problem that the adhesion to metal or molten glass becomes large, and the metal or glass adheres after cooling depending on the composition.
【０００４】この問題を解決する方法として、黒鉛基体
が溶融金属と接する部分の正反射率を調整する方法が提
案されているが（特開平３−１４６４１１号公報）、こ
の方法では、黒鉛基体の表面加工時とガラス状炭素の被
覆時に正反射率の確認を行う必要があったので、量産性
に問題があった。As a method for solving this problem, there has been proposed a method of adjusting the regular reflectance of a portion where the graphite substrate is in contact with the molten metal (Japanese Patent Laid-Open No. 3-146411). Since it was necessary to confirm the regular reflectance at the time of surface processing and coating of glassy carbon, there was a problem in mass productivity.
【０００５】[0005]
【発明が解決しようとする課題】本発明者は、上記問題
を解決するため種々検討した結果、黒鉛基体へのガラス
状炭素被覆層厚み及びその内部への浸透深さと、溶融金
属や溶融ガラスの付着性との間に密接な関係があること
を見いだし、本発明を完成したものである。As a result of various studies to solve the above-mentioned problems, the present inventor has found that the thickness of the glassy carbon coating layer on the graphite substrate and the depth of penetration into the interior thereof, and the molten metal and molten glass They found that there is a close relationship with the adhesiveness, and completed the present invention.
【０００６】[0006]
【課題を解決するための手段】すなわち、本発明は、黒
鉛基体表面に厚さ０．１μｍ以下のガラス状炭素被覆層
を有し、しかも黒鉛基体表面から２００μｍ以上の深さ
にわたってガラス状炭素が含浸されてなることを特徴と
するガラス状炭素被覆物品である。That is, the present invention has a glassy carbon coating layer having a thickness of 0.1 μm or less on the surface of a graphite substrate, and the glassy carbon is spread over a depth of 200 μm or more from the surface of the graphite substrate. A glassy carbon-coated article characterized by being impregnated.
【０００７】以下、さらに詳しく本発明について説明す
る。The present invention will be described in more detail below.
【０００８】黒鉛基体表面へのガラス状炭素被覆層及び
黒鉛基体内部へのガラス状炭素含浸層を形成する方法と
しては、ガラス状炭素の前駆物質である有機重合体の熱
分解物を溶解してコーティングする方法（特公昭５２−
３９６８４号公報）、有機重合体又はその前駆体を溶融
してコ−ティングする方法（特開昭６２−２８３８０７
号公報）等があり、本発明においては、これらの方法が
基本的に採用される。As a method for forming a glassy carbon coating layer on the surface of a graphite substrate and a glassy carbon impregnated layer inside the graphite substrate, a pyrolyzed product of an organic polymer which is a precursor of glassy carbon is dissolved. Coating method (Japanese Patent Publication Sho 52-
39684), a method of melting and coating an organic polymer or a precursor thereof (JP-A-62-283807).
In this invention, these methods are basically adopted.
【０００９】しかしながら、これらの方法を単に採用し
たのでは、ガラス状炭素前駆物質の表面被覆と内部含浸
が同時に進行し、ガラス状炭素被覆層の厚みとガラス状
炭素含浸層の深さには正の相関が生じるので、本発明の
ように、ガラス状炭素被覆層が薄く、しかもガラス状炭
素含浸層の深い物品を得ることはできない。However, if these methods are simply adopted, surface coating and internal impregnation of the glassy carbon precursor proceed simultaneously, and the thickness of the glassy carbon coating layer and the depth of the glassy carbon impregnated layer are positive. Therefore, it is impossible to obtain an article having a thin glassy carbon coating layer and a deep glassy carbon impregnated layer as in the present invention.
【００１０】そこで、本発明では、ガラス状炭素の前駆
物質の溶剤、例えばトリクロルエチレン、ベンゼン、ト
ルエン等に一旦黒鉛基体を浸漬し、その後、ガラス状炭
素前駆物質を含む溶液（コ−ティング材）でコーティン
グするものである。この場合において、ガラス状炭素被
覆層の厚みとガラス状炭素含浸層の深さは、黒鉛基体の
浸漬処理からコーティングするまでの時間調節、ないし
はコーティング材への浸漬時間又はコーティング後にコ
ーティング材を拭き取る等の手段によりコーティング量
を調節することによって、変えることができる。Therefore, in the present invention, the graphite substrate is once immersed in a solvent of the glassy carbon precursor, for example, trichloroethylene, benzene, toluene, etc., and then the solution containing the glassy carbon precursor (coating material). It is to be coated with. In this case, the thickness of the glassy carbon coating layer and the depth of the glassy carbon impregnated layer are controlled by the time from the dipping treatment of the graphite substrate to the coating, or the dipping time in the coating material or the coating material is wiped off after coating, etc. It can be changed by adjusting the coating amount by means of.
【００１１】本発明で使用される黒鉛基体については、
特に制限はないが、嵩密度が低過ぎるとその内部に含浸
された溶剤の蒸発速度が速くなり、一方、嵩密度が高過
ぎると溶剤の含浸量が少なくなり、いずれの場合におい
ても所期の目的を達成することができないので、嵩密度
１．６〜１．９g/cm3 の黒鉛が好ましい。Regarding the graphite substrate used in the present invention,
There is no particular limitation, but if the bulk density is too low, the evaporation rate of the solvent impregnated therein will be fast, while if the bulk density is too high, the impregnated amount of the solvent will be small, and in any case the desired Graphite having a bulk density of 1.6 to 1.9 g / cm 3 is preferable because the purpose cannot be achieved.
【００１２】本発明において、ガラス状炭素被覆層の厚
みが０．１μｍを越えると、溶融金属や溶融ガラスとの
付着防止効果が小さくなり、一方、ガラス状炭素含浸層
の深さが２００μｍ未満では、黒鉛ダストの低減効果な
いし空気中の水分の吸湿又は吸着ガスの防止効果は小さ
くなる。In the present invention, if the thickness of the glassy carbon coating layer exceeds 0.1 μm, the effect of preventing adhesion to molten metal or molten glass becomes small, while if the depth of the glassy carbon impregnated layer is less than 200 μm. In addition, the effect of reducing graphite dust or the effect of absorbing moisture in the air or preventing adsorbed gas becomes small.
【００１３】[0013]
【実施例】以下、実施例と比較例をあげてさらに具体的
に本発明を説明する。 実施例１〜４ 比較例１〜１０ トリクロルエチレンに６時間浸漬された嵩密度１．７５
g/cm3 、形状１０×１０×５ｍｍの黒鉛板に、ポリ塩化
ビニル樹脂を窒素雰囲気中、５００℃の温度で熱分解し
て得られたタール状の前駆物質をトリクロルエチレンに
１０重量％溶解してなるコーティング材を浸漬法により
コーティングした後、真空雰囲気下、温度１０００℃で
焼成してガラス状炭素被覆層とガラス状炭素含浸層を形
成させた。ガラス状炭素被覆層の厚みとガラス状炭素含
浸層の深さの調節は、黒鉛基体をトリクロルエチレンに
浸漬してから上記コーティング材に浸漬するまでの時間
と上記コーティング材への浸漬時間を変えることによっ
て行った。EXAMPLES The present invention will be described in more detail with reference to Examples and Comparative Examples. Examples 1 to 4 Comparative Examples 1 to 10 Bulk density 1.75 soaked in trichloroethylene for 6 hours
10% by weight of tar-like precursor obtained by pyrolyzing polyvinyl chloride resin in a nitrogen atmosphere at a temperature of 500 ° C. on a graphite plate of g / cm 3 and a shape of 10 × 10 × 5 mm was dissolved in trichloroethylene. The coating material thus obtained was coated by a dipping method and then baked at a temperature of 1000 ° C. in a vacuum atmosphere to form a glassy carbon coating layer and a glassy carbon impregnated layer. The thickness of the glassy carbon coating layer and the depth of the glassy carbon impregnated layer can be adjusted by changing the time from the dipping of the graphite substrate in trichlorethylene to the dipping in the coating material and the dipping time in the coating material. Went by.
【００１４】上記とは別に、ガラス状炭素被覆層の厚み
とガラス状炭素含浸層の深さを測定するため、上記コー
ティング材にトレーサーとしてＳｉオイルを０．５重量
％配合したものを用いたこと以外は同様にして黒鉛板に
ガラス状炭素被覆層とガラス状炭素含浸層を形成させ、
ＥＰＭＡ装置によりＳｉの分布状態を測定した。In addition to the above, in order to measure the thickness of the glassy carbon coating layer and the depth of the glassy carbon impregnated layer, a coating material containing 0.5% by weight of Si oil was used as a tracer. In the same manner except for forming a glassy carbon coating layer and a glassy carbon impregnated layer on a graphite plate,
The distribution state of Si was measured by an EPMA apparatus.
【００１５】得られたガラス状炭素被覆板の上に、Ｉ
ｎ、Ｇａ、Ｓｎ、Ｐｂ及び市販の３種類のガラス（Ａ
種：Ｓｉ−Ｚｎ系 Ｂ種：Ｐｂ系 Ｃ種：Ｚｎ−Ｓｉ
系）を載せ、窒素雰囲気中、表１の温度で加熱し冷却
後、それぞれの付着状態を観察した。その結果を表１に
示す。On the obtained glassy carbon-coated plate, I
n, Ga, Sn, Pb and three types of commercially available glass (A
Species: Si-Zn type B type: Pb type C type: Zn-Si type
System), placed in a nitrogen atmosphere, heated at the temperature shown in Table 1 and cooled, and then the state of adhesion of each was observed. The results are shown in Table 1.
【００１６】一方、上記によって得られたガラス状炭素
被覆板の２枚をガラスセルに入れ、振動器で振幅０．０
５ｍｍ、６０Ｈｚの条件で振動させた際に発生したダス
ト量のうち、直径０．３μｍ以上の粒子についてパーテ
ィクルカウンターでその量を測定した。その結果を表１
に示す。On the other hand, two glassy carbon-coated plates obtained as described above were put into a glass cell and the amplitude was adjusted to 0.0 with a vibrator.
Of the amount of dust generated when vibrating under conditions of 5 mm and 60 Hz, the amount of particles having a diameter of 0.3 μm or more was measured with a particle counter. The results are shown in Table 1.
Shown in.
【００１７】[0017]
【表１】 [Table 1]
【００１８】表１から、ガラス状炭素被覆層の厚みが
０．１μｍ以下であれば溶融金属や溶融ガラスとの付着
がなくなることがわかる。また、ダスト発生の低減効果
は、ガラス状炭素含浸層の深さが２００μｍ以上であれ
ば著しくなることがわかる。From Table 1, it can be seen that when the glassy carbon coating layer has a thickness of 0.1 μm or less, adhesion to molten metal or molten glass is eliminated. Further, it can be seen that the effect of reducing dust generation becomes remarkable when the depth of the glassy carbon impregnated layer is 200 μm or more.
【００１９】[0019]
【発明の効果】本発明によれば、溶融金属や溶融ガラス
との付着がなく、また、ダスト発生の低減効果に著しい
ガラス状炭素被覆物品を量産性よく製造することができ
る。According to the present invention, it is possible to mass-produce a glassy carbon-coated article which does not adhere to molten metal or molten glass and has a remarkable effect of reducing dust generation.
Claims (1)
ラス状炭素被覆層を有し、しかも黒鉛基体表面から２０
０μｍ以上の深さにわたってガラス状炭素が含浸されて
なることを特徴とするガラス状炭素被覆物品。1. A glass-like carbon coating layer having a thickness of 0.1 μm or less is formed on the surface of a graphite substrate, and the surface of the graphite substrate is 20 from the surface of the graphite substrate.
A glassy carbon-coated article, characterized by being impregnated with glassy carbon over a depth of 0 μm or more.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4068988A JP2527666B2 (en) | 1992-02-18 | 1992-02-18 | Glassy carbon coated article |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4068988A JP2527666B2 (en) | 1992-02-18 | 1992-02-18 | Glassy carbon coated article |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0733524A true JPH0733524A (en) | 1995-02-03 |
| JP2527666B2 JP2527666B2 (en) | 1996-08-28 |
Family
ID=13389558
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP4068988A Expired - Lifetime JP2527666B2 (en) | 1992-02-18 | 1992-02-18 | Glassy carbon coated article |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2527666B2 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0803897A2 (en) * | 1996-04-22 | 1997-10-29 | Nisshinbo Industries Inc. | Electrode for plasma etching |
| DE19606093B4 (en) * | 1995-02-22 | 2010-06-02 | DENSO CORPORATION, Kariya-shi | A vehicle communication system that uses staggered communication cycles to reduce interference and methods of performing the communication |
| WO2020116584A1 (en) * | 2018-12-07 | 2020-06-11 | ニプロ株式会社 | Device for processing glass member |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5481317A (en) * | 1977-12-13 | 1979-06-28 | Hitachi Chemical Co Ltd | Production of impermeable graphite material |
| JPH01270577A (en) * | 1988-04-20 | 1989-10-27 | Toshiba Ceramics Co Ltd | Ceramic moldings and production thereof |
| JPH03146411A (en) * | 1989-11-02 | 1991-06-21 | Denki Kagaku Kogyo Kk | Metal melting graphite material |
-
1992
- 1992-02-18 JP JP4068988A patent/JP2527666B2/en not_active Expired - Lifetime
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5481317A (en) * | 1977-12-13 | 1979-06-28 | Hitachi Chemical Co Ltd | Production of impermeable graphite material |
| JPH01270577A (en) * | 1988-04-20 | 1989-10-27 | Toshiba Ceramics Co Ltd | Ceramic moldings and production thereof |
| JPH03146411A (en) * | 1989-11-02 | 1991-06-21 | Denki Kagaku Kogyo Kk | Metal melting graphite material |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19606093B4 (en) * | 1995-02-22 | 2010-06-02 | DENSO CORPORATION, Kariya-shi | A vehicle communication system that uses staggered communication cycles to reduce interference and methods of performing the communication |
| EP0803897A2 (en) * | 1996-04-22 | 1997-10-29 | Nisshinbo Industries Inc. | Electrode for plasma etching |
| EP0803897A3 (en) * | 1996-04-22 | 1998-04-01 | Nisshinbo Industries Inc. | Electrode for plasma etching |
| US5951814A (en) * | 1996-04-22 | 1999-09-14 | Nisshinbo Industries, Inc. | Electrode for plasma etching |
| WO2020116584A1 (en) * | 2018-12-07 | 2020-06-11 | ニプロ株式会社 | Device for processing glass member |
| CN113767074A (en) * | 2018-12-07 | 2021-12-07 | 尼普洛株式会社 | Device for processing glass member |
| CN113767074B (en) * | 2018-12-07 | 2023-11-17 | 尼普洛株式会社 | Device for processing glass member |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2527666B2 (en) | 1996-08-28 |
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