JPS6176663A - Graphite crucible for evaporating aluminum - Google Patents
Graphite crucible for evaporating aluminumInfo
- Publication number
- JPS6176663A JPS6176663A JP19759784A JP19759784A JPS6176663A JP S6176663 A JPS6176663 A JP S6176663A JP 19759784 A JP19759784 A JP 19759784A JP 19759784 A JP19759784 A JP 19759784A JP S6176663 A JPS6176663 A JP S6176663A
- Authority
- JP
- Japan
- Prior art keywords
- graphite
- graphite crucible
- crucible
- aluminum
- alumina
- 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
Classifications
-
- 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
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明はアルミニウム蒸着用黒鉛るつほの改良に関する
。DETAILED DESCRIPTION OF THE INVENTION (Industrial Field of Application) The present invention relates to improvement of graphite melt for aluminum deposition.
（従来技術）
アルミニウムの真空蒸着は約１５００°ｃ、ｉｏ−３〜
１０”−’ ｍｍＨｇの条件下で行なわれるのが一般的
であるが、この場合溶融アルミニウムは他の金属に比べ
て黒鉛るつぼの気孔への浸透性が大で、かつ黒鉛と反応
して炭化アルミニウムを生成し、少ない使用回数でるつ
ぼの破壊を生じることがある。(Prior art) Vacuum deposition of aluminum is approximately 1500°C, io-3 ~
It is generally carried out under conditions of 10"-' mmHg, but in this case, molten aluminum has a greater permeability into the pores of the graphite crucible than other metals, and reacts with graphite to form aluminum carbide. The crucible may be destroyed after a small number of uses.
これを防止し、黒鉛るつぼの使用回数を多くするために
種々な検討が加えられている。例えば黒鉛るつぼに硝酸
アルミニウム、又はアルミニウム・ヒドロキシクロライ
ドの水溶液を含浸し、熱処理することによって気孔にア
ルミナ（Ａ１２０３）Ａ充填被覆し、溶融アルミニウム
の浸透を阻止する方法が取られている。Various studies have been made to prevent this and increase the number of times graphite crucibles are used. For example, a method is used in which a graphite crucible is impregnated with an aqueous solution of aluminum nitrate or aluminum hydroxychloride and heat treated to coat the pores with alumina (A1203) A to prevent penetration of molten aluminum.
しかしこの方法では硝酸アルミニウム又はアルミニウム
・ヒドロキシクロライドよシのＡＪｚＯｓ生成歩留生成
歩留比め、溶融アルミニウムの黒鉛るつぼ内部への浸透
防止効果を得るには３〜６回繰り返し処理する必要があ
るが、必ずしも完全な浸透防止を図ることはできない。However, with this method, compared to the AJzOs production yield of aluminum nitrate or aluminum hydroxychloride, it is necessary to repeat the treatment 3 to 6 times to obtain the effect of preventing molten aluminum from penetrating into the graphite crucible. However, it is not always possible to completely prevent penetration.
一方黒鉛るつぼの表面の気孔を埋めるために黒鉛るつぼ
の表面に熱分解黒鉛の層を形成させる方法がある。しか
し熱分解黒鉛の形成層の厚みは生産コストの面より０．
０１＝０．３ｒＭｎ程度が一般的であり、黒鉛るつぼの
使用当初は溶融アルミニウムの浸透を十分に防止できる
が、使用回数が進むにつれて黒鉛るつぼが酸化等で消耗
し、熱分解黒鉛の形成層が無くなった時点で溶融アルミ
ニウムが黒鉛るつぼの気孔に浸透し、以後の使用回数を
極めて短くする。熱分解黒鉛の層を厚く形成すれば黒鉛
るつぼの使用回数を大きくできるが、生産コストが増大
して現実的ではない。On the other hand, there is a method of forming a layer of pyrolytic graphite on the surface of a graphite crucible in order to fill the pores on the surface of the graphite crucible. However, the thickness of the formation layer of pyrolytic graphite is limited to 0.00 mm due to production cost considerations.
01 = about 0.3rMn, which is sufficient to prevent penetration of molten aluminum when the graphite crucible is first used, but as the graphite crucible is used more times, it becomes worn out due to oxidation, etc., and the formation layer of pyrolytic graphite is formed. When it runs out, molten aluminum penetrates into the pores of the graphite crucible, greatly reducing the number of times it can be used thereafter. If the layer of pyrolytic graphite is formed thickly, the number of times the graphite crucible can be used can be increased, but this increases the production cost and is not practical.
（発明の目的）
本発明は前述の問題を解消し、長寿命のアルミニウム蒸
着用黒鉛るつぼを提供することを目的とする。(Objective of the Invention) An object of the present invention is to solve the above-mentioned problems and provide a long-life graphite crucible for aluminum deposition.
（発明の宿成）
本発明は、黒鉛るつぼの気孔にアルミナ及び炭素を充填
した後、該黒鉛るつぼの表面に熱分解黒鉛の層を形成し
たアルミニウム蒸着用黒鉛るつぼに関する。(Embodiment of the Invention) The present invention relates to a graphite crucible for aluminum deposition, in which a layer of pyrolytic graphite is formed on the surface of the graphite crucible after the pores of the graphite crucible are filled with alumina and carbon.
本発明の黒鉛るつぼの材質は人造黒鉛でカサ比重が１．
７８以上のものが好ましい。カサ比重が小さいと気孔率
が大きく充填するアルミナ及び炭素のＡｔ多く必要とす
るからである。The material of the graphite crucible of the present invention is artificial graphite with a bulk specific gravity of 1.
78 or more is preferred. This is because if the bulk specific gravity is small, the porosity is large and a large amount of alumina and carbon are required to be filled.
アルミナの充填は硝酸アルミニウム、アルミニウム・ヒ
ドロキシクロライド等の熱分解してアルミナを残すアル
ミニウム化合物の溶液を公知の真空加圧含浸法等により
含浸し、Ｍ処理する方法を複数回繰ル返す。炭素の充填
は黒鉛るつぼの表面を緻密にして熱分解黒鉛を付着し易
くするために行なうもので、フラン樹脂、フェノール樹
脂、タールピンチのような炭化残量の多い有機材料を液
状にして公知の真空加圧含浸法等にょシ含浸した後熱処
理して炭化するか、カーボンブラックのような微粉末の
炭素を水又は有機溶剤に分散した分散液を含浸する方法
による。取シ扱い易さの点からフラン樹脂を含浸熱処理
することが好ましい。Filling with alumina is performed by impregnating with a solution of an aluminum compound such as aluminum nitrate or aluminum hydroxychloride that leaves alumina after being thermally decomposed by a known vacuum pressure impregnation method, followed by M treatment, which is repeated several times. Filling with carbon is done to make the surface of the graphite crucible denser and make it easier for pyrolytic graphite to adhere to it.It is done by liquefying organic materials with a large amount of carbonization such as furan resin, phenol resin, and tar pinch. The material may be impregnated using a vacuum pressure impregnation method, followed by heat treatment and carbonized, or may be impregnated with a dispersion of finely powdered carbon, such as carbon black, dispersed in water or an organic solvent. From the viewpoint of ease of handling, it is preferable to impregnate and heat-treat the furan resin.
黒鉛るつぼ表面への熱分解黒鉛の層の形成は。Formation of a layer of pyrolytic graphite on the surface of a graphite crucible.
公知の炭化水素等を熱分解して黒鉛を析出させる手段を
用いればよい。Any known means for thermally decomposing hydrocarbons and precipitating graphite may be used.
（作用）
上記のようＫして得られたアルミニウム蒸着用黒鉛るつ
ぼを使用した場合、当初は熱分解黒鉛の層が溶融アルミ
ニウムの浸透を阻止し、熱分解黒鉛が消耗すれば気孔に
充填されたアルミナが溶融アルミニウムの浸透及び溶融
アルミニウムと黒鉛との反応を防止する。(Function) When using a graphite crucible for aluminum evaporation obtained by K as described above, a layer of pyrolytic graphite initially blocks penetration of molten aluminum, and as the pyrolytic graphite is consumed, it fills the pores. Alumina prevents penetration of molten aluminum and reaction of molten aluminum with graphite.
（実施例） 次に実施例を説明する。(Example) Next, an example will be described.
実施例
内径８０ ｍｍ 、外径１００ｍｍ、高さ９０ｍｍ、カ
サ比重１．７８の人造黒鉛のるつぼを製作しオートクレ
ーブに入れ１００−３ｏ＋Ｈｇまで減圧し、゛この圧力
で３０分間保持後硝酸アルミニウム（Ａｔ （Ｎ０３）
ｓ−９Ｈ２０）の５Ｑｗｔ％の水溶液を注入含浸し、更
に５気圧の圧力下で３０分保持して大気圧に戻した。Example A crucible made of artificial graphite with an inner diameter of 80 mm, an outer diameter of 100 mm, a height of 90 mm, and a bulk specific gravity of 1.78 was prepared, placed in an autoclave, and the pressure reduced to 100-3 o + Hg. After holding at this pressure for 30 minutes, aluminum nitrate (At N03)
A 5Qwt% aqueous solution of s-9H20) was injected and impregnated, and the pressure was further maintained at 5 atm for 30 minutes to return to atmospheric pressure.
次に黒鉛るつぼを取り出し２４時間かけて６００℃まで
徐々に昇温しアルミナを気孔中に充填固定した。以上の
含浸及び熱処理操作を２回縁シ返し行なった後、パラト
ルエンスルホンｅ１ｗｔ％メタノール溶液に１時間浸漬
し、乾燥後パラトルエンスルホン酸エチルエステルｉ、
ｓ ｗｔ ％ 配合１．ｆｃフラン樹脂を硝酸アルミニ
ウム含浸と同一条件で減圧含浸後、 ７ ｋｇ ／ ｃ
ｍ２で３０分加圧し大気圧に戻した。Next, the graphite crucible was taken out and the temperature was gradually raised to 600° C. over 24 hours to fill and fix alumina into the pores. After performing the above impregnation and heat treatment operations twice, it was immersed in a 1 wt% methanol solution of para-toluene sulfone e for 1 hour, and after drying, para-toluene sulfonic acid ethyl ester i,
s wt % formulation 1. After impregnating fc furan resin under reduced pressure under the same conditions as aluminum nitrate impregnation, 7 kg/c
The pressure was increased to m2 for 30 minutes and the pressure was returned to atmospheric pressure.
次に黒鉛るりぼｔ−７２時間かけて９００’Ｃまで徐々
に昇温しフラン樹脂を炭化させた。黒鉛るつぼの表面を
清浄にした後石英製反応管中に置き、高周波誘導加熱に
より９００℃に加熱し＋ Ｎ２ガスをキャリヤーガスと
して濃度１３ ｖｏ／％のトリクロロエタンを２ｇ／ｍ
ｉｎのガス流量で５時間送り込み、約０．１−の熱分解
黒鉛の層を形成させ九アルミニウム蒸着用黒鉛るつぼを
得た。Next, the graphite luribo was gradually heated to 900'C over 72 hours to carbonize the furan resin. After cleaning the surface of the graphite crucible, it was placed in a quartz reaction tube, heated to 900°C by high-frequency induction heating, and 2 g/m of trichloroethane with a concentration of 13 vo/% was added using N2 gas as a carrier gas.
The mixture was fed for 5 hours at a gas flow rate of 1.5 in. to form a layer of pyrolytic graphite of about 0.1 - to obtain a graphite crucible for deposition of aluminum.
実施例においてアルミナ充填までを行なったものを比較
例とし実施例と比較例のアルミニウム蒸着用黒鉛るつぼ
について、フィルム材質ポリエステル樹脂、フィルム巻
取速度２００ｍ／ｍｉｎ、蒸着金属純度９９．９．Ａ％
アルミニウム、蒸着膜厚さ４００λ、蒸着温度は１４５
０℃、真空度２ Ｘ １０−’、ｎＨｇ及び蒸着長さ２
５００ｍ／回の条件で試験を行なった結果、その使用回
数（寿命）は比較例のものが２５回、実施例のものが３
８回であった。The graphite crucibles for aluminum evaporation of the Examples and the Comparative Examples were treated as Comparative Examples in which the Example was filled with alumina, and the film material was polyester resin, the film winding speed was 200 m/min, and the purity of the deposited metal was 99.9. A%
Aluminum, evaporation film thickness 400λ, evaporation temperature 145
0°C, degree of vacuum 2 x 10-', nHg and evaporation length 2
As a result of testing under the condition of 500 m/time, the number of uses (life) was 25 times for the comparative example and 3 times for the example example.
It was 8 times.
（発明の効果）
本発明によれば黒鉛るつぼの気孔にアルミナ及び炭素を
充填した後１表面に熱分解黒鉛の層を形成し念のでアル
ミニウム蒸着用るつぼの寿命が大幅に改善される。(Effects of the Invention) According to the present invention, after filling the pores of a graphite crucible with alumina and carbon, a layer of pyrolytic graphite is formed on one surface, thereby greatly improving the life of the crucible for aluminum deposition.
又とノMatatono
Claims (1)
、該黒鉛るつぼの表面に熱分解黒鉛の層を形成したアル
ミニウム蒸着用黒鉛るつぼ。1. A graphite crucible for aluminum evaporation, in which the pores of the graphite crucible are filled with alumina and carbon, and then a layer of pyrolytic graphite is formed on the surface of the graphite crucible.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19759784A JPS6176663A (en) | 1984-09-20 | 1984-09-20 | Graphite crucible for evaporating aluminum |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19759784A JPS6176663A (en) | 1984-09-20 | 1984-09-20 | Graphite crucible for evaporating aluminum |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS6176663A true JPS6176663A (en) | 1986-04-19 |
Family
ID=16377126
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP19759784A Pending JPS6176663A (en) | 1984-09-20 | 1984-09-20 | Graphite crucible for evaporating aluminum |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6176663A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5277934A (en) * | 1990-06-27 | 1994-01-11 | Advanced Ceramico Corporation | Method for protecting a graphite chuck for a starter filament in the manufacture of polycrystalline silicon |
-
1984
- 1984-09-20 JP JP19759784A patent/JPS6176663A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5277934A (en) * | 1990-06-27 | 1994-01-11 | Advanced Ceramico Corporation | Method for protecting a graphite chuck for a starter filament in the manufacture of polycrystalline silicon |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US3713865A (en) | Composite product and method of making same | |
| RU2084425C1 (en) | Method of manufacturing articles from carbon-silicon carbide composite material and carbon-silicon carbide composite material | |
| US4465777A (en) | Composition and method for forming a protective coating on carbon-carbon substrates | |
| US3492153A (en) | Silicon carbide-aluminum nitride refractory composite | |
| US3628984A (en) | Method for the manufacture of heat-resistant carbonaceous products having low permeability | |
| CN112028612B (en) | Magnesia carbon brick applying reinforcing material | |
| US4536358A (en) | Process for the production of high surface area catalyst supports | |
| US5330838A (en) | Coated carbonaceous articles and method for making same | |
| US5518816A (en) | Composition and method for forming a protective coating on carbon-carbon chemical vapor deposition densified substrates | |
| RU2111287C1 (en) | Method of processing carbon-based integrated element of aluminum producing electrolytic cell, preliminarily sintered anode, and electrolytic cell | |
| JP3128149B2 (en) | Carbon composite material for continuous casting, method for producing the same, and die for continuous casting using the same | |
| JPS6176663A (en) | Graphite crucible for evaporating aluminum | |
| US5521001A (en) | Carbide formed on a carbon substrate | |
| JPS62223063A (en) | Manufacture of graphitic crucible | |
| CN110130100B (en) | Continuous sintering method of boron-containing SiC fibers | |
| US2839426A (en) | Method of coating carbonaceous articles with silicon nitride | |
| US6699589B2 (en) | Carbon reinforcements, in particular for use in carbon-fiber reinforced materials, and a method of generating internal protection against oxidation in carbon reinforcements | |
| RU2494998C2 (en) | Method of making articles from carbon-silicon carbide material | |
| JP2519071B2 (en) | Method for producing carbon material with low outgas | |
| JPS61101409A (en) | Manufacture of silicon carbide | |
| RU2101266C1 (en) | Method of production of glass-silicide coatings | |
| JPH0617236A (en) | Vessel for molten metal | |
| JPH01167290A (en) | Method for carrying out oxidation resistance traeatment of carbon material | |
| JPH0725612B2 (en) | Carbon fiber reinforced carbon composite material having oxidation resistance and method for producing the same | |
| JPS62211367A (en) | Production of graphite crucible for vapor deposition of aluminum |