JPH05331643A - Coating method for aluminum by chemical vapor deposition - Google Patents

Coating method for aluminum by chemical vapor deposition

Info

Publication number
JPH05331643A
JPH05331643A JP4138728A JP13872892A JPH05331643A JP H05331643 A JPH05331643 A JP H05331643A JP 4138728 A JP4138728 A JP 4138728A JP 13872892 A JP13872892 A JP 13872892A JP H05331643 A JPH05331643 A JP H05331643A
Authority
JP
Japan
Prior art keywords
reaction vessel
alcl
reaction
hcl
cvd
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
Application number
JP4138728A
Other languages
Japanese (ja)
Other versions
JP3165506B2 (en
Inventor
Masaharu Nakamori
正治 中森
Ichiro Tsuji
一郎 辻
Koji Takahashi
孝二 高橋
Taketoshi Tanimura
武俊 谷村
Satoshi Tsuru
聡 鶴
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.)
KORYO ENG KK
Mitsubishi Heavy Industries Ltd
Original Assignee
KORYO ENG KK
Mitsubishi Heavy Industries 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 KORYO ENG KK, Mitsubishi Heavy Industries Ltd filed Critical KORYO ENG KK
Priority to JP13872892A priority Critical patent/JP3165506B2/en
Publication of JPH05331643A publication Critical patent/JPH05331643A/en
Application granted granted Critical
Publication of JP3165506B2 publication Critical patent/JP3165506B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Landscapes

  • Turbine Rotor Nozzle Sealing (AREA)
  • Chemical Vapour Deposition (AREA)

Abstract

PURPOSE:To provide the coating method which can well coat the inside of the cooling holes of the moving and static vanes of a gas turbine and does not entail a danger on a human body. CONSTITUTION:HCl is supplied into an Al reaction vessel 8 where a metal A 17 is installed to form AlCl3. This AlCl3 is introduced into a CVD reaction vessel 1 where the metal A 17 and work 2 are installed to effect a CVD reaction and to form an Al coating layer on the surface of the work 2, by which the need for direct handling of the AlCl3 by manual labor is eliminated. Since the installation of the metal A 17 in the reaction vessels 8, 1 is merely necessitated, the safety of the operation is greatly improved. In addition, the cost of the operation is drastically reduced. The HCL remaining in the CVD reaction vessel 1 is removed by the metal A 17 and, therefore, the damage to the work 2 and the reaction vessel 1 is prevented.

Description

【発明の詳細な説明】Detailed Description of the Invention

【0001】[0001]

【産業上の利用分野】本発明は、ガスタービン動・静翼
等に適用されるアルミニウム化学蒸着(以下CVDとい
う;Chemical Vapor Deposition)コーティング方法に関
する。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an aluminum chemical vapor deposition (Chemical Vapor Deposition) coating method applied to gas turbine moving and stationary blades.

【0002】[0002]

【従来の技術】コンバインドサイクルプラントに代表さ
れる高効率化された最近の産業用ガスタービンは、ター
ビン入口温度の上昇が著しく1300℃以上となってい
る。この高温ガスに暴露される動・静翼に使用される耐
熱合金は精力的な研究開発が行なわれ、その許容使用温
度も年々上昇しているが、実用合金では850〜900
℃にとどまっている。
2. Description of the Related Art In a recent highly efficient industrial gas turbine represented by a combined cycle plant, the turbine inlet temperature rises significantly at 1300 ° C. or more. The heat-resistant alloys used in moving and stationary blades exposed to this high-temperature gas have undergone vigorous research and development, and their allowable operating temperatures are increasing year by year.
It stays at ℃.

【0003】このため、実機ガスタービンでは、翼内面
に冷却孔を設けて空気を流通させ翼全体の温度を許容温
度以下に保つために、図2に示すようないわゆる空気冷
却翼が使用されている。
For this reason, in an actual gas turbine, a so-called air cooling blade as shown in FIG. 2 is used in order to provide cooling holes on the inner surface of the blade to allow air to flow therethrough and keep the temperature of the entire blade at an allowable temperature or lower. There is.

【0004】しかし、近年のガスタービン入口温度の上
昇は、この空気冷却孔の内面の温度をも上昇させ、なん
らかの高温酸化防止対策を施す必要が生じ、ガスタービ
ン動・静翼に高温耐食・耐酸化性を付与することが行な
われるようになってきている。
However, the recent rise in the temperature of the gas turbine inlet also raises the temperature of the inner surface of the air cooling hole, and it becomes necessary to take some measure against high temperature oxidation, which results in high temperature corrosion resistance and acid resistance of the gas turbine dynamic and stationary blades. It is becoming more common to impart chemical properties.

【0005】上記高温耐食・耐酸化性をガスタービン動
・静翼等に付与する従来の高温酸化・高温腐食防止対策
としては、金属表面技術便覧(金属表面技術協会編、2
50〜255ページ)に記載されているように、アルミ
ナ(Al2 3 )、アルミニウム(Al)、塩化アンモ
ニア(NH4 Cl)の粉末中に被処理材を埋め込み、8
00〜1100℃で還元性ガス(H2 )を通すことによ
り、被処理材の表面にAlを析出させるパックセメンテ
ーションによるAl拡散浸透処理(カロライジング法)
があった。
As a conventional high-temperature oxidation / high-temperature corrosion prevention measure for imparting the above-mentioned high-temperature corrosion resistance / oxidation resistance to a gas turbine dynamic / static blade, etc., there is a Metal Surface Technology Handbook (edited by Metal Surface Technology Association, 2).
As described on pages 50 to 255), the material to be treated is embedded in a powder of alumina (Al 2 O 3 ), aluminum (Al), and ammonium chloride (NH 4 Cl).
Al diffusion and permeation treatment by pack cementation in which Al is deposited on the surface of the material to be treated by passing a reducing gas (H 2 ) at 00 to 1100 ° C. (calorizing method)
was there.

【0006】また、最近では、被処理材の狭隘部にもコ
ーティング層を形成させるものとして、昇華させたAl
Cl3 を減圧した反応炉内にキャリアガスのH2 ガスに
より送り込み、被処理材の表面にコーティング層を形成
させる減圧CVD法が検討されている(第77回講演大
会要旨集に掲載された「減圧CVD法によるNi管内孔
面へのAlコーティングの検討」、金属表面技術協会
編)。
Recently, sublimated Al has been used as a material for forming a coating layer on a narrow portion of a material to be treated.
A low pressure CVD method for forming a coating layer on the surface of a material to be treated by feeding Cl 3 into a reactor in which H 2 gas has been decompressed has been studied (published in the 77th Annual Conference). Examination of Al Coating on Ni Tube Inner Hole Surface by Low Pressure CVD Method ", Metal Surface Technology Association).

【0007】[0007]

【発明が解決しようとする課題】従来の方法において、
パックセメンテーションによるAl拡散浸透処理方法の
場合は、ガスタービン動・静翼はAl等の粉末中へ埋込
まれるが、狭隘な冷却孔内面にコーティング層を形成し
ようとしても粉末が冷却孔内に十分挿入できず、コーテ
ィングが不十分となることがあった。また、コーティン
グ後のこの粉末の除去が不十分な場合には、冷却孔を閉
塞させ重大な事故を招くという欠点があった。
DISCLOSURE OF THE INVENTION In the conventional method,
In the case of the Al diffusion infiltration treatment method by pack cementation, the gas turbine moving and stationary blades are embedded in powder of Al or the like, but even if an attempt is made to form a coating layer on the inner surface of the narrow cooling hole, the powder remains inside the cooling hole. There was a case where it could not be inserted sufficiently and coating was insufficient. Further, if the removal of the powder after coating is insufficient, there is a drawback that the cooling hole is closed and a serious accident occurs.

【0008】前記減圧CVD法は、前記Al拡散浸透処
理方法の欠点を解消するために検討されているものであ
り、Alをガス状の化合物として供給し、冷却孔表面で
Alを析出させようとするものである。Al−CVD反
応としては、前記のようにAlCl3 の利用が知られて
いるが、AlCl3 は空気中の水分を吸って加水分解し
盛んに塩化水素を発生するなど極めて不安定で有害な物
質であり、工業的な取扱いが難しいという課題がある。
The low-pressure CVD method has been studied in order to solve the drawbacks of the Al diffusion and infiltration treatment method, and Al is supplied as a gaseous compound to precipitate Al on the surface of the cooling hole. To do. As mentioned above, the use of AlCl 3 is known as the Al-CVD reaction, but AlCl 3 absorbs moisture in the air and hydrolyzes to actively generate hydrogen chloride, which is an extremely unstable and harmful substance. Therefore, there is a problem that industrial handling is difficult.

【0009】本発明は上記の課題を解決しようとするも
のである。
The present invention is intended to solve the above problems.

【0010】[0010]

【課題を解決するための手段】本発明のAl−CVDコ
ーティング方法は、金属Alが設置されたAl反応容器
内にHClを供給し金属AlへHClを反応させてAl
Cl3 を生成させた後、このAlCl3 と未反応のHC
lを金属Alが設置され被処理材が配設されたCVD反
応容器内へ導入し、CVD反応を生じさせて被処理材の
面にAlコーティング層を形成させることを特徴として
いる。
According to the Al-CVD coating method of the present invention, HCl is supplied into an Al reaction vessel in which metallic Al is installed, and HCl is reacted with metallic Al to form Al.
After generating Cl 3 , the unreacted HC with this AlCl 3
It is characterized in that 1 is introduced into a CVD reaction container in which metallic Al is placed and a material to be treated is arranged to cause a CVD reaction to form an Al coating layer on the surface of the material to be treated.

【0011】[0011]

【作用】上記において、金属Alが設置されたAl反応
容器内にHClが供給されると、次式によりガス状のA
lCl3 が生成される。
In the above, when HCl is supplied into the Al reaction vessel in which the metallic Al is installed, the gaseous A
lCl 3 is produced.

【0012】2Al+6HCl→2AlCl3 +3H2 上記Al反応容器内で生成されたAlCl3 は未反応の
HClとともにCVD反応容器内に導入され、CVD反
応容器内に設置された金属AlをHClに反応させると
ともにAlCl3 に反応させ、AlCl3 は次式に示す
分解反応を行い、3AlCl3 が生成される。
2Al + 6HCl → 2AlCl 3 + 3H 2 AlCl 3 produced in the above Al reaction vessel is introduced into the CVD reaction vessel together with unreacted HCl, and metallic Al placed in the CVD reaction vessel is reacted with HCl. reacted AlCl 3, AlCl 3 performs a decomposition reaction shown in the following equation, 3AlCl 3 is generated.

【0013】2AlCl3 +Al→3AlCl2 上記AlCl2 は、被処理材上で次式の反応を行い、A
lを析出し、 3AlCl2 →2AlCl3 被処理材の面にAlコーティング層を形成する。
2AlCl 3 + Al → 3AlCl 2 The above AlCl 2 undergoes the reaction of the following formula on the material to be treated, and A
l is deposited and an Al coating layer is formed on the surface of the 3AlCl 2 → 2AlCl 3 treated material.

【0014】上記により、AlCl3 の人手による直接
の取扱いを不要とし、反応容器中に金属Alを設置すれ
ばよいものとしたため、作業の安全性の大幅向上を可能
とするとともに、作業コストの大幅低減を可能とする。
また、CVD反応容器中におけるHClの残留を金属A
lにより除去するため、被処理材や反応容器の損傷の防
止が可能となる。
As described above, since it is not necessary to directly handle AlCl 3 by hand and it is only necessary to install metallic Al in the reaction vessel, it is possible to greatly improve the safety of work and greatly reduce the work cost. Enables reduction.
Further, the residue of HCl in the CVD reaction vessel is removed by the metal A.
Since it is removed by l, it is possible to prevent the material to be treated and the reaction container from being damaged.

【0015】[0015]

【実施例】本発明の一実施例の方法に用いる装置を図1
に示す。図1に示す本実施例の方法に用いる装置は、電
気炉4内に設けられたCVD容器1、同CVD容器1内
に設けられその内部に上下に1段動翼である被処理材2
とAl7の入ったAl容器3が配設された反応塔13、
同反応塔13の底部に一端が接続され他端にAr供給ラ
インとH2 供給ラインがそれぞれ流量計10とバルブ9
を介して接続され圧力計6が設けられたガス導入ライン
5、同ガス導入ライン5に接続されAr供給ラインとH
Cl供給ラインがそれぞれ流量計10とバルブ9を介し
て接続され内部にAl7が充填されたAl反応容器8、
上記CVD容器1の底部に接続されたコールドトラップ
11、および同コールドトラップ11に接続されたロー
タリポンプ12を備えている。
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS FIG. 1 shows an apparatus used in the method of one embodiment of the present invention.
Shown in. The apparatus used in the method of the present embodiment shown in FIG. 1 is a CVD container 1 provided in an electric furnace 4, and a material to be treated 2 that is a 1-stage moving blade vertically provided inside the CVD container 1.
And a reaction tower 13 provided with an Al container 3 containing Al7,
One end is connected to the bottom of the reaction tower 13, and the Ar supply line and the H 2 supply line are connected to the other end at the flow meter 10 and the valve 9, respectively.
Gas introduction line 5 connected via a pressure gauge 6 and an Ar supply line and H connected to the gas introduction line 5
An Al reaction vessel 8 in which Cl supply lines are respectively connected to the flowmeter 10 via a valve 9 and Al7 is filled therein,
A cold trap 11 connected to the bottom of the CVD container 1 and a rotary pump 12 connected to the cold trap 11 are provided.

【0016】上記において、Al7が充填されたAl反
応容器8内にはHCl供給ラインよりHClを供給し、
Al7とHClを反応させて次式によりAlCl3 を生
成する。
In the above, HCl is supplied from the HCl supply line into the Al reaction vessel 8 filled with Al7,
Al 7 is reacted with HCl to produce AlCl 3 according to the following formula.

【0017】2Al+6HCl→2AlCl3 +3H2 上記Al反応容器8で生成されたガス状のAlCl
3 は、H2 供給ラインより供給されるキャリアガスのH
2 ガスにより、ガス導入ライン5を介してその必要量が
反応塔13内に導入される。
2Al + 6HCl → 2AlCl 3 + 3H 2 Gaseous AlCl produced in the Al reactor 8
3 is H of carrier gas supplied from the H 2 supply line
The required amount of the two gases is introduced into the reaction tower 13 through the gas introduction line 5.

【0018】上記AlCl3 が導入された反応塔13内
には、Al7がAl容器3内に配置されており、Al反
応容器8内で未反応であったHClをAl7と反応させ
るとともに、次式に示すAlCl3 の分解反応によって
AlCl2 を生成し、HClの生成を防止する。
Al 7 is placed in the Al container 3 in the reaction tower 13 into which AlCl 3 has been introduced. The unreacted HCl in the Al reaction container 8 is reacted with Al 7 and the following formula AlCl 2 is produced by the decomposition reaction of AlCl 3 shown in ( 3 ) and HCl is prevented from being produced.

【0019】2AlCl3 +Al→3AlCl2 上記により生成されたAlCl2 は次式に示す析出反応
を行い、被処理材2の表面にAlのコーティング層を生
成する。
2AlCl 3 + Al → 3AlCl 2 The AlCl 2 produced as described above undergoes a precipitation reaction represented by the following equation to produce an Al coating layer on the surface of the material 2 to be treated.

【0020】3AlCl2 →2AlCl3 +Al 本実施例においては、コーティング材であるAl7を反
応塔13内及びAl反応容器8内に設置すればよいた
め、取扱いが極めて容易であり、人体に対しても無害で
ある。
3AlCl 2 → 2AlCl 3 + Al In the present embodiment, since the coating material Al7 may be installed in the reaction tower 13 and the Al reaction vessel 8, it is extremely easy to handle and is suitable for the human body. It is harmless.

【0021】CVD反応に必要なAlCl3 は、必要に
応じてHClとAl7を反応させることにより必要量生
成するため、容易に分解して水分と激しく反応するAl
Cl 3 を取扱う危険性と手間とが大幅に低減できる。
AlCl required for CVD reaction3In need
Depending on the reaction, HCl and Al7 can be used to generate the required amount.
Al, which decomposes easily and reacts violently with water
Cl 3The risk of handling and labor can be reduced significantly.

【0022】また、AlCl3 はAl反応容器8内で生
成されるものであり、被処理材2のCVD処理後、A
r、H2 又はA2 とH2 によりラインをパージすること
により、Al反応容器8からコールドトラップ11まで
のライン内に残留するAlCl 3 は完全に除去すること
ができる。
In addition, AlCl3Raw in the Al reaction vessel 8
After the CVD processing of the material 2 to be processed,
r, H2Or A2And H2To purge the line by
From Al reaction vessel 8 to cold trap 11
AlCl remaining in the line 3Be completely removed
You can

【0023】更に、反応塔13内にAl7を設置し、反
応ガス中の残留HClをなくし、AlCl3 をAlCl
2 としているため、Al7の析出を容易にするとともに
被処理材2や反応塔13の損傷(塩化腐食)を防止する
ことができる。
Further, Al7 is installed in the reaction tower 13 to eliminate residual HCl in the reaction gas, and AlCl 3 is replaced with AlCl 3 .
Since it is set to 2 , it is possible to facilitate the precipitation of Al 7 and prevent damage to the material to be treated 2 and the reaction tower 13 (chlorination corrosion).

【0024】本実施例の方法においては、コーティング
処理の性能確認のため、上記装置を用いて試験処理1,
2,3を行っており、以下にその内容と結果について説
明する。
In the method of this embodiment, in order to confirm the performance of the coating treatment, the test treatment 1,
A few things have been done, and the contents and results will be explained below.

【0025】上記試験処理1,2は、コーティング基材
として代表的な動翼材IN738LC(Ni−8.3C
o−16Cr−2.5W−3.4Al−3.4Ti−
1.7Ta−1.7Mo−0.1C;各元素に付記した
数字はwt%を示す)、及び静翼材ECY768(Co
−24Cr−10Ni−7W−4Ta−0.5C)を用
い、表1に示す条件でガスタービン翼材へのコーティン
グ処理を行ったものである。
In the test treatments 1 and 2, the typical blade material IN738LC (Ni-8.3C) as a coating substrate is used.
o-16Cr-2.5W-3.4Al-3.4Ti-
1.7Ta-1.7Mo-0.1C; the number added to each element indicates wt%), and the stationary blade material ECY768 (Co
-24Cr-10Ni-7W-4Ta-0.5C) was used to coat the gas turbine blade material under the conditions shown in Table 1.

【0026】また、試験処理3は小型高温ガスタービン
の1段動翼の空気冷却孔内面へ表1に示す条件でコーテ
ィング処理を行ったものである。
Further, in the test treatment 3, the inner surface of the air cooling hole of the first-stage moving blade of the small-sized high-temperature gas turbine was coated under the conditions shown in Table 1.

【0027】[0027]

【表1】 [Table 1]

【0028】上記試験処理により被処理材の表面に形成
されたAlコーティング層の膜厚については、試験片の
断面ミクロ組織検査及び電子プロープX線マイクロアナ
ライザ(EPMA)分析の結果、試験処理1のIN73
8LCでは70〜80μm、ECY768では50〜6
0μm、また、試験処理2のIN738LCで70〜1
00μm、ECY768で60〜80μmのAlコーテ
ィング層(Al拡散浸透層)が形成されていることが確
認された。
Regarding the film thickness of the Al coating layer formed on the surface of the material to be treated by the above-mentioned test treatment, as a result of the cross-sectional microstructure inspection of the test piece and the electronic probe X-ray microanalyzer (EPMA) analysis, IN73
8 to 70 μm for LC, 50 to 6 for ECY768
0 μm, 70 to 1 by IN738LC of test treatment 2
It was confirmed that an Al coating layer (Al diffusion / permeation layer) having a thickness of 00 μm and ECY768 of 60 to 80 μm was formed.

【0029】また、試験処理3では、空気冷却孔内面各
部についてAlコーティング形成量を同様に調査した結
果、60〜80μmの範囲で全域にコーティングされて
いた。
Further, in the test treatment 3, as a result of similarly examining the amount of Al coating formed on each inner surface of the air cooling hole, it was found that the entire area was coated in the range of 60 to 80 μm.

【0030】上記試験処理を行った試験片については、
Alコーティングにより耐酸化性の向上の評価試験を行
った。なお、試験処理1,2,3によるそれぞれの試験
片のAlコーティング厚さ(Al拡散浸透深さ)はほぼ
同等であったため、試験処理1によりコーティング処理
した試験片のみを用いた。
Regarding the test piece which has been subjected to the above test treatment,
An evaluation test for improving the oxidation resistance was performed by the Al coating. Since the Al coating thickness (Al diffusion penetration depth) of each test piece by the test treatments 1, 2, and 3 was almost the same, only the test piece coated by the test treatment 1 was used.

【0031】この試験片と無処理の試験片について、9
00℃空気中で1000Hrの高温酸化試験を行った結
果、その酸化量はIN738LC、ECY768とも
に、無処理材の1/10〜1/5程度であり、すぐれた
耐酸化性を有することが確認された。
Regarding this test piece and the untreated test piece, 9
As a result of a high temperature oxidation test of 1000 hr in air at 00 ° C., the oxidation amounts of both IN738LC and ECY768 were about 1/10 to 1/5 of those of the untreated material, and it was confirmed that they have excellent oxidation resistance. It was

【0032】なお、本実施例の方法においては、被処理
材と接触する反応ガスの流速は、被処理材の大きさ(コ
ーティング範囲)により異なるが、およそ0.1〜1.
0m/sの範囲が適切である。
In the method of this embodiment, the flow rate of the reaction gas contacting the material to be treated varies depending on the size (coating range) of the material to be treated, but is about 0.1 to 1.
A range of 0 m / s is suitable.

【0033】また、Al反応容器の温度は、AlとHC
lとの反応速度、AlCl3 の蒸気圧、ガス導入管の保
温性を考慮すると、250〜450℃が好ましい。CV
D反応における温度は、被処理物の材質により異なる
が、Ni及びCo基合金のガスタービン材料ではNi−
Al、Co−Al化合物の形体とAlの拡散速度より8
00〜1100℃となる。また、圧力及び反応時間はコ
ーティング層の均一性と要求膜厚より決定する(圧力は
常圧又は減圧とも可能)。
The temperature of the Al reaction container is
Considering the reaction rate with 1, the vapor pressure of AlCl 3 , and the heat retaining property of the gas introduction pipe, 250 to 450 ° C. is preferable. CV
The temperature in the D reaction varies depending on the material of the object to be treated, but Ni- and Co-based alloy gas turbine materials are Ni
8 from the form of Al and Co-Al compounds and the diffusion rate of Al
It becomes 00-1100 degreeC. The pressure and reaction time are determined by the uniformity of the coating layer and the required film thickness (pressure can be atmospheric pressure or reduced pressure).

【0034】[0034]

【発明の効果】本発明のガスタービン動・静翼用Al−
CVDコーティング方法は、金属Alが設置されたAl
反応容器内にHClを供給してAlCl3 を生成し、こ
のAlCl3 を金属Alと被処理材が設置されたCVD
反応容器内に導入し、CVD反応を生じさせて被処理材
の面にAlコーティング層を形成させることによって、
AlCl3 の人手による直接の取扱いを不要とし、反応
容器中に金属Alを設置すればよいものとしたため、作
業の安全性の大幅向上を可能とするとともに、作業コス
トの大幅低減を可能とする。また、CVD反応容器中に
おけるHClの残留を金属Alにより除去するため、被
処理材や反応容器の損傷の防止が可能となる。
EFFECT OF THE INVENTION Al-for gas turbine moving / stator blades of the present invention
The CVD coating method uses Al with metallic Al installed.
HCl is supplied into the reaction vessel to generate AlCl 3 , and this AlCl 3 is deposited on the metal Al and the material to be processed by CVD.
By introducing into the reaction vessel and causing a CVD reaction to form an Al coating layer on the surface of the material to be treated,
Since it is not necessary to directly handle AlCl 3 by hand and metal Al may be installed in the reaction vessel, it is possible to greatly improve the safety of the work and significantly reduce the work cost. Further, since the HCl residue in the CVD reaction container is removed by the metal Al, it is possible to prevent the material to be processed and the reaction container from being damaged.

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

【図1】本発明の一実施例の方法に係る装置の説明図で
ある。
FIG. 1 is an explanatory diagram of an apparatus according to a method of an embodiment of the present invention.

【図2】ガスタービン空気冷却翼(第一段動翼)の構造
図である。
FIG. 2 is a structural diagram of a gas turbine air cooling blade (first stage moving blade).

【符号の説明】[Explanation of symbols]

1 CVD容器 2 被処理材 3 Al容器 4 電気炉 5 ガス導入ライン 6 圧力計 7 Al 8 Al反応容器 9 バルブ 10 流量計 11 コールドトラップ 12 ロータリポンプ 13 反応塔 DESCRIPTION OF SYMBOLS 1 CVD container 2 Processed material 3 Al container 4 Electric furnace 5 Gas introduction line 6 Pressure gauge 7 Al 8 Al reaction vessel 9 Valve 10 Flowmeter 11 Cold trap 12 Rotary pump 13 Reaction tower

─────────────────────────────────────────────────────
─────────────────────────────────────────────────── ───

【手続補正書】[Procedure amendment]

【提出日】平成4年7月29日[Submission date] July 29, 1992

【手続補正1】[Procedure Amendment 1]

【補正対象書類名】明細書[Document name to be amended] Statement

【補正対象項目名】0012[Correction target item name] 0012

【補正方法】変更[Correction method] Change

【補正内容】[Correction content]

【0012】2Al+6HCl→2AlCl3 +3H2 上記Al反応容器内で生成されたAlCl3 は未反応の
HClとともにCVD反応容器内に導入され、CVD反
応容器内に設置された金属AlをHClに反応させると
ともにAlCl3 に反応させ、AlCl3 は次式に示す
分解反応を行い、3AlCl 2 が生成される。
2Al + 6HCl → 2AlCl 3 + 3H 2 AlCl 3 produced in the above Al reaction vessel is introduced into the CVD reaction vessel together with unreacted HCl, and metallic Al placed in the CVD reaction vessel is reacted with HCl. reacted AlCl 3, AlCl 3 performs a decomposition reaction shown in the following equation, 3AlCl 2 is generated.

【手続補正2】[Procedure Amendment 2]

【補正対象書類名】明細書[Document name to be amended] Statement

【補正対象項目名】0013[Correction target item name] 0013

【補正方法】変更[Correction method] Change

【補正内容】[Correction content]

【0013】2AlCl3 +Al→3AlCl2 上記AlCl2 は、被処理材上で次式の反応を行い、A
lを析出し、 3AlCl2 →2AlCl 3 +Al 被処理材の面にAlコーティング層を形成する。
2AlCl 3 + Al → 3AlCl 2 The above AlCl 2 undergoes the reaction of the following formula on the material to be treated, and A
l is deposited and an Al coating layer is formed on the surface of the 3AlCl 2 → 2AlCl 3 + Al treated material.

【手続補正3】[Procedure 3]

【補正対象書類名】明細書[Document name to be amended] Statement

【補正対象項目名】0017[Correction target item name] 0017

【補正方法】変更[Correction method] Change

【補正内容】[Correction content]

【0017】2Al+6HCl→2AlCl3 +3H2 上記Al反応容器8で生成されたガス状のAlCl
3 は、Ar供給ラインより供給されるキャリアガスの
ガスにより、ガス導入ライン5を介してその必要量が
反応塔13内に導入される。
2Al + 6HCl → 2AlCl 3 + 3H 2 Gaseous AlCl produced in the Al reactor 8
3 is A of carrier gas supplied from the Ar supply line
The required amount of r gas is introduced into the reaction column 13 via the gas introduction line 5.

【手続補正4】[Procedure amendment 4]

【補正対象書類名】明細書[Document name to be amended] Statement

【補正対象項目名】0022[Name of item to be corrected] 0022

【補正方法】変更[Correction method] Change

【補正内容】[Correction content]

【0022】また、AlCl3 はAl反応容器8内で生
成されるものであり、被処理材2のCVD処理後、A
r、H2 又はAとH2 によりラインをパージすること
により、Al反応容器8からコールドトラップ11まで
のライン内に残留するAlCl 3 は完全に除去すること
ができる。
In addition, AlCl3Raw in the Al reaction vessel 8
After the CVD processing of the material 2 to be processed,
r, H2Or ArAnd H2To purge the line by
From Al reaction vessel 8 to cold trap 11
AlCl remaining in the line 3Be completely removed
You can

───────────────────────────────────────────────────── フロントページの続き (72)発明者 高橋 孝二 兵庫県高砂市荒井町新浜二丁目1番1号 三菱重工業株式会社高砂製作所内 (72)発明者 谷村 武俊 兵庫県高砂市荒井町新浜二丁目8番25号 高菱エンジニアリング株式会社内 (72)発明者 鶴 聡 兵庫県高砂市荒井町新浜二丁目1番1号 中外テクノス株式会社内 ─────────────────────────────────────────────────── ─── Continuation of front page (72) Inventor Koji Takahashi 2-1-1, Niihama, Arai-cho, Takasago, Hyogo Prefecture Mitsubishi Heavy Industries, Ltd. Takasago Works (72) Inventor Taketoshi Tanimura 2--8, Niihama, Arai-cho, Takasago, Hyogo Prefecture No. 25 Takahishi Engineering Co., Ltd. (72) Inventor Satoshi Tsuru 2-1-1, Niihama, Arai Town, Takasago City, Hyogo Prefecture Chugai Technos Co., Ltd.

Claims (1)

【特許請求の範囲】[Claims] 【請求項1】 金属Alが設置されたAl反応容器内に
HClを供給し金属AlへHClを反応させてAlCl
3 を生成させた後、このAlCl3 と未反応のHClを
金属Alが設置され被処理材が配設された化学蒸着反応
容器内へ導入し、化学蒸着反応を生じさせて被処理材の
面にAlコーティング層を形成させることを特徴とする
アルミニウム化学蒸着コーティング方法。
1. HCl is supplied into an Al reaction vessel in which metallic Al is installed, and HCl is reacted with metallic Al to produce AlCl.
After generating 3 , the AlCl 3 and unreacted HCl are introduced into the chemical vapor deposition reaction vessel in which the metal Al is installed and the material to be treated is placed, and a chemical vapor deposition reaction is caused to generate a surface of the material to be treated. An aluminum chemical vapor deposition coating method comprising: forming an Al coating layer on the aluminum.
JP13872892A 1992-05-29 1992-05-29 Aluminum chemical vapor deposition coating method Expired - Lifetime JP3165506B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP13872892A JP3165506B2 (en) 1992-05-29 1992-05-29 Aluminum chemical vapor deposition coating method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP13872892A JP3165506B2 (en) 1992-05-29 1992-05-29 Aluminum chemical vapor deposition coating method

Publications (2)

Publication Number Publication Date
JPH05331643A true JPH05331643A (en) 1993-12-14
JP3165506B2 JP3165506B2 (en) 2001-05-14

Family

ID=15228774

Family Applications (1)

Application Number Title Priority Date Filing Date
JP13872892A Expired - Lifetime JP3165506B2 (en) 1992-05-29 1992-05-29 Aluminum chemical vapor deposition coating method

Country Status (1)

Country Link
JP (1) JP3165506B2 (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115786759A (en) * 2022-11-11 2023-03-14 广州众山精密科技有限公司 Equipment and method for preparing near-net-shape aluminum-based silicon carbide foil by gas-phase aluminizing

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101951383B1 (en) * 2016-12-07 2019-02-22 박은도 Stage equipment having a support body which can transform the shape and control the length

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115786759A (en) * 2022-11-11 2023-03-14 广州众山精密科技有限公司 Equipment and method for preparing near-net-shape aluminum-based silicon carbide foil by gas-phase aluminizing
CN115786759B (en) * 2022-11-11 2024-06-04 广州众山精密科技有限公司 Equipment and method for preparing near-net-shaped aluminum-based silicon carbide foil by gas phase aluminizing

Also Published As

Publication number Publication date
JP3165506B2 (en) 2001-05-14

Similar Documents

Publication Publication Date Title
Rosado et al. Protective behaviour of newly developed coatings against metal dusting
Konys et al. Corrosion of high-temperature alloys in chloride-containing supercritical water oxidation systems
US6725911B2 (en) Corrosion resistance treatment of condensing heat exchanger steel structures exposed to a combustion environment
WO2018169827A1 (en) Boronizing powder compositions for improved boride layer quality in oil country tubular goods and other metal articles
Subramanian et al. Corrosion behaviour of alumina-forming heat resistant alloy with Ti in high temperature steam
Tsipas et al. Boroaluminide coatings on ferritic–martensitic steel deposited by low-temperature pack cementation
Voisey et al. Inhibition of metal dusting using thermal spray coatings and laser treatment
JPH05331643A (en) Coating method for aluminum by chemical vapor deposition
US10870912B2 (en) Method for using boronizing reaction gases as a protective atmosphere during boronizing, and reaction gas neutralizing treatment
JP4598499B2 (en) Manufacturing method of composite layer covering member
US20180057924A1 (en) Coating compositions, methods and articles produced thereby
Leelachao et al. Phase evolution of surface-modified Incoloy 825 superalloy using pack aluminization
Pérez et al. Adhesion properties of aluminide coatings deposited via CVD in fluidised bed reactors (CVD-FBR) on AISI 304 stainless steel
Pan et al. Preparation of a thick NiAl/Al2O3 coating by embedding method and its corrosion resistance under supercritical water environment
Wu et al. Corrosion of Cr23C6 coated Q235 steel in wet atmospheres containing Na2SO4 at 750 C
Agüero Progress in the development of coatings for protection of new generation steam plant components
Marulanda-Arévalo et al. Behavior of aluminum coating by CVD-FBR in steam oxidation at 700 C
US5015535A (en) Article formed from a low carbon iron alloy having a corrosion resistant diffusion coating thereon
Tsipas et al. Thermochemical treatments for protection of steels in chemically aggressive atmospheres at high temperatures
Jang et al. Study on corrosion resistance of gas cylinder materials in HF, HCl and HBr environments
WO2021100415A1 (en) Polycrystalline silicon production device and polycrystalline silicon production method
JP7370263B2 (en) Metal products and their manufacturing methods
EP3684961B1 (en) Improved pre-treatment process of a surface of a metallic substrate
Li et al. Noticeable localized corrosion of solid boric acid on 304 stainless steel
Bogdanov et al. Diffusional chrome plating of steel by iodide transport

Legal Events

Date Code Title Description
A01 Written decision to grant a patent or to grant a registration (utility model)

Free format text: JAPANESE INTERMEDIATE CODE: A01

Effective date: 20010130

FPAY Renewal fee payment (event date is renewal date of database)

Free format text: PAYMENT UNTIL: 20080302

Year of fee payment: 7

FPAY Renewal fee payment (event date is renewal date of database)

Free format text: PAYMENT UNTIL: 20090302

Year of fee payment: 8

FPAY Renewal fee payment (event date is renewal date of database)

Free format text: PAYMENT UNTIL: 20100302

Year of fee payment: 9

FPAY Renewal fee payment (event date is renewal date of database)

Free format text: PAYMENT UNTIL: 20110302

Year of fee payment: 10

FPAY Renewal fee payment (event date is renewal date of database)

Free format text: PAYMENT UNTIL: 20110302

Year of fee payment: 10

FPAY Renewal fee payment (event date is renewal date of database)

Free format text: PAYMENT UNTIL: 20120302

Year of fee payment: 11

FPAY Renewal fee payment (event date is renewal date of database)

Free format text: PAYMENT UNTIL: 20130302

Year of fee payment: 12

EXPY Cancellation because of completion of term
FPAY Renewal fee payment (event date is renewal date of database)

Free format text: PAYMENT UNTIL: 20130302

Year of fee payment: 12