JP3004339B2 - Densification method of thermal spray coating - Google Patents
Densification method of thermal spray coatingInfo
- Publication number
- JP3004339B2 JP3004339B2 JP2272949A JP27294990A JP3004339B2 JP 3004339 B2 JP3004339 B2 JP 3004339B2 JP 2272949 A JP2272949 A JP 2272949A JP 27294990 A JP27294990 A JP 27294990A JP 3004339 B2 JP3004339 B2 JP 3004339B2
- Authority
- JP
- Japan
- Prior art keywords
- thermal spray
- sprayed
- alumina
- spray coating
- deposit
- 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.)
- Expired - Lifetime
Links
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- Coating By Spraying Or Casting (AREA)
Description
【発明の詳細な説明】 〔産業上の利用分野〕 本発明は溶射皮膜の緻密化方法に関する。The present invention relates to a method for densifying a thermal sprayed coating.
〔従来の技術〕 従来の溶射皮膜形成方法においては、第３図の断面図
に示すように、例えばAl2O3,ZrO2−Y2O3,Ni−Cr等の溶
射材料からなる溶射粒子03を、プラズマ又はガス火炎に
よって溶融させながら被溶射物01に吹き付けて堆積させ
溶射皮膜02を形成しており、溶射粒子03は被溶射物01と
の衝突で偏平状態となり、溶射皮膜02は偏平化した粒子
と粒子との堆積となるため、粒界に空孔04ができ全体と
して多孔質の皮膜となる。In [Prior Art] Conventional thermal spray coating forming method, as shown in the sectional view of FIG. 3, for example, Al 2 O 3, ZrO 2 -Y 2 O 3, spray particles consisting of spray material such as Ni-Cr 03 is sprayed and deposited on the object to be sprayed 01 while being melted by plasma or gas flame to form a thermal spray coating 02.The thermal spray particles 03 are flattened by collision with the thermal spray 01, and the thermal spray coating 02 is flat. Since the particles are converted into particles, voids 04 are formed in the grain boundaries, resulting in a porous film as a whole.
このような溶射皮膜02を腐食性の環境にさらすと腐食
物が空孔04を浸透して被溶射物01を腐食してしまい、十
分な耐食性が得られないことがある。そこで従来は、溶
射皮膜02へ樹脂を圧入して空孔04を樹脂で埋め固め、腐
食物が溶射皮膜02を浸透して行かないようにしている。When such a thermal spray coating 02 is exposed to a corrosive environment, corrosive substances penetrate the pores 04 and corrode the thermal spray target 01, so that sufficient corrosion resistance may not be obtained. Therefore, conventionally, a resin is press-fitted into the thermal spray coating 02 to fill the voids 04 with the resin so that corrosive substances do not penetrate the thermal spray coating 02.
しかしながら、高温雰囲気下では、樹脂は溶け落ちる
か又は蒸発してしまうため、腐食物が空孔04内へ侵入し
被溶射物01を腐食させるおそれがあり、従って従来の溶
射皮膜は高温雰囲気の腐食性環境下で十分な耐食効果を
上げることは困難である。However, in a high-temperature atmosphere, the resin melts down or evaporates, so that corrosive substances may enter the pores 04 and corrode the sprayed object 01. It is difficult to achieve a sufficient corrosion resistance effect in a neutral environment.
本発明は、このような事情に鑑みて提案されたもの
で、溶射皮膜の溶射粒子間の空孔内に溶け落ちたり蒸発
したりしない蒸着物を堆積させて溶射皮膜を緻密化し、
高温雰囲気の腐食環境下で溶射皮膜の十分な耐食効果を
得ることができる溶射皮膜の緻密化方法を提供すること
を目的とする。The present invention has been proposed in view of such circumstances, and densifies the thermal spray coating by depositing a deposit that does not melt down or evaporate in the pores between the thermal spray particles of the thermal spray coating,
It is an object of the present invention to provide a method for densifying a sprayed coating capable of obtaining a sufficient corrosion resistance effect of the sprayed coating under a corrosive environment in a high-temperature atmosphere.
そのために本発明の溶射皮膜の緻密化方法は、被溶射
物の表面に形成された溶射皮膜を構成するアルミナの溶
射粒子間の空孔に、化学反応によりアルミナの蒸着物を
生成する水素で希釈した塩化アルミニウムの蒸気ガスと
水素で希釈した水蒸気ガスとをアルミナの蒸着物を生成
するのに必要な混合割合で混合して生成された混合蒸気
ガスを侵入させるとともに、上記溶射皮膜の温度を上記
塩化アルミニウムの蒸気ガスと水蒸気とが反応する温度
にまで加熱保持することにより、上記空孔内でアルミナ
の蒸着物を堆積させることを特徴とする。For this purpose, the method for densifying a sprayed coating of the present invention uses a method of diluting pores between sprayed alumina particles constituting the sprayed coating formed on the surface of the object to be sprayed with hydrogen, which generates an alumina deposit by a chemical reaction. The mixed steam gas generated by mixing the steam gas of aluminum chloride and the steam gas diluted with hydrogen at a mixing ratio necessary to form a deposit of alumina is introduced, and the temperature of the sprayed coating is adjusted to The method is characterized in that alumina is deposited in the pores by heating and maintaining the temperature at which the vapor gas of aluminum chloride and water vapor react with each other.
上述の構成により、被溶射物の表面に形成された溶射
皮膜を構成するアルミナの溶射粒子間の空孔内に溶け落
ちたり蒸発したりしないアルミナの蒸着物を堆積させて
溶射皮膜を緻密化し、高温雰囲気の腐食環境下で溶射皮
膜の十分な耐食効果を得ることができる溶射皮膜の緻密
化方法を得ることができる。According to the above-described configuration, the thermal spray coating is densified by depositing an alumina deposit that does not melt down or evaporate in the pores between the thermal spray particles of the alumina forming the thermal spray coating formed on the surface of the thermal spray coating, It is possible to obtain a method for densifying a sprayed coating capable of obtaining a sufficient corrosion resistance effect of the sprayed coating under a corrosive environment of a high temperature atmosphere.
本発明の溶射皮膜の緻密化方法の一実施例を図面につ
いて説明すると、第１図は実施装置の模式図、第２図は
本方法により得られる溶射皮膜の断面図である。An embodiment of the method for densifying a thermal spray coating according to the present invention will be described with reference to the drawings. FIG. 1 is a schematic view of an apparatus for implementing the method, and FIG. 2 is a sectional view of a thermal spray coating obtained by the present method.
第１図において、雰囲気制御室11は、溶射皮膜２が形
成されている被溶射物１を収容するのに十分な空所を有
するとともに、石英ガラスで製作されており、この雰囲
気制御室11の外周には加熱ヒーター12が設置されるとと
もに、雰囲気制御室11及び加熱ヒーター12を適宜厚さの
断熱材13が囲蔽している。In FIG. 1, an atmosphere control chamber 11 has a sufficient space for accommodating the object 1 on which a thermal spray coating 2 is formed, and is made of quartz glass. A heater 12 is provided on the outer periphery, and a heat insulating material 13 having an appropriate thickness surrounds the atmosphere control chamber 11 and the heater 12.
また雰囲気制御室11の一方の側部には加圧ポンプ14が
連通されるとともに、同加圧ポンプ14に反応ガス混合ボ
ックス15が接続されたうえ、ここに流量形16,17をそれ
ぞれ介した２個の反応ガス供給口18,19が接続され、更
に各反応ガス供給口18,19にはそれぞれ弁20,21が付設さ
れている。なおまた雰囲気制御室11の他方の側部には排
気口22が設けられるとともに、圧力調整弁23が付設され
ている。Further, a pressure pump 14 is connected to one side of the atmosphere control chamber 11, and a reaction gas mixing box 15 is connected to the pressure pump 14, and the reaction gas mixing box 15 is connected to the reaction gas mixing box 15 via flow rate type 16, 17 respectively. The two reaction gas supply ports 18 and 19 are connected, and the reaction gas supply ports 18 and 19 are further provided with valves 20 and 21, respectively. An exhaust port 22 is provided on the other side of the atmosphere control chamber 11, and a pressure regulating valve 23 is additionally provided.
このような装置構成において、溶射材料にアルミナ
（Al2O3）を用いて溶射皮膜２を形成した被溶射物１
を、雰囲気制御室11内に収容させた後、弁20,21を閉め
て圧力調整弁23を開き、排気口22の先の図示せざる真空
ポンプにより雰囲気制御室11から排気する。このときの
排気によって雰囲気制御室11は例えば10−５〜−６Torr
程度の真空度にする。In such an apparatus configuration, a sprayed object 1 having a sprayed coating 2 formed by using alumina (Al 2 O 3 ) as a sprayed material.
Is housed in the atmosphere control chamber 11, the valves 20, 21 are closed, the pressure regulating valve 23 is opened, and the gas is exhausted from the atmosphere control chamber 11 by a vacuum pump (not shown) at the end of the exhaust port 22. At this time, the atmosphere control chamber 11 is evacuated to 10 -5 -6 Torr by the exhaust.
Set the degree of vacuum.
次に弁20,21を開き、反応ガス供給口18に水素で希釈
した塩化アルミニウム（AlCl3）の蒸気ガスを供給する
とともに、反応ガス供給口19に水素で希釈した水蒸気ガ
ス（H2O）を供給する。このとき流量計16,17によって各
ガスの流量を調整し、各ガスの流量は、塩化アルミニウ
ムと水蒸気が化学反応によってアルミナの蒸着物を形成
するように、次の（１）式の化学結合と同じ割合にす
る。つまり塩化アルミニウムと水蒸気が、（１）式の化
学反応を起こすために、塩化アルミニウムと水蒸気の質
量割合を2:3となるように、流量計16,17を調整する。Next, the valves 20 and 21 are opened, a steam gas of aluminum chloride (AlCl 3 ) diluted with hydrogen is supplied to the reaction gas supply port 18, and a steam gas (H 2 O) diluted with hydrogen is supplied to the reaction gas supply port 19. Supply. At this time, the flow rate of each gas is adjusted by the flow meters 16 and 17, and the flow rate of each gas is adjusted to the chemical bond of the following formula (1) so that aluminum chloride and water vapor form an alumina deposit by a chemical reaction. Make the same proportion. That is, the flowmeters 16 and 17 are adjusted so that the mass ratio of aluminum chloride and water vapor becomes 2: 3 so that aluminum chloride and water vapor cause the chemical reaction of the formula (1).
2AlCl3＋3H2O→Al2O3＋6HCl ・・・・・・・・・（１） このような量のアルミニウムの蒸気ガスと水蒸気ガス
を反応ガス混合ボックス15で混合し、混合蒸気ガスを加
圧ポンプ14へ流すと、混合蒸気ガスは加圧ポンプ14によ
って雰囲気制御室11に供給される。その際圧力調整弁23
によって雰囲気制御室11の圧力が常に2Torr前後に保持
されるように調整する。これによって混合蒸気ガスは、
図２における溶射皮膜２内の空孔４内に浸透していくこ
とになる。2AlCl 3 + 3H 2 O → Al 2 O 3 + 6HCl (1) Such amounts of aluminum vapor gas and water vapor gas are mixed in the reaction gas mixing box 15, and the mixed vapor gas is added. When flowing to the pressure pump 14, the mixed vapor gas is supplied to the atmosphere control chamber 11 by the pressure pump 14. At that time, the pressure regulating valve 23
Is adjusted so that the pressure in the atmosphere control chamber 11 is always maintained at about 2 Torr. As a result, the mixed steam gas becomes
2 penetrates into the holes 4 in the thermal spray coating 2 in FIG.
次いで加熱ヒーター12によって、溶射皮膜２の温度を
塩化アルミニウムと水蒸気が反応する温度例えば1100℃
まで加熱調整し約１時間保持する。これによって塩化ア
ルミニウムと水蒸気は空孔４の中で前記（１）式の化学
反応を起こす。その結果、生成したアルミナ（Al2O3）
は、第２図における蒸着物５となり空孔４の壁面に付着
堆積する。Next, the temperature of the thermal spray coating 2 is increased by the heater 12 to a temperature at which aluminum chloride and water vapor react, for example, 1100 ° C.
Adjust until heating and hold for about 1 hour. As a result, the aluminum chloride and water vapor cause the chemical reaction of the above formula (1) in the pores 4. The resulting alumina (Al 2 O 3 )
Becomes the deposit 5 in FIG.
その後、再び真空ポンプによって排気口22から排気
し、アルミナと同時に発生する塩素（HCl）を空孔４か
ら排出させ、新たに塩化アルミニウムの蒸気ガスと水蒸
気を空孔内に供給するために、加熱ヒーター12を切っ
て、溶射皮膜温度を、化学反応が起こらない温度まで下
げる。すなわち、例えば、溶射皮膜温度を500℃へ下
げ、この温度で約15分保持し、そして、再度溶射皮膜温
度を1100℃に上げ約１時間保持する。After that, the air is exhausted again from the exhaust port 22 by the vacuum pump, and the chlorine (HCl) generated simultaneously with the alumina is exhausted from the holes 4, and the heating is performed so that the vapor gas and the water vapor of aluminum chloride are newly supplied into the holes. The heater 12 is turned off to lower the temperature of the thermal spray coating to a temperature at which no chemical reaction occurs. That is, for example, the temperature of the sprayed coating is lowered to 500 ° C., and this temperature is maintained for about 15 minutes, and then the temperature of the sprayed coating is raised again to 1100 ° C. and held for about 1 hour.
かくして、得られる溶射皮膜２は、第２図に示すよう
に、空孔４内と溶射皮膜２の表面に溶射粒子３と同じ材
質のアルミナの蒸着物５が形成されて緻密化され、また
このようなアルミナの蒸着物５は、高温雰囲気の腐食環
境下でも溶け落ちたり蒸発したりすることなく保持さ
れ、十分な耐食効果が得られる。In this way, as shown in FIG. 2, the obtained thermal spray coating 2 is densified by forming an alumina deposit 5 of the same material as the thermal spray particles 3 in the pores 4 and on the surface of the thermal spray coating 2. Such an alumina deposit 5 is retained without being melted down or evaporated even under a corrosive environment of a high temperature atmosphere, and a sufficient corrosion resistance effect can be obtained.
なお、上記実施例では、溶射粒子３と同じ材料の蒸着
物５を形成したが、更に耐熱性のある材料を用いてもよ
い。In the above embodiment, the deposited material 5 of the same material as the thermal sprayed particles 3 is formed, but a material having more heat resistance may be used.
要するに本発明によれば、被溶射物の表面に形成され
た溶射皮膜を構成するアルミナの溶射粒子間の空孔に、
化学反応によりアルミナの蒸着物を生成する水素で希釈
した塩化アルミニウムの蒸気ガスと水素で希釈した水蒸
気ガスとをアルミナの蒸着物を生成するのに必要な混合
割合で混合して生成された混合蒸気ガスを侵入させると
ともに、蒸気溶射皮膜の温度を上記塩化アルミニウムの
蒸気ガスと水蒸気とが反応する温度にまで加熱保持し
て、上記空孔内でアルミナの蒸着物を堆積させることに
より、溶射皮膜のアルミナの溶射粒子間の空孔内に溶け
落ちたり蒸発したりしないアルミナの蒸着物を堆積させ
て溶射皮膜を緻密化し、高温雰囲気の腐食環境下で溶射
皮膜の十分な耐食効果を得ることができる溶射皮膜の緻
密化方法を得るから、本発明は産業上極めて有益なもの
である。In short, according to the present invention, the pores between the spray particles of alumina constituting the spray coating formed on the surface of the object to be sprayed,
A mixed vapor generated by mixing a vapor gas of aluminum chloride diluted with hydrogen and a vapor gas diluted with hydrogen in a mixing ratio necessary to form an alumina deposit, which produces an alumina deposit by a chemical reaction. While allowing gas to enter, heating and maintaining the temperature of the vapor-sprayed coating to a temperature at which the vapor gas of aluminum chloride reacts with water vapor, and depositing a deposit of alumina in the pores, By depositing a deposit of alumina that does not melt down or evaporate in the pores between the sprayed particles of alumina, the sprayed coating is densified, and sufficient corrosion resistance of the sprayed coating can be obtained under a corrosive environment of a high temperature atmosphere. The present invention is extremely useful industrially because a method for densifying a sprayed coating is obtained.
第１図は本発明溶射皮膜の緻密化方法の一実施例におけ
る実施装置の模式図、第２図は本方法により得られる溶
射皮膜の断面図である。 第３図は従来の溶射皮膜の断面図である。 １……被溶射物、２……溶射皮膜、３……溶射粒子、４
……空孔、５……蒸着物、11……雰囲気制御室、12……
加熱ヒーター、13……断熱材、14……加圧ポンプ、15…
…反応ガス混合ボックス、16,17……流量計、18,19……
反応ガス供給口、20,21……弁、22……排気口、23……
圧力調整弁FIG. 1 is a schematic view of an apparatus in one embodiment of the method for densifying a sprayed coating of the present invention, and FIG. 2 is a cross-sectional view of the sprayed coating obtained by the method. FIG. 3 is a sectional view of a conventional thermal spray coating. 1 ... spray target, 2 ... spray coating, 3 ... spray particles, 4
…… Vacancy, 5… Vapor deposit, 11 …… Atmosphere control room, 12 ……
Heater, 13… Insulation material, 14… Pressure pump, 15…
… Reaction gas mixing box, 16,17 …… Flow meter, 18,19 ……
Reactant gas supply port, 20, 21 ... valve, 22 ... exhaust port, 23 ...
Pressure regulating valve
Claims (1)
成するアルミナの溶射粒子間の空孔に、化学反応により
アルミナの蒸着物を生成する水素で希釈した塩化アルミ
ニウムの蒸気ガスと水素で希釈した水蒸気ガスとをアル
ミナの蒸着物を生成するのに必要な混合割合で混合して
生成された混合蒸気ガスを侵入させるとともに、上記溶
射皮膜の温度を上記塩化アルミニウムの蒸気ガスと水蒸
気とが反応する温度にまで加熱保持することにより、上
記空孔内でアルミナの蒸着物を堆積させることを特徴と
する、溶射皮膜の緻密化方法。An aluminum chloride vapor gas and hydrogen diluted with hydrogen, which forms an alumina deposit by a chemical reaction, are filled in pores between sprayed alumina particles forming a thermal spray coating formed on the surface of the object to be sprayed. The mixed steam gas generated by mixing the steam gas diluted with the above at a mixing ratio necessary to generate the deposited material of alumina is caused to penetrate, and the temperature of the sprayed coating is adjusted by the steam gas of the aluminum chloride and the steam. A method for densifying a sprayed coating, comprising heating and maintaining the temperature to a temperature at which a reaction occurs to deposit a deposit of alumina in the pores.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2272949A JP3004339B2 (en) | 1990-10-11 | 1990-10-11 | Densification method of thermal spray coating |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2272949A JP3004339B2 (en) | 1990-10-11 | 1990-10-11 | Densification method of thermal spray coating |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH04147960A JPH04147960A (en) | 1992-05-21 |
| JP3004339B2 true JP3004339B2 (en) | 2000-01-31 |
Family
ID=17521024
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2272949A Expired - Lifetime JP3004339B2 (en) | 1990-10-11 | 1990-10-11 | Densification method of thermal spray coating |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3004339B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP6188004B2 (en) * | 2012-01-16 | 2017-08-30 | 島根県 | Method for forming ceramic spray coating and functional ceramic spray coating |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5690969A (en) * | 1979-12-24 | 1981-07-23 | Nippon Tungsten Co Ltd | Method of making melt-sprayed film dense |
| JPS61147875A (en) * | 1984-12-19 | 1986-07-05 | Seiko Instr & Electronics Ltd | Case of wrist watch |
| JPS63285877A (en) * | 1987-05-19 | 1988-11-22 | Mitsubishi Heavy Ind Ltd | Manufacture of solid electrolyte |
-
1990
- 1990-10-11 JP JP2272949A patent/JP3004339B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH04147960A (en) | 1992-05-21 |
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