JP3605969B2 - Method of producing titanium oxide film for corrosion protection and titanium oxide film for corrosion protection - Google Patents
Method of producing titanium oxide film for corrosion protection and titanium oxide film for corrosion protection Download PDFInfo
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Description
【０００１】
【発明の属する技術分野】
本発明は、防食用チタン酸化膜の作製方法および防食用チタン酸化膜に係わり、特に、原子炉構造材に対して光電極反応を利用して防食を行う技術に関するものである。
【０００２】
【従来の技術】
水を冷却材としている軽水炉では、炉心を囲んでいる原子炉圧力容器内の内部構造物の大部分が、高温状態の原子炉冷却水中に配され、炉心から放射される放射線の雰囲気で使用されるため、構成材料にあっては、原子炉冷却水に対する耐食性を有するとともに、放射線の水分解による影響等を考慮するなど品質管理において格別な配慮が払われている。
【０００３】
防食用チタン酸化膜の作製方法および防食用チタン酸化膜に関連する技術として、例えば、特開平０７−２７０５９２号公報「原子炉構造材およびその防食方法」に、原子炉圧力容器の内部構造物に採用されるチタン酸化膜の作製方法に関連する技術が提案されている。
この技術は、チタン酸化膜の光半導体特性を利用したもので、放射線またはチェレンコフ放射性光の照射時に、非消耗型のアノード反応を生じさせ、チタン酸化膜（光半導体膜）近傍の原子炉構造材の表面の腐食電位を下げて金属の耐食性を高めるようにしている。
【０００４】
また、チタン酸化膜（ＴｉＯ２ 膜）は、酸素の介在雰囲気においてＴｉ粒子を溶射することにより、作製するようにしている。
【０００５】
【発明が解決しようとする課題】
しかしながら、Ｔｉ粒子を溶射させながら酸化させることによりＴｉＯ２ 膜を作製する方法であると、良好な光半導体特性を効率的に得ることが困難である。
【０００６】
一方、ｎ型ＴｉＯ２ は、光半導体特性を有するものとして期待されるが、ｎ型ＴｉＯ２ 粒子を例えば、プラズマ溶射する技術であると、プラズマ流が高温であるために溶融状態となって光半導体としての結晶構造が壊れ、光半導体特性が損なわれてしまうという課題が残されている。
【０００７】
本発明は、このような課題に鑑みてなされたものであり、以下の目的を達成するものである。
▲１▼ ＴｉＯ２ 膜の被防食材への密着性を高めること。
▲２▼ ｎ型ＴｉＯ２ 粒子の形状の残存性を高め、ｎ型ＴｉＯ２ 膜の作製を容易にすること。
▲３▼ ＴｉＯ２ 膜の成膜時の作業性を向上させること。
【０００８】
【課題を解決するための手段】
ｎ型ＴｉＯ２ 粒子をプラズマ流に乗せて被防食材の表面に溶射することにより光半導体特性を有するＴｉＯ２ 膜を作製する際に、ＴｉＯ２ 粒子を溶融して被防食材に溶融凝固層を作製し、プラズマ溶射温度を高温から低温にしてｎ型ＴｉＯ２ 粒子を溶着させることにより粒子層を作製する。この場合にあって、ｎ型ＴｉＯ２ 粒子のみを供給して溶融凝固層および粒子層の双方を形成してもよい。
また、被防食材の表面にあっては、プラズマ溶射温度を高温から低温にしてｎ型ＴｉＯ２ 粒子を溶着させるため、ｎ型ＴｉＯ２ 粒子比率が連続的または段階的に設定されたＴｉＯ２ 膜が作製される。
【０００９】
【発明の実施の形態】
本発明に係る防食用チタン酸化膜の作製方法および防食用チタン酸化膜の一実施形態について、図１ないし図２を参照して説明する。
【００１０】
図１は、防食用チタン酸化膜の作製工程例を示すものである。
また、図２において、１は被防食材、２は溶融凝固層、３は半溶融層、４は粒子層（ｎ型ＴｉＯ２ 粒子層）、ＸはＴｉＯ２ 膜である。
【００１１】
〔Ｓ１：ｎ型ＴｉＯ２ 粒子の製造〕
予め、粒径が数μｍないし数１０μｍのｎ型ＴｉＯ２ 粒子を製造しておく。
【００１２】
〔Ｓ２：ｎ型ＴｉＯ２ 粒子の供給〕
Ｓ１で製造した ｎ型ＴｉＯ２ 粒子を、プラズマ溶射装置に供給する。
【００１３】
〔Ｓ３：プラズマ溶射〕
プラズマガスとしてＡｒガス、２次ガスとしてＨｅガス、Ｈ２ ガス等を使用してプラズマ化し、このときのプラズマ流にｎ型ＴｉＯ２ 粒子を乗せて、鉄系合金やステンレス鋼等の防食材１（図２参照）に、例えば１００％溶解させた状態にして溶射する。
【００１４】
〔Ｓ４：被防食材へのＴｉＯ２ の溶着〕
被防食材１には、溶融状態のＴｉＯ２ が凝固することにより、溶融凝固層２が一体に形成される。
【００１５】
〔Ｓ５：プラズマ温度の調整〕
プラズマ電流を減少させ、かつ、プラズマガス流量を多くして、プラズマ流の温度が低くなるように導く。
この際に、ｎ型ＴｉＯ２ 粒子の供給を継続すると温度が低めに誘導されるために、溶融状態のＴｉＯ２ に一部未溶解状態のＴｉＯ２ 粒子が混合した半溶融層３（図２参照）が形成される。
【００１６】
〔Ｓ６：ｎ型ＴｉＯ２ 粒子の供給〕
以下、プラズマ流の温度を低く誘導した状態でｎ型ＴｉＯ２ 粒子の供給を行う。
【００１７】
〔Ｓ７：プラズマ溶射〕
プラズマ流の温度を低く導いたままｎ型ＴｉＯ２ 粒子を供給すると、ｎ型ＴｉＯ２ 粒子は、全量が溶解されることなく、一部が粒子状態を保持したまま被防食材１に向けて溶射される。
【００１８】
〔Ｓ８：被防食材への粒状ｎ型ＴｉＯ２ の溶着〕
粒状のｎ型ＴｉＯ２ 粒子と溶融状態のＴｉＯ２ とが、混合状態で被防食材１の表面に送り込まれると、溶融状態のＴｉＯ２ の凝固にともないｎ型ＴｉＯ２ 粒子の形状が残されたまま溶着され、半溶融層３の上に粒子層（ｎ型ＴｉＯ２ 粒子層）４が形成される。
【００１９】
このように、プラズマ電流，プラズマガス流量を変えて、実質的にプラズマ流の温度を下げながらｎ型ＴｉＯ２ 粒子を溶着させるようにすると、作製されるＴｉＯ２ 膜Ｘが図２に示すように傾斜構造を有するようになる。
つまり、溶射当初にあっては、ＴｉＯ２ の溶融凝固によりｎ型ＴｉＯ２ 粒子の比率が低くなるが、半溶融層３，粒子層（ｎ型ＴｉＯ２ 粒子層）４が形成されるにしたがって次第にｎ型ＴｉＯ２ 粒子の占める割合が多くなり、最終的にはｎ型ＴｉＯ２ 粒子層の比率が高められた粒子層（ｎ型ＴｉＯ２ 粒子層）４が作製される。
【００２０】
〔他の実施の形態〕
本発明に係わる防食用チタン酸化膜の作製方法にあっては、Ｓ９に示すようにＳ２におけるｎ型ＴｉＯ２ 粒子の供給に代えて、ｎ型ＴｉＯ２ 以外のＴｉＯ２ 粒子を供給し、溶融凝固層２を介在させるようにしてもよい。
【００２１】
【実施例】
プラズマ流の条件を変えて形成されるＴｉＯ２ 膜Ｘの溶融強度について検討した。
〔サンプルＡ〕
プラズマ電流 ４００Ａ，プラズマガス流量 ６０リットル／分
〔サンプルＢ〕
プラズマ電流 ６００Ａ，プラズマガス流量 ５０リットル／分
および、
プラズマ電流 ４００Ａ，プラズマガス流量 ６０リットル／分
（サンプルＢにあっては、溶融凝固層形成後に粒子層を形成）
【００２２】
上記サンプルＡ，Ｂにクロスカットを入れ、セロハンテープを貼り付けて剥離の有無について調べた。
サンプルＡは、セロハンテープの貼付面積のおよそ２０％に剥離が認められた。
サンプルＢは、セロハンテープの貼付部分に剥離が認められなかった。
また、表面状況を観察したところサンプルＡ，Ｂとも粒状のＴｉＯ２ が多量に付着していることが認められた。
これらの結果から、サンプルＢのようにプラズマ流量の条件を変えて溶射することにより、粒子比率を徐々に高くする方法が有効であると結論付けられる。
【００２３】
【発明の効果】
本発明に係る防食用チタン酸化膜の作製方法および防食用チタン酸化膜によれば、以下の効果を奏する。
（１） ＴｉＯ２ 膜の表面の粒子比率を高くすることにより光半導体としての機能を向上させて、防食性を高めることができる。
（２） 被防食材の表面にＴｉＯ２ の溶融凝固層を作製し、その後、粒子比率を高めた傾斜構造とすることにより、ＴｉＯ２ 膜の密着性を高めることができる。
（３） ｎ型ＴｉＯ２ 粒子を連続的に使用して成膜条件を変えることにより、成膜時の作業性を高めることができる。
【図面の簡単な説明】
【図１】本発明に係わる防食用チタン酸化膜の作製方法の一実施形態を示すフローチャートである。
【図２】本発明に係わる防食用チタン酸化膜の一実施形態を示す正断面図である。
【符号の説明】
１ 被防食材
２ 溶融凝固層
３ 半溶融層
４ 粒子層（ｎ型ＴｉＯ２ 粒子層）
Ｘ ＴｉＯ２ 膜[0001]
TECHNICAL FIELD OF THE INVENTION
The present invention relates to a method for producing a titanium oxide film for corrosion protection and a titanium oxide film for corrosion protection, and more particularly to a technique for performing corrosion protection on a reactor structural material using a photoelectrode reaction.
[0002]
[Prior art]
In light water reactors that use water as a coolant, most of the internal structures inside the reactor pressure vessel surrounding the core are placed in high-temperature reactor cooling water and used in an atmosphere of radiation radiated from the core. Therefore, the constituent materials have corrosion resistance to reactor cooling water, and special attention has been paid to quality control, for example, by taking into account the effects of water decomposition of radiation.
[0003]
Examples of a method for producing a corrosion-resistant titanium oxide film and a technique related to the corrosion-resistant titanium oxide film include, for example, Japanese Patent Application Laid-Open No. 07-270592, entitled "Reactor Structural Materials and Corrosion Prevention Method", and Techniques related to a method of manufacturing a titanium oxide film to be employed have been proposed.
This technology utilizes the photo-semiconductor properties of the titanium oxide film, which causes a non-consumable anode reaction when irradiated with radiation or Cerenkov radiant light, and the reactor structural material near the titanium oxide film (photo-semiconductor film) The corrosion potential of the surface is lowered to increase the corrosion resistance of the metal.
[0004]
The titanium oxide film (TiO 2 film) is formed by spraying Ti particles in an atmosphere containing oxygen.
[0005]
[Problems to be solved by the invention]
However, it is difficult to efficiently obtain good optical semiconductor characteristics by a method of producing a TiO 2 film by oxidizing while spraying Ti particles.
[0006]
On the other hand, n-type TiO 2 is expected to have optical semiconductor properties. However, for example, in a technique of plasma spraying n-type TiO 2 particles, the plasma flow is at a high temperature, so that the plasma flow is in a molten state and becomes light. There remains a problem that the crystal structure of the semiconductor is broken and optical semiconductor characteristics are impaired.
[0007]
The present invention has been made in view of such problems, and achieves the following objects.
(1) To improve the adhesion of the TiO 2 film to the material to be protected.
{Circle around (2)} To improve the survivability of the shape of the n-type TiO 2 particles and facilitate the production of the n-type TiO 2 film.
{Circle around (3)} Improving the workability when forming the TiO 2 film.
[0008]
[Means for Solving the Problems]
When producing a TiO 2 film having optical semiconductor characteristics by spraying n-type TiO 2 particles on a plasma flow and spraying the surface of the material to be protected, the TiO 2 particles are melted to form a melt-solidified layer on the material to be protected. Then, the particle layer is formed by lowering the plasma spraying temperature from a high temperature to a low temperature and welding n-type TiO 2 particles. In this case, only the n-type TiO 2 particles may be supplied to form both the melt-solidified layer and the particle layer.
Further, in the surface of the sacrificial material, in order to weld the n-type TiO 2 particles plasma spraying temperature from a high temperature to a low temperature, TiO 2 film n-type TiO 2 particles ratio is continuously or stepwise setting Is produced.
[0009]
BEST MODE FOR CARRYING OUT THE INVENTION
An embodiment of a method for manufacturing a titanium oxide film for corrosion protection and an embodiment of a titanium oxide film for corrosion protection according to the present invention will be described with reference to FIGS.
[0010]
FIG. 1 shows an example of a manufacturing process of a titanium oxide film for corrosion protection.
In FIG. 2, reference numeral 1 denotes a material to be protected, 2 denotes a melt-solidified layer, 3 denotes a semi-molten layer, 4 denotes a particle layer (n-type TiO 2 particle layer), and X denotes a TiO 2 film.
[0011]
[S1: Production of n-type TiO 2 particles]
N-type TiO 2 particles having a particle size of several μm to several tens μm are manufactured in advance.
[0012]
[S2: Supply of n-type TiO 2 particles]
The n-type TiO 2 particles produced in S1 are supplied to a plasma spraying device.
[0013]
[S3: Plasma spraying]
Plasma is formed using Ar gas as a plasma gas, He gas, H 2 gas, or the like as a secondary gas, and n-type TiO 2 particles are placed on the plasma flow at this time, and an anticorrosive material 1 such as an iron-based alloy or stainless steel is placed. (See FIG. 2), for example, in a state where it is dissolved in 100%, and sprayed.
[0014]
[S4: Welding of TiO 2 to the material to be protected]
The molten and solidified layer 2 is formed integrally with the anticorrosion material 1 by solidifying the molten TiO 2 .
[0015]
[S5: Adjustment of plasma temperature]
The plasma current is reduced and the plasma gas flow rate is increased to guide the plasma flow to a lower temperature.
At this time, since the temperature is continued supply of n-type TiO 2 particles are induced to be lower, semi-molten layer 3 (see FIG. 2 TiO 2 particles of partially undissolved was mixed with TiO 2 in a molten state ) Is formed.
[0016]
[S6: Supply of n-type TiO 2 particles]
Hereinafter, n-type TiO 2 particles are supplied in a state where the temperature of the plasma flow is induced to be low.
[0017]
[S7: Plasma spraying]
When n-type TiO 2 particles are supplied while the temperature of the plasma flow is kept low, the entire amount of the n-type TiO 2 particles is sprayed toward the anticorrosion-protected material 1 while a part thereof is maintained without being dissolved. Is done.
[0018]
[S8: Welding of granular n-type TiO 2 to the material to be protected]
When the granular n-type TiO 2 particles and the molten TiO 2 were fed into the surface of the material to be protected 1 in a mixed state, the shape of the n-type TiO 2 particles was left due to the solidification of the molten TiO 2 . The particles are welded as they are, and a particle layer (n-type TiO 2 particle layer) 4 is formed on the
[0019]
As described above, when the n-type TiO 2 particles are welded while changing the plasma current and the flow rate of the plasma gas to substantially lower the temperature of the plasma flow, the TiO 2 film X to be produced becomes as shown in FIG. It has an inclined structure.
That, in the initial spraying, gradually according although the ratio of n-type TiO 2 particles by melting and solidification of TiO 2 is lower,
[0020]
[Other embodiments]
In the manufacturing method of the sacrificial titanium oxide film according to the present invention, instead of the supply of n-type TiO 2 particles in S2, as shown in S9, supplies TiO 2 particles other than n-type TiO 2, the melt-solidified The layer 2 may be interposed.
[0021]
【Example】
The melting strength of the TiO 2 film X formed by changing the conditions of the plasma flow was examined.
[Sample A]
Plasma current 400A, plasma gas flow rate 60 l / min [Sample B]
Plasma current 600A, plasma gas flow rate 50 liter / min and
Plasma current 400A, plasma gas flow rate 60 liter / min (in sample B, a particle layer is formed after the formation of a molten and solidified layer)
[0022]
A cross cut was made in each of the samples A and B, and a cellophane tape was stuck thereon to examine the presence or absence of peeling.
In Sample A, peeling was observed in approximately 20% of the area where the cellophane tape was stuck.
In Sample B, no peeling was observed at the portion where the cellophane tape was attached.
When the surface condition was observed, it was confirmed that a large amount of granular TiO 2 was attached to both samples A and B.
From these results, it can be concluded that a method of gradually increasing the particle ratio by changing the condition of the plasma flow rate and performing thermal spraying as in Sample B is effective.
[0023]
【The invention's effect】
According to the method for producing a corrosion-resistant titanium oxide film and the corrosion-resistant titanium oxide film of the present invention, the following effects can be obtained.
(1) By increasing the particle ratio on the surface of the TiO 2 film, the function as an optical semiconductor can be improved, and the anticorrosion property can be improved.
(2) The adhesion of the TiO 2 film can be enhanced by forming a melt-solidified layer of TiO 2 on the surface of the material to be protected and then forming an inclined structure with an increased particle ratio.
(3) By continuously using the n-type TiO 2 particles and changing the film forming conditions, the workability at the time of film forming can be improved.
[Brief description of the drawings]
FIG. 1 is a flowchart showing one embodiment of a method for producing a titanium oxide film for corrosion protection according to the present invention.
FIG. 2 is a front sectional view showing an embodiment of a titanium oxide film for corrosion protection according to the present invention.
[Explanation of symbols]
DESCRIPTION OF SYMBOLS 1 Corrosion-proof material 2 Melted solidified
X TiO 2 film
Claims (7)
第１のプラズマ溶射温度でＴｉＯ２粒子を溶融して被防食材に溶融凝固層（２）を作製する工程と、
前記第１のプラズマ溶射温度よりも低い第２のプラズマ溶射温度でｎ型ＴｉＯ２粒子を溶着させることにより粒子層（４）を作製する工程と
を有することを特徴とする防食用チタン酸化膜の作製方法。A method of forming a TiO 2 film (X) having optical semiconductor properties by spraying n-type TiO 2 particles on a surface of a material to be protected (1) by placing the particles in a plasma flow,
Melting the TiO 2 particles at a first plasma spraying temperature to produce a melt-solidified layer (2) on the material to be protected;
Producing a particle layer (4) by welding n-type TiO 2 particles at a second plasma spraying temperature lower than the first plasma spraying temperature . Production method.
前記粒子層（４）を作製する工程では、前記第１の電流値よりも低い第２の電流値でプラズマ電流を供給し、前記第１のガス流量よりも多い第２のガス流量でプラズマガスを供給するIn the step of forming the particle layer (4), a plasma current is supplied at a second current value lower than the first current value, and the plasma gas is supplied at a second gas flow rate higher than the first gas flow rate. Supply
ことを特徴とする請求項１に記載の防食用チタン酸化膜の作製方法。The method for producing a titanium oxide film for corrosion protection according to claim 1, wherein:
被防食材に一体に形成されＴｉＯ２粒子を溶融凝固させてなる溶融凝固層（２）と、
該溶融凝固層（２）の上に一体に形成され、前記溶融凝固層（２）のｎ型ＴｉＯ ２ 粒子比率よりも高い比率でｎ型ＴｉＯ ２ 粒子が含まれた粒子層（４）と
を具備することを特徴とする防食用チタン酸化膜。A TiO 2 film (X) having optical semiconductor properties integrally formed on the surface of the material to be protected (1),
A melt-solidified layer (2) formed integrally with the corrosion-resistant material and melt-solidified with the TiO 2 particles;
Is formed integrally on the said melt-solidified layer (2), the melt-solidified layer (2) n-type TiO 2 particles having a particle layer containing the n-type TiO 2 particles at a higher rate than the ratio of the (4) A titanium oxide film for anticorrosion, comprising:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP29088996A JP3605969B2 (en) | 1996-10-31 | 1996-10-31 | Method of producing titanium oxide film for corrosion protection and titanium oxide film for corrosion protection |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| JP29088996A JP3605969B2 (en) | 1996-10-31 | 1996-10-31 | Method of producing titanium oxide film for corrosion protection and titanium oxide film for corrosion protection |
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| Publication Number | Publication Date |
|---|---|
| JPH10130810A JPH10130810A (en) | 1998-05-19 |
| JP3605969B2 true JP3605969B2 (en) | 2004-12-22 |
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| JP29088996A Expired - Fee Related JP3605969B2 (en) | 1996-10-31 | 1996-10-31 | Method of producing titanium oxide film for corrosion protection and titanium oxide film for corrosion protection |
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1996
- 1996-10-31 JP JP29088996A patent/JP3605969B2/en not_active Expired - Fee Related
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|---|---|
| JPH10130810A (en) | 1998-05-19 |
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