JP5201707B2 - A method for producing a photocathode anticorrosion coating structure. - Google Patents
A method for producing a photocathode anticorrosion coating structure. Download PDFInfo
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- JP5201707B2 JP5201707B2 JP2007062795A JP2007062795A JP5201707B2 JP 5201707 B2 JP5201707 B2 JP 5201707B2 JP 2007062795 A JP2007062795 A JP 2007062795A JP 2007062795 A JP2007062795 A JP 2007062795A JP 5201707 B2 JP5201707 B2 JP 5201707B2
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- 239000011248 coating agent Substances 0.000 title claims description 12
- 238000000576 coating method Methods 0.000 title claims description 12
- 238000004519 manufacturing process Methods 0.000 title claims description 6
- 239000002245 particle Substances 0.000 claims description 24
- 239000013078 crystal Substances 0.000 claims description 16
- 239000011941 photocatalyst Substances 0.000 claims description 10
- 239000011232 storage material Substances 0.000 claims description 10
- 239000000758 substrate Substances 0.000 claims description 8
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 6
- 239000010410 layer Substances 0.000 description 6
- 239000007921 spray Substances 0.000 description 6
- 238000003860 storage Methods 0.000 description 5
- 238000005260 corrosion Methods 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 238000004210 cathodic protection Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000002485 combustion reaction Methods 0.000 description 3
- 239000000446 fuel Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 230000001747 exhibiting effect Effects 0.000 description 2
- 238000007749 high velocity oxygen fuel spraying Methods 0.000 description 2
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 238000010248 power generation Methods 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 1
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 229910052980 cadmium sulfide Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910000423 chromium oxide Inorganic materials 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 229910000428 cobalt oxide Inorganic materials 0.000 description 1
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 239000000941 radioactive substance Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical compound [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- 229910001930 tungsten oxide Inorganic materials 0.000 description 1
- 229910001935 vanadium oxide Inorganic materials 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
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- Other Surface Treatments For Metallic Materials (AREA)
Description
本発明は、金属基材の表面に光カソード防食作用を示す光触媒と充放電作用を示す電子貯蔵材料からなる層が形成されてなるフルタイム光カソード防食コーティング構造の製造方法に関する。 The present invention relates to a method for producing a full-time photocathode anticorrosion coating structure in which a layer made of a photocatalyst exhibiting a photocathode anticorrosive action and an electron storage material exhibiting a charge / discharge action is formed on the surface of a metal substrate.
この種フルタイム光カソード防食構造については、特許文献１〜３に示すように従来より公知であり、様々な試みがなされている。
この内、特許文献３の図２（Ｃ）に示される構成は、光励起半導体からなる粉末とエレクトロクロミック材料からなる粉末とを混合物の焼結体の層が示されている。
しかし、これは、これら粉末の焼結体の層であることから、焼結工程が必要となり、対象物の設置現場での作業が不可能となる欠点があった。
また、混合物の焼結は、粉末の相互間で化学反応が生じる恐れがあり、焼結後に所望の作用を発揮する可否かは予測しがたいものである。
もし可能としても、相当の実験に基づく厳格な制御を焼結時に行うべきものであるが、当該文献にはそのようなことを窺わせる記載は一切ない。
これらのことより、当該記載は実現不可能な理想を述べたに過ぎないものであって、空想の域を脱せず技術思想には該当しないものである。
Among these, the structure shown in FIG. 2C of Patent Document 3 shows a layer of a sintered body of a mixture of a powder made of a photoexcited semiconductor and a powder made of an electrochromic material.
However, since this is a layer of a sintered body of these powders, a sintering step is required, and there is a drawback that it is impossible to work on the installation site of the object.
In addition, the sintering of the mixture may cause a chemical reaction between the powders, and it is difficult to predict whether or not a desired effect can be exhibited after sintering.
If possible, strict control based on considerable experimentation should be performed during sintering, but there is no mention in the literature of such a thing.
For these reasons, the description merely describes an ideal that cannot be realized, and does not fall within the scope of fantasy and does not fall under the technical concept.
本発明は、この様な実情に鑑み、理想的な光カソード防食コーティング構造の製造方法を提供することを目的とした。 In view of such circumstances, an object of the present invention is to provide an ideal method for producing a photocathode anticorrosion coating structure.
本発明は、金属基材の表面に光カソード防食作用を有する光触媒と充放電作用を有する電子貯蔵材料からなる層が設けられてなるフルタイム光カソード防食コーティング構造の製造方法であって、粒径が７ｎｍ〜１μｍの範囲の前記光触媒の結晶と、粒径が１０ｎｍ〜１μｍの範囲の前記電子貯蔵材料の結晶と、糊剤を混合して固化させ、粒径２５〜９０μｍの集合粒子とし、この集合粒子を４×１０２〜２５×１０２℃の温度に加熱して超音速で金属基材の表面に吹き付けて、基材表面にて前記集合粒子を衝撃により破砕させて分散させ、各結晶を基材の表面に付着させることを特徴とする。 The present invention relates to a method for producing a full-time photocathode anticorrosion coating structure in which a layer made of a photocatalyst having a photocathode anticorrosive action and an electron storage material having a charge / discharge action is provided on the surface of a metal substrate, There the crystals of the photocatalyst ranging 7Nm～1myuemu, and particle size of the electron storage material in the range of 10nm~1μm crystals, solidified by mixing the sizing agent, and a set particles having a particle diameter 25～90Myuemu, this The aggregated particles are heated to a temperature of 4 × 10 2 to 25 × 10 2 ° C. and sprayed onto the surface of the metal substrate at supersonic speed, and the aggregated particles are crushed and dispersed by impact on the surface of the substrate, and each crystal Is attached to the surface of the substrate.
本発明により、光触媒と電子貯蔵材料とが共にナノ粒子として混在することにより、光触媒からの電子貯蔵材料への移動は、殆ど無抵抗の状態でなされ、極めて効率の良い充電ができる。
また、これらが結晶体を維持していることより、相互の反応は生じにくく、長期に渡り安定した作用を発揮することができる。
また、ウオームスプレー法により吹き付けるので、所望の構造を被処理物表面に形成することができ、その他の処理を必要としないので、被処理物が使用されている現場にて、光カソード防食コーティング構造を作ることができる。
More present invention, by a photocatalyst and an electron storing material is both mixed as nanoparticles, transfer to electronic storage material from the photocatalyst is almost made in non-resistance state, Ru can very efficient charging.
Moreover, since these maintain the crystal body, mutual reaction is hard to occur, and a stable action can be exhibited over a long period of time.
Further, since the blown by warm spray method, it is possible to form the desired structure on the object surface to be treated, does not require other processing at the site where the article to be treated is used, the optical cathodic protection coating structure Ru can make.
図１は、本発明の実施に使用したウオームスプレー用ガンの概要であって、燃料と酸素とを燃焼室（１）に圧入する燃料供給口（２）と酸素供給口（３）を有し、その燃焼室（１）の出口であるノズル（４）近くには、前記燃焼室（１）に不活性ガスを供給する口（５）を設けてある。このようにして、前記不活性ガスの圧入の増減に反比例して、前記酸素と燃料の供給量を増減し、前記ノズル（４）からのガス噴出スピードを余り変動しないようにしながら、その温度を４×１０２〜２５×１０２℃の範囲で調整できるようにしてある。 FIG. 1 is an outline of a worm spray gun used in the practice of the present invention, and has a fuel supply port (2) and an oxygen supply port (3) for press-fitting fuel and oxygen into a combustion chamber (1). A port (5) for supplying an inert gas to the combustion chamber (1) is provided near the nozzle (4) which is the outlet of the combustion chamber (1). In this way, the supply amount of the oxygen and fuel is increased and decreased in inverse proportion to the increase and decrease of the press-fitting of the inert gas, and the temperature is adjusted while keeping the gas ejection speed from the nozzle (4) from fluctuating much. It can be adjusted in the range of 4 × 10 2 to 25 × 10 2 ° C.
また、集合粒子径は、下記実施例に限られるものではなく、最大１００μｍまで可能である。
この粒子径が大きくなるに連れ、集合粒子の作成が困難になる。また、吹き付けた層にむらが生じやすくなる。
また、その糊剤としてはＰＶＡに限らず、アクリル系、ポリエステル系、ポリウレタン系などの従来一般に知られた糊剤を使用することが出来る。また、デンプン質からなる天然又は半合成の糊剤の使用も可能である。
Further, the aggregate particle diameter is not limited to the following examples, and can be up to 100 μm.
As the particle size increases, it becomes difficult to create aggregate particles. Further, unevenness is likely to occur in the sprayed layer.
The paste is not limited to PVA, and conventionally known pastes such as acrylic, polyester, and polyurethane can be used. It is also possible to use natural or semi-synthetic glues made of starch.
光触媒として機能する結晶としては、下記実施例に示す酸化チタンに限らず、酸化亜鉛、酸化タングステン、酸化鉄、チタン酸ストロンチウム、硫化カドミウムなどを用いることが可能である。
また、その結晶粒径も下表１に示したものに限らず、７ｎｍ〜１μｍ以下のものが好ましい。
なお、１μｍを超える大きなものになると触媒活性が著しく低下する恐れがある。
図２は、粒子径の発電能力との関係を示すグラフである。
任意の電位（例えば５００ｍＶ）における電流（Ｃｕｒｒｅｎｔ）は光カソード防食電流に相当するアノード電流を間接的に示すものである。すなわち、この電流が大きいほど、光カソード電流が大きく取れる可能性を示す。
従来手法（ＨＶＯＦ）で＜１μｍの粒子径を有するＴｉＯ２を用いて作製したコーティングに比べて、Ｗａｒｍ Ｓｐｒａｙを用いると同じ粒子径でも電流値は大きく、すなわち光カソード防食性能が向上する。さらに、ＷａｒｍＳｐｒａｙで粒子径を＜１００ｎｍとすると、光カソード防食電流はさらに１０倍近く大きくなっていることが分かる。
The crystal that functions as a photocatalyst is not limited to titanium oxide shown in the following examples, and zinc oxide, tungsten oxide, iron oxide, strontium titanate, cadmium sulfide, and the like can be used.
Further, the crystal grain size is not limited to those shown in Table 1 below, and those having a crystal grain size of 7 nm to 1 μm or less are preferable.
In addition, when it becomes a big thing exceeding 1 micrometer, there exists a possibility that catalyst activity may fall remarkably.
FIG. 2 is a graph showing the relationship between the particle size and the power generation capacity.
A current (Current) at an arbitrary potential (for example, 500 mV) indirectly indicates an anode current corresponding to the photocathode protection current. That is, the larger this current, the greater the possibility of taking a larger photocathode current.
Compared to the coating produced using TiO 2 having a particle size of <1 μm by the conventional method (HVOF), the current value is large even when the Warm Spray is used, that is, the photocathodic anticorrosion performance is improved. Furthermore, when the particle size is <100 nm in WarmSpray, it can be seen that the photocathode anticorrosion current is further increased by almost 10 times.
電子貯蔵材料として用いる結晶としては、酸化鉄に限らず、酸化バナジウム、酸化クロム、酸化マンガン、酸化コバルトなど複数の価数状態において安定で存在しうる遷移金属酸化物であって、電子貯蔵の際に、プロトン（H+）を一緒に取り込むことが可能なものであれば、使用可能である。
また、その結晶粒径も下表１に示したものに限らず、１０ｎｍ〜１μｍのものが使用可能である。
なお、１μｍを超える大きなものになると、電子貯蔵反応も表面積に依存するので、電子貯蔵能力が著しく低下する恐れがある。
図３は、フルタイム光カソード防食コーティングにおける電子貯蔵材料（Ｆｅ２Ｏ３）の充放電特性を示すグラフである。
電流（Ｃｕｒｒｅｎｔ）がマイナス方向にピークが現れているのが充電作用を示しており、ピーク高さが大きいほど、充電容量が大きいことを示す。プラス方向は放電作用を示す。ピーク高さは放電容量に相当する。従来手法（ＨＶＯＦ）で＜１μｍの粒子径を有するＦｅ２Ｏ３を用いて作製したコーティングに比べて、Ｗａｒｍ Ｓｐｒａｙを用いると同じ粒子径でもピークは大きく、すなわち充放電容量が大きくなる。さらに、ＷａｒｍＳｐｒａｙで粒子径を＜１００ｎｍとすると、充放電容量は２倍以上に大きくなっていることが分かる。
The crystals used as the electron storage material are not limited to iron oxide, but are transition metal oxides that can exist stably in a plurality of valence states, such as vanadium oxide, chromium oxide, manganese oxide, and cobalt oxide. In addition, any substance that can incorporate protons (H +) together can be used.
Further, the crystal grain size is not limited to those shown in Table 1 below, and those having a grain size of 10 nm to 1 μm can be used.
In addition, when it becomes a big thing exceeding 1 micrometer, since an electron storage reaction also depends on a surface area, there exists a possibility that an electron storage capability may fall remarkably.
FIG. 3 is a graph showing charge / discharge characteristics of an electron storage material (Fe 2 O 3 ) in a full-time photocathode anticorrosion coating.
A peak in the negative direction of the current (Current) indicates the charging action, and the larger the peak height, the larger the charging capacity. A positive direction indicates a discharge action. The peak height corresponds to the discharge capacity. Compared to the coating prepared using Fe 2 O 3 having a particle diameter of <1 μm by the conventional method (HVOF), the peak is large even when using the Warm Spray, that is, the charge / discharge capacity is increased. Furthermore, when the particle diameter is <100 nm in WarmSpray, it can be seen that the charge / discharge capacity is more than doubled.
下表１の示すように、光触媒用の酸化チタン結晶と電子貯蔵材料である酸化鉄結晶を混合して直径２５〜９０μｍの集合粒子を作成した。（図４、５）
集合粒子を固化するために糊剤として、ＰＶＡを用いた。集合粒子は、糊剤を２質量％結晶混合体に混合して、スプレードライ法にて造粒したものである。
このようにして造粒した集合粒子をウオームスプレー用ガンを用い下表１に条件で基材に吹き付け付着させた。
集合粒子は、付着と同時に破砕され、形成された層はほぼ均一なバラツキで、両結晶が存在した。（図６、７）
下表１において、結果１）２）の○、◎の意味は以下の通りである。
１）◎：光触媒作用高い
１）○：光触媒作用あり
２）◎：電子貯蔵作用高い
２）○：電子貯蔵作用あり
PVA was used as a paste to solidify the aggregated particles. Aggregated particles are obtained by mixing a paste with 2% by mass of a crystal mixture and granulating it by a spray drying method.
The aggregated particles thus granulated were sprayed and adhered to the base material under the conditions shown in Table 1 below using a warm spray gun.
The aggregated particles were crushed simultaneously with the adhesion, and the formed layer was almost uniform and both crystals were present. (Figs. 6 and 7)
In Table 1 below, the meanings of ○ and ◎ in results 1) and 2) are as follows.
1) A: High photocatalytic activity 1) ○: Photocatalytic activity 2) A: High electron storage activity 2) ○: Electron storage activity
鋼橋などの鋼構造物の防食のみならず、容器内の雰囲気制御が重要であるために、通常の犠牲防食システムは採用できない。一方、ステンレス鋼などの高耐食性材料は確率的な局部腐食の危険性を秘めている原子力発電施設等における放射性物質格納容器の防食などに有効に使用できる。 Since it is important not only to prevent corrosion of steel structures such as steel bridges but also to control the atmosphere in the container, a normal sacrificial corrosion protection system cannot be adopted. On the other hand, highly corrosion-resistant materials such as stainless steel can be effectively used for anticorrosion of radioactive substance storage containers in nuclear power generation facilities and the like that have the risk of stochastic local corrosion.
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