WO1992021786A1 - Process for forming passive film on stainless steel, and stainless steel and gas- and liquid-contacting part - Google Patents
Process for forming passive film on stainless steel, and stainless steel and gas- and liquid-contacting part Download PDFInfo
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- WO1992021786A1 WO1992021786A1 PCT/JP1992/000699 JP9200699W WO9221786A1 WO 1992021786 A1 WO1992021786 A1 WO 1992021786A1 JP 9200699 W JP9200699 W JP 9200699W WO 9221786 A1 WO9221786 A1 WO 9221786A1
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- gas
- stainless steel
- passivation film
- treatment
- film
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Classifications
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- 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
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/80—After-treatment
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D6/00—Heat treatment of ferrous alloys
- C21D6/002—Heat treatment of ferrous alloys containing Cr
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- 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
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/02—Pretreatment of the material to be coated
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
Definitions
- the present invention relates to a method for forming a passive film of stainless steel, stainless steel, and gas-contact and liquid-contact parts, and is particularly suitable for ultra-high vacuum equipment, ultra-high cleaning equipment, ultra-pure water equipment, etc.
- the present invention relates to a method for forming a passivation film of an oxidized passivated stainless steel, which can be applied to stainless steel, and stainless steel and gas-contact and liquid-contact parts.
- the dimensions of unit elements are shrinking year by year as LSIs become more highly integrated, and semiconductors with dimensions of 1 / m to sub-micron and less than 0.5 ⁇ Research and development of devices are being actively pursued for practical use.
- a step of forming a thin film, a step of etching the formed thin film into a predetermined circuit pattern, and the like are repeatedly performed. These processes are usually performed in an ultra-high vacuum state or a reduced-pressure atmosphere in which a predetermined gas is introduced. If impurities are mixed in these steps, problems such as deterioration of the film quality of the formed thin film and inability to obtain the precision of fine processing occur. This is why semiconductor manufacturing processes require ultra-high vacuum and ultra-high clean pressure reduction atmospheres.
- FIG. 16 shows the relationship between the total system leakage (the sum of the amount of gas released from the piping system and the inner surface of the reaction chamber and the external leakage) of the system combined with the gas piping system and the reaction chamber in the conventional system, and the gas contamination. It is a graph shown. The multiple lines in the figure show the relationship between the impurity concentration in the atmosphere and the total leak amount of the system when the gas flow rate was changed to various values. -.
- the present inventor has invented an ultra-clean gas Kyoawase system, successfully Mukoto come suppressing leakage amount from the outside of the system the detection limit of the current detector lx ⁇ 0- 11 below To rr ⁇ lZs ec ing.
- leakage from the inside of the system that is, the release of gas from the surface of stainless steel as described above, could not reduce the impurity concentration in the reduced-pressure atmosphere as a result.
- the minimum value of the current surface discharge gas amount obtained by the surface treatment in ultra high vacuum technology in the case of stainless steel, a 1 x 10- 11 T orr ⁇ 1 / sec ⁇ cm 2.
- the surface area exposed to the inside of the chamber for example, even were the smallest observed Seki' and lm 2, 1 X 10 is total "'To rr - Ri Do the leakage amount of 1 / sec, the gas flow rate 10 In the case of cc / min, only gas with an impurity concentration of about 1 pm can be obtained, and if the gas flow rate is further reduced, it goes without saying that the purity is further reduced.
- the stainless steel Degassing from the surface is required to be 1 X 1 0- 15 T orr ⁇ l Z sec ⁇ cm 2 or less. Therefore, there was a strong demand for a technology for treating the surface of stainless steel to reduce the amount of outgassing.
- a relatively stable general gas (0 2, ⁇ 2, A r, H 9, H e) reactivity from a wide variety of gases are used to strong specialty gases corrosive and toxic You.
- some specialty gases such as hydrogen chloride (HC 1), chlorine (C 1 2), boron trichloride (BC 1 3), as such as boron trifluoride (BF q), in the atmosphere If water is present ⁇
- HC 1 hydrogen chloride
- C 1 2 chlorine
- BC 1 3 boron trichloride
- BF q boron trifluoride
- stainless steel is used for piping and chamber materials that handle these gases because of its corrosion resistance, high strength, ease of secondary workability, ease of welding, and ease of inner surface polishing. There are many.
- stainless steel has excellent corrosion resistance in an ultra-high purity atmosphere with a trace amount of moisture, but easily corrodes in a chlorine or fluorine gas atmosphere where moisture is present. For this reason, corrosion-resistant treatment is indispensable after stainless steel surface polishing.
- passivate film formation such as Ni-W-P coating (clean S-coating method) that coats stainless steel with highly corrosion-resistant metal or thin oxide film on metal surface in nitric acid solution
- cleaning S-coating method cleaning method
- an oxidized passivation film formed in a high-purity atmosphere having a water content of about 100 ppb is a passive film formed by a wet method as shown in FIG. b) Compared with), the degassing characteristics are improved. Power, degassing properties are still sufficient Rather, it has reached a point where it can be used as a material for ultra-high vacuum or ultra-high-clean decompression equipment.
- Figure 17 shows the concentration profile of each component atom in the depth direction measured by XPS (X ⁇ photoelectron spectroscopy), and Fig. 18 shows a scanning electron micrograph of the film surface.
- XPS X ⁇ photoelectron spectroscopy
- electropolishing is performed to smooth the surface before the passivation film is formed.
- the surface roughness that can be achieved by electropolishing is limited to Rmax O.05 to 0.1 m. A surface roughness of 0.5 m is used.
- a passivation film is formed after electropolishing, the surface roughness during electropolishing is not maintained and the surface becomes rough. For example, even if the surface of the base material (bulk portion) is finished to Rmax O.05 to 0.1 / m before forming the passivation film, if the passivation film is formed, the surface roughness of the passivation film becomes Rmax It becomes coarser than 0.1. C and surface roughness A stainless ⁇ the passivation film is formed is not currently exist Rmax 0.
- An object of the present invention is to provide a method of forming a passivation film of stainless steel, which achieves ultra-flatness and densification of a passivation film and is excellent in degassing characteristics and corrosion resistance, and a stainless steel and a gas contacting / wetting part.
- a first gist of the present invention is characterized in that after a surface of stainless steel is electropolished, the surface is oxidized in an oxidizing atmosphere gas, and then the iron oxide on the surface is reduced and removed by hydrogen gas. Present in stainless steel passivation film forming method.
- the second gist of the present invention is that the surface of stainless steel is electrolytically polished and then welded. After welding, the surface of the stainless steel is oxidized in an oxidizing atmosphere while heating the welded portion, and then the surface of the surface is oxidized with hydrogen gas.
- a method for forming a passivation film of stainless steel which comprises reducing and removing iron oxide.
- a third aspect of the present invention resides in a stainless steel having a passivation film having a surface roughness of Rmax 0.1 m or less.
- the fourth gist of the present invention is to provide a stainless steel formed by subjecting a surface of stainless steel to electrolytic polishing, oxidizing in an oxidizing atmosphere gas, and subsequently reducing and removing iron oxide on the surface with hydrogen gas. It is present in gas contact parts and liquid contact parts characterized by having a steel passivation film on the surface. Function and example of embodiment
- electropolishing is performed before forming a passivation film.
- a composite electrolytic polishing method may be used.
- the composite electrolytic polishing method is a method in which anodically polished metal to be polished is electrolytically eluted by electrolysis, and a passivated oxide film formed on the surface of the polished metal is mirror-finished by abrasion action of abrasive grains.
- the thickness is 0.05 to 0.1 m.
- Figure 2 shows the change in surface state due to electrolytic polishing.
- Fig. 2 (a) shows the surface condition after polishing
- Fig. 2 (b) shows the surface condition before polishing.
- C As can be seen from Fig. 2, large irregularities in the crystal grains were observed before polishing. Yes, even if an oxidation passivation film is formed in this state, a continuous film cannot be obtained, resulting in a film having poor corrosion resistance. Further, since moisture and the like are absorbed and absorbed between the crystal grains, a film having good degassing properties cannot be obtained. By performing the electropolishing treatment, the surface becomes uneven and the surface becomes smooth. As a result, the surface area is reduced, and the amount of adsorbed and stored moisture is greatly reduced.
- a passivation film forming process immediately preferable that said hot base one king before passivation film formation step t, 0 the hot base one King passivated If performed before the film formation treatment, the chromium concentration on the stainless steel surface side increases, and a dense, highly corrosion-resistant passivation film is formed.
- Hot base one King preprocessing is performed, for example A r, H e, in an inert gas atmosphere such as X 9 gas.
- the time is preferably 1 to 10 hours.
- the processing temperature is preferably from 300 to 600 ° C, more preferably from 400 to 520 ° C. When performed within a temperature range of 400 to 52 ° C, surface roughness is further suppressed, and the formed oxide passivation film becomes denser than when performed at other temperature ranges, and degassed. The characteristics are further improved.
- An oxidation passivation film is also formed in this high-temperature baking. Baking is performed in an inert gas atmosphere. Although the reason why the oxygen passivation film is formed on the surface in spite of baking in an inert gas atmosphere (ie, an atmosphere containing no oxygen) is not always clear, it is not clear by electropolishing. It is thought that an oxide layer formed on the surface of the stainless steel, and the oxygen in the layer is a source of oxygen for the formation of a passivation film. Also formed by high temperature baking The surface roughness of the passivation film after the electropolishing is maintained. The thickness of this passivation film varies depending on the baking temperature, which varies with time.For example, in the case of 500 ° C x 10 hours, the thickness becomes about 3 OA. It can be put to practical use in a state.
- Oxidation Forms a passive film.
- a layer containing a large amount of chromium oxide is formed on the stainless steel surface, and a layer containing a large amount of iron oxide is formed thereon.
- the layer containing much iron oxide is a porous film having cracks and pinholes as described above. The degree of such cracks and pinholes varies depending on the amount of water in the oxidizing atmosphere, and the smaller the water content, the better.
- the oxidizing gas is exhausted, and then hydrogen gas is introduced to reduce and remove the passivation outermost layer.
- hydrogen gas is introduced to reduce and remove the passivation outermost layer.
- the hydrogen concentration in the hydrogen processing gas is 0.1 p ⁇ ⁇ ! ⁇ 10% is preferred, and 0.5 ⁇ 100 ppm is more preferred. In the range of 0.5 to 100 ppm, a dense passivation film having better degassing properties is formed.
- the temperature of the hydrogen treatment is preferably from 200 to 500 ° C, more preferably from 300 to 400 ° C. In this range, the hydrogen embrittlement of stainless steel is suppressed, and a passivation film containing chromium oxide as a main component and having good degassing properties can be obtained.
- the surface roughness of the passivation film produced as described above is extremely smooth.For example, after finishing to 0.05 to 0.1 Zm by electrolytic polishing, Then, if hydrogen gas treatment is performed, a passivation film with a surface roughness of 0.01 zm or less can be obtained.
- the concentration of oxide on the outermost surface of the thermally oxidized passivation film is further increased, and a stainless steel having a passivation film having more excellent corrosion resistance is obtained. can get.
- Annealing is preferably performed at 200 to 500 ° C for 1 to 10 hours, and by performing annealing under these conditions, the surface state of the thermal oxidation passivation film becomes smoother and the chromium oxide concentration on the outermost surface is increased. The corrosion resistance is further improved.
- the inert gas used for the annealing treatment is, for example, Ar, He, X. Isostatic, used.
- a passivation film is formed in an oxidizing atmosphere gas.
- the stainless steel or the stainless steel on which the passivation film is formed by performing the above-described high-temperature baking in an inert gas atmosphere after subjecting the surface of the stainless steel to the electrolytic polishing treatment the surface of the welded portion becomes However, it was found that the film was covered with a passivation film containing more Fe oxide than before welding (Fig. 4).
- a passivation film containing a large amount of Cr oxide can be formed on the welded portion by forming and subsequently reducing and removing iron oxide on the surface with hydrogen gas.
- the surface roughness of the passivation film of the weld formed by method 2 is less than RniaxO. 1 zm.
- the surface roughness is R m . ..0. 1 or less
- Stainless steel having a certain passivation film can be easily produced.
- the method of (1) is a method of finishing the surface roughness to 0.05 to l ⁇ m by electrolytic polishing and performing the high-temperature baking described above.
- the passivation film is formed even by high-temperature baking, and the surface roughness during electrolytic polishing is also maintained by high-temperature baking as described above. . Therefore, if high-temperature baking is performed after electrolytic polishing to a surface roughness of 0.05 to 0.1 / m, a passive film having a surface roughness of 0.05 to 0.1 zm can be obtained.
- this passivation film is extremely rich in chromium and has not less than CrZFe; L. In addition, it has achieved CrZFe of nearly 7 (see Fig. 5). It is a dynamic membrane. -After all, this stainless steel has a surface roughness R m ⁇ . ⁇ It is extremely excellent in degassing because it is less than Y 0.lm and has a dense passive film.
- Another method is a method in which the surface of stainless steel is finished to a surface roughness of RmaxO.05 to 0.0 by electrolytic polishing, and the above-described hydrogen gas treatment (high-temperature baking may be performed before hydrogen gas treatment) is performed. is there.
- a stainless steel having a passivation film having a surface roughness of RmaxO.01 or less can also be produced.
- the Cr / Fe on the passivated surface after the hydrogen gas treatment is larger than the CrZFe on the base metal (see Fig. 6, for example, CrZFe is 0.35 in Fig. 6 (a)). Therefore, stainless steel with excellent degassing properties and corrosion resistance can be obtained.
- the stainless steel of the present invention is, for example, a Fe—Cr system or a Fe—Cr—Ni system.
- the structure may be any of ferritic, martensite, and austenitic stainless steels. S US 316 is particularly preferred.
- the passivated stainless steel produced by the above-described passivation film forming method of the present invention exhibits extremely good degassing characteristics and corrosion resistance, and is used as a constituent material of an ultra-vacuum device, an ultra-high clean pressure reducing device, and the like. It can be used.
- Passivated stainless steel produced by the passivation film forming method of the present invention described above Shows extremely good degassing properties and corrosion resistance, and is suitably used for gas contact parts.
- the stainless steel according to the present invention can be suitably used for liquid contact parts such as a liquid supply pipe and a liquid storage tank.
- a gas supply line system that supplies gas from a gas cylinder to a gas use point such as a film forming apparatus generally has a configuration as shown in FIG.
- 100 is a gas cylinder
- 101 is a gas cylinder valve
- 102 is a regulator
- 110 is a valve
- 104 is an integrated branch valve
- 105 is a mass flow controller.
- Reference numeral 106 denotes a film forming apparatus
- 107 denotes a pipe
- 108 denotes a filter.
- Examples of c- contacting gas parts include a gas cylinder valve, a pressure gauge, a regulator, a lube, a lube, a mass flow controller, and a finole.
- parts such as evening and reguriyu or components constituting these parts include, for example, a valve seat, a valve chamber, a valve body, a diaphragm, a seal ring, and a stem.
- Fig. 8 As the cylinder valve, for example, one having a structure shown in Fig. 8 is exemplified (Japanese Utility Model Laid-Open No. 1-178281).
- Fig. 9 shows a pressure gauge
- Fig. 10 shows a regular valve
- Fig. 11 shows a valve
- Fig. 12 shows a masuff unit controller.
- the surface roughness of the diaphragm is preferably small from the viewpoint of sealing properties.
- elasticity is required to provide deflection.
- the surface roughness is Rmax O. 1 m or less, the sealing property is extremely good.
- a metal having a passivation film is inferior in elasticity to a metal having no passivation film.
- a conventional passivation film was formed in a fatigue test. Excellent fatigue strength compared to stainless steel. Further, in the case of the stainless steel in which the conventional passivation film was formed, a force in which small cracks were observed on the surface was observed.In the case of the stainless steel according to the present invention, a force in which such cracks were not observed, I got it.
- valves such as gas cylinder cylinder valves
- good sealing performance is required.
- the valve of the present invention has better sealing performance than a conventional valve having a passivation film on the gas contact surface, and has a leak.
- the volume has dropped sharply, making it possible to supply ultra-high purity gas.
- a pure water supply pipe was made from the stainless steel according to the present invention, ultrapure water having a specific resistance of about 18 ⁇ cm was supplied into the pipe, and the specific resistance at the outlet was measured. Had not changed.
- Figure 1 shows the degassing characteristics of the oxidized passivated stainless steel tubes manufactured by various methods. rough.
- Fig. 2 is a scanning electron microscope showing the inner surface condition of the stainless steel tube before and after the electrolytic polishing treatment.
- Fig. 3 is a scanning electron microscope photograph showing the inner surface condition of the stainless steel tube after the electrolytic polishing.
- Figure 4 is a graph showing the depth profile in XPS after the weld.
- Fig. 5 is a graph showing XPS depth profile of the electropolished surface after baking in an Ar gas atmosphere.
- Figure 6 shows the depth profile of XPS on the thermal oxidation passivation film surface after hydrogen reduction treatment.
- FIG. 7 is a conceptual diagram showing a gas supply line system.
- FIG. 8 is a sectional view of a cylinder valve according to one embodiment of the present invention.
- FIG. 9 is a sectional view of a pressure gauge according to one embodiment of the present invention.
- FIG. 10 is a cross-sectional view of one embodiment of the present invention.
- FIG. 11 is a sectional view of a valve according to one embodiment of the present invention.
- FIG. 12 is a cross-sectional view of a mass flow controller according to one embodiment of the present invention.
- C FIG. 13 shows an inner surface state of a stainless steel tube after baking in an Ar gas atmosphere.
- Figure 14a shows the surface state of the thermal oxidation passivation film after hydrogen reduction treatment for 10 minutes.
- Figure 14b shows the surface state of the thermal oxidation passivation film after hydrogen reduction treatment for 30 minutes.
- Figure I5 shows the XPS depth profile of the thermal oxidation passivation film surface after Ar annealing treatment. The graph shown.
- Figure 16 shows impurities in atmospheric gas at various gas flow rates in the conventional device.
- 5 is a graph showing a relationship between a concentration and a system leak amount.
- Fig. 17 shows the concentration profile in the depth direction by XPS of the surface of a thermally oxidized passivation film produced by a conventional thermal oxidation method.
- Fig. 18 shows a scanning electron microscope showing the surface state of a thermally oxidized passivation film fabricated by the conventional method.
- a 2m 3/8 "diameter SUS 316L stainless steel tube is electrolytically polished and the surface is a mirror surface with a maximum difference of unevenness (R mnv ) of 0.05 ⁇ m within a circumference of 5m radius.
- This surface state is a smooth surface with grain boundaries as shown in Fig. 3.
- FIG. 13 shows the state of the stainless steel inner surface after heat treatment at various temperatures. As can be seen from Fig. 13, the stainless steel surface remains The mirror surface after polishing was maintained. That, R max 0. 05 was maintained.
- Figure 5 shows the results of XPS measurement of the inner surface of a stainless steel tube baked at 500 ° C. By the above baking treatment, chromium atoms increased on the surface side and iron atoms decreased, and the composition ratio of chromium and iron was reversed from that in the bulk.
- the intersection of the Fe line and the 0 line is the interface between the bulk (base material) and the passivation film.
- the thickness of the passivation film shown in Fig. 5 is about 3 OA.
- about 22 A from the surface (the left end of the graph in Fig. 5) has more chromium oxide than iron oxide. . ..
- FIG. 14 (a) shows the case of hydrogen gas treatment time of 10 minutes
- Fig. 14 (b) Fig. 14 shows the case where the hydrogen gas treatment time is 30 minutes
- the surface of the passive film subjected to the hydrogen reduction treatment has an acid. No cracks and pinholes were observed after the treatment, and the surface became flat, while a high concentration of chromium oxide was present in the passivation film, as shown in Fig. 6, and chromium atoms with respect to iron The ratio was much larger than that in the base metal.
- the thickness of the passivation film shown in FIGS. 6 (a) and 6 (b) was about 6 OA.
- the surface roughness of the passivation film was measured and found to be R maY 0.01 m.
- the hydrogen reduction treatment time is not adversely is little influence on the surface condition and the depth direction of the concentration Brophy Le passivation film, then c was found that the reduction reaction in about 10 minutes is finished, more passivating Test the degassing characteristics of the treated stainless steel tube. Test was carried out. After leaving the stainless steel tube in a clean room at a relative humidity of 50% and a temperature of 20 ° C for one week, Ar gas was flowed at a flow rate of 1.21 / min, and the amount of water contained in the Ar gas was measured at the pipe outlet. (Atmospheric pressure ion mass spectrometer). The results are shown in Fig. 1 (d). After 20 minutes, the water content in the Ar gas was reduced to 1 Oppb, and after 30 minutes it was below the background level of 3 ppb.
- Example 1 an oxidized passivated stainless steel tube was prepared in the same manner as in Example 1 except that the baking treatment in an Ar atmosphere was omitted, and the degassing characteristics were evaluated. The results are shown in Fig. 1 (e).
- the temperature of the hydrogen reduction treatment was set to 600 ° C, and the other treatment conditions were the same as in Example 1, an oxidation passivation film was formed on the inner surface of the stainless steel tube, and the same evaluation was performed.
- the hydrogen reduction treatment gas was 20% hydrogen-containing Ar gas, and other treatment conditions were the same as in Example 1, an oxidation passivation film was formed on the inner surface of the stainless steel tube, and the same evaluation was performed.
- the results are shown in Fig. 1 (g).
- the surface of the passivation film is slightly roughened, and the degassing characteristics are inferior to those of Examples 1 and 2.
- the water content is reduced to 3 ppb in about 70 minutes after gas passage, and is clearly improved compared to the conventional example. Was done.
- the oxidizing atmosphere is an ultra-high-purity atmosphere with a water concentration of 5 ppb.
- An acid-passivated stainless steel tube was prepared in the same manner as in Example 1, and its degassing properties were evaluated. The result is as shown in h) of Fig. 1. After 10 minutes of gas flow, the water content in the Ar gas was below the background level of 3 ppb, and even with the current highest level membrane, the treatment in this example could improve the gas performance. Do you get it.
- Figures 15 (a) to 15 (f) show the depth concentration profile of XPS on the surface of the thermal oxidation passivation film.
- the oxidation passivation film of this example has improved corrosion resistance due to an increase in the chromium concentration on the outermost surface, and exhibits extremely good corrosion resistance even with a strongly corrosive solution of 36% HC ⁇ .
- the present invention it is possible to form a passivation film having extremely excellent degassing properties and corrosion resistance, and to provide an oxidized passivated stainless steel applicable to an ultra-high vacuum, ultra-high clean pressure reducing device, and the like. It is possible to do.
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Abstract
Description
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Priority Applications (2)
Application Number | Priority Date | Filing Date | Title |
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EP19920917389 EP0596121A4 (en) | 1991-05-28 | 1992-05-28 | Process for forming passive film on stainless steel, and stainless steel and gas- and liquid-contacting part. |
JP51015992A JP3181053B2 (en) | 1991-05-28 | 1992-05-28 | Method for forming passive film on stainless steel, and stainless steel and fluid contact parts |
Applications Claiming Priority (6)
Application Number | Priority Date | Filing Date | Title |
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JP15246691 | 1991-05-28 | ||
JP3/152466 | 1991-05-28 | ||
JP19871891 | 1991-07-12 | ||
JP3/198718 | 1991-07-12 | ||
JP3/212592 | 1991-07-30 | ||
JP3212592A JP3045576B2 (en) | 1991-05-28 | 1991-07-30 | Method of forming passive film on stainless steel and stainless steel |
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WO1992021786A1 true WO1992021786A1 (en) | 1992-12-10 |
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EP (1) | EP0596121A4 (en) |
JP (2) | JP3045576B2 (en) |
WO (1) | WO1992021786A1 (en) |
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JP6502225B2 (en) * | 2015-09-30 | 2019-04-17 | 日本特殊陶業株式会社 | Ceramic heater and method of manufacturing the same |
TWI816829B (en) * | 2018-07-06 | 2023-10-01 | 日商富士軟片股份有限公司 | Member, container, chemical solution accommodating body, reaction container, distillation column, filter unit, storage tank, pipeline, method for manufacturing chemical solution |
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JPS6431956A (en) * | 1987-07-25 | 1989-02-02 | Tadahiro Omi | Manufacture of stainless steel member for semiconductor-manufacturing equipment |
JPH0243353A (en) * | 1988-08-04 | 1990-02-13 | Tadahiro Omi | Device and method for metal oxidation treatment |
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US3345218A (en) * | 1964-04-02 | 1967-10-03 | Owens Illinois Inc | Preoxidation of stainless steel for glass-to-metal sealing |
US4078949A (en) * | 1976-09-02 | 1978-03-14 | United States Steel Corporation | Method for improving the surface quality of stainless steels and other chromium-bearing iron alloys |
US4661171A (en) * | 1984-08-29 | 1987-04-28 | Shinko-Pfaudler Company, Ltd. | Method for treating the surface of stainless steel by high temperature oxidation |
JPH0192389A (en) * | 1987-09-30 | 1989-04-11 | Aichi Steel Works Ltd | Method for preventing surface roughening of stainless steel wire rod during pickling |
DE3804359C1 (en) * | 1988-02-12 | 1988-11-24 | Thyssen Edelstahlwerke Ag, 4000 Duesseldorf, De | |
JP2862546B2 (en) * | 1988-11-21 | 1999-03-03 | 神鋼パンテック株式会社 | Equipment piping materials for ultrapure water production and supply equipment |
US5051140A (en) * | 1989-03-23 | 1991-09-24 | Mitsubishi Jidosha Kogyo Kabushiki Kaisha | Surface treatment method for titanium or titanium alloy |
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1991
- 1991-07-30 JP JP3212592A patent/JP3045576B2/en not_active Expired - Lifetime
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1992
- 1992-05-28 EP EP19920917389 patent/EP0596121A4/en not_active Withdrawn
- 1992-05-28 WO PCT/JP1992/000699 patent/WO1992021786A1/en not_active Application Discontinuation
- 1992-05-28 JP JP51015992A patent/JP3181053B2/en not_active Expired - Lifetime
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JPS6431956A (en) * | 1987-07-25 | 1989-02-02 | Tadahiro Omi | Manufacture of stainless steel member for semiconductor-manufacturing equipment |
JPH0243353A (en) * | 1988-08-04 | 1990-02-13 | Tadahiro Omi | Device and method for metal oxidation treatment |
Non-Patent Citations (1)
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO1994023816A1 (en) | 1993-04-14 | 1994-10-27 | Nippon Sanso Corporation | Dissolved oxygen reducing apparatus |
EP0646400A4 (en) * | 1993-04-14 | 1997-05-07 | Nippon Oxygen Co Ltd | Dissolved oxygen reducing apparatus. |
WO1995018246A1 (en) * | 1993-12-30 | 1995-07-06 | Tadahiro Ohmi | Stainless steel and piping system |
JPWO2017188209A1 (en) * | 2016-04-28 | 2019-02-14 | 富士フイルム株式会社 | Purification apparatus, purification method, manufacturing apparatus, chemical manufacturing method, container, and chemical container |
Also Published As
Publication number | Publication date |
---|---|
JP3045576B2 (en) | 2000-05-29 |
JP3181053B2 (en) | 2001-07-03 |
JPH10204526A (en) | 1998-08-04 |
EP0596121A1 (en) | 1994-05-11 |
EP0596121A4 (en) | 1994-11-23 |
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