CN102146559B - Vulcanization method for NiW alloy baseband surface used for coating conductor - Google Patents
Vulcanization method for NiW alloy baseband surface used for coating conductor Download PDFInfo
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- CN102146559B CN102146559B CN2011100564123A CN201110056412A CN102146559B CN 102146559 B CN102146559 B CN 102146559B CN 2011100564123 A CN2011100564123 A CN 2011100564123A CN 201110056412 A CN201110056412 A CN 201110056412A CN 102146559 B CN102146559 B CN 102146559B
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- ammonium sulfide
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Abstract
The invention discloses a vulcanization method for a NiW alloy baseband surface used for a coating conductor. The method comprises the following steps of: performing vulcanization treatment on the NiW alloy baseband surface by adopting ammonium sulfide solution serving as a sulfur source; soaking a NiW alloy baseband in the ammonium sulfide solution for adsorbing sulfur; and performing desulfurization heat treatment. By the vulcanization method, the conventional limitation that an ultra-high vacuum environment is required for vulcanization treatment by taking sulfureted hydrogen as the sulfur source is overcome; and the vulcanization method has simple technical conditions and short treatment time, is simple to operate, contributes to reducing cost, and is suitable for batch vulcanization treatment of NiW long bands.
Description
Technical field
The invention belongs to the Metal Surface Modification Technique field, be specifically related to the vulcanization process on a kind of NiW alloy base belt for coated conductor surface.
Background technology
The NiW alloy is the required main body material of preparation YBCO coating conductor; Adopt the NiW alloy base band that possesses HS, low magnetic of rolling auxiliary biaxial texture technology (RABiTS) preparation; Carrier as coating conductor; Can play the effect of propping up an overfill protection, the texture template being provided, its surface quality and physicochemical property have significant effects for the high-quality oxide buffer layer of epitaxy.Therefore, research NiW alloy base band surface tissue to the epitaxy of steady oxide impact plies, improves the impact plies quality and has played critical effect.
When NiW alloy base band surface preparation oxide buffer layer; The orderly S atom in metal base band surface can form linking layer between oxide compound and metal base band, this orderly linking layer can be realized the control in the epontic oxide compound texture of metal base band.Therefore, carry out sulfidizing on Ni metal base band surface and help of the control of oxidation reinforced thing buffer film at the growth texture on metal base band surface.At present, great majority all concentrate on hydrogen sulfide as the sulphur source about form the research report of c (2 * 2)-S superstructure on Ni base band surface; The Ni base band through after certain vacuum-treat, is exposed in this gas again, makes the H desorption through the thermal treatment that is higher than 200 ℃ then; Promptly adopt method formation c (2 * the 2)-S superstructure of absorption back desorption earlier, this method needs strict UHV condition, is so limited; Cost is higher, is unfavorable for sulfidizing in batches.
Summary of the invention
Technical problem to be solved by this invention is the deficiency to above-mentioned prior art; Provide that a kind of technical qualification are easy, working method is simple; Do not need the restriction of ultra-high vacuum environment, be applicable to the surperficial vulcanization process of NiW alloy base belt for coated conductor of the batch sulfidizing of the long band of NiW.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is: the vulcanization process on a kind of NiW alloy base belt for coated conductor surface is characterized in that this method may further comprise the steps:
(1) ammonium sulfide is handled: the NiW alloy base band is used washed with de-ionized water, dewater with raw spirit then; It is 5%～8% ammonium sulfide solution that NiW alloy base band after the dehydration is put into mass concentration, takes out after soaking 20min～40min, washes the ammonium sulfide solution of surface attachment with deionized water, dries up for use;
(2) desulfurization thermal treatment: the NiW alloy base band after ammonium sulfide is handled in the step (1) is placed tube furnace; In temperature is under 800 ℃～850 ℃ conditions; Argon gas and hydrogen mixed gas protected down, furnace cooling obtains the NiW alloy base band that the surface has c (2 * 2)-S superstructure behind insulation 30min～40min.
The surfaceness of NiW alloy base band is not more than 5nm described in the above-mentioned steps (1).
The temperature of ammonium sulfide solution described in the above-mentioned steps (1) is 30 ℃～50 ℃.
Described in the above-mentioned steps (2) in the mixed gas volumn concentration of hydrogen be 4%, surplus is an argon gas.
The present invention compared with prior art has the following advantages:
1, the present invention adopts ammonium sulfide solution as the sulphur source sulfidizing to be carried out on NiW alloy base band surface, has overcome traditional hydrogen sulfide that utilizes and has carried out the limitation that sulfidizing needs ultra-high vacuum environment as the sulphur source.
2, vulcanization process technical qualification of the present invention are easy, working method is simple, and the treatment time is short, helps reducing cost, and are applicable to the batch sulfidizing of the long band of NiW.
Through embodiment, technical scheme of the present invention is done further detailed description below.
Description of drawings
Fig. 1 is the Auger electron spectrum figure (AES) of the preceding NiW alloy base band of sulfuration.
Fig. 2 is the Auger electron spectrum figure (AES) of the NiW alloy base band of the embodiment of the invention 1 after sulfuration.
Fig. 3 is that the NiW alloy base band of the embodiment of the invention 1 after sulfuration is at refletcion high-energy electron diffraction (RHEED) the detection figure of electron impact direction for < 100 >.
Fig. 4 is that the NiW alloy base band of the embodiment of the invention 1 after sulfuration is at refletcion high-energy electron diffraction (RHEED) the detection figure of electron impact direction for < 110 >.
Fig. 5 is the theoretical model figure of c (2 * 2)-S superstructure.
Embodiment
Embodiment 1
(1) ammonium sulfide is handled: the NiW alloy base band that surfaceness is not more than 5nm is used washed with de-ionized water, dewaters with raw spirit then; To put into mass concentration be 8% with the NiW alloy base band after the dehydration, and temperature is to take out after soaking 30min in 30 ℃ the ammonium sulfide solution, washes the ammonium sulfide solution of surface attachment with deionized water, dries up for use;
(2) desulfurization thermal treatment: the NiW alloy base band after ammonium sulfide is handled in the step (1) is placed tube furnace; In temperature is under 800 ℃ of conditions; (volumn concentration of hydrogen is 4% to the mixed gas of argon gas and hydrogen in the mixed gas; Surplus is an argon gas) to protect down, furnace cooling behind the insulation 30min obtains the NiW alloy base band that the surface has c (2 * 2)-S superstructure.
Fig. 2 is the Auger electron spectrum figure (AES) of the NiW alloy base band after the present embodiment sulfuration; Compare with the AES figure (Fig. 1) that vulcanizes preceding NiW alloy base band; Demonstrate the characteristic peak of element sulphur on the AES curve, explain that NiW base band sample is in the absorption that has produced element sulphur through surface after the sulfidizing.
Fig. 3 and Fig. 4 detect figure for the refletcion high-energy electron diffraction (RHEED) of the NiW alloy base band after the present embodiment sulfuration, and wherein the electron impact direction of Fig. 3 is < 100>direction, and the electron impact direction of Fig. 4 is < 110>direction.From figure, can find; Fringe spacing among Fig. 3 is 0.707 times of fringe spacing of Fig. 4, in conjunction with Fig. 5 the theoretical model of c (2 * 2)-S superstructure is analyzed, and the adjacent atom width between centers of the adjacent atom width between centers of < 100>direction and < 110>direction meets square edge and the relation of hypotenuse in the isosceles right triangle; According to Pythagorean theorem; This hypotenuse and square edge ratio are 0.707, and this result further specifies, and have formed c (2 * 2) superstructure of sulphur on the surface of NiW alloy base band.
NiW alloy base band behind the present embodiment sulfide modifier detects through Auger electron spectrum (AES) and refletcion high-energy electron diffraction (RHEED), has c (2 * 2)-S superstructure.
Embodiment 2
(1) ammonium sulfide is handled: the NiW alloy base band that surfaceness is not more than 5nm is used washed with de-ionized water, dewaters with raw spirit then; To put into mass concentration be 5% with the NiW alloy base band after the dehydration, and temperature is to take out after soaking 40min in 50 ℃ the ammonium sulfide solution, washes the ammonium sulfide solution of surface attachment with deionized water, dries up for use;
(2) desulfurization thermal treatment: the NiW alloy base band after ammonium sulfide is handled in the step (1) is placed tube furnace; In temperature is under 850 ℃ of conditions; (volumn concentration of hydrogen is 4% to the mixed gas of argon gas and hydrogen in the mixed gas; Surplus is an argon gas) to protect down, furnace cooling behind the insulation 35min obtains the NiW alloy base band that the surface has c (2 * 2)-S superstructure.
NiW alloy base band behind the present embodiment sulfide modifier detects through Auger electron spectrum (AES) and refletcion high-energy electron diffraction (RHEED), has c (2 * 2)-S superstructure.
Embodiment 3
(1) ammonium sulfide is handled: the NiW alloy base band that surfaceness is not more than 5nm is used washed with de-ionized water, dewaters with raw spirit then; To put into mass concentration be 7% with the NiW alloy base band after the dehydration, and temperature is in 40 ℃ the ammonium sulfide solution, takes out after soaking 20min, washes the ammonium sulfide solution of surface attachment with deionized water, dries up for use;
(2) desulfurization thermal treatment: the NiW alloy base band after ammonium sulfide is handled in the step (1) is placed tube furnace; In temperature is under 830 ℃ of conditions; (volumn concentration of hydrogen is 4% to the mixed gas of argon gas and hydrogen in the mixed gas; Surplus is an argon gas) to protect down, furnace cooling behind the insulation 40min obtains the NiW alloy base band that the surface has c (2 * 2)-S superstructure.
NiW alloy base band behind the present embodiment sulfide modifier detects through Auger electron spectrum (AES) and refletcion high-energy electron diffraction (RHEED), has c (2 * 2)-S superstructure.
The above; It only is preferred embodiment of the present invention; Be not that the present invention is done any restriction, every according to inventing technical spirit to any simple modification, change and equivalent structure variation that above embodiment did, all still belong in the protection domain of technical scheme of the present invention.
Claims (2)
1. the vulcanization process on NiW alloy base belt for coated conductor surface is characterized in that this method may further comprise the steps:
(1) ammonium sulfide is handled: the NiW alloy base band is used washed with de-ionized water, dewater with raw spirit then; It is 5%～8% ammonium sulfide solution that NiW alloy base band after the dehydration is put into mass concentration, takes out after soaking 20min～40min, washes the ammonium sulfide solution of surface attachment with deionized water, dries up for use; The surfaceness of said NiW alloy base band is not more than 5nm, and the temperature of said ammonium sulfide solution is 30 ℃～50 ℃;
(2) desulfurization thermal treatment: the NiW alloy base band after ammonium sulfide is handled in the step (1) is placed tube furnace; In temperature is under 800 ℃～850 ℃ conditions; Argon gas and hydrogen mixed gas protected down, furnace cooling obtains the NiW alloy base band that the surface has c (2 * 2)-S superstructure behind insulation 30min～40min.
2. the vulcanization process on a kind of NiW alloy base belt for coated conductor according to claim 1 surface is characterized in that, described in the step (2) in the mixed gas volumn concentration of hydrogen be 4%, surplus is an argon gas.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101109063A (en) * | 2007-09-05 | 2008-01-23 | 西北有色金属研究院 | Modifying processing method of vulcanizing surface of metallic base band for coating conductor |
| CN101250705A (en) * | 2008-04-01 | 2008-08-27 | 西南交通大学 | Method for manufacturing nickel-cuprum metallic baseband layer of highly oriented double-shaft texture |
| CN101330110A (en) * | 2008-08-01 | 2008-12-24 | 中南大学 | Light absorption layer material for film solar battery and preparation method thereof |
| US7816303B2 (en) * | 2004-10-01 | 2010-10-19 | American Superconductor Corporation | Architecture for high temperature superconductor wire |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7816303B2 (en) * | 2004-10-01 | 2010-10-19 | American Superconductor Corporation | Architecture for high temperature superconductor wire |
| CN101109063A (en) * | 2007-09-05 | 2008-01-23 | 西北有色金属研究院 | Modifying processing method of vulcanizing surface of metallic base band for coating conductor |
| CN101250705A (en) * | 2008-04-01 | 2008-08-27 | 西南交通大学 | Method for manufacturing nickel-cuprum metallic baseband layer of highly oriented double-shaft texture |
| CN101330110A (en) * | 2008-08-01 | 2008-12-24 | 中南大学 | Light absorption layer material for film solar battery and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 张永军等.涂层导体用金属基带研究进展.《稀有金属材料与工程》.2009,第38卷(第5期),第935-940页. * |
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