CN102154611A - Method for performing vulcanizing modification on surface of NiW alloy base band - Google Patents
Method for performing vulcanizing modification on surface of NiW alloy base band Download PDFInfo
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- CN102154611A CN102154611A CN 201110055300 CN201110055300A CN102154611A CN 102154611 A CN102154611 A CN 102154611A CN 201110055300 CN201110055300 CN 201110055300 CN 201110055300 A CN201110055300 A CN 201110055300A CN 102154611 A CN102154611 A CN 102154611A
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Abstract
The invention discloses a method for performing vulcanizing modification on the surface of a NiW alloy base band. In the method, after simple substance sulphur powder serving as a sulphur source is pressed to form a block, the block is put in a low-temperature area of a tube furnace to form sulphur steam; and the sulphur steam is carried to a high-temperature area of the tube furnace by utilizing current-carrying gas, and is subjected to adsorption and desorption with the surface of the NiW alloy base band positioned in the high-temperature area of the tube furnace to form a c(2*2)-S superstructure. In the method, vulcanizing is performed by taking the simple substance sulphur powder as the sulphur source, so the defect that the vulcanizing is performed by taking the hydrogen sulfide gas as the sulphur source under ultrahigh vacuum environment in the conventional method is overcome; and the technical condition of the method is simple and convenient, the method is easy to operate, and is favorable for reducing cost, and is suitable for the batch vulcanizing of NiW long bands, and processing time is short.
Description
Technical field
The invention belongs to the Metal Surface Modification Technique field, be specifically related to a kind of NiW alloy base band surface sulfide modifier method.
Background technology
The Ni alloy is one of main raw of YBCO used for coating conductor base band, wherein the NiW alloy owing to the low magnetic of its high strength and the characteristics that are easy to obtain cubic texture be subjected to paying close attention to widely.Numerous in the world research groups all adopt rolling auxiliary biaxial texture base band technology (RABiTS) preparation NiW alloy base band, promptly have the base band of sharp keen cubic texture by a series of aximal deformation value processing and recrystallize thermal treatment preparation.As the basis of epitaxy barrier layer and YBCO film, except cubic texture content and sharpness, the surface quality of base band and physicochemical property also will directly influence the growth of buffer layer and YBCO layer.Therefore, improve NiW alloy base band surface property, for the epitaxy of steady oxide buffer layer, to improve the buffer layer quality significant.
2000, Cantoni etc. discovered, can form (2 * 2) superstructure in the ab face on the Ni metal base band of surface clean.Result of study shows that single sulphur layer of chemisorption can form two kinds of ordered structures, p (2 * 2) structure and c (2 * 2) structure.To form p (2 * 2) structure when the fraction of coverage of S is 0.25 monoatomic layer, if when fraction of coverage reaches 0.5 monoatomic layer then form c (2 * 2) structure, this state also is a kind of saturated adsorbed state simultaneously.The crystallographic site of sulphur atom can form good coupling with the oxygen occupy-place in most oxide barrier layers material structures in c (2 * 2) structure, so utilize c (2 * 2)-S superstructure that S forms on base band surface effectively controlled oxidation thing barrier layer improve oxide barrier layers at base band surface forming core and growth conditions in the texture on base band surface.At present, great majority are about forming the research report of c (2 * 2)-S superstructure on Ni base band surface, all concentrate on hydrogen sulfide as the sulphur source, the Ni base band through after the vacuum-treat, is exposed in this gas again, make the H desorption by 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 at above-mentioned the deficiencies in the 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 NiW alloy base band surface sulfide modifier method of the batch sulfidizing of the long band of NiW.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of NiW alloy base band surface sulfide modifier method, it is characterized in that, this method adopts the elemental sulfur powder as the sulphur source, the cold zone that elemental sulfur powder briquetting is placed on tube furnace forms sulfur vapor, utilize current-carrying gas to bring sulfur vapor into the tube furnace high-temperature zone then, adsorb with the NiW alloy base band surface that is positioned at the tube furnace high-temperature zone, desorption formation c (2 * 2)-S superstructure, described current-carrying gas is the mixed gas of argon gas and hydrogen.
Above-mentioned a kind of NiW alloy base band surface sulfide modifier method, this method comprises following concrete steps:
(1) adopts thermopair that tube furnace is carried out the school temperature, demarcate 800 ℃～850 ℃ high-temperature zones and 115 ℃～125 ℃ cold zone positions in the stove respectively;
(2) get 6g～10g elemental sulfur powder and pack in the mould, under the pressure of 8MPa～11MPa, be pressed into block elemental sulfur, then block elemental sulfur is placed the cold zone of tube furnace described in the step (1) to form sulfur vapor;
(3) pending NiW alloy base band is placed the high-temperature zone of tube furnace described in the step (1), mixed gas with argon gas and hydrogen feeds in the tube furnace as current-carrying gas then, the drive that makes sulfur vapor pass through current-carrying gas imports the high-temperature zone and contacts with the NiW alloy base band, and furnace cooling obtains the NiW alloy base band that the surface has c (2 * 2)-S superstructure behind insulation 30min～50min.
Above-mentioned a kind of NiW alloy base band surface sulfide modifier method, the used sulphur powder of per 10 meters NiW alloy base bands surface sulfide modifier is no less than 1g.
Above-mentioned a kind of NiW alloy base band surface sulfide modifier method, the surfaceness of NiW alloy base band is not more than 5nm described in the step (3).
Above-mentioned a kind of NiW alloy base band surface sulfide modifier method, described in the step (3) in the mixed gas volumn concentration of hydrogen be 4%, surplus is an argon gas.
Above-mentioned a kind of NiW alloy base band surface sulfide modifier method, the Ventilation Rate of mixed gas is 150L/h described in the step (3).
The present invention compared with prior art has the following advantages:
1, the present invention adopts the elemental sulfur powder to carry out sulfidizing as the sulphur source, 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, sulfide modifier method and technology condition of the present invention is easy, working method is simple, and the treatment time is short, helps reducing cost, and is applicable to the batch sulfidizing of the long band of NiW.
Below by drawings and Examples, technical scheme of the present invention is described in further detail.
Description of drawings
Fig. 1 is the Auger electron spectrum figure (AES) of the NiW alloy base band before the sulfide modifier.
Fig. 2 is the Auger electron spectrum figure (AES) of the NiW alloy base band of the embodiment of the invention 1 behind sulfide modifier.
Fig. 3 is that the NiW alloy base band before the sulfide modifier is schemed for＜100〉direction refletcion high-energy electron diffraction (RHEED) detection in the electron impact direction.
Fig. 4 is that the NiW alloy base band of the embodiment of the invention 1 behind sulfide modifier schemed for＜100〉direction refletcion high-energy electron diffraction (RHEED) detection in the electron impact direction.
Fig. 5 is the theoretical model figure of c (2 * 2)-S superstructure.
Embodiment
Embodiment 1
(1) adopts thermopair that tube furnace is carried out the school temperature, demarcate 850 ℃ of high-temperature zones and 115 ℃ of cold zone positions in the boiler tube respectively;
(2) get 6g elemental sulfur powder and pack in the mould, adopt spreader bar or cold isostatic press under the pressure of 8MPa, to be pressed into block elemental sulfur, then block elemental sulfur is placed the cold zone of tube furnace described in the step (1) to form sulfur vapor;
(3) the NiW alloy base band (the used sulphur powder of per 10 meters NiW alloy base bands surface sulfide modifier is no less than 1g) that pending surfaceness is not more than 5nm places the high-temperature zone of tube furnace described in the step (1), (volumn concentration of hydrogen is 4% in the mixed gas with the mixed gas of argon gas and hydrogen then, surplus is an argon gas) feed in the tube furnace as the Ventilation Rate of current-carrying gas with 150L/h, the drive that makes sulfur vapor pass through current-carrying gas imports the high-temperature zone and contacts with the NiW alloy base band, and furnace cooling obtains the NiW alloy base band that the surface has c (2 * 2)-S superstructure behind the insulation 40min.
Fig. 2 is the Auger electron spectrum figure (AES) of the NiW alloy base band of present embodiment behind sulfide modifier, compare with the AES figure (Fig. 1) of NiW alloy base band before the sulfide modifier, demonstrate the characteristic peak of element sulphur on the AES curve, illustrate that NiW base band sample is in the absorption that has produced element sulphur through sulfide modifier processing rear surface.
Fig. 4 is that the refletcion high-energy electron diffraction (RHEED) of the NiW alloy base band of present embodiment behind sulfide modifier detects figure, detecting figure (Fig. 3) with the refletcion high-energy electron diffraction (RHEED) of NiW alloy base band before the sulfide modifier compares, sulfide modifier is handled back diffraction fringe spacing and has been reduced to make an appointment with half, illustrate along the spacing of＜100〉the direction atoms of arranging to be that sulfide modifier is handled half of preceding interatomic distance, theoretical model analysis in conjunction with c (2 * 2)-S superstructure of Fig. 5, when forming this kind structure, because the absorption of S atom, interatomic distance on this direction is half before not adsorbing the S atom, further illustrate, 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), obtains c (2 * 2)-S superstructure on NiW base band surface.
Embodiment 2
(1) adopts thermopair that tube furnace is carried out the school temperature, demarcate 800 ℃ of high-temperature zones and 120 ℃ of cold zone positions in the boiler tube respectively;
(2) get 10g elemental sulfur powder and pack in the mould, adopt spreader bar or cold isostatic press under the pressure of 11MPa, to be pressed into block elemental sulfur, then block elemental sulfur is placed the cold zone of tube furnace described in the step (1);
(3) the NiW alloy base band (the used sulphur powder of per 10 meters NiW alloy base bands surface sulfide modifier is no less than 1g) that pending surfaceness is not more than 5nm places the high-temperature zone of tube furnace described in the step (1), (volumn concentration of hydrogen is 4% in the mixed gas with the mixed gas of argon gas and hydrogen then, surplus is an argon gas) feed in the tube furnace as the Ventilation Rate of current-carrying gas with 150L/h, the drive that makes sulfur vapor pass through current-carrying gas imports the high-temperature zone and contacts with the NiW alloy base band, and furnace cooling obtains the NiW alloy base band that the surface has c (2 * 2)-S superstructure behind the insulation 50min.
NiW alloy base band behind the present embodiment sulfide modifier detects through Auger electron spectrum (AES) and refletcion high-energy electron diffraction (RHEED), obtains c (2 * 2)-S superstructure on NiW base band surface.
Embodiment 3
(1) adopts thermopair that tube furnace is carried out the school temperature, demarcate 820 ℃ of high-temperature zones and 125 ℃ of cold zone positions in the boiler tube respectively;
(2) get 8g elemental sulfur powder and pack in the mould, adopt spreader bar or cold isostatic press under the pressure of 9MPa, to be pressed into block elemental sulfur, then block elemental sulfur is placed the cold zone of tube furnace described in the step (1);
(3) the NiW alloy base band (the used sulphur powder of per 10 meters NiW alloy base bands surface sulfide modifier is no less than 1g) that pending surfaceness is not more than 5nm places the high-temperature zone of tube furnace described in the step (1), (volumn concentration of hydrogen is 4% in the mixed gas with the mixed gas of argon gas and hydrogen then, surplus is an argon gas) feed in the tube furnace as the Ventilation Rate of current-carrying gas with 150L/h, the drive that makes sulfur vapor pass through current-carrying gas imports the high-temperature zone and contacts with the NiW alloy base band, and furnace cooling obtains the NiW alloy base band that the surface has c (2 * 2)-S superstructure behind the insulation 30min.
NiW alloy base band behind the present embodiment sulfide modifier detects through Auger electron spectrum (AES) and refletcion high-energy electron diffraction (RHEED), obtains c (2 * 2)-S superstructure on NiW base band surface.
The above; it only is preferred embodiment of the present invention; be not that the present invention is done any restriction, everyly any simple modification that above embodiment did, change and equivalent structure changed, all still belong in the protection domain of technical solution of the present invention according to the invention technical spirit.
Claims (6)
1. NiW alloy base band surface sulfide modifier method, it is characterized in that, this method adopts the elemental sulfur powder as the sulphur source, the cold zone that elemental sulfur powder briquetting is placed on tube furnace forms sulfur vapor, utilize current-carrying gas to bring sulfur vapor into the tube furnace high-temperature zone then, adsorb with the NiW alloy base band surface that is positioned at the tube furnace high-temperature zone, desorption formation c (2 * 2)-S superstructure, described current-carrying gas is the mixed gas of argon gas and hydrogen.
2. a kind of NiW alloy base band according to claim 1 surface sulfide modifier method is characterized in that this method comprises following concrete steps:
(1) adopts thermopair that tube furnace is carried out the school temperature, demarcate 800 ℃～850 ℃ high-temperature zones and 115 ℃～125 ℃ cold zone positions in the stove respectively;
(2) get 6g～10g elemental sulfur powder and pack in the mould, under the pressure of 8MPa～11MPa, be pressed into block elemental sulfur, then block elemental sulfur is placed the cold zone of tube furnace described in the step (1) to form sulfur vapor;
(3) pending NiW alloy base band is placed the high-temperature zone of tube furnace described in the step (1), mixed gas with argon gas and hydrogen feeds in the tube furnace as current-carrying gas then, the drive that makes sulfur vapor pass through current-carrying gas imports the high-temperature zone and contacts with the NiW alloy base band, and furnace cooling obtains the NiW alloy base band that the surface has c (2 * 2)-S superstructure behind insulation 30min～50min.
3. a kind of NiW alloy base band according to claim 2 surface sulfide modifier method is characterized in that the used sulphur powder of per 10 meters NiW alloy base bands surface sulfide modifier is no less than 1g.
4. a kind of NiW alloy base band according to claim 2 surface sulfide modifier method is characterized in that the surfaceness of NiW alloy base band is not more than 5nm described in the step (3).
5. a kind of NiW alloy base band according to claim 2 surface sulfide modifier method is characterized in that, described in the step (3) in the mixed gas volumn concentration of hydrogen be 4%, surplus is an argon gas.
6. a kind of NiW alloy base band according to claim 2 surface sulfide modifier method is characterized in that the Ventilation Rate of mixed gas is 150L/h described in the step (3).
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102127735A (en) * | 2011-02-21 | 2011-07-20 | 中国科学院电工研究所 | Method for modifying metal baseband surface used for YBCO (YBa2Cu3O(7-x)) coating |
| CN103128524A (en) * | 2012-12-29 | 2013-06-05 | 北京工业大学 | Manufacture method for alloy long band with high cubic texture contents, high strength and low magnetism Ni-5at. %W |
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| US5552063A (en) * | 1993-05-12 | 1996-09-03 | Mobil Oil Corporation | Process for treating wastewater containing phenol, ammonia, and cod |
| 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 |
| JP4173123B2 (en) * | 1999-08-30 | 2008-10-29 | Ｔｄｋ株式会社 | Manufacturing method of thin film magnetic head |
| US7777989B2 (en) * | 2006-06-12 | 2010-08-17 | Seagate Technology Llc | Magnetic writer including an electroplated high moment laminated pole |
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2011
- 2011-03-09 CN CN2011100553006A patent/CN102154611B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5552063A (en) * | 1993-05-12 | 1996-09-03 | Mobil Oil Corporation | Process for treating wastewater containing phenol, ammonia, and cod |
| JP4173123B2 (en) * | 1999-08-30 | 2008-10-29 | Ｔｄｋ株式会社 | Manufacturing method of thin film magnetic head |
| US7777989B2 (en) * | 2006-06-12 | 2010-08-17 | Seagate Technology Llc | Magnetic writer including an electroplated high moment laminated pole |
| 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 |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102127735A (en) * | 2011-02-21 | 2011-07-20 | 中国科学院电工研究所 | Method for modifying metal baseband surface used for YBCO (YBa2Cu3O(7-x)) coating |
| CN103128524A (en) * | 2012-12-29 | 2013-06-05 | 北京工业大学 | Manufacture method for alloy long band with high cubic texture contents, high strength and low magnetism Ni-5at. %W |
| CN103128524B (en) * | 2012-12-29 | 2015-07-22 | 北京工业大学 | Manufacture method for alloy long band with high cubic texture contents, high strength and low magnetism Ni-5at. %W |
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