CN106816228A - Preparation method of second-generation high-temperature superconducting tape non-textured metal thin tape - Google Patents
Preparation method of second-generation high-temperature superconducting tape non-textured metal thin tape Download PDFInfo
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- CN106816228A CN106816228A CN201611174265.9A CN201611174265A CN106816228A CN 106816228 A CN106816228 A CN 106816228A CN 201611174265 A CN201611174265 A CN 201611174265A CN 106816228 A CN106816228 A CN 106816228A
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- 239000002184 metal Substances 0.000 title claims abstract description 62
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 69
- 239000000463 material Substances 0.000 claims abstract description 41
- 238000005096 rolling process Methods 0.000 claims abstract description 41
- 238000005097 cold rolling Methods 0.000 claims abstract description 38
- 238000000137 annealing Methods 0.000 claims abstract description 36
- 230000008569 process Effects 0.000 claims abstract description 25
- 239000000956 alloy Substances 0.000 claims abstract description 13
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 12
- 230000001681 protective effect Effects 0.000 claims abstract description 8
- 239000000758 substrate Substances 0.000 claims abstract description 7
- 230000003746 surface roughness Effects 0.000 claims description 14
- 239000000126 substance Substances 0.000 claims description 12
- 238000005498 polishing Methods 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- 230000007704 transition Effects 0.000 claims description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 4
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 238000005229 chemical vapour deposition Methods 0.000 claims description 2
- 238000005240 physical vapour deposition Methods 0.000 claims description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 1
- 239000002887 superconductor Substances 0.000 abstract description 26
- 230000018984 mastication Effects 0.000 abstract description 4
- 238000010077 mastication Methods 0.000 abstract description 4
- 238000010301 surface-oxidation reaction Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 description 11
- 230000009467 reduction Effects 0.000 description 11
- 229910001339 C alloy Inorganic materials 0.000 description 8
- WAIPAZQMEIHHTJ-UHFFFAOYSA-N [Cr].[Co] Chemical compound [Cr].[Co] WAIPAZQMEIHHTJ-UHFFFAOYSA-N 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 7
- 229910001220 stainless steel Inorganic materials 0.000 description 4
- 239000010935 stainless steel Substances 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 125000004429 atom Chemical group 0.000 description 3
- 238000000151 deposition Methods 0.000 description 3
- 230000008021 deposition Effects 0.000 description 3
- 239000010408 film Substances 0.000 description 3
- 238000007517 polishing process Methods 0.000 description 3
- 238000002791 soaking Methods 0.000 description 3
- 230000004888 barrier function Effects 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000005457 optimization Methods 0.000 description 2
- 238000004549 pulsed laser deposition Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000011224 oxide ceramic Substances 0.000 description 1
- 229910052574 oxide ceramic Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000010181 polygamy Effects 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
- H01B13/0026—Apparatus for manufacturing conducting or semi-conducting layers, e.g. deposition of metal
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Superconductors And Manufacturing Methods Therefor (AREA)
Abstract
The present invention relates to a kind of preparation method of second-generation high-temperature superconductor without textured metal strip；High-temperature alloy sheet material is chosen as base material, base material is carried out into surface preparation；Pretreated base material carries out cross-shear rolling, and it is the 101 120% of metal sheet band requirement thickness to roll the thickness of rear substrate；Without high-temperature annealing process in the operation of rolling；According to the requirement of metal sheet band mechanical strength, the base material after cross-shear rolling is carried out into protective atmosphere annealing；Base material after annealing is carried out into minute surface cold rolling, be cold-rolled to and described require thickness.The technique that the inventive method is combined using cross-shear rolling " thinning " and minute surface cold rolling " smooth ", it is to avoid hot mastication annealing repeatedly in traditional cold-rolling process, is considerably reduced to be annealed due to hot mastication and causes the possibility of base band surface oxidation；Surface smoothness of the second-generation high-temperature superconductor without textured metal strip is remarkably improved, the complexity of subsequent technique is reduced.
Description
Technical field
The present invention relates to second-generation high-temperature superconductor preparing technical field, and in particular to a kind of second generation hts band
Preparation method of the material without textured metal strip.
Background technology
Second generation high-temperature superconductor is functional oxide ceramics, and it has good electrical property, but machine below liquid nitrogen temperature
Tool poor performance.Can be with the superconductivity wire of practical application in order to obtain, it is mesh that it is deposited on metal base band in the form of a film
Preceding main technological means.Due in follow-up coating process, to undertake epitaxial film as substrate without textured metal base band and give birth to
Function long, its thickness general one of (i.e. metal sheet band), its important performance indications below 0.15 millimeter are exactly surface matter
Amount.In order to produce nanoscale flat surface without textured metal strip, common technological means is that high-temperature alloy sheet material is (general
More than 0.5 millimeter) rolling it is thinning, then carry out electrobrightening.Whether electrobrightening (is deposited to the initial surface composition of metal sheet band
In oxide) and surface roughness (generally below 30 nanometers) have strict demand.Therefore the rolling of high temperature alloy strip need to be added
Work technique is strictly controlled.High temperature alloy hardness is big, and cold rolling process has obvious processing hardening phenomenon, i.e., by number
The cold rolling high annealing that is accomplished by of passage is otherwise difficult to follow-up cold rolling with softener material.The technique of cold rolling and high annealing will
Be repeated could obtain several times require thickness without textured metal strip.On the other hand, the high temperature of high-temperature alloy material is moved back
Ignition technique is harsh, high to equipment and annealing process requirement.The high-temperature alloy base belt surface oxidation that high annealing causes is production
During common phenomenon.The oxide of high-temperature alloy base belt surface will have a strong impact on entering for follow-up cold-rolling process and electrobrightening
OK, it is greatly lowered final without textured metal Surface Quality of Strip.Which has limited second-generation high-temperature superconductor without textured metal
The reduction of strip production cost.
The content of the invention
The present invention is in order to simplify production technology and reduce production cost, there is provided a kind of second-generation high-temperature superconductor is without texture
The preparation method of metal sheet band.The technology path that the present invention is combined using cross-shear rolling " thinning " with minute surface cold rolling " smooth ",
For obtaining high-quality second-generation high-temperature superconductor without textured metal base band.Present invention mainly solves current second generation high temperature
Superconducting tape is without the technical barrier in textured metal band production process, 1) conventional " minute surface is cold rolling " technique needed to metal base band
" high annealing " several times is carried out to soften, and " high annealing " causes metal base band surface oxidation, reduces its follow-up cold rolling and electricity
Solve the difficulty of glossing；It is 2) independent that cannot to cause that the surface of metal toughness template reaches nanoscale using " cross-shear rolling " smooth
Level.
The purpose of the present invention is achieved through the following technical solutions：
The present invention relates to a kind of preparation method of second-generation high-temperature superconductor without textured metal strip, methods described includes
Following steps：
The base material is carried out surface pre- by S1, selection high-temperature alloy sheet material as the base material of second-generation high-temperature superconductor
Process to remove oxide layer；
S2, the base material that step S1 is obtained is carried out into cross-shear rolling, the thickness for rolling rear substrate be the metal sheet band will
Seek the 101-120% of thickness；Without high-temperature annealing process in the operation of rolling；
S3, the requirement according to the metal sheet band mechanical strength, protective atmosphere annealing is carried out by the base material that step S2 is obtained；
S4, the base material that step S3 is obtained is carried out that minute surface is cold rolling, be cold-rolled to the requirement thickness of the metal sheet band.
Preferably, in step S1, the surface preparation is Chemical cleaning or mechanical grinding, or Chemical cleaning and machinery
Polishing is combined.
Preferably, in step S3, the protective atmosphere is the reducibility gas containing enough ratios, and enough ratios refer to
Be to be able to ensure that oxide-free generation in base band surface in annealing process.
Preferably, the reducibility gas are hydrogen, nitrogen, argon gas or ammonia.
Preferably, in step S3, the temperature of the annealing is 600-1200 DEG C, annealing time is -2 hours 5 minutes.
Preferably, in step S4, the surface roughness of the cold rolling cold rolling mill work roller of minute surface is less than 50 nanometers.
Preferably, in step S4, the requirement thickness of the metal sheet band is 0.01-0.15 millimeters.
The invention further relates to a kind of preparation method of second-generation high-temperature superconductor, methods described comprises the following steps：
A1, second-generation high-temperature superconductor obtained in the method for claim 1 is carried out without textured metal strip
Treatment, makes its surface reach nanoscale flat surface；
A2, surface use physical vaporous deposition deposition oxide transition zone, then in the oxide transition zone table
Face uses pulsed laser deposition, chemical solution method or chemical vapor deposition second generation high-temp. superconducting layer.
Preferably, in step A1, the treatment includes that electrobrightening, chemical polishing, mechanical polishing or chemical solution are put down
Integralization treatment.
Cross-shear rolling is a kind of more advanced strip rolling technique, and current nearly all application is limited to " structural material ",
The product produced using this kind of technology emphasizes mechanical property, to surface roughness without being distinctly claimed.Because second generation high temperature is super
The production of conduction band material metal sheet band belongs to cross discipline, the important performance indexes of such strip be exactly surface roughness with surface into
Point, there is larger difference with conventionally employed cross-shear rolling production product.Therefore, those skilled in the art are difficult to expect using asynchronous
Cold rolling " thinning " prepares second-generation high-temperature superconductor without textured metal with the process route that minute surface cold rolling " smooth " is combined
Strip
Additionally, the crucial of process route that cross-shear rolling " thinning " of the invention is combined with minute surface cold rolling " smooth " also exists
Following technical barrier is mainly solved in it：I) the necessary intermediate annealing of traditional cold rolling processing technology softens；Ii) conventional asynchronous are cold
Roll acquisition second-generation high-temperature superconductor metal sheet band product, the excessive problem of surface roughness.And, using single " asynchronous cold
Roll " technique, it is impossible to reach the requirement of second-generation high-temperature superconductor metal sheet band product surface roughness；Using single " minute surface
It is cold rolling " technique, it is necessary to softened using intermediate annealing, cannot otherwise realize the production of second-generation high-temperature superconductor metal sheet band.
Compared with prior art, the present invention has the advantages that：
1st, the process route that the present invention is combined using cross-shear rolling " thinning " with minute surface cold rolling " smooth ", using asynchronous cold
Roll continuously can carry out cold rolling to high-temperature alloy sheet material, and the characteristics of without high annealing, high efficiency realizes " thinning " base band；Then it is sharp
It is cold rolling with minute surface, realize the planarizing on metal sheet band surface.
2nd, metal sheet band obtained in the method for the present invention can be directly used for electrolytic polishing process or chemical solution planarizing
Technique, obtains metal form band of the surface roughness below 2 nanometers.
3rd, technology path of the invention can reduce to existing second-generation high-temperature superconductor strip production process high temperature
The rigors of annealing process and equipment, simplify cold-rolling process, reduce production cost.
4th, the present invention is a kind of technology path for obtaining high-quality second-generation high-temperature superconductor metal sheet band.
Brief description of the drawings
The detailed description made to non-limiting example with reference to the following drawings by reading, further feature of the invention,
Objects and advantages will become more apparent upon：
During Fig. 1 is embodiment 1, thickness is that surface of 0.05 millimeter of second-generation high-temperature superconductor without textured metal strip is former
Sub- force microscope figure, test scope is 50 micrometre squares；
During Fig. 2 is embodiment 1, the surface atom force microscope figure of metal form band after electrolytic polishing process tests model
It is 1 micrometre square to enclose；
During Fig. 3 is embodiment 1, second generation high-temperature superconductor multi-layer film structure schematic diagram is grown with metal sheet band；
During Fig. 4 is embodiment 3, thickness is 0.15 millimeter of second-generation high-temperature superconductor without textured metal strip, optimization electricity
The surface atom force microscope figure of metal form band after solution glossing, test scope is 50 micrometre squares；
During Fig. 5 is embodiment 2, thickness be 0.01 millimeter of second-generation high-temperature superconductor without the rolling of textured metal strip after
Surface atom force microscope figure, test scope is 50 micrometre squares.
Specific embodiment
With reference to embodiment, the present invention is described in detail.Following examples will be helpful to those skilled in the art
The present invention is further understood, but the invention is not limited in any way.It should be pointed out that to one of ordinary skill in the art
For, without departing from the inventive concept of the premise, can also make certain adjustments and improvements.These belong to guarantor of the invention
Shield scope.
" cross-shear rolling " technique of the present invention, total reduction >=60%, percentage pass reduction 20%~40%, Ke Yiyou
Following methods are realized：Method one, working roll rotating speed is identical, and upper and lower working roll roll neck is different；Method two, upper and lower working roll roll neck
It is identical, but working roll rotating speed is different；Method three, upper and lower work roll diameter is identical, and rotating speed is identical, upper and lower work roll surface and base band
Coefficient of friction it is different.
" minute surface is cold rolling " technique of the present invention, total reduction≤50%, percentage pass reduction 1%~20%, minute surface is cold
The surface roughness of the cold rolling mill work roller for rolling is less than 50 nanometers.
Embodiment 1
The present embodiment is related to a kind of preparation method of second-generation high-temperature superconductor without textured metal strip, methods described bag
Include following steps：
1) selection and pretreatment of high-temperature alloy sheet material：Choose the sheet material conduct of Hastelloy C alloys 276 that thickness is 0.5 millimeter
Base material, is carried out mechanical grinding, removes its surface oxide layer；
2) asymmetrical rolling process：By step 1) obtain the base material of Hastelloy C alloys 276 carry out cross-shear rolling；In the operation of rolling
Without high-temperature annealing process, through six passes, the thickness for rolling base band is 0.06 millimeter；
Six passage cross-shear rollings use method one, i.e., upper and lower working roll roll neck is identical, are realized by the way that working roll rotating speed is different
Asynchronous, the circumferential speed ratio of the upper and lower working roll of asynchronous rolling machine is 1: 1.15, and percentage pass reduction 30%, overall reduction is 88%.
3) annealing process：By step 3) obtain the sheet material of Hastelloy C alloys 276 annealed, protective atmosphere is pure hydrogen；Move back
Fiery temperature is 1200 DEG C, and annealing soaking time is half an hour；
4) minute surface cold-rolled process：By step 3) to carry out minute surface cold rolling for the base material of Hastelloy C alloys 276 that obtains, rolled through a time
System, is cold-rolled to 0.05 millimeter；The surface roughness of minute surface cold rolling mill working roll is 10 nanometers.Final metal sheet band rough surface
It is 17 nanometers to spend, as shown in Figure 1.
The metal sheet band is reduced to 1 nanometer by electrobrightening, metal sheet band surface roughness, as shown in Figure 2；Using thing
Physical vapor deposition deposition oxide transition zone, using pulsed laser deposition superconducting layer, obtains superconducting thin film (structure is as shown in Figure 3)
Critical electric current value be 200 amperes.
Embodiment 2
The present embodiment is related to a kind of preparation method of second-generation high-temperature superconductor without textured metal strip, methods described bag
Include following steps：
1) selection and pretreatment of high-temperature alloy sheet material：Choose the sheet material conduct of Hastelloy C alloys 276 that thickness is 0.3 millimeter
Base material, is carried out mechanical grinding, removes its surface oxide layer；
2) asymmetrical rolling process：By step 1) obtain the base material of Hastelloy C alloys 276 carry out cross-shear rolling；In the operation of rolling
Without high-temperature annealing process, through five passes, the thickness for rolling base band is 0.011 millimeter；Five passage cross-shear rolling use sides
Method one, i.e., upper and lower working roll roll neck is identical, and asynchronous, the week of the upper and lower working roll of asynchronous rolling machine is realized by working roll rotating speed difference
It is 1: 1.15 to speed ratio, percentage pass reduction 30%, overall reduction is 75%；
3) annealing process：By step 3) obtain the sheet material of Hastelloy C alloys 276 annealed, protective atmosphere is pure hydrogen；Move back
Fiery temperature is 600 DEG C, and annealing soaking time is two hours.
4) minute surface cold-rolled process：By step 3) to carry out minute surface cold rolling for the base material of Hastelloy C alloys 276 that obtains, rolled through a time
System, is cold-rolled to 0.01 millimeter；The surface roughness of minute surface cold rolling mill working roll is 10 nanometers.Final metal sheet band rough surface
It is 19 nanometers to spend, as shown in Figure 5.
Embodiment 3
The present embodiment is related to a kind of preparation method of second-generation high-temperature superconductor without textured metal strip, methods described bag
Include following steps：
1) selection and pretreatment of high-temperature alloy sheet material：Selection thickness is 0.5 millimeter of stainless steel materials as base material, general
It carries out mechanical grinding, removes its surface oxide layer；
2) asymmetrical rolling process：By step 1) obtain stainless steel substrate carry out cross-shear rolling；Without high in the operation of rolling
Warm annealing process, through six passes, the thickness for rolling base band is 0.16 millimeter；Five passage cross-shear rollings use method one, i.e.,
Upper and lower working roll roll neck is identical, and asynchronous, the circumferential speed of the upper and lower working roll of asynchronous rolling machine is realized by working roll rotating speed difference
Than being 1: 1.15, percentage pass reduction 30%, overall reduction is 90%.
3) annealing process：By step 3) obtain stainless steel materials annealed, protective atmosphere is pure hydrogen；Annealing temperature
It it is 1000 DEG C, annealing soaking time is one hour；
4) minute surface cold-rolled process：By step 3) to carry out minute surface cold rolling for the stainless steel substrate that obtains, is rolled through a time, cold rolling
To 0.15 millimeter；The surface roughness of minute surface cold rolling mill working roll is 20 nanometers.It is finally golden (after optimization electrolytic polishing process)
Category strip surface roughness is 27 nanometers, as shown in Figure 4.
In sum, the technique that the inventive method is combined using cross-shear rolling " thinning " and minute surface cold rolling " smooth ", keeps away
Hot mastication annealing repeatedly in traditional cold-rolling process is exempted from, has considerably reduced because hot mastication annealing causes base band Surface Oxygen
The possibility of change；The surface smoothness of second-generation high-temperature superconductor metal sheet band is remarkably improved, answering for subsequent technique is reduced
Polygamy.The inventive method simplifies the operation of rolling, reduces the requirement to Equipment for Heating Processing, can save the resources of production and cost,
It is suitable to large-scale industrial production.
Specific embodiment of the invention is described above.It is to be appreciated that the invention is not limited in above-mentioned
Particular implementation, those skilled in the art can within the scope of the claims make various deformations or amendments, this not shadow
Sound substance of the invention.
Claims (9)
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| Application Number | Priority Date | Filing Date | Title |
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| CN201611174265.9A CN106816228B (en) | 2016-12-16 | 2016-12-16 | Preparation method of the second-generation high-temperature superconductor without textured metal strip |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611174265.9A CN106816228B (en) | 2016-12-16 | 2016-12-16 | Preparation method of the second-generation high-temperature superconductor without textured metal strip |
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| CN106816228A true CN106816228A (en) | 2017-06-09 |
| CN106816228B CN106816228B (en) | 2018-08-24 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110797148A (en) * | 2019-10-08 | 2020-02-14 | 上海交通大学 | Superconducting tape suitable for non-insulated coil, non-insulated coil and preparation method thereof |
| CN113046664A (en) * | 2021-02-08 | 2021-06-29 | 中航上大高温合金材料股份有限公司 | Smelting method of C-276 hastelloy |
-
2016
- 2016-12-16 CN CN201611174265.9A patent/CN106816228B/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110797148A (en) * | 2019-10-08 | 2020-02-14 | 上海交通大学 | Superconducting tape suitable for non-insulated coil, non-insulated coil and preparation method thereof |
| CN110797148B (en) * | 2019-10-08 | 2021-07-30 | 上海交通大学 | Superconducting tape suitable for non-insulated coil, non-insulated coil and preparation method thereof |
| CN113046664A (en) * | 2021-02-08 | 2021-06-29 | 中航上大高温合金材料股份有限公司 | Smelting method of C-276 hastelloy |
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| CN106816228B (en) | 2018-08-24 |
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