CN106399757B - A kind of preparation method of low Curie temperature, high intensity, high cubic texture nickel-base alloy base band - Google Patents
A kind of preparation method of low Curie temperature, high intensity, high cubic texture nickel-base alloy base band Download PDFInfo
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- CN106399757B CN106399757B CN201610822371.7A CN201610822371A CN106399757B CN 106399757 B CN106399757 B CN 106399757B CN 201610822371 A CN201610822371 A CN 201610822371A CN 106399757 B CN106399757 B CN 106399757B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
- C22C19/05—Alloys based on nickel or cobalt based on nickel with chromium
- C22C19/051—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W
- C22C19/057—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W with the maximum Cr content being less 10%
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/10—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of nickel or cobalt or alloys based thereon
Abstract
A kind of nickel-base alloy base band of present invention proposition and preparation method thereof, belongs to conductor of high-temperature superconductor coat baseband domain.The ingredient of alloy base band is Ni (89.3 ~ 90.9 wt.%)；Cr (7.3~7.4 wt.%)；Mo (1.6~1.7 wt.%)；Cu (0.1 ~ 1.6 wt.%) can be down to 70K in the composition range base band Curie temperature, and yield strength is between 125 ~ 137 MPa, and cubic texture share is between 82.4% ~ 97.7%.Preparation method is, using pure Ni, Cr, Mo and Cu of 99.95% or more purity, according to proportion ingredient and to smelt into alloy cast ingot；Ingot casting is hot-forged after 1100 °C of -20 h Homogenization Treatments, at 1150 °C；Forging is 30 ~ 40% hot rollings by overall reduction at 1150 °C, after 1100 °C of -10min annealing and pickling processes, it is cold-rolled to 5 mm again, anneal 30 min at 800 °C, then the cold rolling that overall reduction is 95% ~ 98% is carried out again, the alloy base band of about 0.1 mm of thickness is obtained, the above hot rolling, cold rolling pass drafts are 3 ~ 10%.After base band is cleaned by ultrasonic with acetone, under vacuum conditions, 900 ~ 1050 °C is warming up to stove, keeps the temperature 30 min.
Description
Technical field
The present invention relates to a kind of low Curie temperature, high intensity, high cubic texture nickel-base alloy base band used for coating conductor and its
Preparation method belongs to conductor of high-temperature superconductor coat metal base band technical field.
Background technology
It is wide just to have caused people since being found by second generation conductor of high-temperature superconductor coat YBa2Cu3O7-x (YBCO)
General concern and research.Mainly there is the technique that three classes prepare YBCO bands both at home and abroad at present：Ion beam assisted deposition
(IBAD), rolling auxiliary biaxial texture technology (RABiTS) technology and tilted substrates sedimentation (ISD).Since RABiTS technologies exist
There is significant advantage in terms of large-scale production, therefore have been a great concern.
In preparing two generation high-temperature superconducting coating YBCO conducting wire techniques using RABiTS technologies, require metal base band must first
Must have the cubic texture of concentration, in this manner it is possible to which the cubic texture of base band is transitioned into superconduction by the method by epitaxial growth
Layer, to control the variation of superconducting layer critical current density.In addition, load of the metal base band as entire high-temperature superconducting coating material
Body, it is necessary to have higher intensity to play the role of mechanical support.In addition to this, in order to obtain high critical current densities, subtract
Lack superconductor A.C.power loss in practical applications, it is expected that the Curie temperature of metal base band will be less than liquid nitrogen temperature.Therefore, one is prepared
The metal base band that kind takes into account texture, yield strength and each performance of Curie temperature is just particularly important.
Up to the present, Ni-5at.%W strips are the base band being most widely used, and substantially meet and prepare two generation high-temperature superconductors
Requirement of the coating to metal base band intensity and cubic texture, but its Curie temperature is high, the K of Tc=330 ~ 340, this can cause to exchange
Serious A.C.power loss in electricity transmission process.In order to solve the problems, such as base band Curie temperature, addition alloying element be effective method it
One, but this can influence the formation of cubic texture to a certain extent.Studies have shown that adding a small amount of Cr, Mo can significantly reduce
The Curie temperature of nickel-base alloy.With the increase of Cr contents, Curie temperature is by 248 K is found to the system research of Ni-Cr alloy
（7 at.%Cr）It is down to 10 K or less（13 at.%Cr）, but in alloy high-content Cr at a temperature of buffer layer easily
Oxidation, can influence the epitaxial growth of follow-up transition zone and superconducting layer and the formation of texture.Ni-5 at.%Mo alloy research is sent out
Existing, Curie temperature significantly reduces, but the share for recrystallizing cubic texture is decreased obviously.On this basis, to three
The result of study of first alloy Ni-Cr-W and Ni-Cr-V shows that the cubic texture of the base band after Ni-based middle addition alloying element is concentrated
Degree is deteriorated, from the angle design for reducing Curie temperature Ni-Cr-Mo alloys, obtained strip surrender before our seminars
Intensity is about 110 MPa, and cubic texture share is 86.3%.
In order to further take into account Curie temperature, yield strength and the cubic texture share of alloy, the present invention is in ternary alloy three-partalloy
In add the 4th kind of alloying element so that crystal grain is refined, ensure alloy base band yield strength and cubic texture part
Under the premise of volume, Curie temperature is greatly reduced.
Invention content
The object of the present invention is to provide a kind of low Curie temperature, good mechanical properties, the nickel with high share cubic texture
Base alloy baseband and preparation method thereof.By alloying, deformation and recrystallization technique, the nickel-base alloy base band of acquisition has high part
The cubic texture of volume, high yield strength, and it is rendered as paramagnetism under liquid nitrogen temperature.
Invented a kind of low Curie temperature, high intensity, high cubic texture nickel-base alloy base band, the component of this alloy base band and
Weight percentage is specific as follows：
Ni (89.3 ~ 90.9 wt.%)；Cr (7.3 ~7.4 wt.%) ；Mo (1.6 ~1.7 wt.%)；Cu (0.1
~ 1.6 wt.%)。
Invented a kind of low Curie temperature, high intensity, high cubic texture nickel-base alloy base band preparation method, feature exists
In comprising the following steps that：
（a）Alloy smelting and forging
Pure Ni, pure Cr, pure Mo and pure Cu that purity is 99.95% or more weigh matching according to mentioned component proportioning
Material, four kinds of raw material are placed in cold crucible suspension vacuum melting furnace and are smelted, and obtain the nickel-base alloy casting that quality is about 350 g
Ingot.Ingot casting is placed in Muffle furnace, in 1100 °C of 20 h of lower Homogenization Treatments.Then 1150 °C are warming up to stove and keep the temperature 60
It is hot-forged after min, obtains the forging of (70 ~ 80) × (20 ~ 25) × (16 ~ 18) mm；After the completion of hot forging, by forging
10 min are kept the temperature under 1150 °C；
（b）Forging hot rolling and cold rolling
Forging is placed in Muffle furnace, hot rolling after being warming up to 1150 °C and 30 min of heat preservation with stove, reduction in pass 3%
~ 10%, overall reduction is 30% ~ 40%；Hot rolled plate is annealed through 1100 °C of -10 min, after peeling, pickling processes, with passage pressure
Lower amount 3% ~ 10% is cold-rolled to 5 mm, and anneal 30 min at 800 °C, and it is 3% ~ 10% then to carry out reduction in pass again, stagnation pressure
The cold-rolling treatment that lower amount is 95% ~ 98%, it is final to obtain the alloy base band that thickness is about 0.1 mm；
（c）The recrystallization annealing of cold rolling base band
After cold rolling base band is cleaned by ultrasonic oil removing with acetone, under vacuum conditions, heated up with the heating rate of 10 °C/min
To 900 ~ 1050 °C, 30 min are kept the temperature.
The Ni base alloy basebands obtained through the invention have the characteristics that：
1. taking into account the contribution that each alloying element forms mechanical property, Curie temperature and cubic texture, Cr, Mo, Cu are selected
It is added in pure Ni and obtains quaternary alloy, under the premise of guarantee alloy low Curie temperature, significantly improves the mechanical property of alloy
It can be with the share of cubic texture.
2. the cubic texture share of the Ni base alloy basebands obtained through the invention is 97.7%, yield strength 137
MPa, Curie temperature are 70 K, can more meet the actual demand for preparing conductor of high-temperature superconductor coat metal base band.
Description of the drawings
Fig. 1 is the X-ray diffractogram under different holding temperatures in embodiment 1.
After Fig. 2 is alloy base band annealing in embodiment 1（111）Pole figure.
After Fig. 3 is alloy base band annealing in embodiment 2（111）Pole figure.
After Fig. 4 is alloy base band annealing in embodiment 3（111）Pole figure.
After Fig. 5 is alloy base band annealing in embodiment 4（111）Pole figure.
Fig. 6 is the load-deformation curve obtained after alloy base band annealing in embodiment 1,2,3.
Fig. 7 is the graph of relation of the intensity of magnetization and temperature in embodiment 1.
Fig. 8 is the graph of relation of the intensity of magnetization and temperature in embodiment 2.
Specific embodiment
Embodiment 1
By purity be 99.95% or more Ni, Cr, Mo, Cu according to 89.3%, 7.4%, 1.7% and 1.6% weight percent
Dispensing is carried out, the raw material prepared is smelted 5 times repeatedly using cold crucible suspension vacuum melting furnace；It is about 350 by the quality obtained
The ingot casting of g is placed in Muffle furnace, in 1100 °C of 20 h of lower Homogenization Treatments, makes alloy composition more by being spread between atom
Uniformly, it is then hot-forged at a temperature of 1150 °C, obtains the forging that size is 70 × 25 × 18 mm；Forging is warming up to stove
Hot rolling is carried out after 1150 °C of 30 min of heat preservation, reduction in pass is about 10%, finally obtains the hot rolled plate that thickness is 11 mm.Hot rolling
Plate is annealed through 1100 °C of -10 min, after peeling, pickling processes, is carried out the cold-rolling treatment that reduction in pass is 3% ~ 10%, is obtained
To after 5 mm cold-reduced sheets, intermediate annealing is carried out under the conditions of 800 °C of -30 min, then carry out again reduction in pass be 3% ~
10%, the cold rolling that overall reduction is 98% obtains the alloy base band that thickness is 0.1 mm.The ultrasonic cleaning of cold rolling base band acetone is removed
It anneals under vacuum conditions after oil, annealing process is to rise to 900 ~ 1050 °C of heat preservations 30 with the heating rate of 10 °C/min
Min, obtain low Curie temperature, high intensity, high cubic texture metal base band.The X-ray diffraction analysis result of the alloy base band
See that Fig. 1, best annealing temperature are 1000 °C；The base band that best annealing process obtains（111）Pole figure is shown in Fig. 2, cubic texture
It concentrates, and cubic texture share is up to 97.7%；The load-deformation curve of the base band is as shown in fig. 6, yield strength is 137
MPa；The intensity of magnetization of the alloy and the relationship of temperature such as Fig. 7, Curie temperature are 70 K.It is high-strength to illustrate that this alloy base band meets
The requirement of degree, low Curie temperature, high share cubic texture.
Embodiment 2
By purity be 99.95% or more Ni, Cr, Mo, Cu according to 90.1%, 7.4%, 1.7% and 0.8% weight percent
Dispensing is carried out, the raw material prepared is smelted 5 times repeatedly using cold crucible suspension vacuum melting furnace；It is about 350 by the quality obtained
The ingot casting of g is placed in Muffle furnace, in 1100 °C of 20 h of lower Homogenization Treatments, makes alloy composition more by being spread between atom
Uniformly, it is then hot-forged at a temperature of 1150 °C, obtains the forging that size is 75 × 22 × 18 mm；Forging is warming up to stove
Hot rolling is carried out after 1150 °C of 30 min of heat preservation, reduction in pass is about 10%, finally obtains the hot rolled plate that thickness is 11 mm.Hot rolling
Plate is annealed through 1100 °C of -10 min, after peeling, pickling processes, is carried out the cold-rolling treatment that reduction in pass is 3% ~ 10%, is obtained
To after 5 mm cold-reduced sheets, intermediate annealing is carried out under the conditions of 800 °C of -30 min, then carry out again reduction in pass be 3% ~
10%, the cold rolling that overall reduction is 98% obtains the alloy base band that thickness is 0.1 mm.The ultrasonic cleaning of cold rolling base band acetone is removed
It anneals under vacuum conditions after oil, annealing process is to rise to 1000 °C of 30 min of heat preservation with the heating rate of 10 °C/min,
Obtain low Curie temperature, the cube textured base band of high intensity.The alloy base band（111）Pole figure is shown in Fig. 3, cubic texture collection
In, cubic texture share is 96.1%；The load-deformation curve of the alloy base band is as shown in fig. 6, yield strength is 130 MPa.
The intensity of magnetization of the alloy thin band and the relationship of temperature such as Fig. 8, Curie temperature are 80 K.It is more high-strength to illustrate that this alloy base band meets
The requirement of degree and high share cubic texture.
Embodiment 3
Ni, Cr, Mo that purity is 99.95% or more are subjected to dispensing according to 90.9%, 7.4% and 1.7% weight percent,
The raw material prepared is smelted 5 times repeatedly using cold crucible suspension vacuum melting furnace；The ingot casting for being about 350 g by the quality obtained is set
In Muffle furnace, in 1100 °C of 20 h of lower Homogenization Treatments, keep alloy composition more uniform by being spread between atom, then
It is hot-forged at a temperature of 1150 °C, obtains the forging that size is 80 × 20 × 16 mm；Forging is warming up to 1150 °C of guarantors with stove
Hot rolling is carried out after 30 min of temperature, reduction in pass is about 10%, finally obtains the hot rolled plate that thickness is 11 mm.Hot rolled plate passes through
1100 °C of -10 min annealing, is removed the peel, after pickling processes, is carried out the cold-rolling treatment that reduction in pass is 3% ~ 10%, is obtained 5 mm
After cold-reduced sheet, intermediate annealing is carried out under the conditions of 800 °C of -30 min, it is 3% ~ 10% then to carry out reduction in pass again, always
The cold rolling that drafts is 98% obtains the alloy base band that thickness is 0.1 mm.By cold rolling base band with acetone be cleaned by ultrasonic oil removing after
It anneals under vacuum environment, annealing process is to rise to 1000 °C of 30 min of heat preservation with the heating rate of 10 °C/min, is obtained low
Curie temperature, the cube textured base band of high intensity.The alloy base band（111）Pole figure is shown in Fig. 4, and cubic texture is concentrated, cube
Texture share is 85.7%；The alloy base band answers strain curve as shown in fig. 6, yield strength is 125 MPa.Illustrate this alloy
Base band meets the requirement of higher-strength and the cubic texture of higher share.Alloy residence can be reduced due to adding Cu in Ni based alloys
In temperature, under the premise of Cr with Mo contents are consistent, in the present embodiment alloy Curie temperature certainly will be higher than embodiment 1,2, also
It is to say that Curie temperature is higher than 80 K.Therefore, the relationship of the intensity of magnetization of the alloy base band and temperature is not tested.
Embodiment 4
By purity be 99.95% or more Ni, Cr, Mo, Cu according to 89.3%, 7.4%, 1.7% and 1.6% weight percent
Dispensing is carried out, the raw material prepared is smelted 5 times repeatedly using cold crucible suspension vacuum melting furnace；It is about 350 by the quality obtained
The ingot casting of g is placed in Muffle furnace, in 1100 °C of 20 h of lower Homogenization Treatments, makes alloy composition more by being spread between atom
Uniformly, it is then hot-forged at a temperature of 1150 °C, obtains the forging that size is 70 × 25 × 18 mm；Forging is heated up with stove
Hot rolling is carried out after to 1150 °C of 30 min of heat preservation, reduction in pass is about 10%, finally obtains the hot rolled plate that thickness is 11 mm.Heat
It rolls plate to anneal through 1100 °C of -10min, after peeling, pickling processes, carries out the cold-rolling treatment that reduction in pass is 3% ~ 10%, obtain
To after 5 mm cold-reduced sheets, intermediate annealing is carried out under the conditions of 800 °C of -30 min, then carry out again reduction in pass be 3% ~
10%, the cold rolling that overall reduction is 95% obtains the alloy base band that thickness is 0.25 mm.Cold rolling base band is cleaned by ultrasonic with acetone
It anneals under vacuum conditions after oil removing, annealing process is to rise to 1000 °C of heat preservations 30 with the heating rate of 10 °C/min
Min obtains the cube textured base band of low Curie temperature.The alloy thin band（111）Pole figure is shown in Fig. 5, and cubic texture is concentrated, and is stood
Square texture share is 82.4%；The intensity of magnetization of the alloy base band and the relationship of temperature such as Fig. 7, Curie temperature are 70 K.Illustrate this
Alloy can get the cubic texture of higher share under 95% deformation quantity, but compared to the sample of 98% deformation quantity, cubic texture
Share is obviously relatively low.Since the base band cubic texture share obtained under 95% deformation quantity is relatively low, its mechanical property is not carried out
Evaluation.
In conclusion the alloy base band in embodiment 1 is equal at Curie temperature, yield strength and three aspects of cubic texture
It takes advantage.Therefore the preparation process of alloying component and base band is optimal selection in embodiment 1.
Claims (2)
1. a kind of low Curie temperature, high intensity, high cubic texture nickel-base alloy base band, component and mass percent are：Ni
(89.3~90.9wt.%)；Cr (7.3~7.4wt.%)；Mo (1.6~1.7wt.%)；Cu (0.1~1.6wt.%)；It is made
Preparation Method includes the following steps：
(a) alloy smelting and forging
Pure Ni, pure Cr, pure Mo and pure Cu that purity is 99.95% or more are claimed according to said components and mass percent
Four kinds of raw material are placed in cold crucible suspension vacuum melting furnace and smelt by recompounding, obtain the nickel-base alloy that quality is 350g and cast
Ingot casting is placed in Muffle furnace by ingot, and the Homogenization Treatments 20h at 1100 DEG C is then warming up to 1150 DEG C with stove and keeps the temperature 60min
After be hot-forged, obtain the forging of (70~80) × (20~25) × (16~18) mm；After the completion of hot forging, forging is protected at 1150 DEG C
Warm 10min；
(b) forging hot rolling and cold rolling
Forging is placed in Muffle furnace, 1150 DEG C are warming up to stove and keeps the temperature hot rolling after 30min, reduction in pass is 3%~
10%, overall reduction is 30%~40%；Hot rolled plate is annealed through 1100 DEG C of -10min, after peeling, pickling processes, is depressed with passage
Amount 3%~10% is cold-rolled to 5mm, and anneal 30min at 800 DEG C, and it is 3%~10% then to carry out reduction in pass again, under stagnation pressure
Amount is 95%~98% cold-rolling treatment, and the final thickness that obtains is the alloy base band of 0.1mm；
(c) recrystallization annealing of cold rolling base band
After cold rolling base band is cleaned by ultrasonic oil removing with acetone, under vacuum conditions, 900 are warming up to the heating rate of 10 DEG C/min
~1050 DEG C, keep the temperature 30min.
2. the preparation method of a kind of low Curie temperature, high intensity, high cubic texture nickel-base alloy base band, it is characterised in that have with
Lower processing step：
(a) alloy smelting and forging
By the pure Ni of 99.95% or more purity, pure Cr, pure Mo and pure Cu according to nickel-base alloy base band as described in claim 1
Component and mass percent dispensing are smelted in cold crucible suspension vacuum melting furnace, are obtained the nickel-base alloy that quality is 350g and are cast
Ingot；Ingot casting is at 1100 DEG C after Homogenization Treatments 20h, and at 1150 DEG C, hot forging becomes (70~80) × (20~25) × (16~18)
The forging of mm；After the completion of hot forging, forging is kept the temperature into 10min at 1150 DEG C；
(b) forging hot rolling and cold rolling
Forging is warming up to 1150 DEG C with stove and keeps the temperature hot rolling after 30min, reduction in pass is 3%~10%, and overall reduction is
30%~40%；Hot rolled plate is annealed through 1100 DEG C of -10min, after peeling, pickling processes, with 3%~10% cold rolling of reduction in pass
To 5mm；Anneal 30min at 800 DEG C；Then carry out that reduction in pass is 3%~10%, overall reduction is 95%~98% again
Cold rolling, it is final to obtain the alloy base band that thickness is 0.1mm；
(c) recrystallization annealing of cold rolling base band
After cold rolling base band is cleaned by ultrasonic oil removing with acetone, under vacuum conditions, 900 are warming up to the heating rate of 10 DEG C/min
~1050 DEG C, keep the temperature 30min.
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| CN111118422B (en) * | 2019-11-25 | 2021-03-05 | 北京科技大学 | Preparation method of high-tungsten high-cobalt nickel alloy fine-grain plate |
| CN111996477B (en) * | 2020-07-06 | 2021-09-14 | 河南师范大学 | Preparation method of high-strength cube-texture metal base band for coated superconducting strip |
| CN115354251B (en) * | 2022-08-29 | 2023-02-10 | 西安交通大学 | Heat treatment method for improving precipitation degree and inhibiting precipitated phase from coarsening |
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|---|---|---|---|---|
| CN1861388A (en) * | 2006-03-31 | 2006-11-15 | 北京工业大学 | Method for preparing high-temp. superconductive composite Ni alloy base belt |
| CN101514413A (en) * | 2009-04-03 | 2009-08-26 | 西北有色金属研究院 | Preparing method of nickel tungsten base band used for coated conductor |
| CN103952592A (en) * | 2014-04-14 | 2014-07-30 | 上海大学 | Preparation method of non-magnetic cube-textured nickel-based alloy substrate used for high-temperature superconducting coated conductors |
| CN104404306A (en) * | 2014-09-03 | 2015-03-11 | 上海大学 | High-strength cube texture nickel base alloy baseband for coated conductors and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6331199B1 (en) * | 2000-05-15 | 2001-12-18 | Ut-Battelle, Llc | Biaxially textured articles formed by powder metallurgy |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1861388A (en) * | 2006-03-31 | 2006-11-15 | 北京工业大学 | Method for preparing high-temp. superconductive composite Ni alloy base belt |
| CN101514413A (en) * | 2009-04-03 | 2009-08-26 | 西北有色金属研究院 | Preparing method of nickel tungsten base band used for coated conductor |
| CN103952592A (en) * | 2014-04-14 | 2014-07-30 | 上海大学 | Preparation method of non-magnetic cube-textured nickel-based alloy substrate used for high-temperature superconducting coated conductors |
| CN104404306A (en) * | 2014-09-03 | 2015-03-11 | 上海大学 | High-strength cube texture nickel base alloy baseband for coated conductors and preparation method thereof |
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