CN116926394B - Gadolinium-niobium alloy belt with high neutron absorptivity, and preparation method and application thereof - Google Patents
Gadolinium-niobium alloy belt with high neutron absorptivity, and preparation method and application thereof Download PDFInfo
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- CN116926394B CN116926394B CN202311197624.2A CN202311197624A CN116926394B CN 116926394 B CN116926394 B CN 116926394B CN 202311197624 A CN202311197624 A CN 202311197624A CN 116926394 B CN116926394 B CN 116926394B
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- 229910001257 Nb alloy Inorganic materials 0.000 title claims abstract description 85
- RFXPCMBJOLURAK-UHFFFAOYSA-N [Gd].[Nb] Chemical compound [Gd].[Nb] RFXPCMBJOLURAK-UHFFFAOYSA-N 0.000 title claims abstract description 85
- 238000002360 preparation method Methods 0.000 title abstract description 11
- 238000005242 forging Methods 0.000 claims abstract description 91
- 238000000137 annealing Methods 0.000 claims abstract description 58
- 238000005098 hot rolling Methods 0.000 claims abstract description 33
- 238000003723 Smelting Methods 0.000 claims abstract description 32
- 238000005097 cold rolling Methods 0.000 claims abstract description 29
- 229910045601 alloy Inorganic materials 0.000 claims description 77
- 239000000956 alloy Substances 0.000 claims description 77
- 238000000034 method Methods 0.000 claims description 56
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 52
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 claims description 52
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 34
- 229910052758 niobium Inorganic materials 0.000 claims description 31
- 239000010955 niobium Substances 0.000 claims description 31
- 238000010521 absorption reaction Methods 0.000 claims description 28
- 238000005496 tempering Methods 0.000 claims description 19
- 238000005096 rolling process Methods 0.000 claims description 17
- 238000005520 cutting process Methods 0.000 claims description 16
- 238000004321 preservation Methods 0.000 claims description 16
- 239000002994 raw material Substances 0.000 claims description 15
- 230000006698 induction Effects 0.000 claims description 14
- 239000000725 suspension Substances 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 8
- 238000005498 polishing Methods 0.000 claims description 8
- 239000012535 impurity Substances 0.000 claims description 6
- 238000009499 grossing Methods 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 230000000630 rising effect Effects 0.000 claims description 3
- 238000004886 process control Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 5
- 239000011358 absorbing material Substances 0.000 abstract description 11
- 239000011248 coating agent Substances 0.000 abstract description 11
- 238000000576 coating method Methods 0.000 abstract description 11
- 238000013461 design Methods 0.000 abstract description 7
- 238000004458 analytical method Methods 0.000 abstract description 2
- 230000032683 aging Effects 0.000 abstract 1
- 230000035882 stress Effects 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 18
- 239000011888 foil Substances 0.000 description 16
- 239000000463 material Substances 0.000 description 11
- 238000001816 cooling Methods 0.000 description 10
- 230000007547 defect Effects 0.000 description 6
- 238000000265 homogenisation Methods 0.000 description 6
- 229910000831 Steel Inorganic materials 0.000 description 5
- 238000005266 casting Methods 0.000 description 5
- 238000012512 characterization method Methods 0.000 description 5
- 238000007599 discharging Methods 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 238000011534 incubation Methods 0.000 description 5
- 239000011159 matrix material Substances 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 239000010935 stainless steel Substances 0.000 description 5
- 229910001220 stainless steel Inorganic materials 0.000 description 5
- 239000010959 steel Substances 0.000 description 5
- 238000004381 surface treatment Methods 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 229920006351 engineering plastic Polymers 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 2
- 229920003223 poly(pyromellitimide-1,4-diphenyl ether) Polymers 0.000 description 2
- 229920000139 polyethylene terephthalate Polymers 0.000 description 2
- 239000005020 polyethylene terephthalate Substances 0.000 description 2
- 239000002861 polymer material Substances 0.000 description 2
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- YSLWUGPNJFSBON-UHFFFAOYSA-N [Ti].[Gd] Chemical compound [Ti].[Gd] YSLWUGPNJFSBON-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000003252 repetitive effect Effects 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C28/00—Alloys based on a metal not provided for in groups C22C5/00 - C22C27/00
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21J—FORGING; HAMMERING; PRESSING METAL; RIVETING; FORGE FURNACES
- B21J5/00—Methods for forging, hammering, or pressing; Special equipment or accessories therefor
- B21J5/002—Hybrid process, e.g. forging following casting
-
- 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
- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
-
- 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
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
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- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
- G21F1/00—Shielding characterised by the composition of the materials
- G21F1/02—Selection of uniform shielding materials
- G21F1/08—Metals; Alloys; Cermets, i.e. sintered mixtures of ceramics and metals
- G21F1/085—Heavy metals or alloys
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Metallurgy (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Ceramic Engineering (AREA)
- General Engineering & Computer Science (AREA)
- High Energy & Nuclear Physics (AREA)
- Metal Rolling (AREA)
- Measurement Of Radiation (AREA)
Abstract
The invention provides a gadolinium-niobium alloy belt with high neutron absorptivity, a preparation method and application thereof, and belongs to the technical field of neutron collimation spectrometers. The gadolinium-niobium alloy belt with the thickness of 0.1 mm-1 mm and the surface quality is obtained through the preparation steps of component design, smelting, forging, hot rolling, cold rolling, stress relief annealing and the like and the setting of technological parameters of each step, has the tensile strength of higher than 160MPa and the neutron absorptivity of more than 80 percent, has longer service life on the premise of meeting the use performance, fundamentally solves the problems of easy falling and easy aging of the coating of the absorbing material for the existing neutron collimator, and has good application prospect in the fields of neutron analysis, radiology, nuclear industry and the like.
Description
Technical Field
The invention belongs to the technical field of neutron collimation spectrometers, and particularly relates to a gadolinium-niobium alloy belt with high neutron absorptivity, a preparation method and application thereof.
Background
The neutron collimator is a core device of a scattering spectrometer in a large scientific device such as a spallation neutron source and the like, and has the function of absorbing divergent neutrons, so that the neutrons move along a specific angle, the neutrons entering the detector are restrained and collimated, and the resolution of the spectrometer is obviously improved. The neutron collimator affects the intensity, quality, and resolution of the neutron beam utilized by the neutron spectrometer.
The core of the neutron collimator is neutron absorbing material, and the existing neutron absorbing material is Gd with the thickness of 30-100 μm coated on the two sides of a high polymer material (engineering plastic PETP or Kapton film) 2 O 3 Or (b) 10 B 4 The powder C has the problems of low neutron absorptivity, easy falling of a coating, low tensile strength, easy deformation under stress, poor thickness uniformity and the like, and the resolution precision of the neutron collimator is greatly influenced. In addition, the neutron collimator is irradiated by high-energy neutrons in the working process, and the high-molecular materials are accelerated to age, so that the absorption coating is damaged and peeled off, the collimation performance of neutron beams is affected, the service life of the neutron collimator is reduced, and the improvement aspect of the existing neutron collimator is needed.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a gadolinium-niobium alloy belt with high neutron absorptivity, a preparation method and application thereof, and aims to solve the problems of low neutron absorptivity, easy falling of a coating, low tensile strength, easy deformation under stress, poor thickness uniformity and the like of a neutron absorbing material for a neutron collimator at present.
The specific invention comprises the following steps:
in a first aspect, the invention provides a gadolinium-niobium alloy belt with high neutron absorptivity, which consists of high-purity gadolinium and high-purity niobium, wherein the mass ratio of the high-purity gadolinium is 50% -90%.
Optionally, the mass ratio of the high-purity gadolinium is 70% -90%.
Optionally, the thickness of the gadolinium-niobium alloy belt is 0.1 mm-1 mm, the tensile strength is more than 160MPa, and the neutron absorption rate is more than 80%;
the mass percentage of gadolinium element in the high-purity gadolinium is 99.7%, and the mass percentage of niobium element in the high-purity niobium is 99.9%;
the mass ratio of each impurity element in the high-purity gadolinium to the high-purity gadolinium is as follows: ag: <0.02%, al:0.02%, co: <0.01%, cu:0.01%, mg:0.03%, mn:0.03%;
the mass ratio of each impurity element in the high-purity niobium to the high-purity niobium is as follows: ag: <0.005%, al: <0.005%, co:0.02%, cr: 0.02%, cu: <0.01%, mg: <0.005%, mn:0.01%.
In a second aspect, the present invention provides a method for preparing the gadolinium-niobium alloy ribbon with high neutron absorptivity according to the first aspect, the method comprising the following steps:
s1, smelting and ingot pulling by a suspension induction furnace: weighing raw materials of high-purity gadolinium and high-purity niobium, cutting into blocks, mixing, and placing into a suspension induction furnace for smelting and ingot pulling to obtain alloy ingots;
s2, forging: carrying out smoothing treatment on the surface of the alloy ingot, and forging to obtain a plate blank;
s3, hot rolling: treating the cracked edges of the slab, polishing the surface oxide skin clean by a polisher, and then carrying out hot rolling treatment, tempering in the hot rolling process, and annealing after the rolling is completed, so as to obtain a gadolinium-niobium alloy plate completely annealed;
s4, cold rolling: cold rolling the annealed gadolinium-niobium alloy sheet to obtain a cold-rolled gadolinium-niobium alloy strip, wherein the pass processing rate is gradually reduced in the cold rolling process;
s5, stress relief annealing: and carrying out stress relief annealing on the cold-rolled gadolinium-niobium alloy belt under a vacuum condition to obtain the gadolinium-niobium alloy belt with high neutron absorptivity for the neutron collimator.
Optionally, in step S1, the cut thickness of the raw material is not greater than 10 a mm a;
and smelting the suspension induction furnace, wherein the vacuum degree in the furnace is more than 0.01 and Pa when ingot is pulled, and the smelting time is 100-200 min.
Optionally, in step S2, the forging uses a hydraulic forging machine as a forging apparatus; the forging is to perform drawing on the alloy ingot in a direction parallel to ingot pulling; the thickness of the slab is 15 mm-30 mm; the forging process control process conditions include: the initial forging temperature is 750-850 ℃;
finish forging temperature: 700. the temperature is between 800 ℃;
the heat preservation time is set according to the thickness of the alloy and the thickness of the alloy is 5 min/mm;
forging pass: 1-3 times.
Optionally, in step S3, the split edges are cut off by a wire cutting or sawing machine;
the hot rolling is rolling perpendicular to the thickness direction, and the process conditions controlled by the hot rolling process comprise:
rolling temperature: 700. the temperature is between 800 and DEG C;
the processing rate of each pass is less than or equal to 25 percent, and the total processing rate is 80-90 percent;
1-2 times of tempering, wherein the tempering time is set according to the thickness of the slab and the thickness of 4 min/mm;
the thickness of the hot rolled rear plate is 1 mm-2 mm.
Optionally, in step S4, the process conditions controlled in the cold rolling process include:
the processing rate of each pass is controlled to be 5-20 percent;
the thickness of the strip after cold rolling is 0.1 mm-1 mm;
intermediate annealing is carried out for 1-4 times;
the temperature of the intermediate annealing is 520-600 ℃;
the temperature rising rate of the intermediate annealing is 2 ℃/min;
the holding time for the intermediate annealing was 60 min.
Optionally, in step S5, the process conditions controlled by the stress relief annealing process include:
vacuum degree > 10 -3 Pa；
The annealing temperature is 500-550 ℃;
the heat preservation time is 60-120 min.
In a third aspect, the present invention provides an application of the high neutron absorption gadolinium-niobium alloy band according to the first aspect, wherein the Gao Zhongzi absorption gadolinium-niobium alloy band is applied to a neutron collimator.
Compared with the prior art, the invention has the following advantages:
the gadolinium-niobium alloy belt with high neutron absorptivity for the neutron collimator has the thickness of 0.1-mm-1 mm, the tensile strength of higher than 160MPa, the neutron absorptivity of more than 80 percent, and longer service life on the premise of meeting the use performance, and fundamentally solves the problems that the coating of the existing absorbing material for the neutron collimator is easy to fall off and age.
The invention provides a preparation method of a gadolinium-niobium alloy strip with high neutron absorptivity for a neutron collimator, which comprises 5 steps of component design and smelting, forging, hot rolling, cold rolling and stress relief annealing, and the setting of technological parameters of each step, and has the advantages of accurate and controllable obtained thickness, excellent surface quality and good application prospect in the fields of neutron analysis, radiology, nuclear industry and the like.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 shows a flowchart of a preparation method of a gadolinium-niobium alloy tape with high neutron absorptivity provided by the embodiment of the invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. The following description of at least one exemplary embodiment is merely exemplary in nature and is in no way intended to limit the invention, its application, or uses. Any product that is the same as or similar to the present invention, which anyone in the light of the present invention or combines the present invention with other prior art features, falls within the scope of the present invention based on the embodiments of the present invention. And all other embodiments that may be made by those of ordinary skill in the art without undue burden and without departing from the scope of the invention.
Specific experimental steps or conditions are not noted in the examples and may be performed in accordance with the operation or conditions of conventional experimental steps described in the prior art in the field. The reagents used, as well as other instruments, are conventional reagent products available commercially, without the manufacturer's knowledge. Furthermore, the drawings are merely schematic illustrations of embodiments of the invention and are not necessarily drawn to scale. The same reference numerals in the drawings denote the same or similar parts, and thus a repetitive description thereof will be omitted. Some of the block diagrams shown in the figures are functional entities and do not necessarily correspond to physically or logically separate entities.
Techniques, methods and apparatus known to those of ordinary skill in the relevant art may not be discussed in detail, but are intended to be part of the present description where appropriate.
In the description of the present invention, it should be understood that the terms "first," "second," and the like are used for defining the components, and are merely for convenience in distinguishing the corresponding components, and the terms are not meant to have any special meaning unless otherwise indicated, so that the scope of the present invention is not to be construed as being limited.
In addition, the technical features of the different embodiments of the present invention described below may be combined with each other as long as they do not collide with each other.
Because the neutron absorbing material is prepared by coating Gd with the thickness of 30-100 μm on the two sides of the polymer material (engineering plastic PETP or Kapton film) 2 O 3 Or (b) 10 B 4 The neutron absorbing material in the form of the coating has the problems of low neutron absorptivity, easy falling of the coating, low tensile strength, easy deformation under stress, poor thickness uniformity and the like, and the resolution precision of the neutron collimator is greatly influenced. The invention provides a gadolinium-niobium alloy belt with high neutron absorptivity for a neutron collimator, which is composed of gadolinium and niobiumThe gold band is a neutron absorption material, so that the problems of low neutron absorptivity, easy falling of a coating, low tensile strength, easy deformation under stress, poor thickness uniformity and the like caused by using the coating material are avoided. The specific implementation content of the invention is as follows:
in a first aspect, the invention provides a gadolinium-niobium alloy belt with high neutron absorptivity, which consists of high-purity gadolinium and high-purity niobium, wherein the mass ratio of the high-purity gadolinium is 50% -90%.
In the concrete implementation, the neutron absorbing material provided by the invention is a gadolinium-niobium alloy strip, and the gadolinium-niobium alloy strip cannot be directly processed and prepared into a pure metal foil due to the performance of the high-purity metal gadolinium, so that a certain amount of high-purity metal niobium is mixed into the high-purity metal gadolinium to form an alloy under the condition that the performance of the neutron absorbing material is affected by gadolinium, and the gadolinium-niobium alloy has certain plasticity to improve the processability of the strip. And the gadolinium-niobium alloy has certain oxidation resistance and corrosion resistance, and avoids the oxidation loss of high-purity metal niobium caused by high temperature and oxygen environment in the processing process.
In specific implementation, the gadolinium-niobium alloy belt is obtained by smelting, forging, hot rolling, cold rolling, stress relief annealing and other processes from high-purity gadolinium with the mass ratio of 50-90% and high-purity niobium with the mass ratio of 10-50%. The neutron absorbing material exists in the form of gadolinium-niobium alloy band, so that various defects of the neutron absorbing material in the form of a coating are avoided, the collimation performance of neutron beams is improved, and the service life of a neutron collimator is prolonged.
In the concrete implementation, the mass percentage of gadolinium element in the high-purity gadolinium is 99.7%, and the mass percentage of the rest impurity elements is as follows: ag: <0.02%, al:0.02%, co: <0.01%, cu:0.01%, mg:0.03%, mn:0.03%; the mass percentage of niobium element in the high-purity niobium is 99.9%, and the mass percentage of other impurity elements is as follows: ag: <0.005%, al: <0.005%, co:0.02%, cr: 0.02%, cu: <0.01%, mg: <0.005%, mn:0.01%.
In some embodiments, when the mass ratio of the high-purity gadolinium is 70% -90%, the neutron absorption rate of the prepared gadolinium-niobium alloy belt is above 85%, and can even reach 92%. Has high neutron absorptivity.
Further, the gadolinium-niobium alloy belt provided by the invention has the thickness of 0.1-mm-1 mm, the tensile strength of more than 160MPa and the neutron absorptivity of more than 80%;
in a second aspect, the present invention provides a method for preparing a high neutron absorption rate gadolinium-niobium alloy ribbon according to the first aspect, fig. 1 shows a flowchart of a method for preparing a high neutron absorption rate gadolinium-niobium alloy ribbon according to an embodiment of the present invention, and as shown in fig. 1, the method for preparing a high neutron absorption rate gadolinium-niobium alloy ribbon includes the following steps:
s1, smelting and ingot pulling by a suspension induction furnace: weighing raw materials of high-purity gadolinium and high-purity niobium, cutting into blocks, mixing, and placing into a suspension induction furnace for smelting and ingot pulling to obtain alloy ingots;
when the step is specifically implemented, smelting and ingot pulling are performed simultaneously. Further, in order to ensure homogenization of alloy components during smelting, the bulk materials of high-purity gadolinium and high-purity niobium with larger volume are processed into small blocks with the maximum thickness not exceeding 10 mm; the vacuum degree in the furnace is more than 0.01 and Pa when the suspension induction furnace is used for smelting and ingot pulling, and the smelting time is 100-200 min.
S2, forging: carrying out smoothing treatment on the surface of the alloy ingot, and forging to obtain a plate blank;
when the step is specifically implemented, a hydraulic forging machine is adopted as forging equipment for forging; the forging is specifically to draw the alloy ingot in a direction parallel to the ingot drawing direction; the thickness of the slab obtained after the drawing is 15 mm-30 mm; the technological conditions for controlling the forging process specifically comprise: the initial forging temperature is 750-850 ℃; finish forging temperature: 700. the temperature is between 800 ℃; the heat preservation time is set according to the thickness of the alloy and the thickness of the alloy is 5 min/mm; forging pass: 1-3 times.
S3, hot rolling: treating the cracked edges of the slab, polishing the surface oxide skin clean by a polisher, and then carrying out hot rolling treatment, tempering in the hot rolling process, and annealing after the rolling is completed, so as to obtain a gadolinium-niobium alloy plate completely annealed;
when the step is specifically implemented, the processing mode of the split edges can be to cut off the split edges by adopting a linear cutting or sawing machine; the hot rolling is rolling perpendicular to the thickness direction, and the process conditions controlled by the hot rolling process include: rolling temperature: 700. the temperature is between 800 and DEG C; the processing rate of each pass is less than or equal to 25 percent, and the total processing rate is 80-90 percent; 1-2 times of tempering, wherein the tempering time is set according to the thickness of the slab and the thickness of 4 min/mm; the thickness of the hot rolled rear plate is 1 mm-2 mm.
S4, cold rolling: cold rolling the annealed gadolinium-niobium alloy sheet to obtain a cold-rolled gadolinium-niobium alloy strip, wherein the pass processing rate is gradually reduced in the cold rolling process;
when the step is specifically implemented, the process conditions controlled in the cold rolling process include: the processing rate of each pass is controlled to be 5-20 percent; the thickness of the strip after cold rolling is 0.1 mm-1 mm; judging the time of intermediate annealing according to the plate surface condition, wherein the intermediate annealing is performed for 1-4 times; the temperature of the intermediate annealing is 520-600 ℃; the temperature rising rate of the intermediate annealing is 2 ℃/min; the holding time for the intermediate annealing was 60 min.
S5, stress relief annealing: and carrying out stress relief annealing on the cold-rolled gadolinium-niobium alloy belt under a vacuum condition to obtain the gadolinium-niobium alloy belt with high neutron absorptivity for the neutron collimator.
When the step is specifically implemented, stress relief annealing is carried out, so that the finally obtained gadolinium-niobium alloy belt releases redundant stress under the vacuum annealing condition to see i, and the gadolinium-niobium alloy belt obtains better consistency. The process conditions for controlling the stress relief annealing process include: vacuum degree > 10 -3 Pa; the annealing temperature is 500-550 ℃; the heat preservation time is 60-120 min.
In a third aspect, the present invention provides an application of the high neutron absorption gadolinium-niobium alloy band according to the first aspect, wherein the Gao Zhongzi absorption gadolinium-niobium alloy band is applied to a neutron collimator.
In order to make the present invention more clearly understood by those skilled in the art, the following examples will illustrate a gadolinium-niobium alloy ribbon with high neutron absorptivity, a preparation method and applications thereof.
Example 1
The high neutron absorptivity gadolinium-niobium alloy belt for neutron collimator is prepared from high-purity gadolinium and high-purity niobium.
The high-purity gadolinium comprises the following elements in percentage by mass: ag: <0.02%, al:0.02%, co: <0.01%, cu:0.01%, mg:0.03%, mn:0.03%;
the high-purity niobium comprises the following elements in percentage by mass: ag: <0.005%, al: <0.005%, co:0.02%, cr: 0.02%, cu: <0.01%, mg: <0.005%, mn:0.01%.
An embodiment of a preparation method of a gadolinium-niobium alloy belt with high neutron absorptivity is carried out according to the following steps:
(1) Composition design
Gd element is selected as an alloy matrix element, nb element is selected as an alloy element, and Gd is prepared according to the mass ratio: nb=50: 50 the theoretical neutron absorption rate of the alloy strip thickness is 80% and 82% when the thickness of the alloy strip is 0.1mm and 1mm respectively.
(2) Proportioning materials
The weight ratio Gd: nb=50: and 50, weighing high-purity gadolinium and high-purity niobium. To ensure homogenization of the alloy composition during smelting, the relatively large gadolinium block is processed into small gadolinium blocks with a maximum thickness of no more than 10 mm.
(3) Smelting and ingot pulling
And (3) uniformly mixing the raw materials weighed in the step (2), putting the mixture into a suspension induction furnace for smelting, vacuumizing to a vacuum degree higher than 0.01 and Pa, slowly drawing the mixture into an alloy ingot with the thickness of 200mm after the raw materials are melted, cooling the alloy ingot to a temperature below 100 ℃, and discharging the alloy ingot, wherein the alloy ingot has the specification of 200mm and the length of 300mm.
(4) Forging
Cutting off riser and bottom casting defects of the alloy ingot obtained in the step (3) by using a sawing machine, and then smoothing the surface by using a planing machine, wherein the specification of the processed alloy ingot is 190mm multiplied by 290 multiplied by mm (thickness multiplied by length). The hydraulic forging machine is adopted as forging equipment, and the forged alloy is a plate blank with the thickness of 25 mm. The method comprises the steps of adopting 4-pass forging, wherein the initial forging temperature of a first pass is 800 ℃, the final forging temperature is 700 ℃,190 mm-120 mm, the processing rate is 37%, the initial forging temperature of a second pass is 800 ℃, the final forging temperature is 710 ℃,120 mm-70 m, the processing rate is 42%, the initial forging temperature of a third pass is 800 ℃, the final forging temperature is 710 ℃,70 mm-40 mm, the processing rate is 42%, the initial forging temperature of a fourth pass is 800 ℃, the final forging temperature is 710 ℃,40 mm-25 mm, the processing rate is 38%, the total processing rate is 87%, and the heat preservation time is set according to the thickness of an alloy to be 5 min/mm.
(5) Hot rolling
And (3) cutting off the split edges generated in the step (4) by using a sawing machine, and polishing the surface oxide skin by using a polisher. The hot rolling temperature is set to 800 ℃, the rolling is carried out in the vertical thickness direction, the processing rate of each pass is not more than 25%, the total rolling is 20 passes, one tempering is carried out in 1-2 passes, the intermediate tempering time is set according to the thickness of the slab and is set to 4min/mm, the final thickness of the slab after hot rolling is 2mm, and the total processing rate is 88%.
(6) Cold rolling
The annealed gadolinium-niobium alloy is processed into the required width dimension and then cold-rolled, the pass processing rate is gradually reduced along with the increase of the deformation, the processing rate of each pass is controlled to be 5-20%, and the thicknesses of the cold-rolled strips are respectively 0.1mm, 0.2mm, 0.5mm, 0.8mm and 1mm. The temperature of the intermediate annealing is set to 600 ℃, the heating speed is set to 2 ℃/min, the heat preservation time is 60min, and the average cooling speed is set<0.5 At a temperature of 10℃per minute and a vacuum degree of -3 Pa, annealing for 4 times in the cold rolling process.
(7) Stress relief annealing
The cold-rolled gadolinium-niobium alloy strip is processed into a required width size, is laid between stainless steel plates, and the periphery of the plates is fixed by bolts and the like. After the assembly, the steel plate is horizontally placed in a vacuum resistance furnace for stress relief annealing, and the vacuum degree is higher than 10 -3 Pa, the annealing temperature was set to 550℃and the incubation time was set to 60 min.
(8) Characterization of Performance
1) The thickness of the strip obtained in the step (7) is respectively 0.1mm, 0.2mm, 0.5mm, 0.8mm and 1mm measured by a GB/T6462-2005 method;
2) The tensile strength of the strip obtained in the step (7) is 185MPa, 186MPa, 188MPa, 189MPa and 190MPa respectively measured by a GB/T228.1-2010 method;
3) And (3) measuring the roughness of the foil in the step 1) in the vertical grain direction by using a TIME3230 roughness meter to be 0.24+/-0.02 mu m, and measuring the roughness of the foil in the parallel grain direction to be 0.19+/-0.02 mu m.
4) The neutron absorption rates of the strips were 85%, 86%, 87%, 88%, 90%, respectively, as measured using spallation neutron sources.
Example 2
The high neutron absorptivity gadolinium-niobium alloy belt for neutron collimator is prepared from high-purity gadolinium and high-purity niobium.
The high-purity gadolinium comprises the following elements in percentage by mass: ag: <0.02%, al:0.02% Co: <0.01%, cu:0.01% Mg:0.03% Mn:0.03 The%;
the high-purity niobium comprises the following elements in percentage by mass: ag: <0.005%, al: <0.005%, co:0.02% Cr:0.02 % Cu: <0.01%, mg: <0.005%, mn:0.01 Percent of the total weight of the composition.
An embodiment of a method for preparing a gadolinium-niobium alloy belt with high neutron absorptivity for a neutron collimator is carried out according to the following steps:
(1) Composition design
Gd element is selected as an alloy matrix element, nb element is selected as an alloy element, and Gd is prepared according to the mass ratio: nb=60: 40 the theoretical neutron absorption rate of the alloy foil with the thickness of 0.1mm and 1mm is 86 percent and 88 percent respectively.
(2) Proportioning materials
The weight ratio Gd: nb=60: and 40, weighing high-purity gadolinium and high-purity niobium. To ensure homogenization of the alloy composition during smelting, the relatively large gadolinium block is processed into small gadolinium blocks with a maximum thickness of no more than 10 mm.
(3) Smelting and ingot pulling
And (3) uniformly mixing the raw materials weighed in the step (2), putting the mixture into a suspension induction furnace for smelting, vacuumizing to a vacuum degree higher than 0.01 and Pa, slowly drawing the mixture into an alloy ingot with the diameter of 180 mm after the raw materials are completely melted, discharging the alloy ingot from the furnace for air cooling after the furnace is cooled to a temperature below 100 ℃, wherein the alloy ingot has the specification of 180-mm thickness and 350-mm length.
(4) Forging
Cutting off riser and bottom casting defects of the alloy ingot obtained in the step (3) by using a sawing machine, and then smoothing the surface by using a planing machine, wherein the specification of the processed alloy ingot is 170 mm multiplied by 340 mm (thickness multiplied by length). The hydraulic forging machine is adopted as forging equipment, and the forged alloy is a plate blank with the thickness of 20 mm. The method comprises the steps of adopting 4-pass forging, wherein the initial forging temperature of a first pass is 810 ℃, the final forging temperature is 710 ℃,170 mm-110 mm, the processing rate is 35%, the initial forging temperature of a second pass is 810 ℃, the final forging temperature is 710 ℃,110 mm-60 mm, the processing rate is 45%, the initial forging temperature of a third pass is 810 ℃, the final forging temperature is 710 ℃,60 mm-40 mm, the processing rate is 33%, the initial forging temperature of a fourth pass is 810 ℃, the final forging temperature is 710 ℃,40 mm-25 mm, the processing rate is 38%, the total processing rate is 83%, and the heat preservation time is set according to the thickness of an alloy to be 5 min/mm.
(5) Hot rolling
And (3) cutting off the split edges generated in the step (4) by using a sawing machine, and polishing the surface oxide skin by using a polisher. The hot rolling temperature is set to 800 ℃, the rolling is carried out in the vertical thickness direction, the processing rate of each pass is not more than 25%, the total rolling is 20 passes, one tempering is carried out in 1-2 passes, the intermediate tempering time is set according to the thickness of the slab at 4min/mm, the final thickness of the slab after hot rolling is 1.7-mm, and the total processing rate is 90%.
(6) Cold rolling
The annealed gadolinium-niobium alloy plate is processed into the required width dimension and then is cold-rolled, the pass processing rate is gradually reduced along with the increase of the deformation, the processing rate of each pass is controlled to be 5-20%, and the thickness of the cold-rolled strip is respectively 0.1mm, 0.2mm, 0.5mm, 0.8mm and 1mm. The temperature of the intermediate annealing is set to 580 ℃, the heating speed is set to 2 ℃/min, the heat preservation time is 80 min, and the average cooling speed is set<0.5 At a temperature of 10℃per minute and a vacuum degree of -3 Pa, annealing for 4 times in the cold rolling process.
(7) Stress relief annealing
After the cold-rolled gadolinium-niobium alloy belt is processed into the required width size, the gadolinium-niobium alloy belt is paved between stainless steel plates, and the periphery of the plates is fixed by bolts and the like. After the assembly, the steel plate is horizontally placed in a vacuum resistance furnace for stress relief annealing, and the vacuum degree is higher than 10 -3 Pa, the annealing temperature is set to 530 ℃, and the incubation time is set to 90 min.
(8) Characterization of Performance
1) The thickness of the strip obtained in the step (7) is measured by a GB/T6462-2005 method to be 0.1mm, 0.2mm, 0.5mm, 0.8mm and 1mm respectively;
2) The tensile strength of the strip obtained in the step (7) is 183 MPa, 185MPa, 186MPa, 188MPa and 189MPa respectively measured by a GB/T228.1-2010 method;
3) And (3) measuring the roughness of the foil in the step 1) in the vertical grain direction by using a TIME3230 roughness meter to be 0.24+/-0.02 mu m, and measuring the roughness of the foil in the parallel grain direction to be 0.19+/-0.02 mu m.
4) The neutron absorption rates of the strips measured by using spallation neutron sources are 87%, 89%, 90%, 91% and 92%, respectively.
Example 3
The high neutron absorptivity gadolinium-niobium alloy belt for neutron collimator is prepared from high purity gadolinium and high purity titanium.
The high-purity gadolinium comprises the following elements in percentage by mass: ag: <0.02%, al:0.02%, co: <0.01%, cu:0.01%, mg:0.03%, mn:0.03%;
the high-purity niobium comprises the following elements in percentage by mass: ag: <0.005%, al: <0.005%, co:0.02%, cr: 0.02%, cu: <0.01%, mg: <0.005%, mn:0.01%.
An embodiment of a method for preparing a gadolinium-niobium alloy belt with high neutron absorptivity for a neutron collimator is carried out according to the following steps:
(1) Composition design
Gd element is selected as an alloy matrix element, nb element is selected as an alloy element, and Gd is prepared according to the mass ratio: the theoretical neutron absorption rates at 0.1mm and 1mm for nb=70:30 calculated alloy foil thickness were 90% and 95%, respectively.
(2) Proportioning materials
The weight ratio Gd: nb=70:30 high purity gadolinium and high purity niobium were weighed. In order to ensure the homogenization of alloy components during smelting, gadolinium blocks with larger volume are processed into small gadolinium blocks with the maximum thickness of not more than 10 mm.
(3) Smelting and ingot pulling
And (3) uniformly mixing the raw materials weighed in the step (2), putting the mixture into a suspension induction furnace for smelting, vacuumizing to a vacuum degree higher than 0.01Pa, slowly drawing the mixture into an alloy ingot with the diameter of 150mm after the raw materials are completely melted, discharging the alloy ingot from the furnace for air cooling after the furnace is cooled to below 100 ℃, wherein the alloy ingot has the specification of 150mm in diameter and 300mm in length.
(4) Forging
Cutting off riser and bottom casting defects of the alloy ingot obtained in the step (3) by using a sawing machine, and then, carrying out surface treatment on the alloy ingot by using a planing machine to obtain the finished alloy ingot with the specification of 140mm multiplied by 280mm. The hydraulic forging machine is adopted as forging equipment, and the forged alloy is a plate blank with the thickness of 18 mm. 4-pass forging is adopted, the initial forging temperature of the first pass is 800 ℃, the final forging temperature is 700 ℃,140 mm-100 mm, the processing rate is 29%, the initial forging temperature of the second pass is 800 ℃, the final forging temperature is 700 ℃,100 mm-70 mm, the processing rate is 30%, the initial forging temperature of the third pass is 800 ℃, the final forging temperature is 700 ℃,70 mm-45 mm, the processing rate is 36%, the initial forging temperature of the fourth pass is 800 ℃, the final forging temperature is 700 ℃,45 mm-28 mm, the processing rate is 38%, the total processing rate is 80%, and the heat preservation time is set according to the alloy thickness of 5 min/mm.
(5) Hot rolling
And (3) cutting off the split edges generated in the step (4) by using a sawing machine, and polishing the surface oxide skin by using a polisher. The hot rolling temperature is set to 800 ℃, the rolling is carried out in the vertical thickness direction, the processing rate of each pass is not more than 25%, the total rolling is 20 passes, one tempering is carried out in 1-2 passes, the intermediate tempering time is set according to the thickness of the slab and is set to 4min/mm, the final thickness of the slab after hot rolling is 1.5mm, and the total processing rate is 90%.
(6) Cold rolling
The annealed gadolinium-niobium alloy is processed into the required width dimension and then cold-rolled, the pass processing rate is gradually reduced along with the increase of the deformation, the processing rate of each pass is controlled to be 5% -20%, and the thickness of the cold-rolled strip is respectively 0.1mm, 0.2mm, 0.5mm, 0.8mm and 1mm. The temperature of the intermediate annealing is set to 550 ℃, the heating speed is set to 2 ℃/min, the heat preservation time is 100min, and the average cooling speed<0.5 ℃/min and a vacuum degree of 10 -3 Pa, annealing for 4 times in the cold rolling process.
(7) Stress relief annealing
After the cold-rolled gadolinium-niobium alloy belt is processed into the required width size, the gadolinium-niobium alloy belt is laid between stainless steel plates, and the periphery of the plates is fixed by bolts and the likeAnd (5) setting. After the assembly, the steel plate is horizontally placed in a vacuum resistance furnace for stress relief annealing, and the vacuum degree is higher than 10 -3 Pa, the annealing temperature is set to 520 ℃, and the incubation time is set to 100min.
(8) Characterization of Performance
1) The thickness of the strip obtained in the step (7) is respectively 0.1mm, 0.2mm, 0.5mm, 0.8mm and 1mm measured by a GB/T6462-2005 method;
2) The tensile strength of the strip obtained in the step (7) is 185MPa, 186MPa, 188MPa, 189MPa and 190MPa respectively measured by a GB/T228.1-2010 method;
3) And (3) measuring the roughness of the foil in the step 1) in the vertical grain direction by using a TIME3230 roughness meter to be 0.24+/-0.02 mu m, and measuring the roughness of the foil in the parallel grain direction to be 0.19+/-0.02 mu m.
4) The neutron absorption rates of the strips are 88%, 89%, 90% and 92% respectively measured by using spallation neutron sources.
Example 4
The high neutron absorptivity gadolinium-titanium alloy belt for neutron collimator is prepared from high-purity gadolinium and high-purity niobium.
The high-purity gadolinium comprises the following elements in percentage by mass: ag: <0.02%, al:0.02%, co: <0.01%, cu:0.01%, mg:0.03%, mn:0.03%;
the high-purity niobium comprises the following elements in percentage by mass: ag: <0.005%, al: <0.005%, co:0.02%, cr: 0.02%, cu: <0.01%, mg: <0.005%, mn:0.01%.
An embodiment of a method for preparing a gadolinium-niobium alloy belt with high neutron absorptivity for a neutron collimator is carried out according to the following steps:
(1) Composition design
Gd element is selected as an alloy matrix element, ti element is selected as an alloy element, and Gd is prepared according to the mass ratio: theoretical neutron absorption rates at 0.1 and 1mm for nb=80:20 calculated alloy foil thickness are 90% and 95%, respectively.
(2) Proportioning materials
The weight ratio Gd: nb=80:20 high purity gadolinium and high purity niobium were weighed. In order to ensure the homogenization of alloy components during smelting, gadolinium blocks with larger volume are processed into small gadolinium blocks with the maximum thickness of not more than 10 mm.
(3) Smelting and ingot pulling
And (3) uniformly mixing the raw materials weighed in the step (2), putting the mixture into a suspension induction furnace for smelting, vacuumizing to a vacuum degree higher than 0.01Pa, slowly drawing the mixture into an alloy ingot with the diameter of 200mm after the raw materials are completely melted, discharging the alloy ingot from the furnace for air cooling after the furnace is cooled to below 100 ℃, wherein the alloy ingot has the specification of 150mm in diameter and 280mm in length.
(4) Forging
Cutting off riser and bottom casting defects of the alloy ingot obtained in the step (3) by using a sawing machine, and then, carrying out surface treatment on the alloy ingot by using a planing machine to obtain the finished alloy ingot with the specification of 130mm multiplied by 250mm. The hydraulic forging machine is adopted as forging equipment, and the forged alloy is a plate blank with the thickness of 18 mm. The method comprises the steps of adopting 4-pass forging, wherein the initial forging temperature of a first pass is 780 ℃, the final forging temperature is 700 ℃,120 mm-80 mm, the processing rate is 33%, the initial forging temperature of a second pass is 780 ℃, the final forging temperature is 700 ℃,80 mm-50 mm, the processing rate is 38%, the initial forging temperature of a third pass is 780 ℃, the final forging temperature is 700 ℃,50 mm-32 mm, the processing rate is 36%, the initial forging temperature of a fourth pass is 780 ℃, the final forging temperature is 700 ℃,32 mm-20 mm, the processing rate is 34%, the total processing rate is 84%, and the heat preservation time is set according to the thickness of an alloy according to 5 min/mm.
(5) Hot rolling
And (3) cutting off the split edges generated in the step (4) by using a sawing machine, and polishing the surface oxide skin by using a polisher. The hot rolling temperature is set to 750 ℃, the rolling is carried out in the vertical thickness direction, the processing rate of each pass is not more than 25%, 18 passes are carried out in total, one tempering is carried out in 1-2 passes, the intermediate tempering time is set according to the thickness of the slab, the final thickness of the slab after hot rolling is 1.5mm, and the total processing rate is 93%.
(6) Cold rolling
The annealed gadolinium-niobium alloy plate is processed into the required width dimension and then cold-rolled, the pass processing rate is gradually reduced along with the increase of the deformation, the processing rate of each pass is controlled to be 5% -20%, and the thickness of the cold-rolled foil is respectively 0.1mm, 0.2mm, 0.5mm, 0.8mm and 1mm. The temperature of the intermediate annealing is set to 600 ℃, the heating speed is set to 2 ℃/min, the heat preservation time is 60min, and the average cooling speed is set<0.5 ℃/min and a vacuum degree of 10 -3 Pa, annealing for 4 times in the cold rolling process.
(7) Stress relief annealing
After the cold-rolled gadolinium-niobium alloy belt is processed into the required width size, the gadolinium-niobium alloy belt is paved between stainless steel plates, and the periphery of the plates is fixed by bolts and the like. After the assembly, the steel plate is horizontally placed in a vacuum resistance furnace for stress relief annealing, and the vacuum degree is higher than 10 -3 Pa, the annealing temperature is set to 520 ℃, and the incubation time is set to 100min.
(8) Characterization of Performance
1) The thickness of the strip obtained in the step (7) is respectively 0.1mm, 0.2mm, 0.5mm, 0.8mm and 1mm measured by a GB/T6462-2005 method;
2) The tensile strength of the strip obtained in the step (7) is 185MPa, 186MPa, 188MPa, 189MPa and 190MPa respectively measured by a GB/T228.1-2010 method;
3) And (3) measuring the roughness of the foil in the step 1) in the vertical grain direction by using a TIME3230 roughness meter to be 0.24+/-0.02 mu m, and measuring the roughness of the foil in the parallel grain direction to be 0.19+/-0.02 mu m.
4) The neutron absorption rates of the strips are respectively 85%, 88%, 89%, 90% and 91% measured by using spallation neutron sources.
Example 5
The high neutron absorptivity gadolinium-niobium alloy belt for neutron collimator is prepared from high-purity gadolinium and high-purity niobium.
The high-purity gadolinium comprises the following elements in percentage by mass: ag: <0.02%, al:0.02%, co: <0.01%, cu:0.01%, mg:0.03%, mn:0.03%;
the high-purity niobium comprises the following elements in percentage by mass: ag: <0.005%, al: <0.005%, co:0.02%, cr: 0.02%, cu: <0.01%, mg: <0.005%, mn:0.01%.
An embodiment of a method for preparing a gadolinium-niobium alloy belt with high neutron absorptivity for a neutron collimator is carried out according to the following steps:
(1) Composition design
Gd element is selected as an alloy matrix element, nb element is selected as an alloy element, and Gd is prepared according to the mass ratio: theoretical neutron absorption rates at 0.1 and 1mm for nb=90:10 calculated alloy foil thickness are 90% and 95%, respectively.
(2) Proportioning materials
The weight ratio Gd: nb=90:10 high purity gadolinium and high purity niobium were weighed. In order to ensure the homogenization of alloy components during smelting, gadolinium blocks with larger volumes are processed into small blocks with the maximum thickness of not more than 10 mm.
(3) Smelting and ingot pulling
And (3) uniformly mixing the raw materials weighed in the step (2), putting the mixture into a suspension induction furnace for smelting, vacuumizing to a vacuum degree higher than 0.01Pa, slowly drawing the mixture into an alloy ingot with the diameter of 100mm after the raw materials are completely melted, discharging the alloy ingot from the furnace for air cooling after the furnace is cooled to below 100 ℃, wherein the alloy ingot has the diameter of 100mm and the length of 200mm.
(4) Forging
Cutting off riser and bottom casting defects of the alloy ingot obtained in the step (3) by using a sawing machine, and then, carrying out surface treatment on the alloy ingot by using a planing machine to obtain the finished alloy ingot with the specification of 90mm multiplied by 190mm. The hydraulic forging machine is adopted as forging equipment, and the forged alloy is a plate blank with the thickness of 20 mm. 3-pass forging is adopted, the initial forging temperature of the first pass is 780 ℃, the final forging temperature is 700 ℃, 90 mm-60 mm, the processing rate is 34%, the initial forging temperature of the second pass is 780 ℃, the final forging temperature is 700 ℃,60 mm-30 mm, the processing rate is 50%, the initial forging temperature of the third pass is 780 ℃, the final forging temperature is 700 ℃,30 mm-15 mm, the processing rate is 50%, the total processing rate is 84%, and the heat preservation time is set according to the thickness of the alloy and is 5 min/mm.
(5) Hot rolling
And (3) cutting off the split edges generated in the step (4) by using a sawing machine, and polishing the surface oxide skin by using a polisher. The hot rolling temperature is set to 700 ℃, the rolling is carried out in the vertical thickness direction, the processing rate of each pass is not more than 25%, 15 passes are carried out in total, one tempering is carried out in 1-2 passes, the intermediate tempering time is set according to the thickness of the plate blank according to 4min/mm, the final thickness of the plate blank after hot rolling is 1mm, and the total processing rate is 94%.
(6) Cold rolling
The annealed gadolinium-niobium alloy is processed into the required width dimension and then cold-rolled, the pass processing rate is gradually reduced along with the increase of the deformation, and the processing rate of each pass is controlled to be 5-20 percentThe thickness of the strip after cold rolling was 0.1mm, 0.2mm, 0.5mm, 0.8mm and 1mm, respectively. The temperature of the intermediate annealing is set to 520 ℃, the heating speed is set to 2 ℃/min, the heat preservation time is 120min, and the average cooling speed<0.5 ℃/min and a vacuum degree of 10 -3 Pa, annealing for 4 times in the cold rolling process.
(7) Stress relief annealing
After the cold-rolled gadolinium-niobium alloy belt is processed into the required width size, the gadolinium-niobium alloy belt is paved between stainless steel plates, and the periphery of the plates is fixed by bolts and the like. After the assembly, the steel plate is horizontally placed in a vacuum resistance furnace for stress relief annealing, and the vacuum degree is higher than 10 -3 Pa, the annealing temperature is set to 500 ℃, and the incubation time is set to 120min.
(8) Characterization of Performance
1) The thickness of the strip obtained in the step (7) is respectively 0.1mm, 0.2mm, 0.5mm, 0.8mm and 1mm measured by a GB/T6462-2005 method;
2) The tensile strength of the strip obtained in the step (7) is 185MPa, 186MPa, 188MPa, 189MPa and 190MPa respectively measured by a GB/T228.1-2010 method;
3) And (3) measuring the roughness of the foil in the step 1) in the vertical grain direction by using a TIME3230 roughness meter to be 0.24+/-0.02 mu m, and measuring the roughness of the foil in the parallel grain direction to be 0.19+/-0.02 mu m.
4) The neutron absorption rates of the gadolinium-niobium alloy belts are 88%, 89%, 90%, 91% and 92% respectively measured by using a spallation neutron source.
In the description of the present specification, a description referring to terms "one embodiment," "some embodiments," "examples," "specific examples," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms are not necessarily directed to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, one skilled in the art can combine and combine the different embodiments or examples described in this specification.
For the purposes of simplicity of explanation, the methodologies are shown as a series of acts, but one of ordinary skill in the art will recognize that the present invention is not limited by the order of acts described, as some acts may, in accordance with the present invention, occur in other orders and concurrently. Further, those skilled in the art will recognize that the embodiments described in the specification are all of the preferred embodiments, and that the acts and components referred to are not necessarily required by the present invention.
The gadolinium-niobium alloy strip with high neutron absorptivity, the preparation method and the application provided by the invention are described in detail, and specific examples are applied to illustrate the principle and the implementation mode of the invention, and the description of the examples is only used for helping to understand the method and the core idea of the invention; meanwhile, as those skilled in the art will have variations in the specific embodiments and application scope in accordance with the ideas of the present invention, the present description should not be construed as limiting the present invention in view of the above.
Claims (10)
1. The gadolinium-niobium alloy belt with high neutron absorptivity is characterized by comprising high-purity gadolinium and high-purity niobium, wherein the mass ratio of the high-purity gadolinium is 50% -90%, and the neutron absorptivity of the gadolinium-niobium alloy belt is more than 80%.
2. The high neutron absorbing rate gadolinium-niobium alloy ribbon according to claim 1, wherein the high purity gadolinium is 70% to 90% by mass.
3. The high neutron absorption gadolinium-niobium alloy ribbon according to claim 1 or 2, wherein the gadolinium-niobium alloy ribbon has a thickness of 0.1 mm-1 mm, a tensile strength > 160MPa, and a neutron absorption > 80%;
the mass percentage of gadolinium element in the high-purity gadolinium is 99.7%, and the mass percentage of niobium element in the high-purity niobium is 99.9%;
the mass ratio of each impurity element in the high-purity gadolinium to the high-purity gadolinium is as follows: ag: <0.02%, al:0.02%, co: <0.01%, cu:0.01%, mg:0.03%, mn:0.03%;
the mass ratio of each impurity element in the high-purity niobium to the high-purity niobium is as follows: ag: <0.005%, al: <0.005%, co:0.02%, cr: 0.02%, cu: <0.01%, mg: <0.005%, mn:0.01%.
4. A method for preparing the high neutron absorptivity gadolinium-niobium alloy strip according to claim 1, comprising the following steps:
s1, smelting and ingot pulling by a suspension induction furnace: weighing raw materials of high-purity gadolinium and high-purity niobium, cutting into blocks, mixing, and placing into a suspension induction furnace for smelting and ingot pulling to obtain alloy ingots;
s2, forging: carrying out smoothing treatment on the surface of the alloy ingot, and forging to obtain a plate blank;
s3, hot rolling: treating the cracked edges of the slab, polishing the surface oxide skin clean by a polisher, and then carrying out hot rolling treatment, tempering in the hot rolling process, and annealing after the rolling is completed, so as to obtain a gadolinium-niobium alloy plate completely annealed;
s4, cold rolling: cold rolling the annealed gadolinium-niobium alloy sheet to obtain a cold-rolled gadolinium-niobium alloy strip, wherein the pass processing rate is gradually reduced in the cold rolling process;
s5, stress relief annealing: and carrying out stress relief annealing on the cold-rolled gadolinium-niobium alloy belt under a vacuum condition to obtain the gadolinium-niobium alloy belt with high neutron absorptivity for the neutron collimator.
5. The method for producing a high neutron absorption rate gadolinium-niobium alloy strip according to claim 4, wherein in step S1, the cut thickness of the raw material is not more than 10 mm;
and smelting the suspension induction furnace, wherein the vacuum degree in the furnace is more than 0.01 and Pa when ingot is pulled, and the smelting time is 100-200 min.
6. The method for producing a high neutron absorption rate gadolinium-niobium alloy strip according to claim 4, wherein in step S2, the forging uses a hydraulic forging machine as a forging apparatus; the forging is to perform drawing on the alloy ingot in a direction parallel to ingot pulling; the thickness of the slab is 15 mm-30 mm; the forging process control process conditions include: the initial forging temperature is 750-850 ℃;
finish forging temperature: 700. the temperature is between 800 ℃;
the heat preservation time is set according to the thickness of the alloy and the thickness of the alloy is 5 min/mm;
forging pass: 1-3 times.
7. The method for producing a high neutron absorptivity gadolinium-niobium alloy strip according to claim 4, wherein in step S3, the split edges are cut off by a wire cutting or sawing machine;
the hot rolling is rolling perpendicular to the thickness direction, and the process conditions controlled by the hot rolling process comprise:
rolling temperature: 700. the temperature is between 800 and DEG C;
the processing rate of each pass is less than or equal to 25 percent, and the total processing rate is 80-90 percent;
1-2 times of tempering, wherein the tempering time is set according to the thickness of the slab and the thickness of 4 min/mm;
the thickness of the hot rolled rear plate is 1 mm-2 mm.
8. The method for producing a high neutron absorption rate gadolinium-niobium alloy strip according to claim 4, wherein in step S4, the process conditions controlled during the cold rolling process include:
the processing rate of each pass is controlled to be 5-20 percent;
the thickness of the strip after cold rolling is 0.1 mm-1 mm;
intermediate annealing is carried out for 1-4 times;
the temperature of the intermediate annealing is 520-600 ℃;
the temperature rising rate of the intermediate annealing is 2 ℃/min;
the holding time for the intermediate annealing was 60 min.
9. The method for producing high neutron absorbing gadolinium-niobium alloy ribbon according to claim 4, wherein the process conditions for controlling the stress-relief annealing process in step S5 include:
vacuum degree > 10 -3 Pa；
The annealing temperature is 500-550 ℃;
the heat preservation time is 60-120 min.
10. Use of the high neutron absorption gadolinium-niobium alloy ribbon according to claim 1, wherein the Gao Zhongzi absorption gadolinium-niobium alloy ribbon is used in a neutron collimator.
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| CN1676657A (en) * | 2004-04-02 | 2005-10-05 | 中国科学院物理研究所 | Gadolinium-base block amorphous alloy and its preparing method |
| CN114196864A (en) * | 2021-11-25 | 2022-03-18 | 江苏大学 | Y-Gd-based alloy, neodymium cerium iron boron magnet comprising same and preparation method |
| CN116230259A (en) * | 2023-05-09 | 2023-06-06 | 有研资源环境技术研究院(北京)有限公司 | Composite neutron absorption material and preparation method thereof |
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| US20100183475A1 (en) * | 2009-01-21 | 2010-07-22 | Roman Radon | Chromium manganese - nitrogen bearing stainless alloy having excellent thermal neutron absorption ability |
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| CN1676657A (en) * | 2004-04-02 | 2005-10-05 | 中国科学院物理研究所 | Gadolinium-base block amorphous alloy and its preparing method |
| CN114196864A (en) * | 2021-11-25 | 2022-03-18 | 江苏大学 | Y-Gd-based alloy, neodymium cerium iron boron magnet comprising same and preparation method |
| CN116230259A (en) * | 2023-05-09 | 2023-06-06 | 有研资源环境技术研究院(北京)有限公司 | Composite neutron absorption material and preparation method thereof |
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