CN115637352A - Titanium-niobium alloy for neutron scattering experiments and preparation method and application thereof - Google Patents
Titanium-niobium alloy for neutron scattering experiments and preparation method and application thereof Download PDFInfo
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- CN115637352A CN115637352A CN202211241357.XA CN202211241357A CN115637352A CN 115637352 A CN115637352 A CN 115637352A CN 202211241357 A CN202211241357 A CN 202211241357A CN 115637352 A CN115637352 A CN 115637352A
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Abstract
The invention discloses a titanium-niobium alloy for neutron scattering experiments and a preparation method and application thereof. The titanium-niobium alloy comprises 49.5-52.5 wt% of titanium and 47.5-50.5 wt% of niobium, and the preparation method of the titanium-niobium alloy comprises the steps of adopting a vacuum induction furnace to cast or vacuum arc melting alloy raw materials; hot working or hot working. The titanium-niobium alloy is applied to a sample containing container of a neutron experiment, a neutron beam window of neutron experiment related equipment and structural components of the neutron experiment related equipment. The titanium-niobium alloy disclosed by the invention has no neutron diffraction peak, has good processing plasticity and high room temperature theoretical thermal conductivity, can meet the requirements of a neutron scattering experiment on a sample containing container and a neutron beam window and the mechanical processing requirements, meets the requirements of an efficient high-temperature and low-temperature in-situ experiment, enables data obtained by the neutron scattering experiment to be more accurate and reliable, and reduces the cost of the neutron scattering experiment.
Description
Technical Field
The invention relates to the technical field of alloy manufacturing, in particular to a titanium-niobium alloy for neutron scattering experiments and a preparation method and application thereof.
Background
The neutron scattering technology utilizes a neutron scattering method to study the static structure of a substance and the micro-dynamic properties of the substance. Neutrons have the advantages of no electricity, strong penetrating power, capability of identifying isotopes, sensitivity to light elements compared with X-rays, magnetic moment and the like, so that the neutron scattering technology, as a unique characterization means for researching the structure and dynamic characteristics of substances on the atom and molecular scale, has played a role that X-rays cannot replace in the research fields of physics, chemistry, materials, engineering and the like, and becomes an important means for scientific research of substances and research and development of new materials. In the neutron scattering experiment, the test sample is various in form (solid, liquid, powder and the like), a special sample containing container is required to be adopted to arrange a test neutron beam, and in the experiment process, the neutron beam passes through the containing container containing the sample to interact with the sample, so that neutron scattering data is obtained, and the microstructure and the dynamic characteristic of the sample can be analyzed. However, the scattered signals of the sample holding container can cause great trouble to data analysis, and the data quality is seriously influenced. In addition, with the development of neutron scattering technology in the fields of basic scientific research and advanced industrial application, the neutron experimental sample environment occupies an increasingly important position in neutron in-situ test experiments. And the influence of external signals on neutron scattering data is further aggravated by complex structures and metal components in the sample environment. In order to obtain high-quality neutron scattering data, a neutron scattering experiment needs to strictly control a scattering background, and the influence of various background signal sources on the quality of the neutron scattering data is avoided.
At present, vanadium metal and TiZr alloy are generally adopted internationally as sample holding containers, and V or Al is used as a neutron beam window material of a sample environment. However, V and Al have neutron diffraction peaks, which seriously interfere with experimental sample signals and bring difficulty to acquisition of high-quality neutron diffraction data of the sample in the later period. Although the TiZr alloy does not have neutron diffraction peaks, the alloy has poor processing plasticity, so that the sample containing container is high in price, the alloy has poor thermal conductivity, the theoretical thermal conductivity at room temperature is about 6W/(m × K), the temperature rise and fall speed of the sample is slow under the high and low temperature sample environment, and the efficiency of neutron test experiments under the high and low temperature sample environment is greatly limited.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a titanium-niobium alloy for neutron scattering experiments and a preparation method and application thereof.
The technical scheme of the invention is as follows:
according to a first aspect, the invention provides a titanium-niobium alloy for neutron scattering experiments, which comprises 49.5-52.5 wt% of titanium and 47.5-50.5 wt% of niobium.
According to a second aspect, the invention provides a preparation method of a titanium-niobium alloy for neutron scattering experiments, which comprises the following steps:
(1) Casting the alloy raw material by a vacuum induction furnace or vacuum arc melting to obtain a blank;
(2) And carrying out hot working or cold working on the blank to obtain the titanium-niobium alloy.
Preferably, the vacuum induction furnace casting melting in the step (1) comprises primary melting and refining which are carried out in sequence.
Preferably, the alloy raw materials in the step (1) are bulk elemental titanium and elemental niobium.
Preferably, the hot working in the step (2) is one of forging, hot rolling or hot extrusion.
Preferably, the cold working in step (2) is one of rolling, extruding or drawing.
According to a third aspect, the invention provides an application of the titanium-niobium alloy for neutron scattering experiments.
Preferably, the applications include a sample holding container for neutron experiments, a neutron beam window of neutron experiment related equipment and structural components of neutron experiment related equipment.
The invention has the beneficial effects that:
the titanium-niobium alloy disclosed by the invention has no neutron diffraction peak, has good processing plasticity and high room temperature theoretical thermal conductivity, can meet the requirements of a neutron scattering experiment on a sample containing container and a neutron beam window and the mechanical processing requirements, meets the requirements of an efficient high-temperature and low-temperature in-situ experiment, enables data obtained by the neutron scattering experiment to be more accurate and reliable, and reduces the cost of the neutron scattering experiment.
The titanium-niobium alloy has simple preparation process, ensures that the alloy obtains good comprehensive performance, has stable neutron performance, and is convenient for quality control and mass production.
Drawings
FIG. 1 is a graph comparing the thermal conductivity of TiZr and TiNb alloys in an example of the present invention;
FIG. 2 is a graph comparing the mechanical properties of TiZr and TiNb alloys in the examples of the present invention;
FIG. 3 is a neutron spectrum obtained from a neutron test according to an embodiment of the present invention;
FIG. 4 is a neutron spectrum obtained from a neutron test according to example two of the present invention;
FIG. 5 is a neutron spectrum obtained from a neutron test according to an embodiment of the present invention.
Detailed Description
The existing sample container and the existing neutron beam window materials V and Al have neutron diffraction peaks, and the TiZr alloy has the problems of low thermal conductivity and poor processing plasticity, so that the efficiency of neutron experiments is greatly limited. Therefore, it is necessary to develop a new special alloy for neutron diffraction experiments, which has no neutron diffraction peak, high thermal conductivity and can be processed.
The intensity of the neutron brag diffraction peak of the material is related to the coherent scattering cross section of the material. If the coherent scattering cross section of the material is 0, the diffraction intensity is 0, and no neutron diffraction peak occurs. As the scattering cross sections of main different alloy elements on neutrons are different, the coherent scattering cross section of some elements is negative, and the coherent scattering cross section of some elements is positive, the alloy with the coherent scattering cross section of 0 can be obtained through the regulation and control of a certain proportion.
The key point of the invention is to utilize the principle and creatively provide the titanium-niobium alloy with 49.5-52.5 wt% of titanium and 47.5-50.5 wt% of niobium and the preparation method thereof, so as to ensure that the alloy obtains good comprehensive performance, for example, the titanium-niobium alloy prepared by using suspension smelting casting components of 51.11% of titanium and 48.89% of niobium has the advantages of no neutron diffraction peak, good thermal conductivity and tensile elongation rate of more than 20% compared with the existing V, al and TiZr, and meanwhile, through JmatPro phase diagram calculation screening, the theoretical thermal conductivity of the titanium-niobium alloy at room temperature is 30W/(m K), which is about 4.5 times of TiZr, as shown in figure 1. The tensile yield strength of the mechanical property is 400Mpa, and the elongation is more than 20%, as shown in figure 2. Therefore, the alloy can meet the requirements of a neutron scattering experiment on a sample containing container and a neutron beam window, the processing and preparation requirements of the sample containing container and the neutron beam window meet the requirements of efficient high-temperature and low-temperature in-situ experiments.
The preparation method of the titanium-niobium alloy for the neutron scattering experiment comprises the following steps:
(1) Casting the alloy raw material by a vacuum induction furnace or vacuum arc melting to obtain a blank;
(2) And carrying out hot working or cold working on the blank to obtain a titanium-niobium alloy bar with an ideal size or cold working the titanium-niobium alloy bar into an ideal titanium-niobium alloy plate or sheet, and then carrying out neutron test sample container processing test.
In the invention, before casting in a vacuum induction furnace or smelting in an electric arc furnace, alloy raw materials are prepared according to a proportion, and then a surface oxide layer is removed by cleaning.
In the invention, the alloy raw materials are block simple substance titanium (Ti) and simple substance niobium (Nb) with the purity of more than 99.9 percent, oxide skin is easy to remove by adopting the simple substance blocks, and the alloy atomic ratio can be accurately controlled by weighing to obtain the material with stable neutron performance.
In the invention, when the vacuum reaction furnace is adopted for suspension smelting, the method comprises primary smelting and refining which are carried out in sequence, and smelting is carried out repeatedly for more than 4 times in the sequence during smelting, and the vacuum degree is better than 8 x 10 in the smelting process -2 And Pa, cooling along with the furnace for 40 minutes after smelting is finished, and discharging to obtain kilogram-level alloy blanks.
In the invention, the temperature of the primary melting is more than 2000 ℃, preferably 2000 ℃, the refining temperature is more than 2200 ℃, and the refining time is 5-10min.
In the invention, when vacuum arc melting is adopted, high-purity argon with the purity of 99.99 percent is introduced until the gauge pressure in the furnace is-0.05 MPa, the alloy ingot is overturned and melted for more than 7 times, preferably for more than 7 times, the duration time of each time is more than 3 minutes, electromagnetic stirring is started for stirring, and after the melting is finished, the alloy ingot is cooled to room temperature and sampled to obtain gram-grade alloy casting blanks.
In the present invention, the electric current range for arc melting is 300 to 600A, more preferably 200 to 600A, and still more preferably 200 to 400A.
In the present invention, the hot working is one of forging, hot rolling, or hot extrusion.
In the invention, the hot working temperature is 700-1400 ℃, for example, the alloy billet is preferably forged at 700-1250 ℃ to obtain the bar with the ideal size for neutron test sample container processing test.
In the present invention, cold working is one of rolling, extrusion or drawing, and it is preferable to cold-roll the alloy billet to a desired plate or sheet at room temperature.
The invention also provides application of the titanium-niobium alloy for neutron scattering experiments, which is used for preparing a sample holding container for neutron experiments, a neutron beam window of neutron experiment related equipment and a structural component of the neutron experiment related equipment, the alloy has no neutron diffraction peak, reduces interference on experimental sample signals, improves the accuracy of neutron experiment data, has good heat conductivity, avoids the limitation on efficiency of neutron test experiments in high and low temperature sample environments, has good processing plasticity and elongation of more than 20 percent, and reduces the manufacturing difficulty of sample containers, thereby reducing the cost of the sample containers.
The present application will be described in further detail with reference to specific examples. The following examples are intended to be illustrative of the present application only and should not be construed as limiting the present application.
The ingredients of the following examples are shown in table one.
Watch 1
| Melting mode | Ti | Nb |
| Suspension (suspension) | 51.11wt％ | 48.89wt％ |
| Electric arc | 51.08wt％ | 48.92wt％ |
The first embodiment is as follows:
the preparation method of the embodiment is as follows:
50g of TiNb is prepared by adopting an electric arc melting method, melting current of about 200A is adopted, the TiNb alloy ingot is obtained by repeatedly melting for more than 7 times, and a neutron test sample is processed and prepared. And then, testing by using neutrons with the neutron wavelength range of 0.01-4.5A to obtain a neutron spectrum as shown in figure 3, wherein the test shows that the alloy has no neutron diffraction peak and can be used for neutron experimental sample containers or neutron beam window materials.
The second embodiment:
the preparation method of the embodiment is as follows:
preparing 200g of TiNb by adopting an electric arc melting method, repeatedly melting for more than 7 times by adopting melting current of about 300-600A to obtain a TiNb alloy ingot, cold-rolling to 2mm, and processing to prepare a neutron test sample. And then neutron measurement is carried out by using neutrons with the wavelength range of 0.01-4.5A, and the obtained neutron spectrum is shown in figure 4.
Example three:
the preparation method of the embodiment is as follows:
preparing 3KgTiNb by adopting a vacuum suspension smelting method, obtaining a rough blank by adopting vacuum suspension smelting at the smelting temperature of 2000 ℃, then refining for 5-10 minutes by adopting the high temperature of more than 2200 ℃, repeatedly smelting for more than 4 times, and ensuring that the vacuum degree is more than 8 x 10 in the smelting process -2 And Pa or above, discharging the alloy ingot after smelting is finished and is cooled along with the furnace for 40 minutes, obtaining a kilogram-level alloy ingot, forging the bar at the temperature of above 700 ℃, obtaining the bar with an ideal size, processing and preparing the bar into a neutron sample box test, and testing results are shown in figure 5.
The above embodiments are merely preferred embodiments of the present invention, which are not intended to limit the scope of the present invention, and various changes may be made in the above embodiments of the present invention. All simple and equivalent changes and modifications made according to the claims and the content of the specification of the present invention are within the scope of the claims of the present invention. The invention has not been described in detail in order to avoid obscuring the invention.
Claims (9)
1. The titanium-niobium alloy for neutron scattering experiments is characterized by comprising 49.5-52.5 wt% of titanium and 47.5-50.5 wt% of niobium.
2. A preparation method of the titanium-niobium alloy for neutron scattering experiments is used for preparing the titanium-niobium alloy as claimed in claim 1, and is characterized by comprising the following steps of:
(1) Casting the alloy raw material by a vacuum induction furnace or vacuum arc melting to obtain a blank;
(2) And carrying out hot working or cold working on the blank to obtain the titanium-niobium alloy.
3. The method for preparing the titanium-niobium alloy for the neutron scattering experiment in the step (1) is characterized in that the vacuum induction furnace casting melting comprises primary melting and refining which are sequentially carried out.
4. The method for preparing a titanium-niobium alloy for neutron scattering experiments according to claim 3, wherein the preliminary melting and refining are sequentially repeated at least 4 times.
5. The method for preparing the titanium-niobium alloy for the neutron scattering experiment in claim 2, wherein the alloy raw materials in the step (1) are bulk elemental titanium and elemental niobium.
6. The method for preparing the titanium-niobium alloy for the neutron scattering experiment according to claim 2, wherein the hot working temperature in the step (2) is 700 ℃ to 1400 ℃.
7. The method for preparing a titanium-niobium alloy for neutron scattering experiments in claim 2, wherein the hot working in the step (2) is one of forging, hot rolling or hot extrusion.
8. The method for preparing the titanium-niobium alloy for the neutron scattering experiment in claim 2, wherein the cold working in the step (2) is one of rolling, extruding or drawing.
9. Use of the titanium niobium alloy of claim 1 in neutron scattering experiments.
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Citations (5)
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|---|---|---|---|---|
| CN104313363A (en) * | 2014-10-08 | 2015-01-28 | 西安西工大超晶科技发展有限责任公司 | Smelting method for titanium-niobium alloy ingot |
| CN105779819A (en) * | 2015-12-28 | 2016-07-20 | 北京科技大学 | Molybdenum-titanium alloy neutron transparent material and preparation method thereof |
| CN112553501A (en) * | 2020-11-27 | 2021-03-26 | 东南大学 | Titanium-niobium shape memory alloy with adjustable negative thermal expansion and preparation method thereof |
| CN112680681A (en) * | 2020-11-27 | 2021-04-20 | 东南大学 | Preparation method of titanium-niobium alloy with adjustable negative thermal expansion coefficient |
| CN115029570A (en) * | 2022-06-15 | 2022-09-09 | 西部超导材料科技股份有限公司 | Preparation method of titanium-niobium alloy ingot |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104313363A (en) * | 2014-10-08 | 2015-01-28 | 西安西工大超晶科技发展有限责任公司 | Smelting method for titanium-niobium alloy ingot |
| CN105779819A (en) * | 2015-12-28 | 2016-07-20 | 北京科技大学 | Molybdenum-titanium alloy neutron transparent material and preparation method thereof |
| CN112553501A (en) * | 2020-11-27 | 2021-03-26 | 东南大学 | Titanium-niobium shape memory alloy with adjustable negative thermal expansion and preparation method thereof |
| CN112680681A (en) * | 2020-11-27 | 2021-04-20 | 东南大学 | Preparation method of titanium-niobium alloy with adjustable negative thermal expansion coefficient |
| CN115029570A (en) * | 2022-06-15 | 2022-09-09 | 西部超导材料科技股份有限公司 | Preparation method of titanium-niobium alloy ingot |
Non-Patent Citations (2)
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| H.W. WEBER: "Neutron irradiation effects on alloy superconductors", JOURNAL OF NUCLEAR MATERIALS, pages 572 - 584 * |
| K.SCHMELZ等: "Superconductivity of NbTi50 after heavy ion irradiation at low temperature and high fluences", JOURNAL OF NUCLEAR MATERIALS, vol. 67, pages 109 - 118 * |
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