CN110923800A - Preparation method of nickel-uranium pentagallium monocrystal, nickel-uranium pentagallium monocrystal and application of nickel-uranium pentagallium monocrystal - Google Patents
Preparation method of nickel-uranium pentagallium monocrystal, nickel-uranium pentagallium monocrystal and application of nickel-uranium pentagallium monocrystal Download PDFInfo
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Abstract
The invention provides a preparation method of a nickel-uranium pentagallium monocrystal, which comprises the following steps: under a protective atmosphere, loading raw materials into a crucible and placing the crucible with the raw materials into a first quartz tube; vacuumizing and sealing the first quartz tube with the crucible; loading the first quartz tube with the crucible into a second quartz tube; vacuumizing and sealing the second quartz tube with the first quartz tube to obtain a double-layer quartz tube; heating the double-layer quartz tube; and cooling the double-layer quartz tube to obtain the nickel-uranium pentagallium monocrystal. The purity of the nickel-uranium pentagallium monocrystal prepared by the preparation method provided by the invention is high. The invention also provides the nickel-uranium pentagallium monocrystal prepared by the preparation method and application thereof.
Description
Technical Field
The invention relates to the technical field of nickel-uranium pentagallium, and particularly relates to a preparation method of a nickel-uranium pentagallium monocrystal, the nickel-uranium pentagallium monocrystal and application of the nickel-uranium pentagallium monocrystal.
Background
Uranium-based compounds have rich and exotic quantum phenomena such as heavy fermi sub-states, unconventional superconductivity, non-fermi liquid behavior, valence state fluctuations, magnetic ordering, and hidden order. The local-cruise dual characteristics of the 5f electron are key factors for understanding various singular quantum phenomena, and the deep understanding and characterization of the characteristics of the 5f electron require the preparation of high-quality single crystal samples.
UNiGa5(Nickel-uranium pentagallium) has HoCoGa5A tetragonal crystal structure of type having a space group of P4Mm, from AuCu3Model UGa3Layer and NiGa2The layers are stacked in the direction c. UNiGa5The material is in an antiferromagnet state at low temperature, the magnetic transition temperature is 86K, the material has a typical Xel-type magnetic structure, and the arrangement directions of magnetic moments of adjacent U atoms are opposite. The microscopic characteristics of 5f electrons are the basis for understanding the abundant and singular physical properties of the 5f electrons, and advanced electronic structure characterization means such as an angle-resolved photoelectron spectrometer, a scanning tunneling microscope and the like all need to use single crystal samples, so that the preparation of high-quality UNiGa is urgently needed5Single crystal samples to meet experimental requirements.
At present, a preparation method of a single crystal sample in the physical field of condensed state mainly comprises a flux method and a pulling method, the method is difficult to overcome the influence of impurities in the environment on a molten material, and the uranium is very easy to react with other substances (such as water, hydrogen, oxygen and the like) in the environment due to very high activity at high temperature, so that a high-purity single crystal material is difficult to obtain. In addition, uranium has certain radioactivity and needs a special protective environment, and a single-layer sealed crucible method is generally adopted in a conventional single crystal preparation method, so that the phenomena of cracking of a sealing layer and the like are easy to occur at high temperature, and the growth of the radioactive uranium-based material is extremely unfavorable.
Disclosure of Invention
In view of the above, there is a need for a method for preparing a single crystal of nickel-uranium pentagallium, which is high in purity.
In addition, it is necessary to provide a nickel-uranium pentagallium single crystal prepared by the preparation method.
In addition, an application of the nickel-uranium pentagallium monocrystal is also needed to be provided.
The invention provides a preparation method of a nickel-uranium pentagallium monocrystal, which comprises the following steps:
under a protective atmosphere, loading raw materials into a crucible and placing the crucible with the raw materials into a first quartz tube, wherein the raw materials comprise metallic uranium blocks, metallic nickel blocks and metallic gallium particles;
vacuumizing and sealing the first quartz tube with the crucible;
loading the first quartz tube with the crucible into a second quartz tube;
vacuumizing and sealing the second quartz tube with the first quartz tube to obtain a double-layer quartz tube;
heating the double-layer quartz tube so that the metallic uranium blocks, the metallic nickel blocks and the metallic gallium particles are melted and mixed; and
and cooling the double-layer quartz tube to obtain the nickel-uranium pentagallium monocrystal.
The invention also provides a nickel-uranium pentagallium monocrystal prepared by the preparation method of the nickel-uranium pentagallium monocrystal.
The invention also provides application of the nickel-uranium pentagallium monocrystal.
According to the invention, the reaction environment in contact with the metal uranium blocks, the metal nickel blocks and the metal gallium particles is controlled through the double-layer sealed quartz tube, and the vacuum degree of the environment atmosphere is improved, so that the impurities in the environment atmosphere are effectively reduced, and the purity of the nickel-uranium pentagallium monocrystal is high.
Drawings
FIG. 1 is a flow chart of a method for preparing a nickel-uranium pentagallium single crystal in a preferred embodiment of the invention.
Fig. 2 is a schematic view of the connection crucible, the first quartz tube, the first sealing means, and the pump unit in the preparation method shown in fig. 1.
Fig. 3 is a schematic view illustrating the connection of the first quartz tube, the second sealing means, and the pump stack in the manufacturing method shown in fig. 1.
FIG. 4 is a diagram of a crystal of nickel-uranium pentagallium single crystal prepared according to a preferred embodiment of the present invention.
FIG. 5 is a low-energy electron diffraction diagram of the nickel-uranium pentagallium single crystal shown in FIG. 4 after vacuum dissociation.
FIG. 6 is an angle-resolved photoelectron spectrum of the single crystal of nickel-uranium pentagallium oxide shown in FIG. 4.
Description of the main elements
Feedstock 10
Crucible 20
First sealing means 31
Second sealing means 51
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
Referring to fig. 1, a method for preparing a single crystal of nickel-uranium pentagallium according to a preferred embodiment of the present invention includes the following steps:
step S1, referring to fig. 2, the raw material 10 is loaded into a crucible 20 under a protective atmosphere, and the crucible 20 with the raw material 10 is placed in a first quartz tube 30, wherein the raw material 10 includes uranium metal pieces, nickel metal pieces, and gallium metal particles.
In this embodiment, the weight ratio of the metallic uranium nuggets, the metallic nickel nuggets, and the metallic gallium particles is 1:1: 15-17. The purity of the metal uranium blocks is not less than 99.8 wt%, the purity of the metal nickel blocks is not less than 99.9 wt%, and the purity of the metal gallium particles is not less than 99.9999 wt%.
The protective atmosphere is used to reduce the content of water vapor, hydrogen, and oxygen in the environment surrounding the uranium metal chunk, thereby protecting the uranium metal chunk from oxidation. In this embodiment, the protective atmosphere is argon. In other embodiments, the protective atmosphere may be another inert gas.
In this embodiment, prior to loading the uranium metal nuggets into the crucible 20, the uranium metal nuggets are cleaned to remove oxides from the surface of the uranium metal nuggets. Specifically, the metal uranium nuggets may be washed in a dilute nitric acid solution for 5 minutes.
In this embodiment, after the crucible 20 is placed in the first quartz tube 30, a first sealing device 31 is further provided, and the first sealing device 31 is connected to the opening of the first quartz tube 30 under the protective atmosphere. The first sealing device 31 may be a sealing sleeve. The first sealing device 31 is used for preventing water vapor, hydrogen and oxygen in the surrounding environment from entering the first quartz tube 30 when the first quartz tube 30 is subsequently vacuumized.
Wherein the raw material 10 is charged into the crucible 20, the crucible 20 is placed in the first quartz tube 30, and the first sealing means 31 is connected to the first quartz tube 30, all of which can be performed in a glove box. Wherein, the content of the water vapor and the oxygen in the glove box are both required to be lower than 10 ug/g.
In the present embodiment, the material of the crucible 20 is alumina.
Step S2, the first quartz tube 30 with the crucible 20 is evacuated and sealed.
In the present embodiment, the degree of vacuum in the first quartz tube 30 is 1 × 10-5mbar～2×10-5mbar. Wherein the first quartz tube 30 is used as a first layer protective wall.
In this embodiment, a pump unit 40 is used to evacuate the first quartz tube 30. Wherein the pump unit 40 includes a mechanical pump (not shown) and a molecular pump (not shown), and the mechanical pump is connected to the molecular pump to improve the efficiency of the pump unit 40 for drawing vacuum. Specifically, the pump unit 40 passes through the first sealing means 31 through a pipe to evacuate the first quartz tube 30.
In the present embodiment, the first quartz tube 30 is sealed with an oxyhydrogen flame. In particular, sealing may be performed with a water welder.
In step S3, referring to fig. 3, the first quartz tube 30 with the crucible 20 is loaded into a second quartz tube 50.
In this embodiment, after the first quartz tube 30 is installed in the second quartz tube 50, a second sealing means 51 is further provided, and the second sealing means 51 is connected to the opening of the second quartz tube 50. The second sealing device 51 may also be a sealing sleeve. The second sealing device 51 is used for preventing water vapor, hydrogen and oxygen in the surrounding environment from entering the second quartz tube 50 when the second quartz tube 50 is vacuumized subsequently.
Step S4, the second quartz tube 50 with the first quartz tube 30 is vacuumized and sealed to obtain a double-layered quartz tube.
In the present embodiment, the degree of vacuum in the second quartz tube 50 is 1 × 10-5mbar～2×10-5mbar. Wherein the second quartz tube 50 is used as a second layer protective wall.
In this embodiment, the pump unit 40 is used to evacuate the second quartz tube 50. Specifically, the pump unit 40 passes through the second sealing means 51 through a pipe to evacuate the second quartz tube 50.
In the present embodiment, the second quartz tube 50 is sealed with an oxyhydrogen flame. In particular, sealing may be performed with a water welder.
Step S5, heating the double-layer quartz tube, so that the metallic uranium lumps, the metallic nickel lumps, and the metallic gallium particles are melted and mixed.
Specifically, the double-layer quartz tube is placed in a crystal growth furnace, heating the double-layer quartz tube comprises heating the double-layer quartz tube to 1000-1100 ℃ at a heating rate of 200-250 ℃/h, and preserving heat for 40-60h, so that the metal uranium blocks, the metal nickel blocks and the metal gallium particles are completely melted and fully and uniformly mixed, and a mixed solution is obtained.
And step S6, cooling the double-layer quartz tube to obtain the nickel-uranium pentagallium monocrystal.
Specifically, the temperature of the double-layer quartz tube in the step 5 is slowly reduced to 600-650 ℃ at the rate of 0.8-1.2 ℃/h, so as to reduce the temperature of the mixed solution.
After the double-layer quartz tube is cooled, the double-layer quartz tube is placed on a centrifuge for centrifugal separation at the temperature of 600-650 ℃. Because the centrifugal separation is carried out at high temperature, the residual solution of the metal gallium particles (the metal gallium particles can be melted into liquid at the temperature) can be quickly separated from the grown monocrystal, and the phenomenon that the excessive solution of the metal gallium particles is wrapped on the surface of the monocrystal is avoided. Wherein, the rotating speed of the centrifugal machine can be 5000-10000 r/s.
In this embodiment, after the centrifugation, the double-layer quartz tube is removed, that is, the second quartz tube 50 and the first quartz tube 30 are removed, and the crucible 20 is taken out, so that the nickel-uranium pentagallium single crystal is obtained.
The present invention is further illustrated by the following examples.
Examples
Firstly, in an atmospheric environment, a metal uranium block is put into a dilute nitric acid solution for cleaning so as to remove oxides on the surface.
Secondly, in a glove box, the uranium metal blocks, the nickel metal blocks and the gallium metal particles are placed into a crucible 20 according to the weight ratio of 1:1:15, the crucible 20 is placed into a first quartz tube 30, the opening of the first quartz tube 30 is connected with a first sealing device 31, and the first quartz tube 30 and the first sealing device 31 are taken out of the glove box together. Wherein the glove box has an inert atmosphere therein.
Thirdly, pumping the first quartz tube 30 by a pump set 40 connected with a mechanical pump and a molecular pump through the first sealing device 31 through a pipeline, and when the vacuum degree in the first quartz tube 30 reaches 1.5 multiplied by 10-3And when Pa, stopping pumping, and performing high-temperature sealing on the first quartz tube 30 by using a water welding machine, so that the melting part of the first quartz tube 30 is completely attached and sealed.
Fourthly, placing the first quartz tube 30 into a second quartz tube 50, connecting the opening of the second quartz tube 50 with a second sealing device 51, and evacuating the second quartz tube 50 by adopting the third step so that the vacuum degree in the second quartz tube 50 reaches 1.5 x 10-3Pa, and sealing the opening of the second quartz tube 50 according to the third step to obtain a double-layer quartz tube.
And fifthly, putting the double-layer quartz tube into a crystal growth furnace, heating the double-layer quartz tube to 1050 ℃ from room temperature at a speed of 200 ℃/h, and preserving heat for 50h to ensure that the metal uranium blocks, the metal nickel blocks and the metal gallium particles are heated at high temperature and completely melted in the crucible 20, and fully mixing to obtain a uniform mixed solution.
And sixthly, slowly reducing the temperature of the mixed solution obtained in the fifth step to 650 ℃ at the speed of 1 ℃/h, quickly taking out the cooled double-layer sealed quartz tube, and placing the quartz tube into a centrifuge for centrifugal separation, wherein the centrifugal time is about 5 min.
And seventhly, taking the double-layer quartz tube after the centrifugal separation in the sixth step out of the centrifugal machine, destroying the double-layer quartz tube, taking the crucible 20 out, and selecting the nickel-uranium pentagallium monocrystal.
And step eight, adhering the nickel-uranium pentagallium monocrystal to a sample support by using a silver colloid, putting the sample support into an ultrahigh vacuum chamber, and performing vacuum dissociation on the nickel-uranium pentagallium monocrystal by using a manipulator so as to obtain a fresh and clean monocrystal surface.
And step nine, adjusting the energy of low-energy electron diffraction to 80eV, and carrying out a low-energy electron diffraction experiment.
And step ten, adjusting the photon energy of the angle-resolved photoelectron spectrometer to be between 480-560eV, and carrying out an angle-resolved photoelectron spectroscopy experiment.
Referring to fig. 4, the size of the single crystal of nickel-uranium pentagallium is large, the maximum size can reach 5mm × 4mm × 0.8mm, the surface of the single crystal of nickel-uranium pentagallium is very bright, and a condition of obvious specular reflection is presented, which indicates that the quality of the single crystal of nickel-uranium pentagallium is high.
Referring to fig. 5, the structure and the flatness of the surface of the sample of the single crystal of nickel-uranium pentagallium can be distinguished from the figure, so that the quality of the single crystal of nickel-uranium pentagallium can be obtained. Only when the analyzed sample is single crystal, regular lattice arrangement can be generated, so that the nickel-uranium pentagallium monocrystal is known to be of a single crystal structure. The higher the quality of the single crystal, the sharper the diffraction spot will be. As can be seen from the figure, the nickel-uranium pentagallium single crystal has very sharp diffraction spots, which indicates that the nickel-uranium pentagallium single crystal has high crystal quality.
Referring to fig. 6, it can be seen from the figure that the energy band structure of the single crystal of nickel-uranium pentagallium is clear, and the dispersion is obvious, so that the single crystal of nickel-uranium pentagallium can be obtained as a single crystal and has a flat surface. Because if the nickel-uranium pentagallium single crystal is not a single crystal, a dispersion signal cannot be obtained. Furthermore, a flatter band is observed around the fermi energy, mainly due to the heavy quasiparticles bands formed by the hybridization of the f-and conduction band electrons. Another flatter band is observed at the deep level of 2.0eV, which is primarily the energy level position of the localized f-electrons. In addition to this, other dispersion of the conduction band can be observed.
The preferred embodiment of the invention also provides a nickel-uranium pentagallium monocrystal prepared by the preparation method of the nickel-uranium pentagallium monocrystal.
The invention also provides application of the nickel-uranium pentagallium monocrystal.
The invention has the following beneficial effects:
according to the invention, the reaction environment in contact with the metal uranium blocks, the metal nickel blocks and the metal gallium particles is controlled through the double-layer sealed quartz tube, and the vacuum degree of the environment atmosphere is improved, so that the impurities in the environment atmosphere are effectively reduced, and the purity of the grown nickel-uranium pentagallium monocrystal is ensured.
Secondly, under the high-temperature condition, the metal uranium blocks and the metal nickel blocks are melted in the metal gallium particles to form a homogenized high-temperature mixed solution, so that the metal uranium blocks, the metal nickel blocks and the metal gallium particles are fully mixed, and large-size single crystals are easily obtained. Wherein the maximum size of the nickel-uranium pentagallium monocrystal can reach 5mm multiplied by 4mm multiplied by 0.8 mm.
By designing the double-layer quartz tube, the invention effectively prevents the pollution of nuclear materials (namely the uranium metal blocks) to the environment caused by the fracture of the single-layer quartz tube under the high-temperature condition, is particularly suitable for the growth of radioactive materials, and avoids the possible pollution to the environment.
And fourthly, performing centrifugal separation at high temperature, so that the residual solution of the metal gallium particles can be quickly separated from the grown single crystal, and the phenomenon that the excessive solution of the metal gallium particles is wrapped on the surface of the single crystal is avoided.
Although the embodiments of the present invention have been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the spirit and scope of the embodiments of the present invention.
Claims (10)
1. A preparation method of a nickel-uranium pentagallium monocrystal is characterized by comprising the following steps:
under a protective atmosphere, loading raw materials into a crucible and placing the crucible with the raw materials into a first quartz tube, wherein the raw materials comprise metallic uranium blocks, metallic nickel blocks and metallic gallium particles;
vacuumizing and sealing the first quartz tube with the crucible;
loading the first quartz tube with the crucible into a second quartz tube;
vacuumizing and sealing the second quartz tube with the first quartz tube to obtain a double-layer quartz tube;
heating the double-layer quartz tube so that the metallic uranium blocks, the metallic nickel blocks and the metallic gallium particles are melted and mixed; and
and cooling the double-layer quartz tube to obtain the nickel-uranium pentagallium monocrystal.
2. The method for preparing a nickel uranium pentagallium single crystal according to claim 1, wherein the weight ratio of the metal uranium lumps, the metal nickel lumps and the metal gallium particles is 1:1: 15-17.
3. The method for preparing a nickel-uranium pentagallium single crystal as claimed in claim 1, wherein heating the double-layer quartz tube comprises heating the double-layer quartz tube to 1000-1100 ℃ at a heating rate of 200-.
4. The method for preparing a nickel-uranium pentagallium single crystal as defined in claim 1, wherein the cooling the double-layer quartz tube comprises cooling the double-layer quartz tube to 600-650 ℃ at a cooling rate of 0.8-1.2 ℃/h.
5. The method for preparing a nickel-uranium pentagallium single crystal according to claim 1, wherein after the double-layer quartz tube is cooled, the method further comprises:
the double-layer quartz tube was centrifuged at a temperature of 600-650 ℃.
6. The method for preparing a nickel-uranium pentagallium single crystal according to claim 1, wherein the degree of vacuum in each of the first quartz tube and the second quartz tube is 1 x 10-5mbar～2×10-5mbar。
7. The method for producing a nickel uranium pentagallium single crystal according to claim 1, wherein before the loading of the uranium metal chunk into the crucible, the method further comprises the steps of:
and cleaning the uranium metal block to remove oxides on the surface of the uranium metal block.
8. The method for preparing nickel-uranium pentagallium monocrystal according to claim 1, wherein the evacuation is performed by using a pump set, the pump set comprises a mechanical pump and a molecular pump, and the mechanical pump is connected with the molecular pump.
9. A nickel-uranium pentagallium single crystal produced by the method for producing a nickel-uranium pentagallium single crystal according to any one of claims 1 to 8.
10. Use of a nickel uranium pentagallium single crystal according to claim 9.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201911326930.5A CN110923800A (en) | 2019-12-20 | 2019-12-20 | Preparation method of nickel-uranium pentagallium monocrystal, nickel-uranium pentagallium monocrystal and application of nickel-uranium pentagallium monocrystal |
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| CN107731318A (en) * | 2017-10-27 | 2018-02-23 | 中国工程物理研究院材料研究所 | A kind of preparation method of monocrystalline uranium dioxide fuel ball |
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