CN109097652B - Diluted magnetic alloy material RIn3-xFexAnd method for preparing the same - Google Patents
Diluted magnetic alloy material RIn3-xFexAnd method for preparing the same Download PDFInfo
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- CN109097652B CN109097652B CN201810876202.0A CN201810876202A CN109097652B CN 109097652 B CN109097652 B CN 109097652B CN 201810876202 A CN201810876202 A CN 201810876202A CN 109097652 B CN109097652 B CN 109097652B
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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
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- 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
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
- H01F1/147—Alloys characterised by their composition
Abstract
The invention discloses an AuCu3RIn of type structure3‑xFexThe preparation method of the diluted magnetic alloy material comprises the following steps: (1) according to the formula RIn3‑xFexPreparing three elementary substances of R, In and Fe according to the stoichiometric ratio; (2) repeatedly smelting three simple substance elements of R, In and Fe under the protection of inert gas to obtain an ingot-shaped alloy; (3) loading the melted ingot-shaped alloy into a vacuum quartz glass tube in an inert gas environment, and carrying out heat treatment on the quartz glass tube; (4) taking out the heat-treated product for cooling to obtain the product with AuCu3RIn of type structure3‑xFexA diluted magnetic alloy. The method of the invention melts the 3d transition group magnetic element, the 4f rare earth element and the semiconductor element according to the proportion, eliminates the impure phase existing in the casting state by controlling the temperature and the time during the heat treatment, thereby obtaining the AuCu with room temperature ferromagnetism, almost no impure phase and uniform components3RIn of type structure3‑xFexA diluted magnetic alloy material.
Description
Technical Field
The invention belongs to the technical field of diluted magnetic alloy material preparation, and particularly relates to an AuCu alloy3RIn of type structure3-xFexA diluted magnetic alloy material and a preparation method thereof.
Background
Dilute magnetic alloys are generally compounds with magneto-electric coupling composed of magnetic elements (e.g., 3d transition group metals and 4f rare earth metals) and semiconductor elements. By combining a semiconductor material for applying the freedom of electron charge to information storage and a magnetic material for applying the freedom of electron spin to information storage, it is possible to highly integrate the processing and storage of information and to control the spin state of carriers by injecting spin-polarized current into the semiconductor. The material shows very wide application prospect in the field of novel magnetoelectric, magneto-optical and photoelectric material devices, and the diluted magnetic alloy material is used as a novel functional materialThere is a wide range of concerns. However, the key to determining whether a diluted magnetic alloy can be used in practice is whether it can still retain its ferromagnetic properties at and above room temperature. Therefore, the preparation of diluted magnetic alloy materials with room temperature ferromagnetism is called as a hotspot of research. Lethullier et al discovered RIn in 19733Removing PrIn in the system3Besides the subcritical magnetic order, all other alloy compounds have low-temperature antiferromagnetic property, and the temperature range of the low temperature is about 4.5K to 45K. Prior to the study of z.klettowski, little was known about their thermoelectric properties, although there was clear evidence of the effect of crystal fields and magnetic ordering on magnetic and electrical properties in these compounds. Kletowski's study found that, in the temperature interval above 200K, except CeIn3The thermoelectric power of other compounds is increased along with the temperature rise, the compounds can be divided into two groups according to the thermoelectric performance of the compounds at high temperature, one group is light rare earth, the other group is heavy rare earth, and the different thermoelectric behaviors of the two groups of compounds can be explained by different topological structures of a Fisher-Tropsch plane. In 1971 NASU et al treated LaIn at a temperature range of 1.5 to 4.2K3，PrIn3，CeIn3When the specific heat of (A) was investigated, it was found that LaIn3The superconducting properties are exhibited at a Curie point TN of 0.7K. For TbIn3The J.CRANDLE demonstrates TbIn below the Neel temperature TN by means of neutron diffraction3Exhibits antiferromagnetic properties and further measures the magnetic moment of the compound. Subsequently, Lethuillier and Chaussy were measured by CeIn3、PrIn3And NdIn3The paramagnetic susceptibility curve and the specific heat of (b) obtain the corresponding crystal field parameters. For TbIn3、DyIn3、HoIn3And ErIn3These alloy compounds have been studied systematically. In 1993, Satoh et al discovered RIn3The specific heat coefficient of electrons of (R ═ La, Ce, Pr, Nd, Sm, Gd, Tb, Ho) compounds in the temperature range of 0.2 to 2.2K increases with increasing temperature. In RIn3In the system, PrIn3Vanfreik paramagnetic behavior is exhibited over a large temperature range, and nuclear antiferromagnetic order is exhibited only at very low temperatures. Crystals thereofThe field exhibits the singlet ground state, the low temperature susceptibility and the excited state energy level splitting are inversely proportional, independent of temperature. Two electrons not filled in the 4f electron layer in the Pr ion cause it to form a multiple ground state of J ═ 4, and a magnetic moment is generated. PrIn3Another significant feature of (a) is the possession of one large nuclear quaternary interaction at the In atom occupancy (e2qQ/h +228 MHz). A large number of experiments have confirmed NdIn3The compound has a complex magnetic phase diagram, and TN is 5.9K. Czopnik and Czopnik et al found NdIn at zero field3Two consecutive first-order magnetic transitions occur at 5.2K and 4.7K. In RIn3In the system, GdIn3Having a maximum neel temperature, TN of 45K and a lattice parameter value of
AuCu3Cubic structure of type (space group Pm-3 m). When GdIn is to be added3A slight change in the ordering temperature is observed when the value of TN (b) is compared with the value of the tetragonal GdxMINy (x ═ 1 or 2; y ═ 5 or 8; M ═ Rh, Ir, Co), where the compound GdIrIn5(TN 42K) and GdCoIn5(TN 30K). In contrast to the tetragonal phase, in the range of GdIn3Isomorphic SmIn3Similar characteristics can be observed therein, from which a single crystal GdIn is derived3Magnetic and transport properties. From the magnetic susceptibility measurements, the alignment temperature (AFM) can be estimated as TN 45K, with no deviation from the curie-weiss behavior of T41.5TN. The magnetization isotherm shows a linear behavior, which is characteristic of AFM materials. Specific heat shows a well-defined magnetic anomaly characteristic of the lambda type, similar to that of the magnetic transition of TN. By measuring the magnetic susceptibility, after estimating the magnetic contribution of the CP, the magnetic entropy is calculated and it is determined that it is not fully recovered at TN (theoretical value), possibly due to the presence of modulation on the magnetic moment amplitude and/or magnetic contusion. 4f shell electron structure derived from Gd ions. Because the electron half-filled state of the 4f shell causes the Gd ion orbital angular momentum to be frozen (L ═ 0), the magnetic moment can only depend on the unpaired electrons in the 4f shell. Its effective magnetic moment is 8.20 μ B, close to the Gd ion magnetic moment, indicating that the effective magnetic moment is mainly contributed by Gd ions. The paramagnetic Curie-Weiss temperature is-85K.
Disclosure of Invention
Aiming at the problems of operation in the prior art, the invention provides an AuCu with room-temperature ferromagnetism3A diluted magnetic alloy material with a structure and a preparation method thereof.
As one class of magnetoelectronics materials, increasing the Curie temperature of diluted magnetic semiconductors has been a focus of much research, such as GaxMn1-xThe Curie point of the As series of compounds has been reported to approach room temperature by Saito et al. Magnetic semiconductors are currently mainly focused on oxide semiconductors, such as: research on Mn-doped GaAs, ZnO, MgO and SnO2And the like. These semiconductors all exhibit spin-modulated electron transport properties. On the basis of semiconductors, doping transition group magnetic elements is always a hot spot of interest. In the last two decades, people have been on RIn3The research mainly focuses on the influence of the doping of elements on the structure and the magnetism of the alloy, partial doping of rare earth elements and partial replacement of In elements by Sn elements. However, to date, there have been few reports of non-oxide magnetoelectronics materials that modulate both electron charge and electron spin by a 3d transition group magnetic element and a 4f rare earth element. Having AuCu formed by doping a small amount of 3d transition group magnetic element Fe In a semiconductor element In and a rare earth element R3Nonmagnetic two-alloy RIn of type structure3Thereby obtaining a magnetic rare-magnetic alloy. AuCu3The structure is a face-centered cubic structure, and any element combination can form the face-centered cubic structure under the condition of meeting the requirement of forming the face-centered cubic structure, so that AuCu is used3Is more typical and is therefore often referred to as AuCu in face centered cubic structure3And (4) a mold structure. When the material elements are three elements of rare earth elements R, In and Fe, a pseudo-binary alloy RIn is formed3. Rare earth elements in AuCu3Au of the type structure is at the vertex position, In is at the face center position of Cu, and Fe substitutes part of In atoms to occupy the face center position, so that the molecular formula is changed into RIn3-xFexBut the total number of atoms in one molecule is still 4.
The technical scheme of the invention is as follows:
AuCu3Diluted magnetic coupling of structureThe diluted magnetic alloy material has a chemical formula of RIn3-xFex(ii) a Wherein R is Pr, Nd, Gd, or Ho, and x is not more than 0.1 and not more than 0.
Further, the crystal structure of the diluted magnetic alloy material is AuCu3And (5) structure.
Further, the AuCu3The type structure is a face-centered cubic structure.
Further, the diluted magnetic alloy material has room temperature ferromagnetism
AuCu as described above3The preparation method of the diluted magnetic alloy material with the structure comprises the following steps:
(1) according to the formula RIn3-xFexPreparing three elementary substances of R, In and Fe according to the stoichiometric ratio; wherein R is Pr, Nd, Gd or Ho, and x is less than or equal to 0.1 and is not 0.
(2) Repeatedly smelting three simple substance elements of R, In and Fe under the protection of inert gas to obtain an ingot-shaped alloy;
(3) putting the smelted ingot-shaped alloy into a vacuum quartz glass tube in an inert gas environment, and placing the quartz glass tube in a muffle furnace for heat treatment at the temperature of 800-1000 ℃;
(4) taking out the sample after heat treatment, and cooling in cold water to obtain the product with AuCu3A diluted magnetic alloy of structure.
Further, the stoichiometric ratio is R ═ 1, In + Fe ═ 3.
Furthermore, the purities of the R, In and Fe simple substances In the step (1) are more than 99.9%.
Further, the smelting in the step (2) is carried out in a non-consumable arc vacuum smelting furnace, and the smelting current is 40A-200A.
Further, the heat treatment time in the step (3) is 4 to 7 days.
Further, the inert gas in the step (2) and the step (3) is argon.
The invention has the beneficial effects that: the preparation method provided by the invention is characterized in that the 3d transition group magnetic element, the 4f rare earth element and the semiconductor element are smelted according to the proportion, and the temperature and the time during the heat treatment are controlled to obtain the rare earth elementAuCu with heterogeneous phase, uniform components and room temperature ferromagnetism3RIn of type structure3-xFexA diluted magnetic alloy material.
Drawings
FIG. 1 shows RIn prepared according to the present invention2.9Fe0.1And (3) an X-ray diffraction pattern of the diluted magnetic alloy material.
FIG. 2 shows RIn prepared according to the present invention2.9Fe0.1The relation curve of magnetic moment and magnetic field of the diluted magnetic alloy material at room temperature.
FIG. 3 shows RIn prepared according to the present invention2.9Fe0.1The heat capacity of the diluted magnetic alloy material is plotted against the temperature.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and examples.
FIG. 1 shows RIn prepared according to the present invention2.9Fe0.1And (3) an X-ray diffraction pattern of the diluted magnetic alloy material.
FIG. 2 shows RIn prepared according to the present invention2.9Fe0.1The relation curve of magnetic moment and magnetic field of the diluted magnetic alloy material at room temperature is shown, wherein a is PrIn2.9Fe0.1B is NdIn2.9Fe0.1C is GdIn2.9Fe0.1D is HoIn2.9Fe0.1。
FIG. 3 shows RIn prepared according to the present invention2.9Fe0.1The heat capacity of the diluted magnetic alloy material is plotted against the temperature. Wherein a, b, c, d are as defined in figure 2.
Two different magnetic atoms are added into the semiconductor element In for modulation, and the magnetic semiconductor material is prepared. A novel semiconductor-based R (In, Fe)1:3 (R ═ rare earth element) compound In which 4f (rare earth) and 3d (magnetic element) transition group metal Fe are co-doped was studied. The method comprises the steps of preparing an experimental sample by a non-consumable electric arc furnace smelting process, preparing the sample into powder required by testing through physical grinding, performing phase structure analysis on the powder by using an X-ray diffraction technology, and searching an X-ray diffraction card so as to determine the phase structure of an alloy compound. Then, weighing samples with the mass of about 40mg for magnetic measurement, exploring the M-H relation, and performing fitting analysis according to experimental data to determine the magnetic order type, saturation magnetization and effective magnetic moment of each sample. A single magnetic rare earth semiconductor structure is formed by a chemical reaction. Through the interaction of 4f rare earth elements and 3d transition group magnetic elements Fe in the compound (3d-4f and 3d-3d interaction), the magnetic structure can be regulated and controlled to form magnetic anisotropy, so that the antiferromagnetism of the original rare earth semiconductor is changed and the original rare earth semiconductor is converted into a ferromagnetic structure.
Example (b): preparation of RIn2.9Fe0.1A diluted magnetic alloy material.
The implementation steps are as follows:
(1) according to the formula RIn2.9Fe0.1Preparing 12g of three simple substance elements of R, In and Fe In a stoichiometric ratio; wherein, the purities of the three simple substances of R, In and Fe are all more than 99.9%;
(2) a non-consumable vacuum arc melting furnace is used for melting three simple substances of R, In and Fe for 3 times under the protection of argon at the current of 40A and the voltage of 220V to obtain ingot-shaped alloy with uniform components and metallic luster.
(3) And (3) putting the smelted ingot alloy into a vacuum quartz tube filled with argon, and carrying out heat treatment in a muffle furnace at the temperature of 800-1000 ℃ for 4-7 days.
(4) Cooling the heat treated sample in cooling water to obtain the product AuCu with room temperature ferromagnetism3RIn of structure2.9Fe0.1A diluted magnetic alloy material.
Subjecting the RIn obtained in step (4) to a Japanese X-ray diffractometer (XRD, D/max 2500 vertical type)2.9Fe0.1The diluted magnetic alloy material is subjected to an X-ray diffraction experiment, and the X-ray diffraction spectrum is shown in figure 1. As can be seen from FIG. 1, the main phase of the sample is RIn3The phase contains a small amount of second-phase In simple substance which can be ignored. Prepared RIn2.9Fe0.1The relation curve of the magnetic moment and the magnetic field of the diluted magnetic alloy material at room temperature is shown in FIG. 2, and the fitting formula and the fitting parameters are shown in Table 1. From FIG. 2 and Table 1, RIn was prepared2.9Fe0.1The diluted magnetic alloy material has the function of doping a small amount of magnetic element FeHas ferromagnetism at room temperature.
Table 1: RIn2.9Fe0.1Fitting formula and fitting parameters of diluted magnetic alloy material
RIn is measured in a temperature range of 300K to 1000K2.9Fe0.1The DSC curve chart of the diluted magnetic alloy material can find the RIn2.9Fe0.1The diluted magnetic alloy materials are all subjected to magnetic transformation at about 430K, as shown in FIG. 3. As can be seen from the graph of fig. 2 showing the relationship between magnetic moment and magnetic field at room temperature, the transition from ferromagnetic to paramagnetic occurs at a curie temperature of about 430K, and the ferromagnetic property is exhibited at this temperature.
The above embodiments describe the technical solutions of the present invention in detail. It will be clear that the invention is not limited to the described embodiments. Based on the embodiments of the present invention, those skilled in the art can make various changes, but any changes equivalent or similar to the present invention are within the protection scope of the present invention.
Claims (6)
1. AuCu3The preparation method of the diluted magnetic alloy material with the structure is characterized in that the chemical formula of the diluted magnetic alloy material is RIn3-xFex(ii) a Wherein R is Pr, Nd, Gd or Ho, and x is less than or equal to 0.1 and not 0; the method comprises the following steps:
(1) according to the formula RIn3-xFexPreparing three elementary elements of R, In and Fe according to the stoichiometric ratio;
(2) repeatedly smelting three simple substance elements of R, In and Fe under the protection of inert gas to obtain an ingot-shaped alloy; the smelting is carried out in a non-consumable arc vacuum smelting furnace, and the smelting current is 40A-200A;
(3) loading the smelted ingot-shaped alloy into a vacuum quartz glass tube filled with inert gas, and placing the quartz glass tube in a muffle furnace for heat treatment at the temperature of 800-1000 ℃;
（4）taking out the sample after heat treatment, and cooling in cold water to obtain the product with AuCu3A diluted magnetic alloy of structure.
2. The method of claim 1, wherein the AuCu is3The type structure is a face-centered cubic structure.
3. The method of claim 1, wherein the diluted magnetic alloy material has room temperature ferromagnetism.
4. The method according to claim 1, wherein the purity of the R, In and Fe In step (1) is above 99.9%.
5. The method as claimed in claim 1, wherein the heat treatment time in the step (3) is 4 to 7 days.
6. The method of claim 1, wherein the inert gas in steps (2) and (3) is argon.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002363680A (en) * | 2001-06-12 | 2002-12-18 | Tdk Corp | Rare-earth/transition metal alloy material with coating layer |
| CN101168448A (en) * | 2007-08-16 | 2008-04-30 | 北京科技大学 | Low-temperature large specific heat magnetic cold-storage material preparation method thereof |
| CN103468224A (en) * | 2013-08-19 | 2013-12-25 | 杭州电子科技大学 | Application of rare earth RPdIn material to low-temperature magnetic refrigeration |
| CN105523527A (en) * | 2015-12-21 | 2016-04-27 | 华北电力大学 | Diluted magnetic semiconductor material having chalcopyrite structure and preparation method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002363680A (en) * | 2001-06-12 | 2002-12-18 | Tdk Corp | Rare-earth/transition metal alloy material with coating layer |
| CN101168448A (en) * | 2007-08-16 | 2008-04-30 | 北京科技大学 | Low-temperature large specific heat magnetic cold-storage material preparation method thereof |
| CN103468224A (en) * | 2013-08-19 | 2013-12-25 | 杭州电子科技大学 | Application of rare earth RPdIn material to low-temperature magnetic refrigeration |
| CN105523527A (en) * | 2015-12-21 | 2016-04-27 | 华北电力大学 | Diluted magnetic semiconductor material having chalcopyrite structure and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| Structure and magnetic transport properties of GdIn3-xMnx intermetallics;Qiang He et al.;《Journal of Magnetism and Magnetic Materials》;20151009;第44-45页 * |
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