A perovskite polycrystalline oxide ytterbium iron YbFe 1-x Nb x O3 synthesis preparation method

Abstract

The application discloses a synthetic preparation method of a perovskite polycrystal oxide YbFe 1‑x Nb x O3, belongs to the technical field of perovskite-based rare earth ferrite magnetic materials, and relates to a synthetic preparation method of YbFe 1‑x Nb x O3, wherein 0.0<=x<=0.5. The specific synthetic preparation steps are as follows: I. weighing and mixing Yb2O3, Fe2O3 and Nb2O5; II. thoroughly grinding and mixing the obtained mixed powder; III. drying the obtained product; IV. then, performing primary sintering treatment in air; V. then, re-grinding and crushing the obtained powder; mixing the powder with a binder; VI. pressing the obtained product into granules; VII. then, performing preheating treatment on the disc granules; VIII. then, performing secondary sintering treatment in a high-temperature furnace, and the sintering time is <=24 hours; IX. after cooling, YbFe 1‑x Nb x O3 is obtained. Through the above method, the development of the polycrystal is promoted, and the polycrystal is beneficial to application in the fields of data storage devices, energy storage dynamics, sensors and spin electronic devices.

Description

Technical Field

[0001] This invention relates to the field of perovskite-based rare-earth ferrite magnetic materials technology, specifically to a perovskite polycrystalline oxide, ytterbium iron oxide (YbFe). 1-x Nb x Methods for synthesizing and preparing O3. Background Technology

[0002] Since the mid-20th century, rare-earth ferrite materials, represented by the orthorhombic crystal structure of RFeO3 (where R represents a rare-earth element), have been the subject of meticulous research. The ferrite family exhibits unique magnetism, emphasizing non-collinear antiferromagnetic properties and intriguing spin-redirection phase transitions. Pioneering research by renowned scientists, including references to the fundamental work of Rado and Suhl in the 1950s, has laid a solid foundation for understanding the complexity of these materials. The magnetic behavior of rare-earth ferrites, particularly the pulsed laser-induced spin-redirection phase transition, has attracted widespread attention. This dynamic phenomenon involves rapid and reversible changes in magnetic spin alignment, offering enormous potential for applications in advanced magnetic devices and sensors.

[0003] Despite the desirable properties of rare earth orthoferrite, the synthesis of high-quality, pure-phase polycrystalline materials remains challenging. Literature reveals shortcomings in existing methods, highlighting limitations in efficiency, purity, and phase control during synthesis. A comprehensive review of relevant literature, including influential work by renowned authors such as Kimel, underscores the necessity for advancements in rare earth orthoferrite synthesis techniques to fully realize its potential.

[0004] Previous studies on YbFeO3 have focused on a relatively narrow range of compositional doping, potentially overlooking a broader picture of the material's properties. The lack of comprehensive exploration into replacing Fe with Nb may lead to an incomplete understanding of the material's properties. This invention proposes the use of Nb in YbFeO3 oxide ceramics... 5+ Schemes involving ion substitution of Fe sites, such as YbFe 1-x Nb x O3 (where x ranges from 0 to 0.5).

[0005] The study by Polat et al. (2019) explored the electrical properties of YbFeO3 through Co doping, but limited the study to specific Co doping levels (x = 0.01, 0.05, 0.10). In contrast, this invention focuses on Nb-doped YbFeO3 (YbFe 1-x Nb xThe study of Co-doped YbFeO3 extends the scope of exploration to a wider range of doping levels (x = 0 to 0.5). This comprehensive approach allows for a more detailed understanding of how different compositions affect material properties. While Polat et al. primarily focused on the electrical properties of Co-doped YbFeO3, evaluating improvements in conductivity and dielectric constant, this invention explores phase formation and spin reorientation transition temperatures. In this study of Nb-doped YbFeO3, the main focus is on how different doping levels can provide a more versatile and tunable material. This wider tunability allows for more precise control of material properties, offering potential advantages in applications requiring customized characteristics.

[0006] Tran Dinh Trinh et al. (2023) focused on the synthesis conditions and magnetic properties of perovskite-based YbFeO3 nanomaterials. Their research primarily concentrated on the synthesis conditions of YbFeO3 (o-YbFeO3), without exploring the impact of compositional variations on material properties. In contrast, this invention introduces a series of Nb dopant components (YbFeO3-O- ... 1-x Nb x Tran Dinh Trinh et al. (2023) analyzed the effects of synthesis conditions on the crystal structure and magnetic behavior of YbFeO3, but did not delve into the impact of different doping compositions on tunability. In contrast, this invention explicitly addresses this, demonstrating the diversity introduced by different doping levels and their potential applications through the introduction of Nb doping. While both studies explored the magnetism of YbFeO3, Tran Dinh Trinh et al. specifically investigated the effect of synthesis conditions on magnetism. In contrast, this invention focuses on the synthesis and spin reorientation transition temperature of Nb-doped YbFeO3. These parameters provide a more comprehensive understanding of the material's magnetic properties across a range of doping compositions.

[0007] Based on this, the present invention designs a perovskite polycrystalline oxide ytterbium iron oxide (YbFe) 1-x Nb x A method for synthesizing and preparing O3 is proposed to solve the above problems. Summary of the Invention

[0008] To identify the crystal phase, structure, and magnetic properties of YbFeO3 ceramics where Nb ions at Fe sites are not substituted, Nb-doped YbFeO3 was synthesized, with up to 50% Nb doping at the Fe sites (e.g., YbFe). 1-x Nb x O3 (0.0≤x≤0.5). This invention provides a perovskite polycrystalline oxide, ytterbium iron oxide (YbFe). 1-x Nb x Methods for synthesizing and preparing O3.

[0009] To achieve the above objectives, the present invention provides the following technical solution:

[0010] A perovskite polycrystalline oxide, ytterbium iron oxide (YbFe) 1-x Nb x O3 synthesis and preparation methods, YbFe 1-x Nb x In O3, 0.0 ≤ x ≤ 0.5; the specific synthesis and preparation steps are as follows:

[0011] 1. Weigh and mix Yb₂O₃, Fe₂O₃, and Nb₂O₅;

[0012] 2. Thoroughly grind and mix the resulting powder;

[0013] 3. The obtained product is then dried.

[0014] Fourth, the initial sintering process is then carried out in air;

[0015] 5. Then, the resulting powder is re-ground and pulverized; the powder is then mixed with the binder;

[0016] 6. The obtained material is pressed into granules;

[0017] 7. Then, preheat the disc particles;

[0018] 8. Then, it is placed in a high-temperature furnace for secondary sintering treatment, with a sintering time of ≤24 hours;

[0019] 9. After cooling, YbFe can be obtained. 1-x Nb x O3.

[0020] 10. Perform X-ray diffraction for structural analysis; conduct magnetic characterization tests.

[0021] Furthermore, in step two, the mixture is stirred in alcohol and thoroughly ground for 6 hours.

[0022] Furthermore, in step three, the obtained product is dried at 80°C.

[0023] Furthermore, step four specifically involves:

[0024] 4.1, The temperature is uniformly raised from room temperature to 650°C within 65 minutes, and then kept constant at 650°C in an air environment for 2 hours;

[0025] 4.2, and then uniformly raise the temperature to 1000℃ over 50 minutes, and maintain it at a constant temperature of 1000℃ in an air environment for 1 hour;

[0026] 4.3, raise to 1250℃, and maintain a constant temperature in an air environment of 1250℃ for 12 hours.

[0027] 4.4 The mixture is naturally cooled to room temperature in the furnace to prepare a polycrystalline powder composed of ytterbium oxide, iron oxide and niobium oxide.

[0028] Furthermore, in step five, the powder is mixed with 5% polyvinyl alcohol.

[0029] Furthermore, in step six, the resulting material is pressed into disc-shaped particles with a diameter of 10 mm and a thickness of 2 mm under a pressure of 100 MPa.

[0030] Furthermore, in step seven, the disc particles are kept at 650°C for 2 hours, with a heating rate of 10°C / minute.

[0031] Furthermore, in step eight, a secondary sintering treatment is carried out in a high-temperature furnace at 1250°C, with a heating rate of 10°C / minute.

[0032] Furthermore, in step nine, the cooling process involves reducing the temperature to room temperature at a rate of 5°C per minute.

[0033] Beneficial effects

[0034] This invention provides a method for preparing YbFe using a high-temperature sintering synthesis method. 1-x Nb x The precursor was prepared using a solid-state reaction method with O3 (0.0≤x≤0.5), and the magnetic spin redirection transition temperature of the obtained compound was systematically studied for the first time. Nb was introduced by doping the Fe sites of YbFeO3. 5+ This method not only enhances the structural diversity of perovskite oxides, but also allows control over spin orientation within the material.

[0035] Experimental results from X-ray diffraction and magnetization-temperature profiles demonstrate the effectiveness of this method in improving sample quality and magnetic properties. X-ray diffraction analysis revealed the phase formation of YbFeO3, Yb2O3, FeNbO4, and YbNbO4. Unsubstituted ceramics exhibit a pure single-phase YbFeO3; however, with increasing Yb substitution at Fe sites, additional phases of Yb2O3, FeNbO4, and YbNbO4 were observed. Importantly, the spin redirection transition temperature showed a shift to higher temperatures with increasing Nb2O5 substitution. This invention promotes the development of polycrystalline materials, which is beneficial for applications in data storage devices, energy storage dynamics, sensors, and spintronic devices. Attached Figure Description

[0036] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the accompanying drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are merely some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without any creative effort.

[0037] Figure 1 YbFe was displayed 1-x Nb x XRD pattern of O3 (0.0≤x≤0.5).

[0038] Figure 2 YbFe was displayed 1-x Nb x Magnetization-temperature (MT) curves of O3 (0.0≤x≤0.5) in FCC and ZFC modes.

[0039] Figure 3 This indicates that the spin redirection transition in YbFeO3 ceramics changes with Nb 5+ Changes in doping.

[0040] Figure 4 This is a flowchart of the present invention. Detailed Implementation

[0041] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some, not all, of the embodiments of the present invention. All other embodiments obtained by those skilled in the art based on the embodiments of the present invention without creative effort are within the scope of protection of the present invention.

[0042] A perovskite polycrystalline oxide, ytterbium iron oxide (YbFe) 1-x Nb x O3 synthesis and preparation methods, YbFe 1-x Nb x In O3, 0.0 ≤ x ≤ 0.5; the specific synthesis and preparation steps are as follows:

[0043] 1. Weigh and mix Yb₂O₃, Fe₂O₃, and Nb₂O₅;

[0044] 2. Mix the resulting powder in alcohol and grind it thoroughly for 6 hours;

[0045] 3. The obtained product is dried at 80℃; (this step can be omitted)

[0046] IV. Subsequent initial sintering treatment in air; specifically:

[0047] 4.1, The temperature is uniformly raised from room temperature to 650°C within 65 minutes, and then kept constant at 650°C in an air environment for 2 hours;

[0048] 4.2, and then uniformly raise the temperature to 1000℃ over 50 minutes, and maintain it at a constant temperature of 1000℃ in an air environment for 1 hour;

[0049] 4.3 Finally, raise the temperature to 1250°C and maintain it at a constant temperature in an air environment of 1250°C for 12 hours.

[0050] 4.4 The mixture is naturally cooled to room temperature in the furnace to prepare a polycrystalline powder composed of ytterbium oxide, iron oxide and niobium oxide.

[0051] 5. Then, the obtained powder is re-ground and pulverized; the powder is then mixed with 5% polyvinyl alcohol;

[0052] VI. The obtained material is pressed into disc-shaped particles with a diameter of 10 mm and a thickness of 2 mm under a pressure of 100 MPa;

[0053] 7. The disc particles are held at 650℃ for 2 hours, with a heating rate of 10℃ / minute; (this step can be omitted)

[0054] 8. Then, it is placed in a high-temperature furnace at 1250℃ for secondary sintering treatment, with a heating rate of 10℃ / minute and a sintering time of ≤24 hours;

[0055] 9. After cooling, YbFe can be obtained. 1-x Nb x O3 was cooled to room temperature at a rate of 5°C per minute.

[0056] 10. Perform X-ray diffraction for structural analysis; conduct magnetic characterization tests.

[0057] The present invention will be further described below with reference to embodiments.

[0058] Example 1: Synthesis of polycrystalline ytterbium iron oxide (YbFeO3) (x = 0.0) perovskite oxide (Sample 1)

[0059] Using analytically pure Yb₂O₃ (7.1165 g) and Fe₂O₃ (2.8835 g) in a 1:1 molar ratio, each with a purity of 99.99%, the raw materials were accurately weighed and proportioned according to the molecular formula YbFeO₃. The resulting mixed powder was then placed in an agate mortar and thoroughly ground for 6 hours, followed by initial sintering at 650°C in air for 12 hours. The mixture was then naturally cooled to room temperature in a furnace to obtain a polycrystalline powder composed of ytterbium oxide and iron oxide. The resulting powder was then re-ground and calcined at 1250°C for 12 hours. Subsequently, the polycrystalline powder was further ground in an agate mortar, and the powder was mixed with 5% polyvinyl alcohol. The resulting mixture was pressed into disc-shaped particles with a diameter of 10 mm and a thickness of 2 mm under a pressure of 100 MPa. Then, the discs were sintered in a high-temperature furnace at 1250 °C with a heating rate of 10 °C / min for 24 hours, and then cooled to room temperature to obtain the final product—polycrystalline disc-shaped oxide ceramic particles. These particles were removed and finely ground to obtain YbFeO3 powder. X-ray diffraction (XRD) analysis and magnetic observation were performed on the obtained product, and the results are shown in the following figures. Figure 1 , Figure 2 and Figure 3 As shown.

[0060] Figure 1 The X-ray diffraction (XRD) pattern of the product obtained by analyzing the powder using an X-ray diffractometer (Rigaku Ultima IV) with Cu-Kα1 radiation is shown. The scan range was 20°–80°, the scan rate was 5° / min, and the step size was 0.02°. Figure 1 As can be seen, the XRD pattern of the obtained product perfectly matches that of standard YbFeO3 (PDF#47-0070). This indicates that the prepared product is YbFeO3, and the cell parameters are... and

[0061] Figure 2 YbFe was displayed 1-x Nb x The magnetization of O3 samples (x = 0, 0.1, 0.2, 0.3, 0.4, 0.5) is expressed as a function of temperature in both zero-field cooling (ZFC) and field cooling (FCC) modes, and the spin redirection transition temperature (T0) at 9.96 K is represented. SR ).

[0062] Figure 3 The presence of Nb in YbFeO3 ceramics was shown. 5+ Changes in doped spin redirection transitions. Figure 3 Indicates the spin redirection transition temperature (T) SR (The value is between 9 and 35K.)

[0063] Example 2: Synthesis of YbFe Oxide 1-x Nb x O3 (x=0.1) perovskite oxide polycrystalline (sample 2)

[0064] The preparation process differs from that of Sample 1 in that:

[0065] The raw materials were selected with a molar ratio of 1:0.9:0.1, using analytically pure Yb₂O₃ (99.99%), Fe₂O₃ (99.99%), and Nb₂O₅ (99.99%). The raw materials were selected according to the molecular formula YbFe mentioned in Table 1. 0.9 Nb 0.1 Accurately weigh and mix O3.

[0066] The initial sintering process was as follows: the temperature was uniformly raised from room temperature to 650°C within 65 minutes and held constant at 650°C in air for 2 hours; then uniformly raised to 1000°C within 50 minutes and held constant at 1000°C in air for 1 hour; finally, the temperature was raised to 1250°C and held constant at 1250°C in air for 12 hours. The mixture was then naturally cooled to room temperature in the furnace to prepare a polycrystalline powder composed of ytterbium oxide, iron oxide, and niobium oxide.

[0067] The remaining steps are the same as those in Sample 1.

[0068] Table 1 Summary of sample composition and molar ratio

[0069]

[0070] Extract and finely grind to obtain YbFe 0.9 Nb 0.1 O3 powder product. X-ray diffraction (XRD) analysis and magnetic observation were performed on the obtained product, and the results are as follows: Figure 1 , Figure 2 and Figure 3 As shown.

[0071] Figure 1 The X-ray diffraction (XRD) pattern of the product obtained from powder analysis using a Cu-Kα radiation X-ray diffractometer (Rigaku Ultima IV) is shown. The spectral scan was performed at 40 kV and 40 mA, with a scan range of 20°–80°, a scan rate of 5° / min, and a step size of 0.02°. Figure 1 As can be seen, the XRD pattern of the obtained product perfectly matches that of standard YbFeO3 (PDF#47-0070). This indicates that the prepared product is YbFeO3, and the cell parameters are... and

[0072] Figure 2 YbFe was displayed 1-x Nb x The magnetization of O3 samples (x = 0, 0.1, 0.2, 0.3, 0.4, 0.5) as a function of temperature in zero-field cooling (ZFC) and field cooling (FCC) modes is expressed, and is represented by YbFe at 19.41 K. 0.9 Nb 0.1 Spin redirection transition temperature (T) of O3 powder products SR ).

[0073] Figure 3 The presence of Nb in YbFeO3 ceramics was shown. 5+ Changes in doped spin redirection transitions. Figure 3 Indicates the spin redirection transition temperature (T) SR (The value is between 9 and 35K.)

[0074] Example 3: Synthesis of YbFe Oxide 1-x Nb x O3 (x=0.2) perovskite oxide polycrystalline (sample 3)

[0075] Using analytically pure Yb₂O₃ (99.99%), Fe₂O₃ (99.99%), and Nb₂O₅ (99.99%) as raw materials, with a molar ratio of 1:0.8:0.2, the original molecular formula YbFe₂O₃ was used. 0.8 Nb 0.2 Accurately weigh and mix O3. The following process is the same as that for sample 1.

[0076] Remove and grind finely. Obtain YbFe 0.8 Nb 0.2 O3 powder product. The obtained product was analyzed by X-ray diffraction (XRD) and magnetic observation, and the results are as follows: Figure 1 and Figure 2 As shown.

[0077] Figure 1 The X-ray diffraction (XRD) pattern of the product obtained from powder analysis using a Cu-Kα radiation X-ray diffractometer (Rigaku Ultima IV) at 40 kV and 40 mA, with a scan range of 20°–80°, a scan rate of 5° / min, and a step size of 0.02°. Figure 1 As can be seen, the XRD pattern of the obtained product perfectly matches that of standard YbFeO3 (PDF#47-0070). This indicates that the prepared product is YbFeO3, and the cell parameters are... and Other phases include YbNbO4 and Yb2O3.

[0078] Figure 2 This explains YbFe 1-x Nb x The magnetization of O3 samples (x = 0, 0.1, 0.2, 0.3, 0.4, 0.5) as a function of temperature in zero-field cooling (ZFC) and field cooling (FCC) modes is expressed, and YbFe is represented. 0.8 Nb 0.2 The spin orientation transition temperature (T0) of O3 powder products at 25.14 K SR ).

[0079] Figure 3 The presence of Nb in YbFeO3 ceramics was shown. 5+ Changes in doped spin redirection transitions. Figure 3 Indicates the spin redirection transition temperature (T) SR (The value is between 9 and 35K.)

[0080] Example 4: Synthesis of YbFe Oxide 1-x Nb x O3 (x=0.3) perovskite oxide polycrystalline (sample 4)

[0081] Using analytically pure Yb₂O₃ (99.99%), Fe₂O₃ (99.99%), and Nb₂O₅ (99.99%) as raw materials in a molar ratio of 1:0.7:0.3, and with the molecular formula YbFe₂O₃ listed in Table 1 as the raw materials, the raw materials were prepared according to the formulas listed in Table 1. 0.7 Nb 0.3 Accurately weigh and mix O3. The following process is the same as that for sample 1.

[0082] Remove and grind finely to obtain YbFe 0.7 Nb 0.3 O3 powder product. X-ray diffraction (XRD) analysis and magnetic observation were performed on the obtained product, and the results are shown in the following figures. Figure 1 and Figure 2 middle.

[0083] Figure 1 The X-ray diffraction (XRD) pattern of the product obtained from powder analysis using a Cu-Kα radiation X-ray diffractometer (Rigaku Ultima IV) at 40 kV and 40 mA, with a scan range of 20°–80°, a scan rate of 5° / min, and a step size of 0.02°. Figure 1 As can be seen, the XRD pattern of the obtained product perfectly matches that of standard YbFeO3 (PDF#47-0070). This indicates that the prepared product is YbFeO3, and the cell parameters are... and The other phases are YbNbO4 and Yb2O3.

[0084] Figure 2 YbFe was displayed 1-x Nb x The magnetization of O3 samples (x = 0, 0.1, 0.2, 0.3, 0.4, 0.5) as a function of temperature in zero-field cooling (ZFC) and field cooling (FCC) modes is expressed, and YbFe is represented. 0.7 Nb 0.3 The spin redirection transition temperature (T3) of O3 powder products at 28.75 K. SR ).

[0085] Figure 3 The presence of Nb in YbFeO3 ceramics was shown. 5+ Changes in doped spin redirection transitions. Figure 3 Indicates the spin redirection transition temperature (T) SR (The value is between 9 and 35K.)

[0086] Example 5: Synthesis of YbFe Oxide 1-x Nb x O3 (x=0.4) perovskite oxide polycrystalline (sample 5)

[0087] Using analytically pure Yb₂O₃ (99.99%), Fe₂O₃ (99.99%), and Nb₂O₅ (99.99%) as raw materials in a molar ratio of 1:0.6:0.4, the raw materials were prepared according to the molecular formula YbFe₂O₃ mentioned in Table 1. 0.6 Nb 0.4 Accurately weigh and mix O3. The following process is the same as that for sample 1.

[0088] Remove and grind finely to obtain YbFe 0.6 Nb 0.4 O3 powder product. X-ray diffraction (XRD) analysis and magnetic observation were performed on the obtained product, and the results are as follows: Figure 1 and Figure 2 As shown.

[0089] Figure 1 The X-ray diffraction (XRD) pattern of the product obtained by powder analysis using a Cu-Kα radiation X-ray diffractometer (Rigaku Ultima IV) is shown. The spectrum was obtained at 40 kV and 40 mA, with a scan range of 20°–80°, a scan rate of 5° / min, and a step size of 0.02°. Figure 1 As can be seen, the XRD pattern of the obtained product perfectly matches that of standard YbFeO3 (PDF#47-0070). This indicates that the prepared product is YbFeO3, and the cell parameters are... and The other phases are YbNbO4, Yb3NbO7 and Yb2O3.

[0090] Figure 2 This explains YbFe 1-x Nb x The magnetization of O3 samples (x = 0, 0.1, 0.2, 0.3, 0.4, 0.5) as a function of temperature in zero-field cooling (ZFC) and field cooling (FCC) modes is expressed, and YbFe is represented. 0.6 Nb 0.4 The spin redirection transition temperature (T3) of the O3 powder product at 32.76 K SR ).

[0091] Figure 3 The presence of Nb in YbFeO3 ceramics was shown. 5+ Changes in doped spin redirection transitions. Figure 3 Indicates the spin redirection transition temperature (T) SR (The value is between 9 and 35K.)

[0092] Example 6: Synthesis of YbFe Oxide 1-x NbxO3 (x=0.5) perovskite oxide polycrystalline (sample 6)

[0093] YbFe 0.5 Nb 0.5 The synthesis of polycrystalline O3 perovskite oxide involves a meticulous preparation process. Analytically pure Yb₂O₃ (99.99%), Fe₂O₃ (99.99%), and Nb₂O₅ (99.99%) were used as raw materials in a molar ratio of 1:0.5:0.5. The raw materials were prepared according to the molecular formula YbFe₂O₃ mentioned in Table 1. 0.5 Nb 0.5 Accurately weigh and mix O3. The following process is the same as that for sample 1.

[0094] Remove and grind finely to obtain YbFe 0.5 Nb 0.5 O3 powder product. The obtained product was analyzed by X-ray diffraction (XRD) and magnetic observation, and the results are as follows: Figure 1 and Figure 2 As shown.

[0095] Figure 1 The X-ray diffraction (XRD) pattern of the product obtained from powder analysis using a Cu-Kα radiation X-ray diffractometer (Rigaku Ultima IV) is shown. The spectrum was obtained at 40 kV and 40 mA, with a scan range of 20°–80°, a scan rate of 5° / min, and a step size of 0.02°. Figure 1 As can be seen, the XRD pattern of the obtained product perfectly matches that of standard YbFeO3 (PDF#47-0070). This indicates that the prepared product is YbFeO3, and the cell parameters are... and The other phases are YbNbO4, FeNbO4 and Yb2O3.

[0096] Figure 2 YbFe was displayed 1-x Nb x The magnetization of O3 samples (x = 0, 0.1, 0.2, 0.3, 0.4, 0.5) as a function of temperature in zero-field cooling (ZFC) and field cooling (FCC) modes is expressed, and YbFe is represented. 0.5 Nb 0.5 The spin redirection transition temperature (T3) of O3 powder products at 34.78 K. SR ).

[0097] Figure 3 The presence of Nb in YbFeO3 ceramics was shown. 5+ Changes in doped spin redirection transitions. Figure 3 Indicates the spin redirection transition temperature (T) SR (The value is between 9 and 35K.)

[0098] In summary, Figure 1 X-ray diffraction (XRD) analysis showed that the obtained product was completely identical to standard YbFeO3 (PDF#47-0070), confirming its structural integrity. The initial YbFeO3 and YbFe... 0.9 Nb 0.1 The O3 samples exhibited a pure phase, while different Nb doping levels (x = 0.2, 0.3, 0.4, 0.5) introduced additional phases, as detailed in Table 2. The observed trends indicate that Nb... +5 Ion doping leads to the formation of composite materials. YbFe2 under both zero-field cooling (ZFC) and field cooling (FCC) modes... 1-x Nb x The magnetization curves of the O3 samples (x = 0, 0.1, 0.2, 0.3, 0.4, 0.5) reveal the spin redirection transition temperature (T) in YbFeO3. SR The K value is approximately T ~ 9.96 K. The results show that in YbFe... 1-x Nb x T in O3 samples (x = 0, 0.1, 0.2, 0.3, 0.4, 0.5) SR Within the 9-35K range. Nb 5+ The substitution of ions leads to T SR This is the first observed fine-tuning of the transition to higher temperatures. The temperature (T) was modulated by the Nb ion doping concentration. SR This innovative approach opens up new possibilities for customizing the magnetism of YbFeO3-based perovskite ceramics.

[0099] Table 2 YbFe 1-x Nb x Phase formation and lattice parameters of O3 ceramics, spin orientation transformation (T) SR Temperature Summary

[0100]

[0101] This invention systematically explores the effects of different Nb doping compositions on YbFeO3 from a more nuanced perspective through in-depth research on a wider range of doping elements. This broader exploration not only reveals new aspects of the material's behavior but also lays the foundation for customizing its properties to meet specific needs. Introducing various doping levels allows for a thorough analysis of the material's tunability and versatility, significantly improving upon the limitations imposed by previous studies.

[0102] The above embodiments are only used to illustrate the technical solutions of the present invention, and are not intended to limit it. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some of the technical features. Such modifications or substitutions will not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims

1. A perovskite polycrystalline oxide, ytterbium iron oxide (YbFe) 1-x Nb x The method for synthesizing and preparing O3 is characterized by, YbFe 1- x Nb x In O3, 0.0 < x ≤0.5; The specific synthesis and preparation steps are as follows:

1. Weigh and mix Yb₂O₃, Fe₂O₃, and Nb₂O₅; 2. Thoroughly grind and mix the resulting powder; Third, a preliminary sintering treatment in air is then performed; specifically: The temperature was uniformly increased from room temperature to 650°C over 65 minutes and held constant at 650°C in air for 2 hours; then uniformly increased to 1000°C over 50 minutes and held constant at 1000°C in air for 1 hour; then increased to 1250°C and held constant at 1250°C in air for 12 hours; the mixture was then allowed to cool naturally to room temperature in the furnace to prepare a polycrystalline powder composed of ytterbium oxide, iron oxide, and niobium oxide.

4. Then, the resulting powder is re-ground and pulverized; the powder is then mixed with the binder.

5. The obtained material is pressed into granules; 6. Then, it is placed in a high-temperature furnace for secondary sintering treatment, with a sintering time of ≤24 hours; Seven, after cooling, YbFe 1-x Nb x O3.

2. The perovskite polycrystalline oxide ytterbium iron oxide (YbFe) according to claim 1 1-x Nb x The method for synthesizing and preparing O3 is characterized by, In step two, mix in alcohol and grind thoroughly for 6 hours.

3. The perovskite polycrystalline oxide ytterbium iron oxide (YbFe) according to claim 2 1-x Nb x The method for synthesizing and preparing O3 is characterized by, Between step two and step three, the following step is also included: the obtained product is dried at 80°C.

4. The perovskite polycrystalline oxide ytterbium iron oxide (YbFe) according to claim 3 1-x Nb x The method for synthesizing and preparing O3 is characterized by, In step four, the powder is mixed with 5% polyvinyl alcohol.

5. The perovskite polycrystalline oxide ytterbium iron oxide (YbFe) according to claim 4 1-x Nb x The method for synthesizing and preparing O3 is characterized by, In step five, the resulting material is pressed into disc-shaped particles with a diameter of 10 mm and a thickness of 2 mm under a pressure of 100 MPa.

6. The perovskite polycrystalline oxide ytterbium iron oxide (YbFe) according to claim 5 1-x Nb x The method for synthesizing and preparing O3 is characterized by, In step six, a secondary sintering treatment is carried out in a high-temperature furnace at 1250℃, with a heating rate of 10℃ / minute.

7. The perovskite polycrystalline oxide ytterbium iron oxide (YbFe) according to claim 6 1-x Nb x The method for synthesizing and preparing O3 is characterized by, Between steps five and six, the following step is also included: then preheating the disc particles.

8. The perovskite polycrystalline oxide ytterbium iron oxide (YbFe) according to claim 7 1-x Nb x The method for synthesizing and preparing O3 is characterized by, The disc particles were kept at 650℃ for 2 hours, with a heating rate of 10℃ / minute.

9. The perovskite polycrystalline oxide ytterbium iron oxide (YbFe) according to claim 8 1-x Nb x The method for synthesizing and preparing O3 is characterized by, In step seven, the cooling process involves reducing the temperature to room temperature at a rate of 5°C per minute.

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