CN116514536A - High-entropy YIG ferrite with high saturation magnetization and preparation method thereof - Google Patents
High-entropy YIG ferrite with high saturation magnetization and preparation method thereof Download PDFInfo
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- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 77
- 230000005415 magnetization Effects 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 59
- 238000001035 drying Methods 0.000 claims abstract description 27
- 238000000498 ball milling Methods 0.000 claims abstract description 26
- 238000005245 sintering Methods 0.000 claims abstract description 11
- 238000007873 sieving Methods 0.000 claims abstract description 7
- 238000005303 weighing Methods 0.000 claims abstract description 7
- 238000000748 compression moulding Methods 0.000 claims abstract description 3
- 239000002002 slurry Substances 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
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- 239000010959 steel Substances 0.000 claims description 6
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 claims description 5
- 229910021193 La 2 O 3 Inorganic materials 0.000 claims description 5
- 229910017493 Nd 2 O 3 Inorganic materials 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 239000002223 garnet Substances 0.000 abstract description 13
- 239000000463 material Substances 0.000 abstract description 11
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 6
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- 238000005516 engineering process Methods 0.000 description 2
- MTRJKZUDDJZTLA-UHFFFAOYSA-N iron yttrium Chemical compound [Fe].[Y] MTRJKZUDDJZTLA-UHFFFAOYSA-N 0.000 description 2
- 230000005389 magnetism Effects 0.000 description 2
- -1 oxygen ion Chemical class 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 229910006404 SnO 2 Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
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- 229910052760 oxygen Inorganic materials 0.000 description 1
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- 239000000243 solution Substances 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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- C04B35/26—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on ferrites
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Abstract
The invention discloses a high-entropy YIG ferrite with high saturation magnetization and a preparation method thereof, comprising the following steps: s1, weighing different oxide powders, placing the powder into a ball mill, and placing the slurry into a drying oven to obtain uniform powder after ball milling is finished; s2, sieving the powder dried in the step S1, and placing the sieved powder in a muffle furnace for presintering; s3, placing the powder pre-sintered in the step S2 into a ball mill for secondary ball milling and drying; s4, granulating the powder dried in the step S3, and then performing compression molding to obtain a ferrite green body; and S5, placing the ferrite green body obtained in the step S4 into a muffle furnace for sintering to obtain the high-entropy YIG ferrite. The high-entropy YIG ferrite with high saturation magnetization and the preparation method thereof are adopted, and the ferrite material has more excellent performance by combining the high entropy with the garnet type ferrite structure.
Description
Technical Field
The invention relates to the technical field of ferrite materials, in particular to a high-entropy YIG ferrite with high saturation magnetization and a preparation method thereof.
Background
With the continuous development of communication technology, the coverage of the global 5G signal is also expanding, the technical level of 5G in China and the construction progress of base stations are in the forefront of the world, and gyromagnetic ferrite is an important raw material for manufacturing radio frequency devices, and the position importance of gyromagnetic ferrite is increasingly outstanding. With the development of satellite remote sensing technology, the positioning and navigation of smart phones, smart homes, smart automobiles and other devices are becoming popular, and with the demands of the fields of industry, medical treatment, military and the like, the development space of the industry is wide, and the development potential of the industry is also becoming larger. The use of garnet-type ferrites in ferrites has been rapidly developing since the discovery of ferrites in 1956. At present, it has been widely applied to various microwave devices such as circulators, isolators, filters, and the like.
In garnet ferrite crystal structures, the cations fully occupy oxygen ion vacancies, which makes it difficult for charged particles to move, thereby having lower ferroresonance linewidths and dielectric losses than other crystal structures. Meanwhile, the garnet structure has three positions occupied by ions, and Y 3+ Is a non-magnetic particle, the magnetism of the material is formed by Fe 3+ Contribution of Fe at different positions 3+ Two secondary lattices are formed, the magnetic moment of which is different in size and opposite in direction, so that the net magnetic moment of the material is not zero. And the particles at three positions can be replaced by different ions, so that the saturation magnetization, coercive force, ferromagnetic resonance line width and other magnetic properties of the particles can be changed to meet the requirements of various applications.
The high entropy is a new material design concept which is developed in recent years, is originally developed from high entropy alloy, forms a single-phase solid solution by proportionally dissolving various alloy elements together, is a hot spot for material research, and is expanded to the fields of high entropy ceramics, high entropy polymers, high entropy composite materials and the like. The high-entropy material has four core effects of thermodynamic high entropy effect, structural lattice distortion effect, kinetic hysteresis effect and performance 'cocktail' effect, and has more excellent performance due to the core effects. However, there have been few studies on the combination of high entropy and garnet-type ferrite structures in the prior art.
Disclosure of Invention
The invention aims to provide a high-entropy YIG ferrite with high saturation magnetization and a preparation method thereof, and the ferrite material has more excellent performance by combining the high entropy with a garnet type ferrite structure.
In order to achieve the above object, the present invention provides a high entropy YIG ferrite having high saturation magnetization and a method for preparing the same, comprising the steps of:
s1, weighing different oxide powders, placing the powder into a ball mill, and placing the slurry into a drying oven for drying after the ball milling is finished;
s2, sieving the powder dried in the step S1, and placing the sieved powder in a muffle furnace for presintering;
s3, placing the powder pre-sintered in the step S2 into a ball mill for secondary ball milling and drying;
s4, granulating the powder dried in the step S3, and then performing compression molding to obtain a ferrite green body;
and S5, placing the ferrite green body obtained in the step S4 into a muffle furnace for sintering to obtain the high-entropy YIG ferrite.
Preferably, in step S1, the oxide powder is La 2 O 3 、Yb 2 O 3 、Er 2 O 3 、Tm 2 O 3 、Ho 2 O 3 、Dy 2 O 3 、Gd 2 O 3 、Sm 2 O 3 、Nd 2 O 3 、Ce 2 O 3 、Eu 2 O 3 、Bi 2 O 3 、Y 2 O 3 And Fe (Fe) 2 O 3 One or more of the following;
oxide molar ratio in powder material followsStudy type (Re) x Ce y Eu y Bi z Y 3-x-2y-z )Fe 5 O 12 Wherein x, y, z > 0, x+2y+z=1; re is one of La, yb, tm, er, ho, dy, gd, sm, nd, lu.
Preferably, in step S1, the purity of the oxide powder is not less than 99.9%.
Preferably, in the steps S1 and S3, the ball mill uses steel balls as grinding media, pure water is used as dispersing agent for ball milling, the rotating speed of the ball mill is 100-200 rad/min, the effective ball milling time is 20-24 h, and powder in the ball mill is prepared by the following steps: ball: the water ranges from 1:2:1 to 1:3:1.5.
Preferably, in the steps S1 and S3, the drying temperature is 135-165 ℃ and the drying time is 6-10h.
Preferably, the calcination temperature in the muffle furnace in the step S2 is 950-1150 ℃ and the calcination time is 2-4 h.
Preferably, the binder used in the granulation in the step S4 is a PVA aqueous solution with the weight percent of 5-7, and the dosage of the binder is 10-15 percent of the mass of ferrite powder.
Preferably, in the step S4, the pressing is performed by using a hydraulic press, the pressure of the hydraulic press is 100-150 Mpa, and the pressure holding time is 0.1-5 min.
Preferably, the sintering in step S5 is performed at a sintering temperature of 1250-1400 ℃ for 2-4 hours.
A preparation method of high-entropy YIG ferrite with high saturation magnetization.
The invention has the beneficial effects that:
1. the invention prepares the high-entropy YIG ferrite material by using six oxide powders: (Re) x Ce y Eu y Bi z Y 3-x-2y-z )Fe 5 O 12 Wherein x, y, z > 0, x+2y+z=1; re is one of La, yb, tm, er, ho, dy, gd, sm, nd, lu, wherein Re represents rare earth element ion and Ce 3+ 、Eu 3+ And Bi (Bi) 3+ Because of the larger ionic radius, all occupy the dodecahedral position in the garnet lattice, replace part Y 3+ By introducing Bi 3+ Can effectively reduce garnetSynthesis temperature, introduction of Eu 3+ Can improve the spontaneous magnetization intensity of the spherical crystal, and in Ce 3+ In presence of 4f 1 And 4f 0 5d 1 Intra-ionic electric dipole transitions between configurations, contributing to Faraday Rotation (FR), the remaining rare earth ions can improve the magnetic properties of garnet ferrite to some extent;
2. according to the yttrium iron garnet ferrite provided by the invention, through the summation of various oxides, the whole Gibbs free energy of the material is minimized, and the stable single-phase high-entropy ferrite is obtained, and the mechanical property, the thermal property, the electrical property, the magnetism, the optical property and the corrosion resistance of the ferrite are improved to a certain extent;
3. the high-entropy yttrium iron garnet ferrite provided by the invention not only has a stable single phase, but also has higher saturation magnetization (more than 1700 Gs) and lower coercivity, and can meet the application requirements of 5G microwave devices;
4. the high-entropy YIG ferrite provided by the invention has stable single phase, higher saturation magnetization, higher dielectric constant and lower dielectric loss.
The technical scheme of the invention is further described in detail through the drawings and the embodiments.
Drawings
FIG. 1 is an X-ray diffraction chart of the high entropy YIG ferrite prepared in example 2 of the present invention;
FIG. 2 is an X-ray diffraction pattern of the conventional YIG-doped ferrite prepared in comparative example 1 of the present invention.
Detailed Description
The invention will be further described with reference to examples. Unless defined otherwise, technical or scientific terms used herein should be given the ordinary meaning as understood by one of ordinary skill in the art to which this invention belongs. The above-mentioned features of the invention or the features mentioned in the specific examples can be combined in any desired manner, and these specific examples are only intended to illustrate the invention and are not intended to limit the scope of the invention.
Example 1
S1, according to the chemical formula (La 0.25 Ce 0.25 Eu 0.25 Bi 0.25 Y 2 )Fe 5 O 12 Weighing Y in proportion 2 O 3 、Ce 2 O 3 、Eu 2 O 3 、Bi 2 O 3 、La 2 O 3 、Fe 2 O 3 The powder is placed in a ball mill, ball milling is carried out by taking steel balls as grinding media and pure water as dispersing agent, the ball-water ratio in the ball mill is 1:2:1, the rotation speed of a central shaft is 100rad/min, and the ball milling time is 24 hours. The temperature of the drying oven is 135 ℃, and the drying time is 8 hours.
S2, sieving the dried powder, and placing the sieved powder in a muffle furnace for presintering, and calcining for 4 hours at 950 ℃.
S3, placing the presintered powder in a ball mill for secondary ball milling, wherein parameters are unchanged, and the time is 24 hours; and after ball milling, placing the mixture in a drying oven at 135 ℃ for drying for 8 hours.
S4, placing ferrite powder into a mortar for granulation, and dropwise adding a PVA aqueous solution with the weight percent of 5 percent while manually grinding, wherein the dosage of the adhesive is 10 percent of the mass of the powder; placing the granulated powder into a die, applying pressure to 100Mpa by using a hydraulic press, maintaining the pressure for 0.5min, and demoulding to obtain ferrite green blanks.
S5, placing the ferrite green body in a muffle furnace, wherein the sintering process comprises the following steps: the room temperature is 1h to 120 ℃, the temperature is 10h to 330 ℃, the glue is discharged by slowly heating, the temperature is 10h to 1200 ℃, the temperature is 1h to 1250 ℃, the heat is preserved for 2h to 1200 ℃, the temperature is preserved for 2h, and the temperature is preserved for 1h to 1100 ℃ and then the furnace is cooled. Obtaining the high-entropy ferrite with garnet structure.
Example 2
S1, according to the chemical formula (La 0.25 Ce 0.25 Eu 0.25 Bi 0.25 Y 2 )Fe 5 O 12 Weighing Y in proportion 2 O 3 、Ce 2 O 3 、Eu 2 O 3 、Bi 2 O 3 、La 2 O 3 、Fe 2 O 3 The powder is placed in a ball mill, ball milling is carried out by taking steel balls as grinding media and pure water as dispersing agent, the ball-water ratio in the ball mill is 1:2.8:1.3, the rotation speed of a central shaft is 150rad/min, and the ball milling time is 24 hours. The temperature of the drying oven is 150 ℃ and the drying time is 8 hours.
S2, sieving the dried powder, placing the sieved powder in a muffle furnace for presintering, and calcining for 4 hours at 1100 ℃.
S3, placing the presintered powder in a ball mill for secondary ball milling, wherein parameters are unchanged, and the time is 24 hours; and (5) after ball milling, placing the mixture in a drying oven at 150 ℃ for drying for 8 hours.
S4, placing ferrite powder into a mortar for granulation, and dropwise adding 7wt% of PVA aqueous solution while manually grinding, wherein the dosage of the adhesive is 12% of the mass of the powder; placing the granulated powder into a die, applying pressure to 100Mpa by using a hydraulic press, maintaining the pressure for 1min, and then demolding to obtain ferrite green blanks.
S5, placing the ferrite green body in a muffle furnace, wherein the sintering process comprises the following steps: the room temperature is 1h to 120 ℃, the temperature is 10h to 330 ℃, the glue is discharged by slowly heating, the temperature is 10h to 1200 ℃, the temperature is 1h to 1250 ℃, the heat is preserved for 2h to 1200 ℃, the temperature is preserved for 2h, and the temperature is preserved for 1h to 1100 ℃ and then the furnace is cooled. Obtaining the high-entropy ferrite with garnet structure. Fig. 1 is an X-ray diffraction diagram of the high-entropy YIG ferrite prepared in example 2 of the present invention, and as can be seen from fig. 1, a high-entropy ferrite of single-phase garnet structure is finally obtained.
Example 3
S1, according to the chemical formula (La 0.25 Ce 0.25 Eu 0.25 Bi 0.25 Y 2 )Fe 5 O 12 Weighing Y in proportion 2 O 3 、Ce 2 O 3 、Eu 2 O 3 、Bi 2 O 3 、La 2 O 3 、Fe 2 O 3 The powder is placed in a ball mill, ball milling is carried out by taking steel balls as grinding media and pure water as dispersing agent, the ball-water ratio in the ball mill is 1:3:1.5, the rotation speed of a central shaft is 200rad/min, and the ball milling time is 24 hours. The temperature of the drying oven is 150 ℃ and the drying time is 8 hours.
S2, sieving the dried powder, and placing the sieved powder in a muffle furnace for presintering, and calcining for 4 hours at 1150 ℃.
S3, placing the presintered powder in a ball mill for secondary ball milling, wherein parameters are unchanged, and the time is 24 hours; and (5) after ball milling, placing the mixture in a drying oven at 165 ℃ and drying for 8 hours.
S4, placing ferrite powder into a mortar for granulation, and dropwise adding 7wt% of PVA aqueous solution while manually grinding, wherein the dosage of the adhesive is 15% of the mass of the powder; placing the granulated powder into a die, applying pressure to 100Mpa by using a hydraulic press, maintaining the pressure for 5min, and then demolding to obtain ferrite green blanks.
S5, placing the ferrite green body in a muffle furnace, wherein the sintering process comprises the following steps: the room temperature is 1h to 120 ℃, the temperature is 10h to 330 ℃, the glue is discharged by slowly heating, the temperature is 10h to 1200 ℃, the temperature is 1h to 1250 ℃, the heat is preserved for 2h to 1200 ℃, the temperature is preserved for 2h, and the temperature is preserved for 1h to 1100 ℃ and then the furnace is cooled. Obtaining the high-entropy ferrite with garnet structure.
Comparative example 1
The preparation method of the conventional YIG-doped ferrite comprises the following steps:
s1 is according to the chemical formula Y 2.85 Ca 0.15 Fe 4.489 Sn 0.15 O 12 Weighing Y in proportion 2 O 3 、CaCO 3 、SnO 2 、Fe 2 O 3 The powder is placed in a ball mill, ball milling is carried out by taking steel balls as grinding media and pure water as dispersing agent, the ball-water ratio in the ball mill is 1:2.8:1.3, the rotation speed of a central shaft is 150rad/min, and the ball milling time is 24 hours. The temperature of the drying oven is 150 ℃ and the drying time is 8 hours.
S2, sieving the dried powder, placing the sieved powder in a muffle furnace for presintering, and calcining for 4 hours at 1300 ℃.
S3, placing the presintered powder in a ball mill for secondary ball milling, wherein parameters are unchanged, and the time is 24 hours. And (5) after ball milling, placing the mixture in a drying oven at 150 ℃ for drying for 8 hours.
S4, granulating ferrite powder in a mortar, and dropwise adding 7wt% of PVA aqueous solution while manually grinding, wherein the dosage of the adhesive is 12% of the mass of the powder. Placing the granulated powder into a die, applying pressure to 100Mpa by using a hydraulic press, maintaining the pressure for 15s, and demoulding to obtain ferrite green blanks.
S5, placing the ferrite green body in a muffle furnace, wherein the sintering process comprises the following steps: the temperature is slowly raised to be 1h to 120 ℃ and 10h to 330 ℃ for glue discharging, 10h to 1300 ℃,5h to 1450 ℃, 2h to 1430 ℃ and 2h to 1330 ℃ and 2.5h to 1100 ℃ and then is cooled along with the furnace. As can be seen from fig. 2, a conventional YIG-doped ferrite is finally obtained. Fig. 2 is an X-ray diffraction pattern of the conventional YIG ferrite doped with the comparative example 1 of the present invention, which is also a ferrite of a single-phase garnet structure as can be seen from fig. 2.
The performance of the garnet-structured high-entropy ferrite prepared in example 2 was compared with that of the conventional YIG-doped ferrite prepared in comparative example 1, and the comparison data are shown in Table 1.
Table 1 shows the ferrite performance data of example 2 and comparative example 1
As can be seen from table 1, the magnetic properties of the high entropy YIG ferrite in example 2 are superior to those of the conventional YIG ferrite doped in comparative example 1.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention and not for limiting it, and although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that: the technical scheme of the invention can be modified or replaced by the same, and the modified technical scheme cannot deviate from the spirit and scope of the technical scheme of the invention.
Claims (10)
1. The preparation method of the high-entropy YIG ferrite with high saturation magnetization is characterized by comprising the following steps of:
s1, weighing different oxide powders, placing the powder into a ball mill, and placing the slurry into a drying oven to obtain uniform powder after ball milling is finished;
s2, sieving the powder dried in the step S1, and placing the sieved powder in a muffle furnace for presintering;
s3, placing the powder pre-sintered in the step S2 into a ball mill for secondary ball milling and drying;
s4, granulating the powder dried in the step S3, and then performing compression molding to obtain a ferrite green body;
and S5, placing the ferrite green body obtained in the step S4 into a muffle furnace for sintering to obtain the high-entropy YIG ferrite.
2. The method for preparing the YIG ferrite with high saturation magnetization according to claim 1, wherein the method comprises the following steps: in step S1, the oxide powder is La 2 O 3 、Yb 2 O 3 、Er 2 O 3 、Tm 2 O 3 、Ho 2 O 3 、Dy 2 O 3 、Gd 2 O 3 、Sm 2 O 3 、Nd 2 O 3 、Ce 2 O 3 、Eu 2 O 3 、Bi 2 O 3 、Y 2 O 3 And Fe (Fe) 2 O 3 One or more of the following;
the molar ratio of the oxides in the powder follows the formula (Re) x Ce y Eu y Bi z Y 3-x-2y-z )Fe 5 O 12 Wherein x, y, z > 0, x+2y+z=1; re is one of La, yb, er, tm, ho, dy, gd, sm, nd.
3. The method for preparing the YIG ferrite with high saturation magnetization according to claim 1, wherein the method comprises the following steps: in the step S1, the purity of the oxide powder is more than or equal to 99.9 percent.
4. The method for preparing the YIG ferrite with high saturation magnetization according to claim 1, wherein the method comprises the following steps: in the steps S1 and S3, the ball mill uses steel balls as grinding media, pure water is used as dispersing agent for ball milling, the rotating speed of the ball mill is 100-200 rad/min, the effective ball milling time is 20-24 h, and powder in the ball mill is obtained: ball: the water ranges from 1:2:1 to 1:3:1.5.
5. The method for preparing the YIG ferrite with high saturation magnetization according to claim 1, wherein the method comprises the following steps: in the steps S1 and S3, the drying temperature is 135-165 ℃ and the drying time is 6-10h.
6. The method for preparing the YIG ferrite with high saturation magnetization according to claim 1, wherein the method comprises the following steps: in the step S2, the calcination temperature in the muffle furnace is 950-1150 ℃ and the calcination time is 2-4 h.
7. The method for preparing the YIG ferrite with high saturation magnetization according to claim 1, wherein the method comprises the following steps: the adhesive used for pelleting in the step S4 is PVA water solution with the weight percent of 5-7 percent, and the dosage of the adhesive is 10-15 percent of the mass of ferrite powder.
8. The method for preparing the YIG ferrite with high saturation magnetization according to claim 1, wherein the method comprises the following steps: in the step S4, the pressing is performed by using a hydraulic press, the pressure of the hydraulic press is 100-150 Mpa, and the pressure holding time is 0.1-5 min.
9. The method for preparing the YIG ferrite with high saturation magnetization according to claim 1, wherein the method comprises the following steps: the sintering temperature in the step S5 is 1250-1400 ℃, and the sintering time is 2-4 h.
10. A high-entropy YIG ferrite produced by the production method of a high-entropy YIG ferrite having a high saturation magnetization as claimed in any one of claims 1 to 9.
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