CN117026376A - Garnet type ferrite single crystal material with small line width, high temperature coefficient and high saturation magnetization intensity - Google Patents
Garnet type ferrite single crystal material with small line width, high temperature coefficient and high saturation magnetization intensity Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 79
- 239000013078 crystal Substances 0.000 title claims abstract description 55
- 230000005415 magnetization Effects 0.000 title claims abstract description 42
- 239000002223 garnet Substances 0.000 title claims abstract description 27
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 18
- 229910017493 Nd 2 O 3 Inorganic materials 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims description 24
- 239000000203 mixture Substances 0.000 claims description 22
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 15
- 239000002253 acid Substances 0.000 claims description 15
- 238000002360 preparation method Methods 0.000 claims description 10
- 238000005303 weighing Methods 0.000 claims description 10
- 238000009835 boiling Methods 0.000 claims description 9
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 238000013461 design Methods 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000010411 cooking Methods 0.000 claims description 4
- 238000007580 dry-mixing Methods 0.000 claims description 2
- 230000004907 flux Effects 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 238000002844 melting Methods 0.000 claims description 2
- 230000008018 melting Effects 0.000 claims description 2
- 238000000034 method Methods 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 230000005350 ferromagnetic resonance Effects 0.000 abstract description 24
- 239000003795 chemical substances by application Substances 0.000 abstract description 9
- 230000005291 magnetic effect Effects 0.000 abstract description 9
- 238000012360 testing method Methods 0.000 description 29
- 230000000052 comparative effect Effects 0.000 description 16
- 238000011056 performance test Methods 0.000 description 8
- 238000002441 X-ray diffraction Methods 0.000 description 7
- 238000009472 formulation Methods 0.000 description 4
- 238000010583 slow cooling Methods 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 229910052738 indium Inorganic materials 0.000 description 3
- 239000008188 pellet Substances 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 2
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229910052596 spinel Inorganic materials 0.000 description 2
- 239000011029 spinel Substances 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910003437 indium oxide Inorganic materials 0.000 description 1
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/22—Complex oxides
- C30B29/28—Complex oxides with formula A3Me5O12 wherein A is a rare earth metal and Me is Fe, Ga, Sc, Cr, Co or Al, e.g. garnets
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B9/00—Single-crystal growth from melt solutions using molten solvents
- C30B9/04—Single-crystal growth from melt solutions using molten solvents by cooling of the solution
- C30B9/08—Single-crystal growth from melt solutions using molten solvents by cooling of the solution using other solvents
- C30B9/12—Salt solvents, e.g. flux growth
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- Chemical & Material Sciences (AREA)
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- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
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- Inorganic Chemistry (AREA)
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Abstract
The application discloses a garnet type ferrite single crystal material with small line width, high temperature coefficient and high saturation magnetization intensity, which comprises the following main components in percentage by mole: fe (Fe) 2 O 3 （20.8～20.2%）、In 2 O 3 （0.8～1.4%）、Nd 2 O 3 (0.1～0.2%)、Y 2 O 3 (8.2-8.3%) and a fluxing agent component; the saturation magnetization Ms 147-157 kA/m and the temperature coefficient of the garnet ferrite single crystal material of the applicationαThe ferromagnetic resonance line width delta H is less than or equal to 48A/m and less than 2.0 per mill/DEG C, and the ferromagnetic resonance line width delta H has the characteristics of remarkable small line width, high temperature coefficient, high saturation magnetization intensity and the like in a garnet type single crystal material system, thereby meeting the use requirements of a C-band magnetic tuning filter on wide bandwidth and low loss.
Description
Technical Field
The application relates to the field of microwave ferrite materials, in particular to a garnet type ferrite single crystal material with small line width, high temperature coefficient and high saturation magnetization intensity.
Background
In recent years, for the wide-band development in the fields of electronic countermeasure, electronic reconnaissance, millimeter wave precision guidance and the like, a magnetic tuning device serving as a core wide-band component of an electronic warfare system is provided with the technical characteristics of high temperature stability, ultra-wide band and the like while keeping low loss. Therefore, a wider-band, ultra-low power consumption and high temperature stability magnetic tuning device is a general trend of development of the magnetic tuning device in the current and future 5-10 years.
The C wave band is one of the main frequency bands of the electronic countermeasure system, and the garnet type ferrite single crystal material is used as a key functional material applied to a conventional C wave band magnetic tuning device and has the characteristics of small ferromagnetic resonance line width (delta H), low loss and the like. However, from published reports, the saturation magnetization of the practical garnet ferrite material products is generally smaller than 1850Gs (147 kA/m), and the saturation magnetization is a key factor affecting the bandwidth of the device, so that the existing materials cannot meet the requirement of a part of filter products for a specific broadband (> 50 MHz); the spinel type single crystal material is used, and the broadband and temperature characteristic requirements of the device can be realized, but the ferromagnetic resonance line width of the material determines the device loss, and the ferromagnetic resonance line width of the material does not meet the practical use requirements of the device (the device requirement is less than or equal to 48A/m; the minimum line width of the spinel single crystal is about 160A/m, which is 4-5 times that of the garnet single crystal); in few literature researches, mn element and other doping are used for improving the saturation magnetization intensity of garnet, but the inventor actually tests to find that the ferromagnetic resonance line width and the temperature coefficient of the garnet are obviously deteriorated (see comparative example 5), the temperature coefficient directly influences the frequency drift of a device, and further, the temperature stability of the device is greatly influenced, and the device requirement is that: and less than 2.0 per mill/. Degree.C, thus the use requirement is not met.
Therefore, development of a single crystal material with the characteristics of small linewidth, high temperature coefficient and high saturation magnetization is needed to meet the use requirements of a wide-bandwidth, low-loss and high-temperature stability C-band magnetic tuning filter.
Disclosure of Invention
One of the purposes of the present application is to provide a garnet type ferrite single crystal material with small linewidth, high temperature coefficient and high saturation magnetization, so as to solve the defects existing in the prior art.
In order to achieve the above purpose, the technical scheme adopted by the application is as follows:
a garnet type ferrite single crystal material with small line width, high temperature coefficient and high saturation magnetization intensity comprises the following main components in percentage by mole:
Fe 2 O 3 20.2～20.8 %
Nd 2 O 3 0.1～0.2%
In 2 O 3 0.8～1.4%
Y 2 O 3 8.2-8.3%；
the flux also comprises the following components in mole percent:
PbO 36～38%
PbF 2 27～30%
B 2 O 3 1.0～7.0%。
the saturation magnetization of the common garnet type ferrite single crystal material is 16 kA/m-141 kA/m, and the saturation magnetization is continuously increased on the basis, so that the magnetic loss of the material is obviously increased, the temperature coefficient is increased, and the like, and the performance deterioration of the C-band magnetic tuning filter with wide bandwidth, low loss and high temperature stability cannot be met.
According to the application, trace Nd element is doped to replace Y element at tetrahedral position, so that the material temperature stability of single crystal is improved (temperature coefficient is reduced); the proper amount of In replaces Fe element at the octahedral position, so that the saturation magnetization of the material is increased and the smaller ferromagnetic resonance line width is kept.
The second purpose of the application is to provide a preparation method of the garnet type ferrite single crystal material with small line width, high temperature coefficient and high saturation magnetization intensity, which comprises the following steps:
(1) Weighing: according to the formula design result of claim 1, calculating and weighing various required high-purity raw materials, wherein each raw material is weighed with the precision: less than or equal to +/-0.05 g;
(2) Dry mixing: stirring and uniformly mixing the raw materials weighed in the step (1), and placing the raw materials into a crucible for 20-30 min;
(3) Pre-burning the chemical material: carrying out high-temperature presintering on the mixture obtained in the step (2);
(4) Crystal growth: and (3) carrying out high-temperature slow cooling growth on the presintering raw material after the material melting in the step (3), heating to 1350-1450 ℃, preserving heat for 4-8 hours, cooling to 850-950 ℃ at a speed of 0.3-1 ℃/h, and naturally cooling to room temperature to obtain a crystal mixture.
(5) And (3) separating crystals: and (3) carrying out acid cooking on the crystal mixture obtained in the step (4) by using boiling acid mixed liquor for 6-7 days to obtain a crystal material.
As a preferable technical scheme: in the step (1), the purity of the high-purity raw material is more than or equal to 99.99 percent.
As a preferable technical scheme: in the step (3), the presintering temperature is 900-1000 ℃, and the temperature is kept for 10-12 hours.
As a preferable technical scheme: in the step (5), the composition of the acid mixed solution is nitric acid and acetic acid, and the volume ratio is 1:1-2:1.
Compared with the prior art, the application has the advantages that: the application researches garnet ferrite single crystal materials with high saturation magnetization to obtain the saturation magnetization Ms 147-157 kA/m and the temperature coefficientαThe single crystal material with the ferromagnetic resonance line width delta H less than or equal to 48A/m and the characteristics of small line width, high temperature coefficient and the like is less than 2.0 per mill/DEGC, and through device trial, the single crystal material meets the use requirements of a C band magnetic tuning filter with wide bandwidth, low loss and high temperature stability; the preparation method disclosed by the application is reasonable in process and suitable for mass production, popularization and application.
Drawings
FIG. 1 is an XRD pattern measured after directional cutting of single crystal materials obtained in examples 1,2 and 3 of the present application.
Description of the embodiments
The application will be further illustrated with reference to examples.
Example 1:
the garnet type ferrite single crystal material with small line width, high temperature coefficient and high saturation magnetization intensity comprises the following main components in percentage by mole: fe (Fe) 2 O 3 20.2 %、Nd 2 O 3 0.1 %、In 2 O 3 1.4%、Y 2 O 3 8.3%; the fluxing agent comprises the following components: pbO 36%, pbF 2 30%、B 2 O 3 4.0 %；
According to the formula design result, calculating and weighing various required high-purity raw materials with purity of 99.99 percent, wherein each raw material has the weighing precision: less than or equal to +/-0.05 g; stirring and uniformly mixing the weighed various raw materials, and putting the materials into a crucible for 20min; carrying out high-temperature presintering on the obtained mixture, wherein the presintering temperature is 900 ℃, and preserving the heat for 12 hours; the presintering raw materials after preheating the material are subjected to high-temperature slow cooling growth, firstly, the temperature is raised to 1350 ℃, the temperature is kept for 8 hours, then the temperature is lowered to 950 ℃ at the speed of 0.3 ℃/h, and then the mixture is naturally cooled to room temperature, so as to obtain a crystal mixture; and then the boiling acid mixed solution (nitric acid: acetic acid volume ratio is 1:1) is used for carrying out acid boiling on the obtained crystal mixture, and the acid boiling time is 6 days, so that the crystal material is obtained. And finally, performing performance test.
Measuring saturation magnetization Ms, temperature coefficient using Vibrating Sample Magnetometer (VSM)αTest results are as follows; the ferromagnetic resonance linewidth deltah was tested using a single crystal pellet linewidth test system according to GJB4410-2002,all test results are shown in table 1; the prepared single crystal material was subjected to phase analysis by X-ray diffraction (XRD), and the results are shown in fig. 1.
Table 1 example 1 material property test
From the test results, all diffraction peaks in the XRD spectrum of the material of the example 1 are (l 00) series (l=4n, n=1, 2), no impurity peak caused by the second phase compound is observed, and all diffraction peaks belong to the characteristic peak positions of the cubic garnet, so that the material is in a single-phase garnet structure; in addition, the saturation magnetization intensity of the material is 148.5kA/m, the temperature coefficient is 1.96 per mill/DEG C, and the ferromagnetic resonance line width is 38.8A/m, which shows that the material has the characteristics of small line width, high temperature coefficient, high saturation magnetization intensity and the like.
Example 2:
the garnet type ferrite single crystal material with small line width, high temperature coefficient and high saturation magnetization intensity comprises the following main components in percentage by mole: fe (Fe) 2 O 3 20.5 %、Nd 2 O 3 0.15 %、In 2 O 3 1.1%、Y 2 O 3 8.25 The%; the fluxing agent comprises the following components: pbO 37%, pbF 2 28 %、B 2 O 3 5.0 %；
According to the formula design result, calculating and weighing various required high-purity raw materials with purity of 99.99 percent, wherein each raw material has the weighing precision: less than or equal to +/-0.05 g; stirring and uniformly mixing the weighed various raw materials, and putting the materials into a crucible for 25min; carrying out high-temperature presintering on the obtained mixture, wherein the presintering temperature is 950 ℃, and preserving the heat for 13 hours; the presintering raw materials after preheating the material are subjected to high-temperature slow cooling growth, firstly, the temperature is raised to 1400 ℃, the temperature is kept for 6 hours, then the temperature is lowered to 900 ℃ at the speed of 0.5 ℃/h, and then the temperature is naturally cooled to room temperature, so that a crystal mixture is obtained; and then the boiling acid mixed solution (nitric acid: acetic acid volume ratio is 1.5:1) is used for carrying out acid cooking on the obtained crystal mixture, and the acid cooking time is 6 days, so that the crystal material is obtained. And finally, performing performance test.
Measuring saturation magnetization Ms, temperature coefficient using Vibrating Sample Magnetometer (VSM)αTest results are as follows; the ferromagnetic resonance linewidth Δh was tested according to GJB4410-2002 using a single crystal pellet linewidth test system, all test results are shown in table 2; the prepared single crystal material was subjected to phase analysis by X-ray diffraction (XRD), and the results are shown in fig. 1.
Table 2 example 2 material property test
From the test results, all diffraction peaks in the XRD spectrum of the material of the example 2 are (l 00) series (l=4n, n=1, 2), no impurity peak caused by the second phase compound is observed, and all diffraction peaks belong to the characteristic peak positions of the cubic garnet, so that the material is in a single-phase garnet structure; in addition, the saturation magnetization intensity of the material is 155.7 kA/m, the temperature coefficient is 1.90 per mill/DEG C, and the ferromagnetic resonance line width is 43.7A/m, which indicates that the material has the characteristics of small line width, high temperature coefficient, high saturation magnetization intensity and the like.
Example 3:
the garnet type ferrite single crystal material with small line width, high temperature coefficient and high saturation magnetization intensity comprises the following main components in percentage by mole: fe (Fe) 2 O 3 20.8 %、Nd 2 O 3 0.2 %、In 2 O 3 0.8%、Y 2 O 3 8.2 The%; the fluxing agent comprises the following components: pbO 39%, pbF 2 27 %、B 2 O 3 4.0 %；
According to the formula design result, calculating and weighing various required high-purity raw materials with purity of 99.99 percent, wherein each raw material has the weighing precision: less than or equal to +/-0.05 g; stirring and uniformly mixing the weighed various raw materials, and putting the materials into a crucible for 30min; carrying out high-temperature presintering on the obtained mixture, wherein the presintering temperature is 1000 ℃, and preserving the heat for 12 hours; the presintering raw materials after preheating the material are subjected to high-temperature slow cooling growth, firstly, the temperature is raised to 1450 ℃, the temperature is kept for 5 hours, then the temperature is lowered to 850 ℃ at the speed of 1.0 ℃/h, and then the temperature is naturally cooled to room temperature, so that a crystal mixture is obtained; and then the boiling acid mixed solution (nitric acid: acetic acid volume ratio is 2:1) is used for carrying out acid boiling on the obtained crystal mixture, and the acid boiling time is 7 days, so that the crystal material is obtained. And finally, performing performance test.
Measuring saturation magnetization Ms, temperature coefficient using Vibrating Sample Magnetometer (VSM)αTest results are as follows; the ferromagnetic resonance linewidth Δh was tested according to GJB4410-2002 using a single crystal pellet linewidth test system, all test results are shown in table 3; the prepared single crystal material was subjected to phase analysis by X-ray diffraction (XRD), and the results are shown in fig. 1.
Table 3 example 3 material property test
From the test results, all diffraction peaks in the XRD spectrum of the material of the example 2 are (l 00) series (l=4n, n=1, 2), no impurity peak caused by the second phase compound is observed, and all diffraction peaks belong to the characteristic peak positions of the cubic garnet, so that the material is in a single-phase garnet structure; in addition, the saturation magnetization intensity of the material is 147.4 kA/m, the temperature coefficient is 1.82 per mill/DEG C, and the ferromagnetic resonance line width is 47.8A/m, which indicates that the material has the characteristics of small line width, high temperature coefficient, high saturation magnetization intensity and the like.
In order to demonstrate the technical advantages of the present application, the present inventors have made a corresponding one-factor comparative test.
Comparative example 1
Influence of not carrying out Nd element doping
In the comparative example, nd element doping was not performed in the formulation as compared with example 1, and Nd was continuously maintained 2 O 3 And Y 2 O 3 The total molar ratio was unchanged (Nd 2 O 3 0 mol %, Y 2 O 3 8.4 mol%) and the mole percentage of the rest main components and the fluxing agent are kept unchanged, and meanwhile, the preparation process is kept unchanged. Temperature coefficient and saturation are carried out through a vibration sample magnetometer and a single crystal ball linewidth testing systemAnd magnetization intensity and ferromagnetic resonance line width tests, the test results are shown in table 4, the saturation magnetization intensity and ferromagnetic resonance line width of the material are not changed greatly, and the requirements are met; but the temperature coefficient is obviously increased to be more than 2.0 per mill/DEG C, and the use requirement is not met.
Table 4 comparative example 1 material performance test
Comparative example 2
Influence of excessive Nd element doping
In this comparative example, compared with example 1, nd was maintained while excessively doping Nd element in the formulation 2 O 3 And Y 2 O 3 The total molar ratio is unchanged ((Nd) 2 O 3 0.3 mol %, Y 2 O 3 8.1 mol%) of the rest of the main components and the fluxing agent remain unchanged, and the preparation process remains unchanged. The temperature coefficient, the saturation magnetization and the ferromagnetic resonance linewidth are tested by a vibration sample magnetometer and a single crystal ball linewidth testing system, the test results are shown in table 5, the temperature coefficient is reduced by 0.13 per mill/°c, and the requirements are met; but the saturation magnetization of the material is slightly reduced to 147 kA/m or less, the ferromagnetic resonance line width is obviously increased and exceeds 48A/m, and the use requirement is not met.
Table 5 comparative example 2 material performance test
Comparative example 3
Effect of small amount of In element doping
In this comparative example, in was maintained while doping In element In a small amount In the formulation as compared with example 1 2 O 3 And Fe (Fe) 2 O 3 The total molar ratio was unchanged (In 2 O 3 0.6mol%, Fe 2 O 3 21.0 mol%) and the mole percentage of the rest main components and fluxing agent are kept unchanged, and the preparation process is also kept unchanged. Single crystal ball line by vibrating sample magnetometerThe wide test system tests the temperature coefficient, the saturation magnetization and the ferromagnetic resonance line width, the test results are shown in table 6, the ferromagnetic resonance line width and the temperature coefficient of the material are reduced, and the requirements are met; but the saturation magnetization of the material is obviously reduced and is lower than 147A/m, which does not meet the use requirement.
Table 6 comparative example 3 material performance test
Comparative example 4
Influence of excessive In-element doping
In this comparative example, in was maintained while the In element was excessively doped In the formulation, as compared with example 1 2 O 3 And Fe (Fe) 2 O 3 The total molar ratio was unchanged (In 2 O 3 1.6mol%, Fe 2 O 3 20.0mol percent) of the other main components and fluxing agents are kept unchanged, and the preparation process is kept unchanged. The temperature coefficient, the saturation magnetization and the ferromagnetic resonance linewidth are tested by a vibration sample magnetometer and a single crystal ball linewidth testing system, the test results are shown in table 7, the ferromagnetic resonance linewidth of the material is increased and still less than 48A/m, and the requirements are met; but the temperature coefficient of the material is more than 2.0 per mill/. Degree.C, the saturation magnetization of the material is obviously reduced and is lower than 147A/m, and the use requirement is not met.
Table 7 comparative example 4 material performance test
Comparative example 5
Influence of Mn element doping
Compared with the example 1, the high-purity manganese dioxide is used for replacing indium oxide in the formula, the doping amount is unchanged, the mole percentage of the rest main components and fluxing agent is unchanged, and the preparation process is also unchanged. The temperature coefficient, the saturation magnetization and the ferromagnetic resonance linewidth are tested by a vibration sample magnetometer and a single crystal ball linewidth testing system, the test results are shown in table 8, the saturation magnetization of the material is obviously reduced and is slightly higher than 147A/m, and the requirement is met; but the ferromagnetic resonance line width of the material is obviously increased and is more than 48A/m, the temperature coefficient of the material is more than 2.0 per mill/DEG C, and the use requirement is not met.
Table 8 comparative example 5 material performance test
The foregoing description of the preferred embodiments of the application is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the application.
Claims (5)
1. A garnet type ferrite single crystal material with small line width, high temperature coefficient and high saturation magnetization intensity is characterized in that the main components of the formula are as follows in mole percent:
Fe 2 O 3 20.2～20.8%
Nd 2 O 3 0.1～0.2%
In 2 O 3 0.8～1.4%
Y 2 O 3 8.2-8.3%；
the flux also comprises the following components in mole percent:
PbO 36～39%
PbF 2 27～30%
B 2 O 3 1.0～7.0%。
2. the method for preparing the garnet type ferrite single crystal material with small line width and high temperature coefficient and high saturation magnetization according to claim 1, comprising the following steps:
(1) Weighing: according to the formula design, calculating and weighing various required high-purity raw materials, wherein each raw material is weighed with the precision: less than or equal to +/-0.05 g;
(2) Dry mixing: stirring and uniformly mixing the raw materials weighed in the step (1), and placing the raw materials into a crucible for 20-30 min;
(3) Pre-burning the chemical material: carrying out high-temperature presintering on the mixture obtained in the step (2);
(4) Crystal growth: slowly cooling the presintering raw material subjected to the material melting in the step (3) to grow at a high temperature, firstly heating to 1350-1450 ℃, preserving heat for 4-8 hours, cooling to 850-950 ℃ at a speed of 0.3-1 ℃/h, and naturally cooling to room temperature to obtain a crystal mixture;
(5) And (3) separating crystals: and (3) carrying out acid cooking on the crystal mixture obtained in the step (4) by using boiling acid mixed liquor for 6-7 days to obtain a crystal material.
3. The preparation method according to claim 2, characterized in that: in the step (1), the purity of the high-purity raw material is more than or equal to 99.99 percent.
4. The preparation method according to claim 2, characterized in that: in the step (3), the presintering temperature is 900-1000 ℃, and the temperature is kept for 10-12 hours.
5. The preparation method according to claim 2, characterized in that: in the step (5), the composition of the acid mixed solution is nitric acid and acetic acid, and the volume ratio is 1:1-2:1.
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|---|---|---|---|
| CN202310989600.4A CN117026376A (en) | 2023-08-08 | 2023-08-08 | Garnet type ferrite single crystal material with small line width, high temperature coefficient and high saturation magnetization intensity |
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| CN202310989600.4A CN117026376A (en) | 2023-08-08 | 2023-08-08 | Garnet type ferrite single crystal material with small line width, high temperature coefficient and high saturation magnetization intensity |
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