CN117328143A - Growth method of medium saturation magnetization Ge-doped BiCaV ferrite single crystal material - Google Patents
Growth method of medium saturation magnetization Ge-doped BiCaV ferrite single crystal material Download PDFInfo
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- CN117328143A CN117328143A CN202311215577.XA CN202311215577A CN117328143A CN 117328143 A CN117328143 A CN 117328143A CN 202311215577 A CN202311215577 A CN 202311215577A CN 117328143 A CN117328143 A CN 117328143A
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- 239000013078 crystal Substances 0.000 title claims abstract description 55
- 239000000463 material Substances 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 33
- 230000005415 magnetization Effects 0.000 title claims abstract description 31
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 29
- 239000002223 garnet Substances 0.000 claims abstract description 7
- 230000004907 flux Effects 0.000 claims abstract 3
- 239000003795 chemical substances by application Substances 0.000 claims description 15
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 8
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- 238000000498 ball milling Methods 0.000 claims description 6
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 claims description 5
- 229910005793 GeO 2 Inorganic materials 0.000 claims description 5
- 238000010583 slow cooling Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- 229910052697 platinum Inorganic materials 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 229960000583 acetic acid Drugs 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- 238000009835 boiling Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 239000012362 glacial acetic acid Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 238000011049 filling Methods 0.000 claims description 2
- 239000011812 mixed powder Substances 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- 230000005350 ferromagnetic resonance Effects 0.000 abstract description 13
- 238000012360 testing method Methods 0.000 description 7
- 238000013461 design Methods 0.000 description 4
- 230000005291 magnetic effect Effects 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 238000009472 formulation Methods 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 238000005204 segregation Methods 0.000 description 3
- 229910005191 Ga 2 O 3 Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000003780 insertion Methods 0.000 description 2
- 230000037431 insertion Effects 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000012797 qualification Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000006184 cosolvent Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000002902 ferrimagnetic material Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
- H01F41/0266—Moulding; Pressing
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Abstract
The invention discloses a method for growing a medium saturation magnetization Ge-doped BiCaV ferrite single crystal material, which belongs to the technical field of ferrite single crystal materials and comprises the steps of passing Ge 4+ Ion doping and growth of garnet Bi using PbO flux x‑y3‑2 Ca x+2 y V x Fe x y5‑‑ Ge y O 12 Single crystal, ge prepared by the invention: the BiCaV ferrite single crystal material has saturation magnetization of 800-1000 Gs, belongs to the range of medium saturation magnetization, has good element doping concentration distribution uniformity and high saturation magnetization uniformity, has a ferromagnetic resonance line width of less than 0.9Oe, and can be applied to S-C wave band microwave ferrite devices.
Description
Technical Field
The invention relates to the technical field of ferrite single crystal materials, in particular to a growth method of a medium saturation magnetization Ge-doped BiCaV ferrite single crystal material.
Background
The garnet type BiCaV ferrite single crystal material is a ferrimagnetic material, has the characteristics of excellent saturation magnetization uniformity, narrow ferromagnetic resonance line width, low dielectric loss and the like, is an excellent gyromagnetic material, and is widely applied to various microwave devices with low frequency, high Q value and low insertion loss.
However, conventional BiCaV and In doped BiCaV ferrite single crystal materials have low saturation magnetization, generally no higher than 600 Gs, which is only used In P-L band magnetically tuned microwave devices. For devices above the S band, the In doped BiCaV ferrite single crystal material has low stopband depth of the device (such as a magnetic tuning band-stop filter) due to the low saturation magnetization intensity, so that the practical application is difficult. For magnetically tuned microwave devices in the S-C band, ga-doped YIG ferrite single crystal materials of medium saturation magnetization (. Gtoreq.800 Gs) are generally used, however, ga: the YIG single crystal material has the defects that Ga element doping is uneven due to segregation phenomenon, saturation magnetization uniformity is poor, a wide distribution range is presented, and further the use qualification rate of devices is low.
In view of the above technical problems, korean in 1991Shiquan (Han Zhiquan. In-substituted BiCaVGeIG research 1991. Magnetic materials and devices: 22 (3)) studied In-substitution and Ge-substitution on Bi using common ceramic sintering processes z Ca -3 z Ge x In y Fe z x y3.5+0.5-0.5- V z x1.5-0.5-0.5 O 12 The (BiCaVGeIG) polycrystalline garnet material has the effects of parameters such as saturation magnetization intensity, ferromagnetic resonance line width, curie temperature and the like, the 0K theoretical saturation magnetization intensity is 750-1200 Gs, and the 77K experimental value is 700-1050Gs. However, although the ferromagnetic resonance linewidth of the bicavgiig polycrystalline material decreases dramatically with increasing Ge content, the minimum ferromagnetic resonance linewidth still reaches 12Oe, which is not suitable for low insertion loss magnetically tuned microwave devices.
Therefore, in order to meet the application requirements of S-C band magnetic tuning microwave devices, a novel ferrite single crystal material with saturation magnetization of 800-1000 Gs, uniform saturation magnetization distribution and small ferromagnetic resonance line width needs to be found.
Disclosure of Invention
Aiming at the problems of low saturation magnetization and high ferromagnetic resonance linewidth of the garnet type BiCaV ferrite single crystal material grown by the existing fluxing agent method, the invention provides a growth method of a medium saturation magnetization Ge-doped BiCaV ferrite single crystal material.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
medium saturation magnetization Ge: the growth method of the BiCaV ferrite single crystal material comprises the following steps:
(1) According to the formula Bi x-y3-2 Ca x+y2 V x Fe x y5-- Ge y O 12 Calculating the solute Bi 2 O 3 、CaCO 3 、V 2 O 5 、GeO 2 、Fe 2 O 3 And the mass proportion of the fluxing agent PbO, respectively accurately weighing the solute and the fluxing agent and uniformly mixing;
(2) Filling the mixed powder obtained in the step (1) into a container, compacting the powder, and sealing the container;
(3) Placing the sealed container in the step (2) in a molten salt furnace vertically for slow cooling growth;
(4) After the growth is finished, taking out the crystals in the container in the step (3), and removing the fluxing agent to obtain garnet type Ge: biCaV ferrite single crystal.
As a preferable embodiment, in the step (1), the solute molar quantity ratio is Bi 2 O 3 ：CaCO 3 ：V 2 O 5 ：GeO 2 ：Fe 2 O 3 =1.1~1.2(3-2x-y)：0.35~0.38(2x+y)：0.28~0.3x：y：0.5~0.52(5-x-y) Wherein, the method comprises the steps of, wherein,x，yv, ge in the molecular formula, both satisfy 1.0<x<1.5，0≤y<1，2x+y<3。
To be used forx=1.40，yFor example, =0.05, the solute molar quantity ratio can be specifically calculated as Bi 2 O 3 ：CaCO 3 ：V 2 O 5 ：GeO 2 ：Fe 2 O 3 =3.30~3.60：19.95~21.66：7.84~8.40：1：35.50~36.92。
As a preferred technical scheme, in the step (1), the purity of the raw material is more than 99.99%.
As a preferable technical scheme, in the step (1), the molar ratio of the fluxing agent PbO to the solute is 1: 2.3-1: 3.
In the preferred embodiment, in the step (1), the mixing mode is ball milling.
As a further preferable technical scheme, the ball milling time is 4-6 hours.
In the preferred technical scheme, in the step (2), the container is a platinum crucible.
As a preferable technical scheme, in the step (3), the slow cooling growth process is as follows: raising the temperature to 1200-1250 ℃ at a heating rate of 100-120 ℃/h, preserving heat for 10-12 h, and lowering the temperature to 950 ℃ at a cooling rate of 0.5-1.0 ℃/h. If the growth cut-off temperature is too high, solute precipitation is less, and the crystal size is difficult to grow; if the growth cut-off temperature is too low, hexagonal magnetoplumbite impurity phase is liable to occur in the crystallized product.
In the present invention, the growth cut-off temperature mainly affects the crystal yield without affecting 4piM S And deltaHValues.
As a preferable technical solution, in the step (4), the method for removing the fluxing agent is as follows: boiling in nitric acid and glacial acetic acid mixed acid solution until the fluxing agent is completely removed.
The formula design and the growth process of the Ge doping and fluxing agent provided by the invention are used for preparing medium saturation magnetization garnet type Ge: the BiCaV ferrite single crystal material has important significance for the development of S-C band magnetic tuning microwave devices.
In the invention, pbO mainly plays a role in reducing the melting point of solute, but excessive PbO can influence the yield and quality of crystals, so the invention also has the following effects on PbO and Ge: the ratio between BiCaV is regulated to find the crystal with proper melting point.
In addition, in the PbO fluxing agent of the invention, geO 2 Has a segregation coefficient of less than Ga 2 O 3 The variation of the doping amount of Ge element in the crystal along with the crystal growth is smaller, so that the distribution uniformity of saturated magnetization intensity is better.
In addition, as is well known in the art, the linewidth of the single crystal ferrite material is far lower than that of the polycrystalline material, so that the linewidth of the ferroresonance of the single crystal material prepared by the method is obviously lower than that of the traditional polycrystalline material.
Compared with the prior art, the invention has the advantages that: the fluxing agent with proper proportion adopted by the invention effectively reduces Ge: the melting point of BiCaV, and design the slow cooling growth process, avoid impurity defects such as wrappage in the crystal, and effectively promote the saturation magnetization intensity by doping a proper amount of Ge element; the monocrystalline material obtained by the invention contains the following components In: compared with BiCaV single crystal material, ge: the BiCaV monocrystal has higher saturation magnetization intensity and can be used in a microwave device with higher frequency; and Ga: due to GeO compared with YIG single crystal material 2 Has a segregation coefficient of less than Ga 2 O 3 Thus Ge: the BiCaV single crystal has more uniform element doping, better saturation magnetization distribution uniformity and can be effectively usedThe product qualification rate is improved, and the cost is reduced; compared to bicavgiig poly-crystal, ge: the BiCaV monocrystal has lower ferromagnetic resonance line width and can be used for low-insertion-loss magnetic tuning microwave devices.
Drawings
FIG. 1 shows Ge prepared in example 1: photograph of appearance of BiCaV ferrite single crystal;
fig. 2 shows Ge prepared in example 1: a photo of a BiCaV ferrite spherical harmonic oscillator;
fig. 3 shows Ge prepared in example 1, example 2, and example 3: XRD pattern of BiCaV ferrite single crystal;
fig. 4 shows Ge prepared in example 1: EDS test results of BiCaV ferrite single crystals;
fig. 5 shows Ge prepared in example 1: room temperature hysteresis loop of BiCaV ferrite single crystal;
fig. 6 shows Ge prepared in example 1: ferromagnetic resonance linewidth of BiCaV ferrite single crystal.
Description of the embodiments
The invention will be further described with reference to the accompanying drawings.
Example 1
Medium saturation magnetization Ge: the growth method of the BiCaV ferrite single crystal material comprises the following steps:
respectively weighing the required Bi according to the formula 2 O 3 (weight 125 g), caCO 3 (weight 300 g), V 2 O 5 (weight 110 g), geO 2 (weight 15 g), fe 2 O 3 (weight 420 g), pbO (weight 530 g), and ball-milling for 4 hours by using a ball mill, so that the materials are uniformly mixed; then placing the ball-milling raw materials into a platinum crucible, grinding a pestle, compacting forcefully, and covering and sealing the crucible by using a platinum crucible cover; setting a process curve: raising the temperature to 1200 ℃ at a heating rate of 120 ℃/h, then preserving the temperature for 10 hours, and then lowering the temperature to 950 ℃ at a rate of 0.5 ℃/h; cooling to room temperature along with the furnace, and after the growth is finished, performing acid boiling on the crystal by using a mixed solution of nitric acid (300 ml), glacial acetic acid (200 ml) and water (500 ml) to remove residual fluxing agent;
the morphology photo diagram of the obtained bulk single crystal is shown in fig. 1, the crystal size can reach the centimeter level, and the maximum linear dimension is 2.0 cm. To characterize the resulting single crystalThe physical and chemical properties of the single crystal are tested and analyzed by XRD and EDS respectively, and the test results are shown in figure 3 and figure 4, which show that the obtained single crystal has good structural integrity and low defect and the chemical composition is Bi 0.15 Ca 2.85 V 1.4 Ge 0.05 Fe 3.55 O 12 The method meets the expected design; the obtained single crystal is processed in batch, polished and spherical harmonic oscillator, as shown in figure 2, the saturation magnetization 4 pi Ms of the test sample ball according to GB/T9633-2012, "method for measuring gyromagnetic Material Performance for microwave frequency application" is 800 Gs+ -20 Gs (shown in figure 5), the ferromagnetic resonance linewidth DeltaH at 3GHz is lower than 0.9Oe (shown in figure 6), and the microwave parameter distribution is superior to that of Ga prepared by the traditional cosolvent method: YIG single crystal.
Example 2
In this example, as compared with example 1, only "the required Bi was weighed according to the formulation 2 O 3 (weight 82 g), caCO 3 (weight 317.5 g), V 2 O 5 (weight 112 g), geO 2 (weight 22 g), fe 2 O 3 (weight 433.5 g) and PbO (weight 533 g) ", the remainder being the same as in example 1.
Example 3
In this example, as compared with example 1, only "the required Bi was weighed according to the formulation 2 O 3 (weight 36.5 g), caCO 3 (weight 335 g), V 2 O 5 (weight 114.5 g), geO 2 (weight 29 g), fe 2 O 3 (weight 447 g) and PbO (weight 538 g) ", the remainder being the same as in example 1.
XRD tests were performed on the single crystal materials grown in the foregoing examples 1, 2, and 3, and the test results are shown in fig. 3, where an increase in the Ge doping amount causes Ge: the XRD diffraction peak position of the BiCaV single crystal material slightly shifts left, because Ge ions replace part of Fe ions so that the lattice constant becomes smaller and the unit cell volume is reduced. Three kinds of Ge were tested by vibrating magnetometer and ferroresonance method, respectively: the BiCaV single crystal materials were tested for saturation magnetization and ferromagnetic resonance linewidth for 5 single crystal pellets, and the test results are shown in Table 1, indicating Ge prepared by the formulation design and growth process of the present invention: the BiCaV ferrite single crystal material has the saturation magnetization intensity covering 800-1000 Gs, good element doping uniformity, saturation magnetization intensity deviation smaller than +/-20 Gs and ferromagnetic resonance line width smaller than 0.9Oe.
TABLE 1 results of testing saturation magnetization and ferromagnetic resonance linewidth of single crystal materials grown in examples
The foregoing description of the preferred embodiments of the invention 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 invention.
Claims (9)
1. A method for growing a medium saturation magnetization Ge-doped BiCaV ferrite single crystal material, the method comprising the steps of:
(1) According to the formula Bi x-y3-2 Ca x+y2 V x Fe x y5-- Ge y O 12 Calculating the solute Bi 2 O 3 、CaCO 3 、V 2 O 5 、GeO 2 、Fe 2 O 3 And the mass proportion of the fluxing agent PbO, respectively accurately weighing the solute and the fluxing agent and uniformly mixing;
(2) Filling the mixed powder obtained in the step (1) into a container, compacting the powder, and sealing the container;
(3) Placing the sealed container in the step (2) in a molten salt furnace vertically for slow cooling growth;
(4) After the growth is finished, taking out the crystals in the container in the step (3), and removing the fluxing agent to obtain garnet type Ge: biCaV ferrite single crystal.
2. The method according to claim 1, wherein in the step (1), the solute molar quantity ratio is Bi 2 O 3 ：CaCO 3 ：V 2 O 5 ：GeO 2 ：Fe 2 O 3 =（1.1~1.2）×(3-2x-y)：（0.35~0.38）×(2x+y)：（0.28~0.3）×x：y：（0.5~0.52）×(5-x-y) Wherein, the method comprises the steps of, wherein,x，yv, ge in the molecular formula, both satisfy 1.0<x<1.5，0≤y<1，2x+y<3。
3. The process of claim 1, wherein in step (1) the feedstock is >99.99% pure.
4. The method of claim 1, wherein in step (1), the molar ratio of flux PbO to solute is between 1: 2.3-1: 3.
5. The method of claim 1, wherein in step (1), the mixing is ball milling.
6. The method of claim 5, wherein the ball milling time is 4-6 hours.
7. The method of claim 1, wherein in step (2), the container is a platinum crucible.
8. The method of claim 1, wherein in step (3), the slow cooling growth process is: raising the temperature to 1200-1250 ℃ at a heating rate of 100-120 ℃/h, preserving heat for 10-12 h, and lowering the temperature to 950 ℃ at a cooling rate of 0.5-1.0 ℃/h.
9. The method of claim 1, wherein in step (4), the flux is removed by: boiling in nitric acid and glacial acetic acid mixed acid solution until the fluxing agent is completely removed.
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