CN113943154A - Method for adjusting coercive force of garnet rotational-moment magnetic ferrite material - Google Patents

Method for adjusting coercive force of garnet rotational-moment magnetic ferrite material Download PDF

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CN113943154A
CN113943154A CN202111333558.8A CN202111333558A CN113943154A CN 113943154 A CN113943154 A CN 113943154A CN 202111333558 A CN202111333558 A CN 202111333558A CN 113943154 A CN113943154 A CN 113943154A
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garnet
less
ferrite material
adjusting
coercive force
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王文鑫
黄凡彧
杨雷
翁兆平
李之琦
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Nanjing Glarun Microwave Devices Co ltd
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Nanjing Glarun Microwave Devices Co ltd
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Abstract

The invention discloses a method for adjusting the coercive force of a garnet rotational moment magnetic ferrite material, which uses Co2+‑Si4+Ionic association substitution of Fe in garnet ferrite materials3+Ion of the formula Y3‑a‑2c‑hGdhCaa+2cAaFe5‑a‑b‑c‑2σ‑θ(CoSi)σMnbVcO12Wherein A is a 4-valent ion Sn4+And Zr4+A is more than 0 and less than or equal to 3, h is more than or equal to 0 and less than 3, b is more than 0 and less than 1, c is more than 0 and less than 1, sigma is more than 0 and less than 0.06, theta is more than 0 and less than 0.5, and theta is the iron-deficiency, or Mn is firstly added into the garnet ferrite material3+Ion, regulating remanence ratio of material, and using Co2+‑Si4+Ionic association substitution of Fe in garnet ferrite materials3+Ion of the formula Y3‑lGdlAlm(CoSi)αMnpFe5‑m‑p‑2α‑θO12Wherein l is more than or equal to 0 and less than 3, m is more than 0 and less than 3, p is more than 0 and less than 0.15, alpha is more than 0 and less than 0.06, theta is more than 0 and less than 0.5, the cubic anisotropy is superposed with local uniaxial anisotropy, so that a domain wall generates a freezing effect, an irreversible domain wall displacement pinning field mechanism of coercive force is generated, and the aim of regulating the coercive force of the garnet ferrite material is fulfilled.

Description

Method for adjusting coercive force of garnet rotational-moment magnetic ferrite material
Technical Field
The invention belongs to the technical field of microwave technology and magnetic materials, and particularly relates to a rotational moment magnetic material technology of a lock type phase shifter or a microwave switch in a microwave system.
Background
As a microwave ferrite material for phase shifters or microwave switches, it is required to have not only excellent gyromagnetic properties but also good rectangular magnetic properties, mainly in that the material has a high remanence ratio and a coercive force of an appropriate size.
Garnet ferrites have higher power resistance, lower losses and lower coercivity than spinel ferrites. The small coercive force is beneficial to reducing the driving power and the switching time of the phase shifter, and the garnet material selected in the low-frequency band has great advantages.
Garnet gyromagnetic ferrite materials are reported in domestic and foreign documents or patents. Garnet ferrite material applied to the phase shifter as described in the currently published patent CN108191423A, which has a chemical formula: y is3-x- 2yGdxCa2yVyInzCoξSiξFe5-2ξ-y-z-θO12By using Co2+The influence of the ion-regulated magnetocrystalline anisotropy on the remanence ratio improves the rectangular magnetic property of the material. CN 201510802358, using Mn3+The ion doping improves the remanence ratio of the material. Ce3+Ions are also often used to improve the paramagnetic properties of garnet ferrite materials, with small amounts of Ce3+Substituted Y3+Or a small amount of Mn3+Substituted Fe3+The magnetostriction coefficient can be reduced, the remanence ratio is improved, and the moment magnetic property of the material is improved.
For the moment magnetic property of the ferrite material, people usually only pay attention to the remanence ratio, but the coercive force property of the material is neglected, and attention should be paid to the garnet ferrite material with adjustable coercive force.
The coercive force of the ferromagnetic material is mainly influenced by the retardation of domain wall displacement, the retardation of irreversible rotation of magnetic moment and the retardation of growth of diamagnetic nuclei. In order to obtain a garnet ferrite material with small coercivity, a garnet material with a positive component is generally prepared to reduce the influence of a reverse magnetization core, and a garnet material with large and uniform grains and high density is obtained from the process to reduce the influence of domain wall displacement on the coercivity.
In general, the coercivity determined by irreversible rotation of the magnetic moment is larger than the coercivity determined by the displacement of the irreversible domain wall. The hindered moment rotation is mainly due to material anisotropy, such as magnetocrystalline anisotropy, shape anisotropy, and induced anisotropy. As a polycrystalline ferrite material, the magnetization process is dominated by the domain wall displacement mechanism.
Disclosure of Invention
The invention provides a method for adjusting the coercive force of a garnet rotational moment magnetic ferrite material in order to solve the problems in the prior art, and adopts the following technical scheme in order to achieve the purpose.
Addition of Co to garnet ferrite materials2+The ion changes the property of the magnetic ion and the symmetry and strength of the crystal field of the crystal position, adjusts the magnetocrystalline anisotropy constant of the material, compensates the positive and negative magnetocrystalline anisotropy, and adjusts the coercive force of the garnet material.
Further, with Co2+-Si4+Ionic association substitution of Fe in garnet ferrite materials3+Ion of the formula Y3-a-2c-hGdhCaa+2cAaFe5-a-b-c-2σ-θ(CoSi)σMnbVcO12Wherein A is a 4-valent ion Sn4+And Zr4+A is more than 0 and less than or equal to 3, h is more than or equal to 0 and less than 3, b is more than 0 and less than 1, c is more than 0 and less than 1, sigma is more than 0 and less than 0.06, theta is more than 0 and less than 0.5, and theta is the iron deficiency.
Adding Mn to garnet ferrite material3+Ion, regulating remanence ratio of material, and using Co2+-Si4+Ion co-extractionFe in garnet ferrite material3+Ion of the formula Y3-lGdlAlm(CoSi)αMnpFe5-m-p-2α-θO12Wherein l is more than or equal to 0 and less than 3, m is more than 0 and less than 3, p is more than 0 and less than 0.15, alpha is more than 0 and less than 0.06, and theta is more than 0 and less than 0.5.
In particular, Co2+The range of the substitution amount is more than 0 and less than or equal to 0.06.
With analytically pure Gd2O3，Y2O3，CaCO3，V2O5，MnCO3，Co2O3，SiO2，Al2O3，ZrO2，SnO2，Fe2O3As a raw material.
Further, by using the traditional ceramic process, the garnet ferrite material with high remanence ratio is obtained through primary ball milling, drying, presintering, secondary ball milling, secondary drying, granulation, press molding and sintering.
Particularly, the garnet system is GdSn (Zr) CaVMn-YIG or GdAl-YIG ferrite material, the GdSn (Zr) CaVMn-YIG system obtains the ferrite material with extremely low coercive force and high remanence ratio, and the GdAl-YIG system obtains the ferrite material with high remanence ratio and adjustable coercive force.
The invention has the beneficial effects that: material introduction of Co2+Ions, local uniaxial anisotropy is superposed on the cubic anisotropy, so that a domain wall generates a freezing effect, an irreversible domain wall displacement pinning field mechanism of coercive force is generated, and Co is adjusted2+And ions are used for achieving the purpose of adjusting the coercive force of the garnet ferrite material.
Detailed Description
The technical scheme of the invention is specifically described by three embodiments.
Example one
According to the chemical formula Y3-a-2c-hGdhCaa+2cAaFe5-a-b-c-2σ-θ(CoSi)σMnbVcO12Wherein A is Sn, a is 0.3, b is 0.04, c is 0.05, h is 0,θ is 0.08, and σ is 0, 0.015, 0.025 and 0.035, respectively. Respectively calculating the required amount of each raw material according to the molecular formula, performing primary ball milling mixing, drying, presintering at 1200 ℃, preserving heat for 6 hours, performing secondary ball milling, drying, granulating, performing dry pressing molding, and sintering at 1430 ℃ for 8 hours to obtain a sample, wherein the test parameters are as follows:
Figure BDA0003349834150000021
due to Co2+-Si4+Combined substitution of trace amounts of garnet ferrite material with Co2+-Si4+The replacement amount was increased, the remanence ratio and the coercive force were decreased first and then increased, the coercive force reached the minimum value near the replacement amount of 0.02, and at the replacement amount of 0.015, the coercive force was 0.17 Oe.
The magnetization process of polycrystalline ferrite is dominated by the domain wall displacement mechanism, and experimental results may be due to Co, as in soft ferrite 2+The presence of the material superimposes a local uniaxial anisotropy on the cubic anisotropy, causing a domain wall to have a freezing effect. Irreversible domain wall displacement pinning field mechanism of coercivity, along with Co2+The increase in the content is locally a function of the uniaxial anisotropy Ku, from negative to positive, resulting in HcBy adjusting Co2+And ions are used for achieving the purpose of adjusting the coercive force of the garnet ferrite material.
Example two
According to the chemical formula Y3-a-2c-hGdhCaa+2cAaFe5-a-b-c-2σ-θ(CoSi)σMnbVcO12Where a is Zr, let a be 0.3, b be 0.04, c be 0.05, h be 0, θ be 0.08, σ be 0, 0.011, 0.023, and 0.035, respectively. Respectively calculating the required amount of each raw material according to the molecular formula, performing primary ball milling mixing, drying, presintering at 1200 ℃, preserving heat for 6 hours, performing secondary ball milling, drying, granulating, performing dry pressing molding, and sintering at 1430 ℃ for 8 hours to obtain a sample, wherein the test parameters are as follows:
Figure BDA0003349834150000031
remanence ratio and coercive force follow Co2+-Si4+The substitution amount is increased after being reduced, and is adjusted by Co2+And ions also achieve the purpose of adjusting the coercive force of the garnet ferrite material.
EXAMPLE III
According to the chemical formula Y3-lGdlAlm(CoSi)αMnpFe5-m-p-2α-θO12Let l be 0, m be 0.82, p be 0.1, θ be 0.05, and α be 0 and 0.005, respectively. Respectively calculating the required amount of each raw material according to the molecular formula, performing primary ball milling mixing, drying, presintering at 1200 ℃, preserving heat for 6 hours, performing secondary ball milling, drying, granulating, performing dry pressing molding, and sintering at 1460 ℃ for 8 hours to obtain a sample, wherein the test parameters are as follows:
Figure BDA0003349834150000032
Remanence ratio and coercive force follow Co2+-Si4+The substitution amount is increased, and the coercive force is obviously increased because of the fact that in the GdAl-YIG system, Co2+The ion action is outstanding, so that the magnetocrystalline anisotropy field of the material is increased, a strong irreversible domain wall displacement pinning field mechanism is generated, the coercive force is increased rapidly, and the aim of adjusting the coercive force of the material is fulfilled.
The above-described embodiments are not intended to limit the present invention, and any modifications, equivalents, improvements, etc. made within the spirit and principle of the present invention are included in the scope of the present invention.

Claims (7)

1. A method for adjusting the coercive force of a garnet rotary-moment magnetic ferrite material is characterized by comprising the following steps: addition of Co to garnet ferrite materials2+Ions, pairs of crystal fields changing the nature and crystal position of magnetic ionsThe symmetry and the strength of the garnet material are adjusted, the magnetocrystalline anisotropy constant of the material is adjusted, the positive and negative magnetocrystalline anisotropy is compensated, and the coercive force of the garnet material is adjusted.
2. The method of adjusting the coercivity of a garnet-spiral ferrite material as claimed in claim 1, wherein said adding Co to the garnet ferrite material2+Ions, comprising: by Co 2+-Si4+Ionic association substitution of Fe in garnet ferrite materials3+Ion of the formula Y3-a-2c-hGdhCaa+2cAaFe5-a-b-c-2σ-θ(CoSi)σMnbVcO12Wherein A is a 4-valent ion Sn4+And Zr4+A is more than 0 and less than or equal to 3, h is more than or equal to 0 and less than 3, b is more than 0 and less than 1, c is more than 0 and less than 1, sigma is more than 0 and less than 0.06, theta is more than 0 and less than 0.5, and theta is the iron deficiency.
3. The method of adjusting the coercivity of a garnet-spiral ferrite material as claimed in claim 2, wherein said adding Co to the garnet ferrite material2+Ions, comprising: adding Mn to garnet ferrite material3+Ion, regulating remanence ratio of material, and using Co2+-Si4+Ionic association substitution of Fe in garnet ferrite materials3+Ion of the formula Y3-lGdlAlm(CoSi)αMnpFe5-m-p-2α-θO12Wherein l is more than or equal to 0 and less than 3, m is more than 0 and less than 3, p is more than 0 and less than 0.15, alpha is more than 0 and less than 0.06, and theta is more than 0 and less than 0.5.
4. The method of adjusting the coercivity of a garnet-spin-torque magnetic ferrite material as claimed in claim 3, wherein said Co is selected from the group consisting of Co, Co2+The range of the substitution amount is more than 0 and less than or equal to 0.06.
5. The method of adjusting the coercivity of a garnet-type magnetic ferrite material as set forth in claim 1, further comprising: with analytically pure Gd2O3，Y2O3，CaCO3，V2O5，MnCO3，Co2O3，SiO2，Al2O3，ZrO2，SnO2，Fe2O3As a raw material.
6. The method of adjusting the coercivity of a garnet-rotation rectangular magnetic ferrite material as set forth in claim 5, further comprising: the garnet ferrite material is obtained by the traditional ceramic process through primary ball milling, drying, pre-sintering, secondary ball milling, secondary drying, granulation, press molding and sintering.
7. The method of adjusting the coercivity of a garnet rotational ferrite material as claimed in claim 6, wherein the system of garnet ferrite materials is a GdSn (Zr) CaVMn-YIG or GdAl-YIG ferrite material.
CN202111333558.8A 2021-11-11 2021-11-11 Method for adjusting coercive force of garnet rotational-moment magnetic ferrite material Pending CN113943154A (en)

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Application publication date: 20220118