CN117282645A - Ferrite thick film material with low ferromagnetic resonance line width and high dielectric constant and preparation method thereof - Google Patents

Ferrite thick film material with low ferromagnetic resonance line width and high dielectric constant and preparation method thereof Download PDF

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CN117282645A
CN117282645A CN202311193606.7A CN202311193606A CN117282645A CN 117282645 A CN117282645 A CN 117282645A CN 202311193606 A CN202311193606 A CN 202311193606A CN 117282645 A CN117282645 A CN 117282645A
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ferrite
thick film
dielectric constant
line width
ferromagnetic resonance
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卢冰
王帅
李颉
孙凯
陈一鑫
刘颖力
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University of Electronic Science and Technology of China
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University of Electronic Science and Technology of China
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Abstract

The invention belongs to the field of electronic materials, and provides a ferrite thick film material with low ferromagnetic resonance line width and high dielectric constant and a preparation method thereof; firstly, the Bi-Ca-Sn-Zr ion substituted YIG ferrite material is used as the base, and the ferrite material is utilizedPreparation of Y by conventional solid phase sintering method 2.0‑x Bi 1.0 Ca x Fe 5‑2x Sn x Zr x O 12 The ferrite material has the advantages that the Bi-Ca ions in the components are substituted, so that the dielectric constant of the material can be improved, the material has high dielectric constant characteristics (dielectric constant epsilon'. Gtoreq.20) in the frequency range of 1 MHz-500 MHz, the Sn-Zr ions in the components are substituted to promote the material to reduce magnetocrystalline anisotropy and loss, the influence of the internal stress and air holes of the material on the ferromagnetic resonance line width is improved, the magnetic loss of ferrite in the high frequency range is reduced, and the material has lower ferromagnetic resonance line width (delta H is less than or equal to 100 Oe); however, the ferrite thick film material is prepared by adopting a spin coating process, and the ferrite thick film material with low ferromagnetic resonance line width and high dielectric constant is obtained by annealing and forming under the orientation of a magnetic field, so that the requirements of microwave devices are met.

Description

Ferrite thick film material with low ferromagnetic resonance line width and high dielectric constant and preparation method thereof
Technical Field
The invention belongs to the field of electronic materials, and particularly provides a ferrite thick film material with low ferromagnetic resonance line width and high dielectric constant and a preparation method thereof.
Background
With the rapid development of the fields of high-frequency wireless communication and information big data, a microwave high-frequency device for wireless communication becomes one of key devices, and based on the requirements of an integral microwave system, the requirements of high integration, chip type and high performance are put forward for the microwave device, the research on the substrate material of the microwave device is carried out, and the design of a miniaturized microwave device becomes one of the international hot spot problems. Materials with low ferroresonance linewidth and high dielectric constant are used as the substrate of microwave devices, and the development is carried out based on the influence of electromagnetic parameters of the materials on the size and the performance of the devices. Along with the improvement of the transmission efficiency, the transmission loss requirement of the microwave device is lower and stricter, and the lower ferromagnetic resonance linewidth requirement of the material is higher and stricter from the basis material, so that the microwave device has lower microwave loss in the application process and higher transmission efficiency is obtained; the high dielectric constant performance of the material can meet the application requirements of miniaturized microwave devices; in addition, devices are required to be gradually developed in the direction of chip formation in order to meet the space requirements of the integration level and the microwave system.
For substrate materials with low ferroresonance linewidth and high dielectric constant, much research has been focused mainly on yttrium iron garnet (Y 3 Fe 5 O 12 YIG) material aspect; for example, patent document 202110239907.3 discloses a high dielectric constant microwave ferrite material, a preparation method and application thereof, wherein Sn-Al-Sm synergistic ion substitution is adopted to improve the dielectric constant (more than 18) of YIG ferrite, meanwhile, better magnetic performance is maintained, bi element ion substitution is adopted to maintain the large size of crystal grains, and the ferromagnetic resonance line width is reduced; in addition, as disclosed In patent document 202210164462.1, a medium saturation magnetization power type high dielectric constant garnet material and a preparation method thereof are disclosed, and the dielectric constant (dielectric constant is 25-26) of YIG material is regulated and controlled by adopting various ions such as Bi-Ca-Dy-Zr-Sn-In-Sb and the like, and meanwhile, the magnetic properties such as good saturation magnetization and the like are maintained; and as disclosed in patent document 202110324952.9, the low-temperature sintered YIG gyromagnetic ferrite material and the preparation method thereof adopt Bi-Zn-V plasma to regulate and control the sintering temperature and magnetic property of YIG, and the YIG material sintered and formed below 960 ℃ is obtained, and the material has certain saturated magnetization intensity, low coercive force and low loss. However, the YIG materials prepared in the above patent documents are YIG powder, and in order to meet the high integration requirement of a microwave system, the invention forms a thick film material by a spin coating process based on ferromagnetic resonance line width and high dielectric constant ferrite, thereby further meeting the higher requirement of a microwave device.
Disclosure of Invention
The invention aims to provide a ferrite thick film material with low ferromagnetic resonance line width and high dielectric constant and a preparation method thereof, firstly, bi-Ca-Sn-Zr ion substituted Y is adopted 3 Fe 5 O 12 (YIG) ferrite material is used as a base to prepare Y by a traditional solid phase sintering method according to stoichiometric ratio 2.0-x Bi 1.0 Ca x Fe 5-2x Sn x Zr x O 12 The Bi-Ca ions in the ferrite material are substituted, so that the dielectric constant of the material can be improved, the material has high dielectric constant characteristics (dielectric constant epsilon'. Gtoreq.20) in the frequency band of 1 MHz-500 MHz, and the Sn-Zr ions in the ferrite material are substituted with the accelerating materialThe material reduces magnetocrystalline anisotropy and loss, improves the influence of internal stress and air holes of the material on the ferromagnetic resonance line width, integrally reduces the magnetic loss of ferrite in a high frequency band, and ensures that the material has lower ferromagnetic resonance line width (delta H is less than or equal to 100 Oe); however, preparing a ferrite material thick film by adopting a spin coating process, and preparing a ferrite thick film material with uniform thickness; finally, the ferrite thick film material with low ferromagnetic resonance line width and high dielectric constant is prepared by adopting magnetic field orientation annealing molding, thereby meeting the requirements of microwave devices.
In order to achieve the above purpose, the invention adopts the following technical scheme:
a ferrite thick film material with low ferromagnetic resonance line width and high dielectric constant is characterized in that the ferrite thick film material is composed of Y 2.0-x Bi 1.0 Ca x Fe 5-2x Sn x Zr x O 12 Ferrite material is formed on a carrier substrate through a spin coating process and is annealed and formed under the orientation of a magnetic field, wherein x=0.1-0.5.
Further, the thickness of the ferrite thick film material is 10-50 μm.
Further, the preparation method of the ferromagnetic resonance line width high dielectric constant ferrite thick film material is characterized by comprising the following steps:
step 1, according to Y 2.0-x Bi 1.0 Ca x Fe 5-2x Sn x Zr x O 12 The stoichiometric ratio of ferrite material weighs the reactants: yttria (Y) 2 O 3 ) Bismuth oxide (Bi) 2 O 3 ) Calcium carbonate (CaCO) 3 ) Tin dioxide (SnO) 2 ) Zirconium oxide (ZrO) 2 ) And ferric oxide (Fe) 2 O 3 ) Wherein x=0.1 to 0.5;
step 2, preparing the raw materials in the step 1 into Y by a solid-phase sintering method 2.0-x Bi 1.0 Ca x Fe 5-2x Sn x Zr x O 12 Ferrite powder, the sintering temperature of the solid phase sintering method is 900-1100 ℃ and the heat preservation time is 1-6 hours;
step 3, mixing and stirring the ferrite powder obtained in the step 2, toluene, ethanol, a dispersing agent and a plasticizer together to form slurry; wherein, toluene: ethanol: dispersing agent: and (3) a plasticizer: the mass ratio of the ferrite powder is 4:6:1:1:15, stirring for 3-5 hours to obtain slurry; then weighing PVA adhesive accounting for 8-12 wt% of the ferrite powder component, adding the PVA adhesive into the slurry, and continuously stirring for 1 hour to obtain a spin-coating powder slurry;
step 4, placing the spin-coating powder slurry obtained in the step 3 into a spin-coating machine, adopting a silicon substrate, a glass substrate or a silicon dioxide substrate and the like as carriers, spin-coating on the carriers for spin-coating, taking down a sample after spin-coating for 20-40 seconds at the rotating speed of 500-1500 rpm of the spin-coating machine, and carrying out heat treatment, wherein the heat treatment is carried out, and the heat treatment is carried out specifically, the heat is preserved for 10-15 minutes at 250 ℃ and the heat is preserved for 10 minutes at 800-1000 ℃; taking out the sample, and then carrying out spin coating again, and repeating for a plurality of times to obtain a primary sample of the ferrite thick film;
and 5, annealing the primary sample of the ferrite thick film obtained in the step 4 under a magnetic field, wherein the annealing is specifically as follows: setting the magnetic field to 300-1000 Oe, and preserving the temperature at 600-700 ℃ for 0.5-3 hours under the protection of nitrogen to obtain the low ferromagnetic resonance line width high dielectric ferrite thick film material.
Compared with the prior art, the invention has the beneficial effects that:
1. the ferrite thick film material with low ferromagnetic resonance line width and high dielectric constant is prepared by using Y 2.0-x Bi 1.0 Ca x Fe 5- 2x Sn x Zr x O 12 Ferrite is used as a base material, and the ferromagnetic resonance line width and the dielectric constant of the material are regulated and controlled through material component design, so that the application requirement of a microwave device is met;
2. the ferrite thick film material with low ferromagnetic resonance line width and high dielectric constant has high dielectric constant characteristics (dielectric constant epsilon'. Gtoreq.20) in a frequency band of 1 MHz-500 MHz, and has lower ferromagnetic resonance line width (delta H is less than or equal to 100 Oe);
3. the low ferromagnetic resonance line width high dielectric ferrite thick film material is applied as a substrate of a microwave device, has the advantages of small size, large bias magnetic field and the like compared with a common powder substrate based on the low ferromagnetic resonance line width and high dielectric constant characteristics, can improve the high transmission efficiency of the microwave device, and provides a new material for application of high-frequency and integrated small-size communication equipment.
Drawings
FIG. 1 is a flow chart of a method for preparing a low ferromagnetic resonance linewidth high dielectric ferrite thick film material of the present invention.
Fig. 2 is an XRD test pattern of low ferroresonance linewidth high dielectric ferrite thick film materials of examples 1, 2 and 3 of the present invention.
Fig. 3 is a dielectric constant test chart of low ferroresonance linewidth high dielectric ferrite thick film materials of examples 1, 2 and 3 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantageous effects of the present invention more apparent, the present invention will be described in further detail with reference to the accompanying drawings and examples.
Example 1
The embodiment provides a low ferromagnetic resonance line width high dielectric ferrite thick film material, the preparation method is shown in fig. 1, and the method specifically comprises the following steps:
step 1, according to Y 2.0-x Bi 1.0 Ca x Fe 5-2x Sn x Zr x O 12 Stoichiometric ratio of ferrite the reactants were weighed, x=0.1 was chosen, and yttria (Y 2 O 3 ) 10.73g, bismuth oxide (Bi) 2 O 3 ) 11.65g of calcium carbonate (CaCO) 3 ) 0.5g, tin dioxide (SnO) 2 ) 0.75g, zirconia (ZrO 2 ) 0.62g and ferric oxide (Fe 2 O 3 )19.16g；
Step 2, preparing ferrite powder from the raw materials in the step 1 according to a solid phase sintering method, and adopting a conventional ball milling method, wherein the sintering temperature is 1030 ℃ and the heat preservation time is 3 hours to obtain Y 1.9 Bi 1.0 Ca 0.1 Fe 4.8 Sn 0.1 Zr 0.1 O 12 Ferrite powder;
and 3, mixing and stirring the powder obtained in the step 2 with toluene, ethanol, a dispersing agent and a plasticizer to form slurry, wherein the toluene: ethanol: dispersant (M1135 type): plasticizer (M1125 type): the mass ratio of the ferrite powder is 4:6:1:1:15, stirring for 4 hours to obtain slurry; weighing 10wt% of B74001 type PVA adhesive of ferrite component, adding into the slurry, and continuously stirring for 1 hour to obtain spin-coating powder slurry;
step 4, placing the spin-coating powder slurry obtained in the step 3 into a spin-coating machine, spin-coating by using a silicon substrate, a glass substrate or a silicon dioxide substrate and the like as carriers, taking down a sample after spin-coating for 30 seconds at the rotation speed of 800 rpm, performing heat treatment, keeping the temperature at 250 ℃ for 12 minutes and the temperature at 900 ℃ for 10 minutes, taking out the sample, performing secondary spin-coating, and repeating for three times by adopting a spin-heat treatment method to obtain a primary sample of ferrite thick film, wherein the primary sample is consistent with the parameters;
and 5, annealing the preliminary sample of the ferrite thick film obtained in the step 4 under a magnetic field, keeping the magnetic field at 800Oe and 650 ℃ for 1 hour under the protection of nitrogen, and obtaining the ferrite thick film material with the thickness of 30 mu m and the low ferromagnetic resonance line width and the high dielectric constant.
Example 2
This embodiment differs from embodiment 1 in that: the process of the step 1 is as follows: according to Y 2.0-x Bi 1.0 Ca x Fe 5- 2x Sn x Zr x O 12 Stoichiometric ratio of ferrite the reactants were weighed, x=0.3 was chosen, and yttria (Y 2 O 3 ) 9.60g, bismuth oxide (Bi) 2 O 3 ) 11.65g of calcium carbonate (CaCO) 3 ) 1.5g, tin dioxide (SnO) 2 ) 2.26g, zirconia (ZrO 2 ) 1.85g and ferric oxide (Fe 2 O 3 ) 17.57g of ferrite material was prepared, and the rest of the procedure was the same as in example 1.
Example 3
This embodiment differs from embodiment 1 in that: the process of the step 1 is as follows: according to Y 2.0-x Bi 1.0 Ca x Fe 5- 2x Sn x Zr x O 12 Stoichiometric ratio of ferrite the reactants were weighed, x=0.5 was chosen, and yttria (Y 2 O 3 ) 8.47g of bismuth oxide(Bi 2 O 3 ) 11.65g of calcium carbonate (CaCO) 3 ) 2.5g, tin dioxide (SnO) 2 ) 3.77g, zirconia (ZrO 2 ) 3.08g and ferric oxide (Fe) 2 O 3 ) 15.97g of ferrite material was prepared and the rest of the procedure was the same as in example 1.
XRD tests are carried out on the ferrite thick film materials prepared in the embodiment 1, the embodiment 2 and the embodiment 3, the XRD patterns are shown in the figure 2, and the (a), (b) and (c) in the figure 2 correspond to the embodiment 1, the embodiment 2 and the embodiment 3 in sequence; the graph shows that the ferrite material prepared by the invention has single phase formation, no other impurity phase appears, and the garnet structure of YIG ferrite is maintained.
The ferrite thick film materials prepared in example 1, example 2 and example 3 were subjected to ferromagnetic resonance line width and dielectric constant tests, the ferromagnetic resonance line width test results are shown in table 1, the dielectric constant test results are shown in fig. 3, and (a), (b) and (c) in fig. 3 correspond to examples 1, 2 and 3 in sequence; the ferromagnetic resonance line width of the ferrite thick film material is tested by adopting a waveguide resonant cavity method at 9.56GHz, and the dielectric constant is tested at 1 MHz-1 GHz. According to the result, the ferrite thick film material provided by the invention has a lower ferromagnetic resonance line width and a high dielectric constant, and can be used as a substrate material of a microwave device.
TABLE 1
Sample of Example 1 Example 2 Example 3
Line width of ferromagnetic resonance ΔH＝87.85Oe ΔH＝86.37Oe ΔH＝83.41Oe
While the invention has been described in terms of specific embodiments, any feature disclosed in this specification may be replaced by alternative features serving the equivalent or similar purpose, unless expressly stated otherwise; all of the features disclosed, or all of the steps in a method or process, except for mutually exclusive features and/or steps, may be combined in any manner.

Claims (3)

1. A ferrite thick film material with low ferromagnetic resonance line width and high dielectric constant is characterized in that the ferrite thick film material is composed of Y 2.0-x Bi 1.0 Ca x Fe 5-2x Sn x Zr x O 12 Ferrite material is formed on a carrier substrate through a spin coating process, and is annealed and formed under the orientation of a magnetic field, wherein x=0.1-0.5.
2. The low ferromagnetic resonance linewidth high dielectric constant ferrite thick film material of claim 1 wherein said ferrite thick film material has a thickness of 10-50 μm.
3. The method for preparing the ferromagnetic resonance line width high dielectric constant ferrite thick film material according to claim 1, comprising the following steps:
step 1, according to Y 2.0-x Bi 1.0 Ca x Fe 5-2x Sn x Zr x O 12 The stoichiometric ratio of ferrite material weighs the reactants: yttria (Y) 2 O 3 ) Bismuth oxide (Bi) 2 O 3 ) Calcium carbonate (CaCO) 3 ) Tin dioxide (SnO) 2 ) Zirconium oxide (ZrO) 2 ) And ferric oxide (Fe) 2 O 3 ) Wherein x=0.1 to 0.5;
step 2, preparing the raw materials in the step 1 according to a solid-phase sintering methodPreparing Y 2.0-x Bi 1.0 Ca x Fe 5-2x Sn x Zr x O 12 Ferrite powder, the sintering temperature of the solid phase sintering method is 900-1100 ℃ and the heat preservation time is 1-6 hours;
step 3, mixing and stirring the ferrite powder obtained in the step 2, toluene, ethanol, a dispersing agent and a plasticizer together to form slurry; wherein, toluene: ethanol: dispersing agent: and (3) a plasticizer: the mass ratio of the ferrite powder is 4:6:1:1:15, stirring for 3-5 hours to obtain slurry; then weighing PVA adhesive accounting for 8-12 wt% of the ferrite powder component, adding the PVA adhesive into the slurry, and continuously stirring for 1 hour to obtain a spin-coating powder slurry;
step 4, placing the spin-coating powder slurry obtained in the step 3 into a spin-coating machine, adopting a silicon substrate, a glass substrate or a silicon dioxide substrate and the like as carriers, spin-coating on the carriers for spin-coating, taking down a sample after spin-coating for 20-40 seconds at the rotating speed of 500-1500 rpm of the spin-coating machine, and carrying out heat treatment, wherein the heat treatment is carried out, and the heat treatment is carried out specifically, the heat is preserved for 10-15 minutes at 250 ℃ and the heat is preserved for 10 minutes at 800-1000 ℃; taking out the sample, and then carrying out spin coating again, and repeating for a plurality of times to obtain a primary sample of the ferrite thick film;
and 5, annealing the primary sample of the ferrite thick film obtained in the step 4 under a magnetic field, wherein the annealing is specifically as follows: setting the magnetic field to 300-1000 Oe, and preserving the temperature at 600-700 ℃ for 0.5-3 hours under the protection of nitrogen to obtain the low ferromagnetic resonance line width high dielectric ferrite thick film material.
CN202311193606.7A 2023-09-15 2023-09-15 Ferrite thick film material with low ferromagnetic resonance line width and high dielectric constant and preparation method thereof Pending CN117282645A (en)

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