CN116854460A - Microwave ferrite material with high dielectric constant, high Curie temperature and low loss and preparation method thereof - Google Patents
Microwave ferrite material with high dielectric constant, high Curie temperature and low loss and preparation method thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 84
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 238000000498 ball milling Methods 0.000 claims abstract description 63
- 239000002994 raw material Substances 0.000 claims abstract description 35
- 239000000843 powder Substances 0.000 claims abstract description 32
- 239000006247 magnetic powder Substances 0.000 claims abstract description 23
- 238000001035 drying Methods 0.000 claims abstract description 18
- 239000000203 mixture Substances 0.000 claims abstract description 15
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 239000002002 slurry Substances 0.000 claims abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 6
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000010959 steel Substances 0.000 claims abstract description 6
- 238000005303 weighing Methods 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 29
- 238000005245 sintering Methods 0.000 claims description 28
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 22
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- 239000002245 particle Substances 0.000 claims description 12
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- 238000012216 screening Methods 0.000 claims 2
- 230000005350 ferromagnetic resonance Effects 0.000 abstract description 17
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Abstract
The invention discloses a high dielectric constant high Curie temperature low-loss microwave ferrite material and a preparation method thereof, and the preparation method specifically comprises the following steps: s1, firstly, according to chemical formula Bi a Ca b Y (3‑a‑b) Zr c Sn d In e Ta f Fe (5‑c‑d‑e‑f‑δ) O 12 Weighing raw material magnetic powder, and drying the raw material magnetic powder; s2, adding raw material magnetic powder into a ball milling tank, adding pure water or alcohol and carrying out ball milling and mixing on the steel balls or zirconium balls for the first time; s3, drying the primary ball milling slurry, sieving, and adding pure water accounting for 0.5-5% of the weight of the powder into the sieved powder to uniformly mix; s4, pressing the powder into blocks by using the pressure of 1-20 MPa; the invention relates to the technical field of microwave ferrite materials. The high dielectric constant and the high CurieThe microwave ferrite material with high dielectric constant, low ferromagnetic resonance linewidth, high Curie temperature and excellent comprehensive performance of proper magnetic moment is prepared by the temperature low-loss microwave ferrite material and the preparation method thereof, so that the miniaturized application of the microwave device is practically applied, and the material preparation process is suitable for mass production.
Description
Technical Field
The invention relates to the technical field of microwave ferrite materials, in particular to a high-dielectric-constant high-Curie-temperature low-loss microwave ferrite material and a preparation method thereof.
Background
The microwave ferrite device plays an important role in microwave technology and has wide application in the fields of aerospace, satellite communication, electronic countermeasure, mobile communication, medical treatment and the like. As the core of the microwave ferrite device, the microwave ferrite material is applied to devices such as a circulator, an isolator, a phase shifter, a variable polarizer and the like, and realizes the functions of isolating, selecting a passage, shifting phase, controlling polarization state, switching, modulating, doubling frequency, amplifying and the like of microwave transmission in a microwave system.
With the development of microwave technology, the requirements for device miniaturization are higher, and for microwave ferrite materials applied to microwave devices such as circulators and isolators, the improvement of the dielectric constant of the materials is a main direction of device miniaturization, and meanwhile, the microwave devices also have higher requirements for characteristics such as insertion loss, intermodulation and temperature stability, so that the microwave ferrite materials are required to have high dielectric constants, low ferroresonance line width, high curie temperature and proper saturation magnetization. The most widely used YIG (i.e. Y 3 Fe 5 O 12 ) In the microwave ferrite material, bi3+ is generally adopted to replace Y of part dodecahedron position 3 +to increase the dielectric constant, zr is used 4+ Or Sn (Sn) 4+ Or I n 3+ Plasma-substituted part of octahedral Fe 3+ To reduce line width, but these methods suffer from two drawbacks: 1. bi is a low-melting-point substance, and is subjected to liquid phase sintering in the sintering process, so that abnormal grain growth is easy to cause, and the grain size in the final sintered body is uneven, so that the ferromagnetic resonance line width is influenced; 2. excessive Zr 4+ Or Sn (Sn) 4+ Or I n 3+ Of other ions of the plasmaSubstitution weakens the super-exchange effect between tetrahedral and octahedral Fe-O-Fe, so that the Curie temperature of the material is reduced, and the temperature stability of the microwave device is affected; therefore, the invention provides a microwave ferrite material with high dielectric constant, high Curie temperature and low loss and a preparation method thereof, so as to solve the problems.
Disclosure of Invention
(one) solving the technical problems
Aiming at the defects of the prior art, the invention provides a compound with a chemical formula of Bi a Ca b Y (3-a-b) Zr c Sn d I n e Ta f Fe (5-c-d-e-f) O 12 The microwave ferrite material and the preparation method thereof solve the problems of high ferromagnetic resonance line width and low Curie temperature of the YIG microwave ferrite material with high dielectric constant.
(II) technical scheme
In order to achieve the above purpose, the invention is realized by the following technical scheme: the preparation method of the microwave ferrite material with high dielectric constant, high Curie temperature and low loss comprises the following steps:
s1, firstly, according to chemical formula Bi a Ca b Y (3-a-b) Zr c Sn d I n e Ta f Fe (5-c-d-e-f-δ) O 12 Weighing raw material magnetic powder, and drying the raw material magnetic powder;
s2, adding raw material magnetic powder into a ball milling tank, adding pure water or alcohol and carrying out ball milling and mixing on the steel balls or zirconium balls for the first time;
s3, drying the primary ball milling slurry, sieving, and adding pure water accounting for 0.5-5% of the weight of the powder into the sieved powder to uniformly mix;
s4, pressing the powder into blocks by using the pressure of 1-20 MPa, and preserving the temperature of the pressed blocks at 700-1000 ℃ for 2-6 hours for presintering;
s5, crushing the presintering material, sieving, and performing secondary ball milling on the sieved powder;
s6, adding a binder into the secondary ball milling material for granulating, and pressing the granulated granules to form blanks with the required size;
s7, finally, the blank is sintered into a required product at the temperature of 800-1200 ℃ for 6-20 hours, and the sintering heating rate is controlled to be 0.5-5 ℃/min, so as to prepare the microwave ferrite.
Preferably, the raw material magnetic powder in the step S1 is oxide, specifically Bi 2 O 3 、CaCO 3 Or CaO, Y 2 O 3 、ZrO 2 、SnO 2 、I n 2 O3、Ta 2 O 5 、Fe 2 O 3 。
Preferably, the ball milling time in the step S2 is 1-10 h, the ball milling speed is 150-250 revolutions/min, and the direction is changed every 30 min.
Preferably, in the step S3, a sieve with 30-200 meshes is adopted, and in the step S5, a sieve with 30-60 meshes is adopted.
Preferably, the secondary ball milling time in the step S5 is 4-30 hours, and the average particle size of the ball milling material is controlled to be 0.9-1.6 mu m.
Preferably, the binder in the step S6 is 5-12% pva glue.
Preferably, the sintering process in the step S7 specifically includes the following steps:
(1) And (3) heating: the temperature rise is slower at 0-500 ℃ and is 1 ℃/min;
(2) And (3) heat preservation: preserving heat at 500 ℃ for 360min;
(3) And a cooling stage, namely cooling the temperature from 1450 ℃ to 1200 ℃, wherein the cooling rate is 2 ℃/min.
A high dielectric constant high Curie temperature low loss microwave ferrite material, the chemical formula of the microwave ferrite is Bi a Ca b Y (3-a-b) Zr c Sn d I n e Ta f Fe (5-c-d-e-f-δ) O 12 Wherein a is more than or equal to 0.6 and less than or equal to 1.6,0.1 and less than or equal to 1.0, c is more than or equal to 0 and less than or equal to 0.4, d is more than or equal to 0 and less than or equal to 0.4, e is more than or equal to 0 and less than or equal to 0.4, f is more than or equal to 0 and less than or equal to 0.3, and delta is the iron deficiency considered during ball milling.
(III) beneficial effects
The invention provides a microwave ferrite material with high dielectric constant, high Curie temperature and low loss and a preparation method thereof. Compared with the prior art, the method has the following beneficial effects:
(1) According to the high-dielectric constant high-Curie temperature low-loss microwave ferrite material and the preparation method thereof, powder after primary ball milling is subjected to briquetting and presintering, so that the contact area between powder particles can be increased, the activity of solid phase reaction is enhanced, the presintering temperature is reduced, and volatilization of Bi with a low melting point in the presintering process is effectively prevented.
(2) According to the high-dielectric constant high-Curie temperature low-loss microwave ferrite material and the preparation method thereof, zr, sn, I n and Ta ions are used for replacing Fe ions, so that the magnetocrystalline anisotropy of the material can be effectively reduced, the ferromagnetic resonance line width of the material is reduced, meanwhile, ta can also inhibit abnormal growth of crystal grains in the sintering process, and the problems of abnormal growth of crystal grains and non-uniformity of the crystal grains caused by adding Bi in the material are solved; the microwave ferrite material with high dielectric constant, low ferromagnetic resonance line width, high Curie temperature and excellent comprehensive performance of proper magnetic moment is prepared, so that the miniaturized application of the microwave device is practically applied, and the material preparation process is suitable for mass production.
Drawings
FIG. 1 is a graph of burn-in temperature for the present invention;
FIG. 2 is a sintering graph of the present invention;
FIG. 3 shows dielectric loss test results for different sintering temperatures in an embodiment of the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Referring to fig. 1-3, the embodiments of the present invention provide three technical solutions:
example 1:
the preparation method of the microwave ferrite material with high dielectric constant, high Curie temperature and low loss comprises the following steps:
s1, firstly, according to chemical formula Bi a Ca b Y (3-a-b) Zr c Sn d I n e Ta f Fe (5-c-d-e-f-δ) O 12 Weighing raw material magnetic powder, and drying the raw material magnetic powder; because the raw materials generally contain a certain amount of moisture, particularly water-absorbing materials, the raw materials need to be dried before being compounded, the drying temperature is 120 ℃, and the drying time is 120 mi.
S2, adding raw material magnetic powder into a ball milling tank, adding pure water or alcohol and carrying out ball milling and mixing on the steel balls or zirconium balls for the first time;
s3, sieving the primary ball milling slurry after drying, sieving with a 30-mesh sieve, and adding pure water accounting for 0.5% of the weight of the powder into the powder after sieving;
s4, pressing the powder into blocks under the pressure of 1MPa, and preserving the heat of the pressed blocks at 700 ℃ for 2 hours for presintering; the powder after one-time ball milling is presintered through the pressing block, so that the contact area between powder particles can be increased, the activity of solid phase reaction is enhanced, the presintering temperature is reduced, and the volatilization of low-melting-point Bi in the presintering process is effectively prevented.
S5, crushing the presintering material, sieving the presintering material with a 30-mesh sieve, and performing secondary ball milling on the sieved powder, wherein the secondary ball milling time is 4 hours, and the average granularity of the ball milling material is controlled to be 0.9 mu m; after presintering, only part of the raw materials are converted into ferrite, and the components are unevenly distributed, so that the whole components are uniformly mixed by crushing and mechanical mixing, and the raw materials are fully contacted in the sintering process, thereby being beneficial to solid phase reaction. The pre-sintered material has high hardness and large particles, the post-forming can be completed only by crushing, the particle size can be reduced by secondary ball milling, the sintering power is improved, the grain growth and the air hole reduction are facilitated, and the microstructure is optimized.
S6, adding a binder into the secondary ball milling material for granulating, wherein the binder is 5% PVA glue; pressing the granulated granules to form blanks with the required size; as a further technical scheme, after the secondary ball milling is carried out for a certain time, the mixture is sieved by a sieve with 50-100 meshes, only the mixture with 50-100 meshes is taken for forming, and the mixture with more than 50 meshes and less than 100 meshes is continuously ground until all the mixture is positioned between 50 meshes and 100 meshes, and the granulation is completed.
S7, finally, the blank is sintered into a required product after heat preservation for 6 hours at 800 ℃, and the sintering heating rate is controlled at 0.5 ℃/min, so that the microwave ferrite is prepared. After sintering, the grain growth is completed, the air holes are discharged as much as possible, the grain boundary disappears, and the densification degree is highest.
In the embodiment of the present invention, the raw material magnetic powder in step S1 is an oxide, specifically Bi 2 O 3 、CaCO 3 Or CaO, Y 2 O 3 、ZrO 2 、SnO 2 、I n 2 O3、Ta 2 O 5 、Fe 2 O 3 。
In the embodiment of the invention, the ball milling time in the step S2 is 1h, the ball milling speed is 150 revolutions per mi n, and the direction is changed every 30mi n.
In the embodiment of the present invention, the sintering process in step S7 is specifically as follows:
(1) And (3) heating: the temperature rise is slower at 0-500 ℃ and is 1 ℃/min; in the process, moisture introduced by the adhesive and the like is gradually removed, and the compactness is affected by the too fast temperature rise;
(2) And (3) heat preservation: preserving heat at 500 ℃ for 360min; because the temperature is the volatilization temperature of the adhesive, the adhesive needs to be discharged, after the adhesive is volatilized, crystal grains continue to grow in the period, air holes are discharged, and the densification degree is further improved.
(3) And a cooling stage, namely cooling the temperature from 1450 ℃ to 1200 ℃, wherein the cooling rate is 2 ℃/min. The influence caused by too fast cooling is effectively avoided.
A high dielectric constant high Curie temperature low loss microwave ferrite material is characterized in that: the chemical formula of the microwave ferrite is Bi a Ca b Y (3-a-b) Zr c Sn d I n e Ta f Fe (5-c-d-e-f-δ) O 12 Wherein a is more than or equal to 0.6 and less than or equal to 1.6,0.1 and less than or equal to 1.0, c is more than or equal to 0 and less than or equal to 0.4, d is more than or equal to 0 and less than or equal to 0.4, e is more than or equal to 0 and less than or equal to 0.4, f is more than or equal to 0 and less than or equal to 0.3, and delta is the iron deficiency considered during ball milling，0≤δ≤0.3。
In the technical scheme, bi replaces Y to improve the dielectric constant, but when the Bi replacement quantity a is smaller than 0.6, the dielectric constant epsilon is smaller than 16, the application effect of the microwave device can not be achieved, and when the Bi replacement quantity a is larger than 1.6, the ferromagnetic resonance line width is obviously increased, and the practical application can not be achieved.
Zr, sn, I n and Ta ions replace Fe ions, so that magnetocrystalline anisotropy of the material can be effectively reduced, ferromagnetic resonance line width of the material is reduced, meanwhile Ta can inhibit abnormal growth of crystal grains in the sintering process, and the problems of abnormal growth of the crystal grains and non-uniformity of the crystal grains caused by adding Bi into the material are solved. However, the substitution amount c, d, e, f of Zr, sn, I n and Ta ions cannot be too large, the Curie temperature of the material is obviously reduced after the substitution amount is large, and the temperature stability of the microwave device in practical application is poor.
The microwave ferrite material with high dielectric constant, low ferromagnetic resonance line width, high Curie temperature and excellent comprehensive performance of proper magnetic moment is prepared, so that the miniaturized application of a microwave device is practically applied, and the material preparation process is suitable for mass production. The material performance indexes are as follows: magnetic moment 4pi Ms=1650-2100 Gs; the line width delta H of the ferromagnetic resonance is less than or equal to 40Oe; dielectric constant epsilon=16 to 32; dielectric loss tan delta less than or equal to 4 x 10 -4 The method comprises the steps of carrying out a first treatment on the surface of the The Curie temperature Tc is more than or equal to 260 ℃.
Example 2:
the preparation method of the microwave ferrite material with high dielectric constant, high Curie temperature and low loss comprises the following steps:
s1, firstly, according to chemical formula Bi a Ca b Y (3-a-b) Zr c Sn d I n e Ta f Fe (5-c-d-e-f-δ) O 12 Weighing raw material magnetic powder, and drying the raw material magnetic powder; because the raw materials generally contain a certain amount of moisture, particularly water-absorbing materials, the raw materials need to be dried before being compounded, the drying temperature is 120 ℃, and the drying time is 120 mi.
S2, adding raw material magnetic powder into a ball milling tank, adding pure water or alcohol and carrying out ball milling and mixing on the steel balls or zirconium balls for the first time;
s3, sieving the primary ball milling slurry after drying, sieving with a 115-mesh sieve, and adding pure water accounting for 2.8% of the weight of the powder into the powder after sieving;
s4, pressing the powder into blocks under the pressure of 10MPa, and preserving the temperature of the pressed blocks at 850 ℃ for 4 hours for presintering; the powder after one-time ball milling is presintered through the pressing block, so that the contact area between powder particles can be increased, the activity of solid phase reaction is enhanced, the presintering temperature is reduced, and the volatilization of low-melting-point Bi in the presintering process is effectively prevented.
S5, crushing the presintering material, sieving the presintering material with a 45-mesh sieve, and performing secondary ball milling on the sieved powder, wherein the secondary ball milling time is 17 hours, and the average granularity of the ball milling material is controlled to be 1.2 mu m; after presintering, only part of the raw materials are converted into ferrite, and the components are unevenly distributed, so that the whole components are uniformly mixed by crushing and mechanical mixing, and the raw materials are fully contacted in the sintering process, thereby being beneficial to solid phase reaction. The pre-sintered material has high hardness and large particles, the post-forming can be completed only by crushing, the particle size can be reduced by secondary ball milling, the sintering power is improved, the grain growth and the air hole reduction are facilitated, and the microstructure is optimized.
S6, adding a binder into the secondary ball milling material for granulating, wherein the binder is 8.5% PVA glue; pressing the granulated granules to form blanks with the required size; as a further technical scheme, after the secondary ball milling is carried out for a certain time, the mixture is sieved by a sieve with 50-100 meshes, only the mixture with 50-100 meshes is taken for forming, and the mixture with more than 50 meshes and less than 100 meshes is continuously ground until all the mixture is positioned between 50 meshes and 100 meshes, and the granulation is completed.
S7, finally, the blank is sintered into a required product after heat preservation for 13 hours at the temperature of 1000 ℃, and the sintering heating rate is controlled at 2.7 ℃/min, so that the microwave ferrite is prepared. After sintering, the grain growth is completed, the air holes are discharged as much as possible, the grain boundary disappears, and the densification degree is highest.
In the embodiment of the present invention, the raw material magnetic powder in step S1 is an oxide, specifically Bi 2 O 3 、CaCO 3 Or CaO, Y 2 O 3 、ZrO 2 、SnO 2 、I n 2 O3、Ta 2 O 5 、Fe 2 O 3 。
In the embodiment of the invention, the ball milling time in the step S2 is 5.5 hours, the ball milling speed is 200 revolutions/min, and the direction is changed every 30 min.
In the embodiment of the present invention, the sintering process in step S7 is specifically as follows:
(1) And (3) heating: the temperature rise is slower at 0-500 ℃ and is 1 ℃/min; in the process, moisture introduced by the adhesive and the like is gradually removed, and the compactness is affected by the too fast temperature rise;
(2) And (3) heat preservation: preserving heat at 500 ℃ for 360min; because the temperature is the volatilization temperature of the adhesive, the adhesive needs to be discharged, after the adhesive is volatilized, crystal grains continue to grow in the period, air holes are discharged, and the densification degree is further improved.
(3) And a cooling stage, namely cooling the temperature from 1450 ℃ to 1200 ℃, wherein the cooling rate is 2 ℃/min. The influence caused by too fast cooling is effectively avoided.
A high dielectric constant high Curie temperature low loss microwave ferrite material is characterized in that: the chemical formula of the microwave ferrite is Bi a Ca b Y (3-a-b) Zr c Sn d I n e Ta f Fe (5-c-d-e-f-δ) O 12 Wherein a is more than or equal to 0.6 and less than or equal to 1.6,0.1 and less than or equal to 1.0, c is more than or equal to 0 and less than or equal to 0.4, d is more than or equal to 0 and less than or equal to 0.4, e is more than or equal to 0 and less than or equal to 0.4, f is more than or equal to 0 and less than or equal to 0.3, and delta is the iron deficiency considered during ball milling.
In the technical scheme, bi replaces Y to improve the dielectric constant, but when the Bi replacement quantity a is smaller than 0.6, the dielectric constant epsilon is smaller than 16, the application effect of the microwave device can not be achieved, and when the Bi replacement quantity a is larger than 1.6, the ferromagnetic resonance line width is obviously increased, and the practical application can not be achieved.
Zr, sn, I n and Ta ions replace Fe ions, so that magnetocrystalline anisotropy of the material can be effectively reduced, ferromagnetic resonance line width of the material is reduced, meanwhile Ta can inhibit abnormal growth of crystal grains in the sintering process, and the problems of abnormal growth of the crystal grains and non-uniformity of the crystal grains caused by adding Bi into the material are solved. However, the substitution amount c, d, e, f of Zr, sn, I n and Ta ions cannot be too large, the Curie temperature of the material is obviously reduced after the substitution amount is large, and the temperature stability of the microwave device in practical application is poor.
The microwave ferrite material with high dielectric constant, low ferromagnetic resonance line width, high Curie temperature and excellent comprehensive performance of proper magnetic moment is prepared, so that the miniaturized application of a microwave device is practically applied, and the material preparation process is suitable for mass production. The material performance indexes are as follows: magnetic moment 4pi Ms=1650-2100 Gs; the line width delta H of the ferromagnetic resonance is less than or equal to 40Oe; dielectric constant epsilon=16 to 32; dielectric loss tan delta less than or equal to 4 x 10 -4 The method comprises the steps of carrying out a first treatment on the surface of the The Curie temperature Tc is more than or equal to 260 ℃.
Example 3:
the preparation method of the microwave ferrite material with high dielectric constant, high Curie temperature and low loss comprises the following steps:
s1, firstly, according to chemical formula Bi a Ca b Y (3-a-b) Zr c Sn d I n e Ta f Fe (5-c-d-e-f-δ) O 12 Weighing raw material magnetic powder, and drying the raw material magnetic powder; because the raw materials generally contain a certain amount of moisture, particularly water-absorbing materials, the raw materials need to be dried before being compounded, the drying temperature is 120 ℃, and the drying time is 120 mi.
S2, adding raw material magnetic powder into a ball milling tank, adding pure water or alcohol and carrying out ball milling and mixing on the steel balls or zirconium balls for the first time;
s3, drying the primary ball milling slurry, sieving the slurry with a 200-mesh sieve, and adding pure water accounting for 5% of the weight of the powder into the powder which is sieved, and uniformly mixing the powder;
s4, pressing the powder into blocks by using 20MPa, and preserving the temperature of the pressed blocks at 700-1000 ℃ for 6 hours for presintering; the powder after one-time ball milling is presintered through the pressing block, so that the contact area between powder particles can be increased, the activity of solid phase reaction is enhanced, the presintering temperature is reduced, and the volatilization of low-melting-point Bi in the presintering process is effectively prevented.
S5, crushing the presintering material, sieving the presintering material with a 60-mesh sieve, and performing secondary ball milling on the sieved powder, wherein the secondary ball milling time is 30 hours, and the average granularity of the ball milling material is controlled to be 1.6 mu m; after presintering, only part of the raw materials are converted into ferrite, and the components are unevenly distributed, so that the whole components are uniformly mixed by crushing and mechanical mixing, and the raw materials are fully contacted in the sintering process, thereby being beneficial to solid phase reaction. The pre-sintered material has high hardness and large particles, the post-forming can be completed only by crushing, the particle size can be reduced by secondary ball milling, the sintering power is improved, the grain growth and the air hole reduction are facilitated, and the microstructure is optimized.
S6, adding a binder into the secondary ball milling material for granulating, wherein the binder is 12% PVA glue; pressing the granulated granules to form blanks with the required size; as a further technical scheme, after the secondary ball milling is carried out for a certain time, the mixture is sieved by a sieve with 50-100 meshes, only the mixture with 50-100 meshes is taken for forming, and the mixture with more than 50 meshes and less than 100 meshes is continuously ground until all the mixture is positioned between 50 meshes and 100 meshes, and the granulation is completed.
And S7, finally, preserving the heat of the blank at 1200 ℃ for 20 hours, and sintering the blank to obtain the required product, wherein the sintering heating rate is controlled at 5 ℃/min, so as to prepare the microwave ferrite. After sintering, the grain growth is completed, the air holes are discharged as much as possible, the grain boundary disappears, and the densification degree is highest.
In the embodiment of the present invention, the raw material magnetic powder in step S1 is an oxide, specifically Bi 2 O 3 、CaCO 3 Or CaO, Y 2 O 3 、ZrO 2 、SnO 2 、I n 2 O3、Ta 2 O 5 、Fe 2 O 3 。
In the embodiment of the invention, the ball milling time in the step S2 is 10 hours, the ball milling speed is 250 revolutions per minute (Mi), and the direction is changed every 30 Mi.
In the embodiment of the present invention, the sintering process in step S7 is specifically as follows:
(1) And (3) heating: the temperature rise is slower at 0-500 ℃ and is 1 ℃/min; in the process, moisture introduced by the adhesive and the like is gradually removed, and the compactness is affected by the too fast temperature rise;
(2) And (3) heat preservation: preserving heat at 500 ℃ for 360min; because the temperature is the volatilization temperature of the adhesive, the adhesive needs to be discharged, after the adhesive is volatilized, crystal grains continue to grow in the period, air holes are discharged, and the densification degree is further improved.
(3) And a cooling stage, namely cooling the temperature from 1450 ℃ to 1200 ℃, wherein the cooling rate is 2 ℃/min. The influence caused by too fast cooling is effectively avoided.
A high dielectric constant high Curie temperature low loss microwave ferrite material is characterized in that: the chemical formula of the microwave ferrite is Bi a Ca b Y (3-a-b) Zr c Sn d I n e Ta f Fe (5-c-d-e-f-δ) O 12 Wherein a is more than or equal to 0.6 and less than or equal to 1.6,0.1 and less than or equal to 1.0, c is more than or equal to 0 and less than or equal to 0.4, d is more than or equal to 0 and less than or equal to 0.4, e is more than or equal to 0 and less than or equal to 0.4, f is more than or equal to 0 and less than or equal to 0.3, and delta is the iron deficiency considered during ball milling.
In the technical scheme, bi replaces Y to improve the dielectric constant, but when the Bi replacement quantity a is smaller than 0.6, the dielectric constant epsilon is smaller than 16, the application effect of the microwave device can not be achieved, and when the Bi replacement quantity a is larger than 1.6, the ferromagnetic resonance line width is obviously increased, and the practical application can not be achieved.
Zr, sn, I n and Ta ions replace Fe ions, so that magnetocrystalline anisotropy of the material can be effectively reduced, ferromagnetic resonance line width of the material is reduced, meanwhile Ta can inhibit abnormal growth of crystal grains in the sintering process, and the problems of abnormal growth of the crystal grains and non-uniformity of the crystal grains caused by adding Bi into the material are solved. However, the substitution amount c, d, e, f of Zr, sn, I n and Ta ions cannot be too large, the Curie temperature of the material is obviously reduced after the substitution amount is large, and the temperature stability of the microwave device in practical application is poor.
The microwave ferrite material with high dielectric constant, low ferromagnetic resonance line width, high Curie temperature and excellent comprehensive performance of proper magnetic moment is prepared, so that the miniaturized application of a microwave device is practically applied, and the material preparation process is suitable for mass production. The material performance indexes are as follows: magnetic moment 4pi Ms=1650-2100 Gs; the line width delta H of the ferromagnetic resonance is less than or equal to 40Oe; dielectric constant epsilon=16 to 32; dielectric loss tan delta less than or equal to 4 x 10 -4 The method comprises the steps of carrying out a first treatment on the surface of the The Curie temperature Tc is more than or equal to 260 ℃.
And all that is not described in detail in this specification is well known to those skilled in the art.
It is noted that relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. The preparation method of the microwave ferrite material with high dielectric constant, high Curie temperature and low loss is characterized by comprising the following steps:
s1, firstly, according to chemical formula Bi a Ca b Y (3-a-b) Zr c Sn d In e Ta f Fe (5-c-d-e-f-δ) O 12 Weighing raw material magnetic powder, and drying the raw material magnetic powder;
s2, adding raw material magnetic powder into a ball milling tank, adding pure water or alcohol and carrying out ball milling and mixing on the steel balls or zirconium balls for the first time;
s3, drying the primary ball milling slurry, sieving, and adding pure water accounting for 0.5-5% of the weight of the powder into the sieved powder to uniformly mix;
s4, pressing the powder into blocks by using the pressure of 1-20 MPa, and preserving the temperature of the pressed blocks at 700-1000 ℃ for 2-6 hours for presintering;
s5, crushing the presintering material, sieving, and performing secondary ball milling on the sieved powder;
s6, adding a binder into the secondary ball milling material for granulating, and pressing the granulated granules to form blanks with the required size;
s7, finally, the blank is sintered into a required product at the temperature of 800-1200 ℃ for 6-20 hours, and the sintering heating rate is controlled to be 0.5-5 ℃/min, so as to prepare the microwave ferrite.
2. The high dielectric constant, high curie temperature, low loss microwave ferrite material of claim 1, wherein: the raw material magnetic powder in the step S1 is oxide, specifically Bi 2 O 3 、CaCO 3 Or CaO, Y 2 O 3 、ZrO 2 、SnO 2 、In 2 O3、Ta 2 O 5 、Fe 2 O 3 。
3. The high dielectric constant, high curie temperature, low loss microwave ferrite material of claim 1, wherein: the ball milling time in the step S2 is 1-10 h, the ball milling speed is 150-250 r/min, and the direction is changed every 30 min.
4. The high dielectric constant, high curie temperature, low loss microwave ferrite material of claim 1, wherein: and screening with a 30-200 mesh sieve in the step S3, and screening with a 30-60 mesh sieve in the step S5.
5. The high dielectric constant, high curie temperature, low loss microwave ferrite material of claim 1, wherein: the secondary ball milling time in the step S5 is 4-30 hours, and the average particle size of the ball milling material is controlled to be 0.9-1.6 mu m.
6. The high dielectric constant, high curie temperature, low loss microwave ferrite material of claim 1, wherein: the binder in the step S6 is 5-12% PVA glue.
7. The high dielectric constant, high curie temperature, low loss microwave ferrite material of claim 1, wherein: the sintering process in the step S7 specifically includes the following steps:
(1) And (3) heating: the temperature rise is slower at 0-500 ℃ and is 1 ℃/min;
(2) And (3) heat preservation: preserving heat at 500 ℃ for 360min;
(3) And a cooling stage, namely cooling the temperature from 1450 ℃ to 1200 ℃, wherein the cooling rate is 2 ℃/min.
8. A high dielectric constant, high curie temperature, low loss microwave ferrite material according to any of claims 1-8, characterized in that: the chemical formula of the microwave ferrite is Bi a Ca b Y (3-a-b) Zr c Sn d In e Ta f Fe (5-c-d-e-f-δ) O 12 Wherein a is more than or equal to 0.6 and less than or equal to 1.6,0.1 and less than or equal to 1.0, c is more than or equal to 0 and less than or equal to 0.4, d is more than or equal to 0 and less than or equal to 0.4, e is more than or equal to 0 and less than or equal to 0.4, f is more than or equal to 0 and less than or equal to 0.3, and delta is the iron deficiency considered during ball milling.
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20120133452A1 (en) * | 2010-11-30 | 2012-05-31 | Skyworks Solutions, Inc. | Effective substitutions for rare earth metals in compositions and materials for electronic applications |
| CN102976740A (en) * | 2012-11-14 | 2013-03-20 | 东阳富仕特磁业有限公司 | Production method of garnet microwave ferrite with narrow line width and high dielectric constant |
| CN103649384A (en) * | 2011-06-06 | 2014-03-19 | 天工方案公司 | Rare earth reduced garnet systems and related microwave applications |
| US20140175327A1 (en) * | 2010-11-30 | 2014-06-26 | Skyworks Solutions, Inc. | Effective substitutions for rare earth metals in compositions and materials for electronic applications |
| CN112159218A (en) * | 2020-09-23 | 2021-01-01 | 横店集团东磁股份有限公司 | Preparation method of low-cost high-performance permanent magnetic ferrite material |
| CN112456998A (en) * | 2020-10-28 | 2021-03-09 | 北京无线电测量研究所 | Garnet ferrite material with high dielectric constant and preparation method thereof |
| CN112679204A (en) * | 2020-12-28 | 2021-04-20 | 横店集团东磁股份有限公司 | High-saturation high-dielectric-constant low-linewidth microwave ferrite material and preparation method thereof |
| CN116409988A (en) * | 2023-04-12 | 2023-07-11 | 电子科技大学 | Garnet ferrite material with high dielectric medium saturation magnetization and preparation method thereof |
-
2023
- 2023-07-31 CN CN202310946239.7A patent/CN116854460A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20120133452A1 (en) * | 2010-11-30 | 2012-05-31 | Skyworks Solutions, Inc. | Effective substitutions for rare earth metals in compositions and materials for electronic applications |
| US20140175327A1 (en) * | 2010-11-30 | 2014-06-26 | Skyworks Solutions, Inc. | Effective substitutions for rare earth metals in compositions and materials for electronic applications |
| CN103649384A (en) * | 2011-06-06 | 2014-03-19 | 天工方案公司 | Rare earth reduced garnet systems and related microwave applications |
| CN102976740A (en) * | 2012-11-14 | 2013-03-20 | 东阳富仕特磁业有限公司 | Production method of garnet microwave ferrite with narrow line width and high dielectric constant |
| CN112159218A (en) * | 2020-09-23 | 2021-01-01 | 横店集团东磁股份有限公司 | Preparation method of low-cost high-performance permanent magnetic ferrite material |
| CN112456998A (en) * | 2020-10-28 | 2021-03-09 | 北京无线电测量研究所 | Garnet ferrite material with high dielectric constant and preparation method thereof |
| CN112679204A (en) * | 2020-12-28 | 2021-04-20 | 横店集团东磁股份有限公司 | High-saturation high-dielectric-constant low-linewidth microwave ferrite material and preparation method thereof |
| CN116409988A (en) * | 2023-04-12 | 2023-07-11 | 电子科技大学 | Garnet ferrite material with high dielectric medium saturation magnetization and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN118026662A (en) * | 2024-01-24 | 2024-05-14 | 东阳富仕特磁业有限公司 | High-performance microwave ferrite material and preparation method thereof |
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