CN115331907B - Gyromagnetic ferrite material applied to high-power microwave device and preparation method thereof - Google Patents
Gyromagnetic ferrite material applied to high-power microwave device and preparation method thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 70
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 238000000498 ball milling Methods 0.000 claims abstract description 58
- 239000002994 raw material Substances 0.000 claims abstract description 52
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 46
- 238000005245 sintering Methods 0.000 claims abstract description 28
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 24
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- 238000003825 pressing Methods 0.000 claims abstract description 19
- 238000000227 grinding Methods 0.000 claims abstract description 18
- 239000000203 mixture Substances 0.000 claims abstract description 17
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 15
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- 239000000126 substance Substances 0.000 claims abstract description 10
- 229910018626 Al(OH) Inorganic materials 0.000 claims abstract description 9
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- 238000005303 weighing Methods 0.000 claims abstract description 9
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 5
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/10—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials non-metallic substances, e.g. ferrites, e.g. [(Ba,Sr)O(Fe2O3)6] ferrites with hexagonal structure
- H01F1/11—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials non-metallic substances, e.g. ferrites, e.g. [(Ba,Sr)O(Fe2O3)6] ferrites with hexagonal structure in the form of particles
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/0302—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity characterised by unspecified or heterogeneous hardness or specially adapted for magnetic hardness transitions
- H01F1/0311—Compounds
- H01F1/0313—Oxidic compounds
- H01F1/0315—Ferrites
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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
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Abstract
The invention provides a preparation method of gyromagnetic ferrite material applied to a high-power microwave device, which uses Fe 2 O 3 、Y 2 O 3 、Gd 2 O 3 、Dy 2 O 3 、V 2 O 5 、ZrO 2 、Al(OH) 3 、CaCO 3 、MnCO 3 Calculating the mass ratio of each raw material according to a chemical formula, and weighing the raw materials; putting the weighed raw materials into a stainless steel ball grinding tank, adding a proper amount of steel balls and absolute ethyl alcohol, sealing the ball grinding tank, and ball-milling; after ball milling the mixed raw materials for one time, drying absolute ethyl alcohol, pressing the mixed raw materials into a round cake, and presintering in a high-temperature electric furnace; crushing the presintered mixture, putting the crushed mixture into a stainless steel ball milling tank, adding a proper amount of steel balls and absolute ethyl alcohol, sealing and ball milling; drying the mixed powder after the second ball milling, and adding a polyvinyl alcohol solution for granulating; pressing into a green body; placing the green body into a high-temperature electric furnace, introducing oxygen and sintering.
Description
Technical Field
The invention belongs to the technical field of electronic ceramic materials, and particularly relates to a gyromagnetic ferrite material applied to a high-power microwave device and a preparation method thereof.
Background
Ferrite is a nonmetallic magnetic material, typically a composite oxide of iron and other metallic elements. The resistivity rho of ferrite can reach 10 2 ～10 11 Omega cm. In terms of dielectric properties, the dielectric constant is generally 8 to 16, and the dielectric loss tangentCan generally reach 10 -3 ～10 -4 The saturation magnetization 4 pi Ms is generally in the range of 200 to 5500Gauss and the Curie temperature is generally in the range of 100 to 600 ℃. Ferrite can be classified into three types according to crystal structure: spinel type, garnet type and magnetoplumbite type. Ferrite can be classified into five types according to its characteristics and uses: soft magnetic ferrite, hard magnetic ferrite, gyromagnetic ferrite, rectangular magnetic ferrite and piezomagnetic ferrite. Gyromagnetic ferrite material, other soft magnetic, hard magnetic, etcFerrite materials are different, and other magnetic materials generally work by utilizing the characteristic of magnetism; the gyromagnetic ferrite material does not show magnetism, and under the action of an external magnetic field, the gyromagnetic ferrite material shows tensor magnetic permeability, ferromagnetic resonance, faraday rotation, field shift effect and other characteristics on a microwave signal, and various microwave magnetic devices with excellent performances, such as an isolator, a circulator, an electric control phase shifter, an electric control switch, a polarization transformer, an electric modulation filter, an oscillator, a delay line and the like, can be manufactured by utilizing the characteristics. The garnet-type gyromagnetic ferrite material is one of the indispensable magnetic materials used in a large number of domestic and foreign military and civil electronic equipment in the current and future for a long time, has excellent performances of low loss, high resistivity, narrow resonance line width and the like in a microwave frequency band, and has extremely high application value.
The microwave circulator/isolator works in the range of-55 ℃ to +85 ℃ generally, so that gyromagnetic ferrite materials used for the circulator/isolator are required to keep good performance in a wider temperature range. In practical application, there are many garnet gyromagnetic ferrite materials, their saturation magnetization (4pi Ms) changes greatly along with the change of temperature, especially in high-power microwave devices, not only the saturation magnetization of ferrite is affected by the change of ambient temperature, but also the heat productivity of the ferrite material is larger because the working power of the device is larger, and the heat dissipation rate of the ferrite substrate is not faster than that of an externally applied magnetic field because the ferrite substrate is positioned near the center of the microwave device, so that the temperature of the ferrite material is higher than that of the externally applied magnetic field, the change amplitude of 4pi Ms of the ferrite material is always larger than that of the externally applied magnetic field, and at the moment, the saturation magnetization of the ferrite substrate in the circulator/isolator changes greatly, thereby deteriorating the performance index of the circulator/isolator.
For a high-power microwave device, not only the saturation magnetization intensity of ferrite is affected by the change of the ambient temperature, but also the heating value of the ferrite material is larger due to the larger working power of the device, and the temperature of the ferrite substrate is higher than the temperature of an externally-applied magnetic field due to the fact that the ferrite substrate is positioned near the center of the microwave device, so that the change amplitude of 4pi Ms of the ferrite material is always larger than the change amplitude of the intensity of the externally-applied magnetic field.
Disclosure of Invention
The invention aims to solve the problems in the prior art, and provides a gyromagnetic ferrite material applied to a high-power microwave device and a preparation method thereof.
A preparation method of gyromagnetic ferrite material applied to a high-power microwave device comprises the following steps:
step one: by Fe 2 O 3 、Y 2 O 3 、Gd 2 O 3 ，Dy 2 O 3 ，V 2 O 5 ，ZrO 2 ，Al(OH) 3 ，CaCO 3 、MnCO 3 As raw material according to the chemical formula Y 2.54-x-y-z Ca x+0.46 Gd z Dy y V 0.23 Zr x Al 0.2 Mn 0.03 Fe 4.54-x-δ O 12 Calculating the mass ratio of the raw materials, wherein x is more than or equal to 0.1 and less than or equal to 0.3, y is more than or equal to 0 and less than or equal to 0.1,0.1, z is more than or equal to 0 and less than or equal to 0.4,is iron deficiency and is less than or equal to 0.15%>Weighing according to the calculated mass ratio, wherein the mass ratio is less than or equal to 0.25;
step two: putting the weighed raw materials into a stainless steel ball grinding tank, adding a proper amount of steel balls and absolute ethyl alcohol, sealing the ball grinding tank, and putting the ball grinding tank on a roller ball mill for ball grinding to obtain powder after primary ball grinding;
step three: after the mixed raw materials are ball-milled for one time, the absolute ethyl alcohol is dried, the mixed raw materials are pressed into round cakes, the round cakes are presintered in a high-temperature electric furnace, the presintered temperature of the high-temperature electric furnace is 1130-1180 ℃, and the heat preservation time is 4-6 hours;
step four: crushing the presintered mixture, putting the crushed mixture into a stainless steel ball milling tank, adding a proper amount of steel balls and absolute ethyl alcohol, sealing, and putting the mixture on a roller ball mill for ball milling for 20-28 hours;
step five: drying the mixed powder after the second ball milling, adding a proper amount of polyvinyl alcohol solution for granulating;
step six: pressing the material into a green body with a certain shape and size according to the device requirement, wherein the pressing pressure is 30-80 MPa;
step seven: placing the green body into a high-temperature electric furnace, introducing oxygen, sintering at 1340-1390 ℃, and preserving heat at the sintering temperature for 5-8 hours.
Further, in the first step, raw materials are weighed by adopting an iron-deficiency formula, the purity of the raw materials is not lower than 99.95%, and the iron deficiency of the formula is 0.15-0.25.
Further, the ball milling time of the ball milling tank on the roller ball mill in the second step is 16-24 hours, the weight ratio of the added raw materials to the steel balls is 1:1.5-1:2.8, and the weight ratio of the added raw materials to the absolute ethyl alcohol is 1:0.8-1:1.4.
Further, the rotation speed of the ball milling tank is 90-130 rpm.
Further, before the powder material dried by the absolute ethyl alcohol in the third step is pressed into a cake, a proper amount of deionized water is added, the amount of the added deionized water is 12-20% of the mass of the raw material, and the mixture is uniformly stirred and then pressed.
Further, in the fourth step, the diameter of the crushed material block of the mixture is smaller than 8mm, and the weight ratio of the added crushed material block to the steel ball is 1: 1.5-1:2.8, the weight ratio of the crushed material blocks to the absolute ethyl alcohol is 1:0.6-1:1, and the rotating speed of the ball milling tank is 90-130 r/min.
Further, the concentration of the polyvinyl alcohol solution in the fifth step is 5wt%, and the mass of the added PVA solution is 7-15% of the mass of the mixed powder after secondary ball milling.
Further, the electric furnace sintering method in the step seven is as follows:
step one: the temperature rising process is room temperature to 400 ℃, and the temperature rising rate is 1.5 ℃/min;
step two: the temperature rising process is 400-600 ℃, and the temperature rising rate is 1 ℃/min;
step three: the temperature rise process is 600-1200 ℃, and the temperature rise rate is 3 ℃/min;
step four: the temperature rise process is 1200-sintering temperature, the temperature rise rate is 1.5 ℃/min, and the sintering temperature is 1340-1390 ℃;
step five: the heat preservation process is kept at the sintering temperature for 5 to 8 hours;
step six: the temperature reduction process is that the sintering temperature is between 1200 ℃ and the temperature reduction rate is 2 ℃/min;
step seven: the temperature reduction process is 1200-room temperature.
Further, in the seventh step, the temperature is reduced from 1200 ℃ to room temperature in a natural temperature reduction mode.
The beneficial effects of the invention are as follows:
the product adopts a compound ion substitution technology, designs the formula of the ferrite material, and is matched with a solid phase reaction preparation process, so that the produced gyromagnetic ferrite material has the advantages of smaller temperature coefficient, smaller ferromagnetic resonance line width and higher temperature stability and smaller loss under the high-power condition;
the temperature coefficient is smaller between-55 ℃ and +85 ℃, the ferromagnetic resonance line width delta H is small, and the ferrite material can be applied to ferrite materials of high-power microwave devices, so that the high-power circulator/isolator can keep stable performance indexes.
Drawings
The accompanying drawings are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate the invention and together with the embodiments of the invention, serve to explain the invention. In the drawings:
FIG. 1 is a temperature profile of a ferrite material sintering process in a fifth embodiment of the present invention;
FIG. 2 is a flow chart of the production process of the present invention;
FIG. 3 is a graph of a related parameter of a comparative example of the present invention;
FIG. 4 is a graph of a comparative example II related parameter of the present invention;
FIG. 5 is a graph of comparative example three related parameters of the present invention;
FIG. 6 is Y of the present invention 3 Fe 5 O 12 A graph of saturation magnetization as a function of temperature;
FIG. 7 is a graph of related parameters according to an embodiment of the present invention;
FIG. 8 is a graph of related parameters for an embodiment of the present invention;
FIG. 9 is a graph of related parameters according to an embodiment of the present invention;
FIG. 10 is a graph of four related parameters of an embodiment of the present invention;
FIG. 11 is a graph of a fifth related parameter of an embodiment of the present invention;
FIG. 12 is an X-ray diffraction pattern of a sample according to an embodiment of the present invention;
FIG. 13 is an X-ray diffraction pattern of a second sample of the present invention;
FIG. 14 is an X-ray diffraction pattern of a third sample of the present invention;
FIG. 15 is an X-ray diffraction pattern of a fourth sample of the present invention;
FIG. 16 is an X-ray diffraction pattern of a fifth sample of the present invention.
Detailed Description
Example 1
As shown in fig. 2, a preparation method of gyromagnetic ferrite material applied to a high-power microwave device comprises the following steps:
step one: by Fe 2 O 3 、Y 2 O 3 、Gd 2 O 3 ，Dy 2 O 3 ，V 2 O 5 ，ZrO 2 ，Al(OH) 3 ，CaCO 3 、MnCO 3 As raw material according to the chemical formula Y 2.54-x-y-z Ca x+0.46 Gd z Dy y V 0.23 Zr x Al 0.2 Mn 0.03 Fe 4.54-x-δ O 12 Calculating the mass ratio of the raw materials, wherein x is more than or equal to 0.1 and less than or equal to 0.3, y is more than or equal to 0 and less than or equal to 0.1,0.1, z is more than or equal to 0 and less than or equal to 0.4,in order to achieve the iron deficiency amount,and is not less than 0.15%>Weighing according to the calculated mass ratio, wherein the mass ratio is less than or equal to 0.25;
step two: putting the weighed raw materials into a stainless steel ball grinding tank, adding a proper amount of steel balls and absolute ethyl alcohol, sealing the ball grinding tank, putting the ball grinding tank on a roller ball mill for ball grinding, and obtaining powder after primary ball grinding, wherein the rotating speed of the ball grinding tank is 90-130 r/min;
step three: after the mixed raw materials are ball-milled for one time, the absolute ethyl alcohol is dried, the mixed raw materials are pressed into round cakes, the round cakes are presintered in a high-temperature electric furnace, the presintered temperature of the high-temperature electric furnace is 1130-1180 ℃, and the heat preservation time is 4-6 hours;
step four: crushing the presintered mixture, putting the crushed mixture into a stainless steel ball milling tank, adding a proper amount of steel balls and absolute ethyl alcohol, sealing, and putting the mixture on a roller ball mill for ball milling for 20-28 hours;
step five: drying the mixed powder after the second ball milling, adding a proper amount of polyvinyl alcohol solution for granulating;
step six: pressing the material into a green body with a certain shape and size according to the device requirement, wherein the pressing pressure is 30-80 MPa;
step seven: placing the green body into a high-temperature electric furnace, introducing oxygen, sintering at 1340-1390 ℃ for 5-8 hours.
In the first step, raw materials are weighed by adopting an iron-deficiency formula, the purity of the raw materials is not lower than 99.95 percent, and the iron deficiency of the formula is 0.15 to 0.25.
In the second step, the ball milling time of the ball milling tank on the roller ball mill is 16-24 hours, the weight ratio of the added raw materials to the steel balls is 1:1.5-1:2.8, and the weight ratio of the added raw materials to the absolute ethyl alcohol is 1:0.6-1:1.
And thirdly, adding a proper amount of deionized water into the powder after the absolute ethyl alcohol is dried before the powder is pressed into a cake, wherein the amount of the added deionized water is 12-20% of the mass of the raw materials, uniformly stirring, and then pressing.
In the fourth step, the diameter of the crushed material block of the mixture is smaller than 8mm, and the weight ratio of the added crushed material block to the steel ball is 1: 1.5-1:2.8, the weight ratio of the crushed material blocks to the absolute ethyl alcohol is 1:0.6-1:1, and the rotating speed of the ball milling tank is 90-130 r/min.
In the fifth step, the concentration of the polyvinyl alcohol solution is 5wt%, and the mass of the added PVA solution is 7-15% of the mass of the mixed powder after secondary ball milling.
As shown in fig. 1, the electric furnace sintering method is as follows:
step one: the temperature rising process is room temperature to 400 ℃, and the temperature rising rate is 1.5 ℃/min;
step two: the temperature rising process is 400-600 ℃, and the temperature rising rate is 1 ℃/min;
step three: the temperature rise process is 600-1200 ℃, and the temperature rise rate is 3 ℃/min;
step four: the temperature rise process is 1200-sintering temperature, the temperature rise rate is 1.5 ℃/min, and the sintering temperature is 1340-1390 ℃;
step five: the heat preservation process is kept at the sintering temperature for 5 to 8 hours;
step six: the temperature reduction process is that the sintering temperature is between 1200 ℃, the temperature reduction rate is 2 ℃/min, and the temperature reduction speed is controlled, so that the performance of the material is improved;
step seven: the temperature reduction process is 1200-room temperature, and the sintering temperature is reduced from 1200 ℃ to room temperature by adopting a natural temperature reduction mode.
With chemical formula Y 3 Fe 5 O 12 For example, the garnet type ferrite material has the 4 pi Ms value of 2020 Gauss at the temperature of minus 55 ℃ and has the 4 pi Ms value of 1510 Gauss at the temperature of +85 ℃, the decreasing amplitude of 25 percent, and the curve of the 4 pi Ms changing along with the temperature is shown as figure 6;
rotary magnet oxygen applied to high-power deviceThe bulk material, in actual operation, often exhibits a large insertion loss, the ferromagnetic resonance linewidth of the gyromagnetic ferrite materialClosely related to insertion loss, so material +.>The magnitude of the insertion loss in practical applications can be shown.
The current gyromagnetic ferrite material is prepared from the raw materials of the composite material,small, cannot tolerate high power, cannot be applied to high power devices; material for high-power devices, which is +.>The value is generally large, often reaching 100 +.>The above.
To express the intensity of saturation magnetization 4pi Ms along with the change of temperature T, a temperature coefficient is usedTo characterize the temperature stability of the saturation magnetization of the ferrite material:
wherein (4pi Ms) max AND (4pi Ms) min Respectively the maximum value and the minimum value of 4pi Ms in the interval of the temperature T1 to T2; (4 pi Ms) rt The 4 pi MS values at room temperature are shown.
From the above equation, the smaller the value of the temperature coefficient, the better the temperature stability of the material.
In the chemical formula, x=0.1, y=0, z=0.1,=0.15, calculated Fe according to total mass 2kg 2 O 3 、Y 2 O 3 、Gd 2 O 3 ，Dy 2 O 3 ，V 2 O 5 ，ZrO 2 ，Al(OH) 3 ，CaCO 3 、MnCO 3 The dosage of each raw material;
accurately weighing raw materials, putting the raw materials into a ball milling tank, performing wet ball milling, and taking absolute ethyl alcohol as a dispersing agent to obtain powder: steel ball: mixing and ball milling the raw materials for 20 hours, wherein the mass ratio of the absolute ethyl alcohol is 1:2:0.6;
after uniform mixing, drying absolute ethyl alcohol, adding 300g of deionized water into the dried powder, uniformly mixing, and pressing into a cake on a hydraulic press under the pressure of about 10MPa;
presintering the pressed round cakes in a high-temperature furnace to 1140 ℃, and preserving heat for 5 hours;
crushing the presintered round cakes, wherein the particle size of the crushed presintered material is smaller than 8mm;
filling the crushed presintered materials into a ball milling tank for secondary ball milling, and obtaining powder materials: steel ball: the mass ratio of the absolute ethyl alcohol is 1:2:0.6; secondary ball milling for 24 hours, pouring out feed liquid and drying alcohol;
adding 200g of PVA solution with the concentration of 5wt% into the dried powder, granulating, and then pressing into a green body with the diameter of 13.5mm, wherein the pressure applied to the green body is 50MPa when the green body is pressed;
and (3) putting the pressed green body into a high-temperature furnace, heating to 1350 ℃, and preserving heat for 6 hours.
Analysis of sample phase composition by X-ray powder diffractometer, measurement of 4 pi Ms, T of product by vibrating sample magnetic field meter c And 4 pi Ms-T curve at minus 60 ℃ to plus 120 ℃, dielectric constant of the sample is measured at 8-12 GHz by using dielectric column resonance method r And dielectric loss->Measuring the line width of ferromagnetic resonance by waveguide resonant cavity perturbation method at 9.5GHz>。
Comparative example one:
as shown in fig. 3, according to the 4 pi Ms-T curve disclosed in the comparative example, it was measured that (4 pi Ms) max=1236 Gauss, (4 pi Ms) min=1137 Gauss, the disclosed room temperature saturation magnetization was 1200Guass, and the above data was calculated by substituting the above data into the formula, the comparative example one was between-55 ℃ and +85 ℃, 4πMs =5.89*10-4。
comparative example two:
as shown in fig. 4, according to the 4 pi Ms-T curve disclosed in the comparative example two, it was measured that (4 pi Ms) max=1236 Gauss, (4 pi Ms) min=1129 Gauss, the disclosed room temperature saturation magnetization was 1200Guass, and the above data was calculated by substituting the above data into the formula, the comparative example two was between-55 ℃ and +85 ℃, 4πMs =6.37*10-4。
comparative example three:
as shown in fig. 5, according to the 4 pi Ms-T curve disclosed in the comparative example three, it was measured that the (4 pi Ms) max=1304 Gauss, (4 pi Ms) min=1132 Gauss, the disclosed room temperature saturation magnetization was 1250Guass, and the above data was substituted into the formula, and the comparative example three was calculated between-55 ℃ and +85 ℃, 4πMs =9.83*10-4。
embodiment one:
as shown in fig. 7 and 12, 4pi ms=1200 Gauss for the sample at-55 ℃ and 4pi ms=1128 Gauss for the sample at +85 ℃ and 4pi ms=1200 Gauss for the sample at room temperature (25 ℃) were obtained by substituting the above data into the formula, the temperature coefficient of ferrite in example one 4πMs =5.48*10-4。
The performance of example one versus the other comparative examples is as follows:
as can be seen from the above table and FIG. 3, comparative example one is a published product of SKYWORKS corporation and is assigned the designation G1001;
as can be seen from the above table and FIG. 4, comparative example II is a product of the company SKYWORKS and has a brand name of G4257;
as can be seen from the above table and FIG. 5, comparative example III is a product of the company Charcroft Electronics (original TEMEX CERAMICS) and is assigned the designation Y13.
The sintered samples of example one were tested with the remaining properties: curie temperature T C Dielectric constant=261 ℃, dielectric loss tangent=14.6, dielectric loss tangent=0.0002, all measured at room temperature.
Example two
In the chemical formula, x=0.2, y=0, z=0.3,=0.16, calculated Fe according to total mass 2kg 2 O 3 、Y 2 O 3 、Gd 2 O 3 ，Dy 2 O 3 ，V 2 O 5 ，ZrO 2 ，Al(OH) 3 ，CaCO 3 、MnCO 3 The dosage of each raw material;
accurately weighing raw materials, putting the raw materials into a ball milling tank, performing wet ball milling, and taking absolute ethyl alcohol as a dispersing agent to obtain powder: steel ball: mixing and ball milling the raw materials for 20 hours according to the mass ratio of the absolute ethyl alcohol of 1:2:0.6;
after uniform mixing, drying absolute ethyl alcohol, adding 300g of deionized water into the dried powder, uniformly mixing, and pressing into a cake on a hydraulic press under the pressure of about 10MPa;
presintering the pressed round cakes in a high-temperature furnace to 1160 ℃, and preserving heat for 5 hours;
crushing the presintered round cakes, wherein the particle size of the crushed presintered material is smaller than 8mm;
filling the crushed presintered materials into a ball milling tank for secondary ball milling, and obtaining powder materials: steel ball: the mass ratio of the absolute ethyl alcohol is 1:2:0.6; secondary ball milling for 24 hours, pouring out feed liquid and drying alcohol;
adding 200g of PVA solution with the concentration of 5wt% into the dried powder, granulating, and then pressing into a green body with the diameter of 13.5mm, wherein the pressure applied to the green body is 50MPa when the green body is pressed;
and (3) putting the pressed green body into a high-temperature furnace, heating to 1370 ℃, and preserving heat for 6 hours.
As shown in fig. 8 and 13, 4pi ms=1222 Gauss for the sample at-55 ℃ and 4pi ms=1134 Gauss for the sample at +85 ℃ and 4pi ms=1200 Gauss for the sample at room temperature (25 ℃) are obtained by substituting the above data into the formula, and the temperature coefficient of ferrite in the second example is obtained 4πMs =5.24*10-4。
The performance of example two versus the other comparative examples is compared as follows:
the sample after sintering in the second embodiment is tested, and the rest performances are as follows: curie temperature T C Dielectric constant of =235℃=14.7, dielectric loss tangent +.>=0.0003。
Example III
In the chemical formula, taking x=0.2, y=0.1, z=0.1, δ=0.18, fe is calculated from the total mass of 2kg 2 O 3 、Y 2 O 3 、Gd 2 O 3 ，Dy 2 O 3 ，V 2 O 5 ，ZrO 2 ，Al(OH) 3 ，CaCO 3 、MnCO 3 The dosage of each raw material;
accurately weighing raw materials, putting the raw materials into a ball milling tank, performing wet ball milling, and taking absolute ethyl alcohol as a dispersing agent to obtain powder: steel ball: mixing and ball milling the raw materials for 20 hours according to the mass ratio of the absolute ethyl alcohol of 1:2:0.7;
after uniform mixing, drying absolute ethyl alcohol, adding 300g of deionized water into the dried powder, uniformly mixing, and pressing into a cake on a hydraulic press under the pressure of about 10MPa;
presintering the pressed round cakes in a high-temperature furnace to 1150 ℃, and preserving heat for 5 hours;
crushing the presintered round cakes, wherein the particle size of the crushed presintered material is smaller than 8mm;
filling the crushed presintered materials into a ball milling tank for secondary ball milling, and obtaining powder materials: steel ball: the mass ratio of the absolute ethyl alcohol is 1:2:0.7, the secondary ball milling is carried out for 24 hours, the feed liquid is poured out, and the alcohol is dried;
adding 200g of PVA solution with the concentration of 5wt% into the dried powder, granulating, and then pressing into a green body with the diameter of 13.5mm, wherein the pressure applied to the green body is 50MPa when the green body is pressed;
and (3) putting the pressed green body into a high-temperature furnace, heating to 1360 ℃, and preserving heat for 6 hours.
As shown in fig. 9 and 14, 4pi ms=1250 Gauss for the sample at-55 ℃, 4pi ms=1162 Gauss for the sample at +85 ℃, 4pi ms=1230 Gauss for the sample at room temperature (25 ℃) are obtained by substituting the above data into the formula, and the temperature coefficient of ferrite in the third embodiment is obtained 4πMs =5.11*10-4。
The performance of example three versus the other comparative examples is compared as follows:
the sample after sintering in example three was tested, and the remaining properties were: curie temperature T C Dielectric constant of =236℃=14.5, dielectricLoss tangent +.>=0.0002。
Example IV
In the chemical formula, taking x=0.2, y=0.05, z=0.2, δ=0.20, fe is calculated according to the total mass of 2kg 2 O 3 、Y 2 O 3 、Gd 2 O 3 ，Dy 2 O 3 ，V 2 O 5 ，ZrO 2 ，Al(OH) 3 ，CaCO 3 、MnCO 3 The dosage of each raw material;
accurately weighing raw materials, putting the raw materials into a ball milling tank, performing wet ball milling, and taking absolute ethyl alcohol as a dispersing agent to obtain powder: steel ball: mixing and ball milling the raw materials for 20 hours according to the mass ratio of the absolute ethyl alcohol of 1:2:0.8;
after uniform mixing, drying absolute ethyl alcohol, adding 300g of deionized water into the dried powder, uniformly mixing, pressing into round cakes on a hydraulic press under the pressure of about 10MPa, presintering the pressed round cakes in a high-temperature furnace to 1160 ℃, and preserving heat for 5 hours;
crushing the presintered round cakes, wherein the particle size of the crushed presintered material is smaller than 8mm;
filling the crushed presintered materials into a ball milling tank for secondary ball milling, and obtaining powder materials: steel ball: the mass ratio of the absolute ethyl alcohol is 1:2:0.8, the secondary ball milling is carried out for 24 hours, the feed liquid is poured out, and the alcohol is dried;
adding 200g of PVA solution with the concentration of 5wt% into the dried powder, granulating, and then pressing into a green body with the diameter of 13.5mm, wherein the pressure applied to the green body is 50MPa when the green body is pressed;
and (3) putting the pressed green body into a high-temperature furnace, heating to 1370 ℃, and preserving heat for 6 hours.
As shown in fig. 10 and 15, 4pi ms=1230 Gauss for the sample at-55 ℃ and 4pi ms=1147 Gauss for the sample at +85 ℃ and 4pi ms=1210 Gauss for the sample at room temperature (25 ℃) were obtained by substituting the above data into the formula, and the temperature coefficient of ferrite in example four was obtained 4πMs =4.90*10-4。
The performance of example four versus the other comparative examples is compared as follows:
the sample after sintering in example four was tested, and the remaining properties were: curie temperature T C Dielectric constant of =235℃=14.6, dielectric loss tangent +.>=0.0002。
Example five
In the chemical formula, taking x=0.25, y=0.08, z=0.3, δ=0.21, fe is calculated according to the total mass of 2kg 2 O 3 、Y 2 O 3 、Gd 2 O 3 ，Dy 2 O 3 ，V 2 O 5 ，ZrO 2 ，Al(OH) 3 ，CaCO 3 、MnCO 3 The dosage of each raw material;
accurately weighing raw materials, putting the raw materials into a ball milling tank, performing wet ball milling, and taking absolute ethyl alcohol as a dispersing agent to obtain powder: steel ball: mixing and ball milling the raw materials for 20 hours according to the mass ratio of the absolute ethyl alcohol of 1:2:0.8;
after uniform mixing, drying absolute ethyl alcohol, adding 300g of deionized water into the dried powder, uniformly mixing, and pressing into a cake on a hydraulic press under the pressure of about 10MPa;
presintering the pressed round cakes in a high-temperature furnace to 1170 ℃, and preserving heat for 5 hours;
crushing the presintered round cakes, wherein the particle size of the crushed presintered material is smaller than 8mm;
filling the crushed presintered materials into a ball milling tank for secondary ball milling, and obtaining powder materials: steel ball: the mass ratio of the absolute ethyl alcohol is 1:2:0.8, the secondary ball milling is carried out for 24 hours, the feed liquid is poured out, and the alcohol is dried;
adding 200g of PVA solution with the concentration of 5wt% into the dried powder, granulating, and then pressing into a green body with the diameter of 13.5mm, wherein the pressure applied to the green body is 50MPa when the green body is pressed;
and (3) putting the pressed green body into a high-temperature furnace, heating to 1380 ℃, and preserving heat for 6 hours.
As shown in fig. 11 and 16, 4pi ms=1220 Gauss for the sample at-55 ℃, 4pi ms=1144 Gauss for the sample at +85 ℃, 4pi ms=1200 Gauss for the sample at room temperature (25 ℃) are obtained by substituting the above data into the formula, and the temperature coefficient of ferrite in the fifth embodiment is obtained 4πMs =4.52*10-4。
The performance of example five compared to other comparative examples is as follows:
the sample after sintering in example five was tested, and the remaining properties were: curie temperature T C Dielectric constant of =222℃=14.5, dielectric loss tangent +.>=0.0005。
The foregoing description is only a preferred embodiment of the present invention, and the present invention is not limited thereto, but it is to be understood that modifications and equivalents of some of the technical features described in the foregoing embodiments may be made by those skilled in the art, although the present invention has been described in detail with reference to the foregoing embodiments. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. The preparation method of the gyromagnetic ferrite material applied to the high-power microwave device is characterized by comprising the following steps of:
step one: by Fe 2 O 3 、Y 2 O 3 、Gd 2 O 3 ，Dy 2 O 3 ，V 2 O 5 ，ZrO 2 ，Al(OH) 3 ，CaCO 3 、MnCO 3 As raw material according to the chemical formula Y 2.54-x-y-z Ca x+0.46 Gd z Dy y V 0.23 Zr x Al 0.2 Mn 0.03 Fe 4.54-x-δ O 12 Calculating the mass ratio of the raw materials, wherein x is more than or equal to 0.1 and less than or equal to 0.3, y is more than or equal to 0 and less than or equal to 0.1,0.1, z is more than or equal to 0 and less than or equal to 0.4,is iron deficiency and is less than or equal to 0.15%>Weighing according to the calculated mass ratio, wherein the mass ratio is less than or equal to 0.25;
step two: putting the weighed raw materials into a stainless steel ball grinding tank, adding a proper amount of steel balls and absolute ethyl alcohol, sealing the ball grinding tank, and putting the ball grinding tank on a roller ball mill for ball grinding to obtain powder after primary ball grinding;
step three: after the mixed raw materials are ball-milled for one time, the absolute ethyl alcohol is dried, the mixed raw materials are pressed into round cakes, the round cakes are presintered in a high-temperature electric furnace, the presintered temperature of the high-temperature electric furnace is 1130-1180 ℃, and the heat preservation time is 4-6 hours;
step four: crushing the presintered mixture, putting the crushed mixture into a stainless steel ball milling tank, adding a proper amount of steel balls and absolute ethyl alcohol, sealing, and putting the mixture on a roller ball mill for ball milling for 20-28 hours;
step five: drying the mixed powder after the second ball milling, adding a proper amount of polyvinyl alcohol solution for granulating;
step six: pressing the material into a green body with a certain shape and size according to the device requirement, wherein the pressing pressure is 30-80 MPa;
step seven: placing the green body into a high-temperature electric furnace, introducing oxygen, sintering at 1340-1390 ℃ for 5-8 hours at the sintering temperature.
2. The method for preparing gyromagnetic ferrite material for high-power microwave devices as claimed in claim 1, wherein the raw materials are weighed according to the iron-deficiency formula in the first step, the purity of the raw materials is not lower than 99.95%, and the iron deficiency of the formula is 0.15-0.25.
3. The method for preparing gyromagnetic ferrite material for high-power microwave devices according to claim 1, wherein the ball milling time of the ball milling tank on the roller ball mill in the second step is 16-24 hours, the weight ratio of the added raw materials to the steel balls is 1:1.5-1:2.8, and the weight ratio of the added raw materials to the absolute ethyl alcohol is 1:0.8-1:1.4.
4. The method for preparing gyromagnetic ferrite material for high-power microwave devices as claimed in claim 1, wherein in the second step, the rotation speed of the ball milling tank is 90-130 rpm.
5. The method for preparing gyromagnetic ferrite material for high-power microwave devices as claimed in claim 1, wherein the powder material after drying absolute ethyl alcohol in the third step is added with a proper amount of deionized water before being pressed into a cake, and the amount of the added deionized water is 12% -20% of the mass of the raw material, and the mixture is stirred uniformly and then pressed.
6. The method for preparing gyromagnetic ferrite material for high-power microwave devices as claimed in claim 1, wherein the diameter of the broken material block of the mixture in the fourth step is less than 8mm, and the weight ratio of the broken material block to the steel ball is 1: 1.5-1:2.8, the weight ratio of the crushed material blocks to the absolute ethyl alcohol is 1:0.6-1:1, and the rotating speed of the ball milling tank is 90-130 r/min.
7. The method for preparing gyromagnetic ferrite material for high-power microwave devices as claimed in claim 1, wherein the concentration of the polyvinyl alcohol solution in the fifth step is 5wt%, and the mass of the added PVA solution is 7% -15% of the mass of the mixed powder after secondary ball milling.
8. The method for preparing gyromagnetic ferrite material for high-power microwave devices as claimed in claim 1, wherein the electric furnace sintering method in the seventh step is:
step one: the temperature rising process is room temperature to 400 ℃, and the temperature rising rate is 1.5 ℃/min;
step two: the temperature rising process is 400-600 ℃, and the temperature rising rate is 1 ℃/min;
step three: the temperature rise process is 600-1200 ℃, and the temperature rise rate is 3 ℃/min;
step four: the temperature rise process is 1200-sintering temperature, the temperature rise rate is 1.5 ℃/min, and the sintering temperature is 1340-1390 ℃;
step five: the heat preservation process is kept at the sintering temperature for 5 to 8 hours;
step six: the temperature reduction process is that the sintering temperature is between 1200 ℃ and the temperature reduction rate is 2 ℃/min;
step seven: the temperature reduction process is 1200-room temperature.
9. The method for preparing gyromagnetic ferrite material for high-power microwave devices as claimed in claim 8, wherein in step seven, the sintering temperature is lowered from 1200 ℃ to room temperature in a natural cooling mode.
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