CN110803921A - Composite microwave ferrite magnetic sheet and preparation method and application thereof - Google Patents
Composite microwave ferrite magnetic sheet and preparation method and application thereof Download PDFInfo
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- CN110803921A CN110803921A CN201911311423.4A CN201911311423A CN110803921A CN 110803921 A CN110803921 A CN 110803921A CN 201911311423 A CN201911311423 A CN 201911311423A CN 110803921 A CN110803921 A CN 110803921A
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- microwave ferrite
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- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 147
- 230000005291 magnetic effect Effects 0.000 title claims abstract description 113
- 239000002131 composite material Substances 0.000 title claims abstract description 81
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000000919 ceramic Substances 0.000 claims abstract description 83
- 238000013329 compounding Methods 0.000 claims abstract description 5
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 31
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 30
- 239000002270 dispersing agent Substances 0.000 claims description 30
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- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 13
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- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 10
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 7
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 6
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical group N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 4
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims description 4
- 229910052593 corundum Inorganic materials 0.000 claims description 4
- 239000011656 manganese carbonate Substances 0.000 claims description 4
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 claims description 4
- FKTOIHSPIPYAPE-UHFFFAOYSA-N samarium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Sm+3].[Sm+3] FKTOIHSPIPYAPE-UHFFFAOYSA-N 0.000 claims description 4
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 4
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 claims description 2
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- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 5
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- UPWOEMHINGJHOB-UHFFFAOYSA-N oxo(oxocobaltiooxy)cobalt Chemical compound O=[Co]O[Co]=O UPWOEMHINGJHOB-UHFFFAOYSA-N 0.000 description 2
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- H01—ELECTRIC ELEMENTS
- H01P—WAVEGUIDES; RESONATORS, LINES, OR OTHER DEVICES OF THE WAVEGUIDE TYPE
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Abstract
The invention provides a composite microwave ferrite magnetic sheet and a preparation method and application thereof. The composite microwave ferrite magnetic sheet comprises a microwave ferrite magnetic sheet and a microwave ceramic dielectric sheet sleeved outside the microwave ferrite magnetic sheet. The preparation method comprises the following steps: (1) preparing microwave ferrite; (2) preparing microwave ceramics; (3) and compounding the microwave ferrite and the microwave ceramic to obtain the composite microwave ferrite magnetic sheet. The composite microwave ferrite magnetic sheet provided by the invention adopts the mode that the microwave ceramic dielectric sheet is sleeved outside the microwave ferrite magnetic sheet, achieves the effect of improving the overall dielectric constant under the condition of not changing the dielectric constant of the microwave ferrite magnetic sheet, has extremely small size and meets the requirement of a 5G base station isolator.
Description
Technical Field
The invention belongs to the technical field of ferrite, and relates to a composite microwave ferrite magnetic sheet, and a preparation method and application thereof.
Background
The circulator/isolator for 5G single communication base station can reach more than 100, and is 8 to 10 times of that of 4G communication base station, the frequency band used by 5G mobile communication is higher, the data transmission rate is faster, the performance and the size of the circulator and the isolator used in the communication base station are correspondingly higher, the performance of the microwave ferrite material used in the circulator and the isolator is also higher, 1, the saturation magnetization (4 n ms) is higher (1800-1950 oe), 2, the ferromagnetic resonance line width (△ H) is narrow, 3, the Curie Temperature (TC) is high, 4, the dielectric constant (epsilon') is high, and 5, the dielectric loss (tan delta epsilon) is low.
Since the number of isolators used in a 5G base station is significantly increased compared to 4G and the number of isolators to be mounted on one substrate is significantly increased, the isolators and the gyromagnetic materials used therefor are required to be significantly reduced in size.
Under the premise of fixed use frequency, the dielectric constant of the gyromagnetic material needs to be improved to reduce the size, and the difficulty of improving the dielectric constant of the YIG gyromagnetic material is very high.
CN107021747A provides a high-temperature co-firing method of microwave ferrite material and microwave dielectric ceramic. The method comprises the following steps: (a) preparing a microwave dielectric ceramic material and a microwave ferrite material; (b) respectively adding an auxiliary agent into a microwave dielectric ceramic material and a microwave ferrite material, then grinding to respectively obtain microwave ceramic dielectric powder and microwave ferrite powder, and controlling the particle size of the obtained powder in the grinding process; (c) preparing a transition layer material; (d) carrying out casting molding, laminating and isostatic pressing on the microwave ceramic dielectric powder, the microwave ferrite powder and the transition layer material to obtain a multilayer heterogeneous ceramic green body; (e) sintering the multilayer heterogeneous ceramic green body by a space limitation method to obtain the multilayer heterogeneous ceramic.
CN107564656A provides a microwave ferrite composite material and a preparation process thereof, the basic formula is BaCO3.0.45Co2O3.1.1ZnO.8Fe2O3The raw material is BaCO3、Co2O3、ZnO、Fe2O3Preparing according to the proportion of each component, preparing microwave ferrite (BaMe) by ball milling, draining, briquetting, sintering, crushing and sieving2Fe16O27Me is a divalent metal ion) powder.
However, the above solutions all have the problem that the dielectric constant of ferrite material is not large enough to reduce the size to meet the requirement of 5G base station isolator.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a composite microwave ferrite magnetic sheet and a preparation method and application thereof. The composite microwave ferrite magnetic sheet provided by the invention achieves the effect of improving the overall dielectric constant under the condition of not changing the dielectric constant of the microwave ferrite magnetic sheet, and meets the requirement of a 5G base station isolator.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the invention provides a composite microwave ferrite magnetic sheet, which comprises a microwave ferrite magnetic sheet and a microwave ceramic dielectric sheet sleeved outside the microwave ferrite magnetic sheet.
The composite microwave ferrite magnetic sheet provided by the invention adopts the mode that the microwave ceramic dielectric sheet is sleeved outside the microwave ferrite magnetic sheet, achieves the effect of improving the overall dielectric constant under the condition of not changing the dielectric constant of the microwave ferrite magnetic sheet, has extremely small size and meets the requirement of a 5G base station isolator.
The principle is that the electromagnetic wave passes through the microwave ceramic dielectric ring (with high dielectric constant), the wavelength of the electromagnetic wave is correspondingly reduced, so that the electromagnetic wavelength incident to the microwave ferrite magnetic sheet is reduced, and the size of the isolator device can be greatly reduced.
The following is a preferred technical solution of the present invention, but not a limitation to the technical solution provided by the present invention, and the technical objects and advantageous effects of the present invention can be better achieved and achieved by the following preferred technical solution.
As the preferable technical scheme of the invention, the microwave ferrite magnetic sheet and the microwave ceramic dielectric sheet are mutually bonded and fixed through the adhesive.
Preferably, the adhesive is glue;
preferably, the microwave ferrite magnetic sheet comprises the following raw materials: fe2O3、Y2O3、CaCO3、ZrO2And MnCO3. Wherein each component has the function of Fe2O3And Y2O3As a base material, they form garnet crystals, wherein Fe is a magnetic element, Y is a non-magnetic element, ZrO2Substituted Fe2O3Playing a role in reducing the magnetic anisotropy constant, MnCO3Substituted Fe2O3Acting to reduce the dielectric constant of the material, CaCO3Has the functions of electricity price compensation and combustion assistance.
Preferably, the microwave ferrite magnetic sheet comprises the following raw materials in parts by weight:
for example, Fe2O3Is 49 parts, 50 parts, 51 parts, 52 parts, 53 parts, 54 parts, 55 parts or 56 parts, etc., Y2O339 parts, 40 parts, 41 parts, 42 parts, 43 parts, 44 parts, 45 parts, 46 parts, 47 parts or 48 parts, CaCO, and the like3Is 0.1 part, 0.3 part, 0.5 part, 0.8 part, 1 part, 1.5 parts, 1.8 parts or 2.1 parts, etc., ZrO20.1 part, 0.3 part, 0.5 part, 0.8 part, 1 part, 1.5 parts, 1.8 parts or 2.1 parts, etc., MnCO30.01 part, 0.05 part, 0.1 part, 0.2 part, 0.3 part, 0.4 part, 0.5 part, etc.
Preferably, the microwave ceramic dielectric sheet comprises the following raw materials: CaCO3、TiO2、Sm2O3、Al2O3And CeO2. Wherein the functions of each component are respectively as follows, wherein Al2O3Being a base component of a ceramic material, TiO2、Sm2O3Functioning to adjust the dielectric constant, CeO2Can optimize the Q value, CaCO of the material3The function of reducing the sintering temperature is achieved.
In the invention, in order to better achieve the purpose of improving the overall dielectric constant to reduce the size of the microwave ceramic dielectric plate to meet the requirement of a 5G device, the dielectric constant of the microwave ceramic dielectric plate is preferably 20-50, the quality factor Qxfo (1GHZ) is more than or equal to 55000, and the temperature coefficient tau f (ppm/DEG C-40-85 ℃) is-6.
Preferably, the microwave ceramic dielectric sheet comprises the following raw materials in parts by weight:
for example, CaCO333 parts, 34 parts, 35 parts, 36 parts, 37 parts or 38 parts of TiO225 parts, 27 parts, 29 parts, 31 parts, 33 parts or 35 parts of Sm2O320, 21, 22, 23, 24, 25, 26, 27 or 28 parts, etc., Al2O3Is 7, 8, 9, 10 or 11 parts of CeO20.2 part, 0.3 part, 0.4 part, 0.5 part, 0.6 part, 0.7 part, 0.8 part and the like.
In a second aspect, the present invention provides a method of preparing a composite microwave ferrite magnetic sheet according to the first aspect, the method comprising the steps of:
(1) preparing microwave ferrite;
(2) preparing microwave ceramics;
(3) and (3) compounding the microwave ferrite obtained in the step (1) with the microwave ceramic obtained in the step (2) to obtain the composite microwave ferrite magnetic sheet.
As a preferred technical scheme of the invention, the method for preparing the microwave ferrite in the step (1) comprises the following steps:
mixing the raw materials according to the formula ratio, performing primary crushing, pre-sintering, secondary crushing, granulating, molding and sintering to obtain the microwave ferrite.
In the method for preparing microwave ferrite, the purpose of pre-sintering is to prepare for sintering of the following material, the powder after pre-sintering is already partially crystallized, the powder is easy to form, and the shrinkage rate of final sintering is reduced, and the purpose of post-sintering is to make the material completely crystallized and have proper mechanical strength and performance.
As a preferred technical scheme of the invention, the first crushing is ball milling.
Preferably, the first crushing is wet ball milling.
Preferably, in the wet ball milling, the mass ratio of the material, the steel balls and the water is 1 (1.5-4.5): (0.9-1), such as 1:1.5:0.9, 1:2:1, 1:3:0.9, 1:3.5:1, 1:4:0.9 or 1:4.5: 1.
Preferably, the time for the first disruption is 15-20h, such as 15h, 16h, 17h, 18h, 19h or 20h, etc.
Preferably, the first disruption is followed by sieving and drying at 150 ℃. sup.200 ℃.
Preferably, the pre-sintering temperature is 1050-.
Preferably, the pre-sintering time is 6-10h, such as 6h, 7h, 8h, 9h or 10 h.
Preferably, the raw material after the first crushing is sieved before the pre-sintering.
Preferably, the second crushing is ball milling.
Preferably, the second crushing is wet ball milling.
Preferably, in the wet ball milling, the mass ratio of the material, the steel balls and the water is 1 (1.5-4.5): (0.9-1), such as 1:1.5:0.9, 1:2:1, 1:3:0.9, 1:3.5:1, 1:4:0.9 or 1:4.5: 1.
Preferably, the time of the second crushing is 20-30h, such as 20h, 22h, 24h, 26h, 28h or 30h, etc.
Preferably, the granulation is dry granulation.
Preferably, a binder is added during the granulation.
Preferably, the forming method is to place the granules in a mould for compression forming.
Preferably, the pressure of the molding is 500-2E.g. 500kg/cm2、600kg/cm2、700kg/cm2、800kg/cm2、900kg/cm2Or 1000kg/cm2And the like.
Preferably, the forming forms the particulate material into a cylindrical blank.
Preferably, the sintering temperature is 1390-.
Preferably, the sintering time is 6-10h, such as 6h, 7h, 8h, 9h or 10h, etc.
Preferably, the sintering is performed in an oxygen-containing atmosphere.
Preferably, the method for preparing microwave ferrite further comprises the step of performing external cylindrical grinding on the obtained product after sintering.
As a preferable technical scheme of the invention, the method for preparing the microwave ceramic in the step (2) comprises the following steps:
mixing the raw materials according to the formula ratio, performing primary crushing, calcining, secondary crushing, granulating, molding and sintering to obtain the microwave ceramic.
In the method for preparing microwave ceramics, the purpose of calcination is to prepare the sintering of the following material, the powder after pre-sintering is partially crystallized, the powder is easy to form, and the shrinkage rate of the final sintering is reduced, and the purpose of the following sintering is to make the material completely crystallized and have proper mechanical strength and performance.
As a preferable technical scheme of the invention, the first crushing is wet ball milling.
Preferably, in the wet ball milling, the mass ratio of the materials, water, the dispersing agent and the zirconia balls is (190-210): 140-160): 1: (1040-1060), such as 190:140:1:1040, 200:150:1:1050, 210:160:1:1060, and the dispersing agent comprises ammonia water.
Preferably, the time for the first disruption is 6-10h, such as 6h, 7h, 8h, 9h or 10h, etc.
Preferably, the first disruption is followed by drying at 200 ℃ and 250 ℃.
Preferably, the drying time is 15-20h, such as 15h, 16h, 17h, 18h, 19h or 20h, etc.
Preferably, the temperature of the calcination is 1260-.
Preferably, the calcination is carried out for a period of time of 5 to 7 hours, such as 5 hours, 5.5 hours, 6 hours, 6.5 hours, 7 hours, or the like.
Preferably, the second crushing is ball milling.
Preferably, the second crushing is wet ball milling.
Preferably, in the wet ball milling, the mass ratio of the materials, water, the dispersing agent and the zirconia balls is (190-210): 150-170): 1: (1180-1220), such as 190:170:1:1180, 200:150:1:1220, 210:160:1:1200 and the like, and the dispersing agent comprises ammonia water.
Preferably, the time of the second crushing is 12-18h, such as 12h, 13h, 14h, 15h, 16h, 17h or 18h, etc.
Preferably, the granulation method is spray granulation.
Preferably, the feed liquid for spray granulation comprises materials, water, a dispersing agent, a binder, a plasticizer and a release agent.
Preferably, the dispersant is ammonia.
Preferably, the binder comprises glue, preferably polyvinyl alcohol, such as PVA217 (15).
Preferably, the plasticizer comprises polyethylene glycol, such as PEG400, PEG20K (20).
Preferably, the release agent comprises LU 6418.
Preferably, the forming is performed by a press.
Preferably, the molding forms the granules into a circular ring shape.
Preferably, the sintering temperature is 1350-.
Preferably, the sintering time is 3-5h, such as 3h, 3.5h, 4h, 4.5h or 5h, etc.
Preferably, the sintering is performed in an oxygen-containing atmosphere.
Preferably, the method for preparing microwave ceramics further comprises the step of carrying out internal grinding and external grinding on the obtained product after sintering.
As a preferred technical solution of the present invention, the compounding method in the step (3) includes:
and (3) coating an adhesive on the microwave ferrite obtained in the step (1), sleeving the microwave ceramic obtained in the step (2) on the microwave ferrite coated with the adhesive, and drying to obtain the composite microwave ferrite magnetic sheet.
Preferably, the preparation method of the composite microwave ferrite magnetic sheet further comprises the following steps: and slicing the composite microwave ferrite magnetic sheet and carrying out double-sided grinding.
As a further preferable technical scheme of the preparation method, the method comprises the following steps:
(1) mixing the raw materials according to the formula ratio, carrying out wet ball milling for 15-20h, then sieving, drying at the temperature of 150-2Pressing the obtained product into a cylindrical blank, sintering the cylindrical blank for 6 to 10 hours at the temperature of 1390-;
(2) mixing the raw materials according to the formula ratio, carrying out wet ball milling for 6-10h, drying for 15-20h, calcining for 5-7h at 1260-1300 ℃, carrying out wet ball milling for 12-18h for the second time, carrying out spray granulation, preparing the obtained granular material into a ring shape by using a press, sintering for 3-5h at 1370 ℃ in an oxygen-containing atmosphere, and carrying out inner circle grinding and outer circle grinding on the sintered product to obtain the microwave ceramic;
(3) and (3) coating an adhesive on the microwave ferrite obtained in the step (1), sleeving the microwave ceramic obtained in the step (2) on the microwave ferrite coated with the adhesive, drying, slicing and grinding the two sides to obtain the composite microwave ferrite magnetic sheet.
In a third aspect, the present invention provides the use of a composite microwave ferrite magnetic sheet as described in the first aspect for an isolator for a 5G base station.
Compared with the prior art, the invention has the following beneficial effects:
(1) the composite microwave ferrite magnetic sheet provided by the invention adopts the mode that the microwave ceramic dielectric sheet is sleeved outside the microwave ferrite magnetic sheet, achieves the effect of improving the overall dielectric constant under the condition of not changing the dielectric constant of the microwave ferrite magnetic sheet, has extremely small size and meets the requirement of a 5G base station isolator. After the composite microwave ferrite magnetic sheet provided by the invention is assembled in an isolator, the isolation degree can reach-24.2 DB at 2.6GHz, and the insertion loss is only-0.21 DB; the isolation degree can reach-25.6 DB at 2.7GHz, and the insertion loss is only-0.19 DB; the isolation can reach-24.6 DB at 2.8GHz, and the insertion loss is only-0.20B.
(2) The preparation method provided by the invention is simple to operate, short in flow and suitable for industrial large-scale production.
Drawings
FIG. 1 is a schematic view of a microwave ferrite magnetic sheet provided in example 1;
FIG. 2 is a schematic view of a microwave ceramic dielectric sheet provided in example 1;
FIG. 3 is a schematic view of a composite microwave ferrite magnetic sheet provided in embodiment 1.
Detailed Description
In order to better illustrate the present invention and facilitate the understanding of the technical solutions of the present invention, the present invention is further described in detail below. The following examples are merely illustrative of the present invention and do not represent or limit the scope of the claims, which are defined by the claims.
The following are typical but non-limiting examples of the invention:
example 1
The embodiment provides a composite microwave ferrite magnetic sheet, which comprises a microwave ferrite magnetic sheet and a microwave ceramic dielectric sheet sleeved outside the microwave ferrite magnetic sheet, wherein the microwave ferrite magnetic sheet and the microwave ceramic dielectric sheet are mutually bonded and fixed through AB mixed glue. The composite microwave ferrite magnetic sheet is in a shape of a circular sheet, and the thickness of the composite microwave ferrite magnetic sheet is 0.65 mm.
In the composite microwave ferrite magnetic sheet provided in this embodiment, the schematic diagram of the microwave ferrite magnetic sheet is shown in fig. 1, the schematic diagram of the microwave ceramic dielectric sheet is shown in fig. 2, and the schematic diagram of the composite microwave ferrite magnetic sheet is shown in fig. 3.
In the composite microwave ferrite magnetic sheet provided in this embodiment, the microwave ferrite magnetic sheet comprises the following raw materials in parts by weight:
in the composite microwave ferrite magnetic sheet provided in this embodiment, the microwave ceramic dielectric sheet comprises the following raw materials in parts by weight:
the results of the performance tests of the composite microwave ferrite magnetic sheet provided in this example are shown in Table 1.
The embodiment also provides a preparation method of the composite microwave ferrite magnetic sheet, which comprises the following specific steps:
preparing microwave ferrite:
1. weighing the raw materials according to the mass ratio of the formula and mixing.
2. One-step ball milling
Mixing the raw materials weighed in the step 1, putting the mixture into a stainless steel ball milling tank, adding a steel ball and deionized water according to the proportion of the materials, namely the ball and the water, of 1:4.5:0.9, and carrying out wet ball milling for the first time: for 18 hours.
3. Drying by baking
And (3) passing the ball-milled materials through a 100-mesh screen, and drying for 15 hours at 150 ℃ to obtain dry materials.
4. Pre-sintering
And (3) screening the dried powder through a 30-mesh screen, putting the powder into a bowl, putting the bowl into a high-temperature electric furnace, presintering at 1150 ℃ and preserving heat for 10 hours.
5. Secondary ball milling
And crushing the pre-sintered mixture, putting the crushed mixture into a stainless steel ball milling tank, and adding steel balls and deionized water according to the proportion of the materials to the balls to water of 1:4:0.9 to perform secondary wet ball milling for 25 hours.
6. Granulating
And (5) drying and granulating the slurry obtained in the step (5), and adding a binder during granulation, wherein the binder is a polyvinyl alcohol aqueous solution with the concentration of 5 wt%.
7. Shaping of
And (3) putting the granules obtained in the step (6) into a die for compression molding, wherein the sizes are as follows: 8mm, 15mm in height and 800kg/cm in molding pressure2。
8. Sintering
And (4) placing the product blank formed by pressing in the step (7) into a high-temperature electric furnace for oxygenation and sintering, wherein the sintering temperature is 1420 ℃, and the temperature is kept for 8 hours.
9. Cylindrical grinder
And (3) cylindrical grinding is carried out on the cylindrical product sintered in the step (8) by using a centerless grinder, and the outer diameter size is as follows: 6.6 ± 0.01mm, height: 13 mm.
(II) preparing a microwave ceramic tube:
1. weighing the raw materials according to the mass ratio of the formula and mixing.
2. Mixing
Mixing by using a horizontal ball mill, and feeding the powder, the deionized water, the dispersing agent and the zirconia balls according to the weight ratio of 200:150:1:1050, wherein the ball milling time is 8 hours.
The dispersant used was ammonia water, and the zirconia balls had a diameter of 5 mm.
3. Drying
And drying the mixed slurry at 225 ℃ for 17 hours.
4. Calcination of
And (3) putting the dried powder into an air sintering furnace for calcination at 1280 ℃ for 6 hours.
5. Fine grinding
And (3) placing the calcined powder into a ball mill for fine grinding, wherein the powder is fed according to the weight ratio of deionized water, a dispersing agent and zirconia balls of 100:80:0.5:600, the dispersing agent is ammonia water, and the ball milling time is 15 hours.
6. Spray granulation
Uniformly stirring 200kg of powder, 157kg of powder, 1.0kg of powder, 10.5kg of powder, 11.3kg of powder and 1.9kg of powder, deionized water, a dispersing agent, glue, a plasticizer and a release agent in a weight ratio, and then carrying out spray granulation. The used dispersing agents are ammonia water, glue PVA217(15), plasticizer PEG400 and release agent LU 6418.
7. Shaping of
The molded product was formed into a circular ring shape by using a 100 ton press, and had an inner diameter of 7mm, an outer diameter of 11.5mm and a height of 15.2 mm.
8. Sintering
And (3) sintering the formed ceramic tube by high-temperature air at 1360 ℃ for 4 hours.
9. Internal grinding mill
And (3) carrying out internal grinding on the sintered ceramic tube to reduce the internal roughness of the ceramic tube, wherein the internal diameter size is 6.62mm, and the internal diameter size precision reaches +/-0.01 mm.
10. Cylindrical grinder
And (3) performing external grinding on the ceramic tube after internal grinding to reduce the external roughness of the ceramic tube, wherein the external diameter size is 9.3mm, and the external diameter size precision reaches +/-0.01 mm.
The microwave ceramic tube is prepared according to the steps, and the size of the ceramic tube is as follows: outer diameter: 9.3 plus or minus 0.01mm, 6.6 plus or minus 0.01mm in inner diameter and 13mm in height.
(III) preparing the composite magnetic sheet:
1. and uniformly coating glue (AB mixed glue) on the excircle of the cylindrical microwave ferrite.
2. And sleeving the microwave ferrite coated with the glue into a microwave ceramic tube.
3. And (3) drying the composite material obtained in the step (2) at the temperature of 150 ℃.
4. Slicing the composite material, wherein the slicing thickness is as follows: 0.72 mm.
5. Carrying out double-side grinding on the cut composite material wafer, wherein the thickness after grinding is as follows: 0.65mm, and reducing the surface roughness to prepare the composite microwave ferrite magnetic sheet.
Example 2
The composite microwave ferrite magnetic sheet provided in this example has the same structure, the same kinds of raw materials, and the same preparation method as those of example 1, except that the raw material ratio is different from that of example 1.
In the composite microwave ferrite magnetic sheet provided in this embodiment, the microwave ferrite magnetic sheet comprises the following raw materials in parts by weight:
in the composite microwave ferrite magnetic sheet provided in this embodiment, the microwave ceramic dielectric sheet comprises the following raw materials in parts by weight:
the results of the performance tests of the composite microwave ferrite magnetic sheet provided in this example are shown in Table 1.
Example 3
The composite microwave ferrite magnetic sheet provided in this example has the same structure, the same kinds of raw materials, and the same preparation method as those of example 1, except that the raw material ratio is different from that of example 1.
In the composite microwave ferrite magnetic sheet provided in this embodiment, the microwave ferrite magnetic sheet comprises the following raw materials in parts by weight:
in the composite microwave ferrite magnetic sheet provided in this embodiment, the microwave ceramic dielectric sheet comprises the following raw materials in parts by weight:
the results of the performance tests of the composite microwave ferrite magnetic sheet provided in this example are shown in Table 1.
Example 4
The embodiment provides a composite microwave ferrite magnetic sheet, which comprises a microwave ferrite magnetic sheet and a microwave ceramic dielectric sheet sleeved outside the microwave ferrite magnetic sheet, wherein the microwave ferrite magnetic sheet and the microwave ceramic dielectric sheet are mutually bonded and fixed through AB mixed glue. The composite microwave ferrite magnetic sheet is in a shape of a circular sheet, and the thickness of the composite microwave ferrite magnetic sheet is 0.65 mm.
In the composite microwave ferrite magnetic sheet provided in this embodiment, the microwave ferrite magnetic sheet comprises the following raw materials in parts by weight:
in the composite microwave ferrite magnetic sheet provided in this embodiment, the microwave ceramic dielectric sheet comprises the following raw materials in parts by weight:
the results of the performance tests of the composite microwave ferrite magnetic sheet provided in this example are shown in Table 1.
The embodiment also provides a preparation method of the composite microwave ferrite magnetic sheet, which comprises the following specific steps:
preparing microwave ferrite:
1. weighing the raw materials according to the mass ratio of the formula and mixing.
2. One-step ball milling
Mixing the raw materials weighed in the step 1, putting the mixture into a stainless steel ball milling tank, adding a steel ball and deionized water according to the proportion of the materials, namely the ball and the water, of 1:1.5:0.9, and carrying out wet ball milling for the first time: for 20 hours.
3. Drying by baking
And (3) passing the ball-milled materials through a 100-mesh screen, and drying for 15 hours at 200 ℃ to obtain dry materials.
4. Pre-sintering
And (3) sieving the dried powder through a 30-mesh sieve, putting the powder into a bowl, presintering the powder in a high-temperature electric furnace at 1050 ℃, and preserving the heat for 8 hours.
5. Secondary ball milling
And crushing the pre-sintered mixture, putting the crushed mixture into a stainless steel ball milling tank, and adding steel balls and deionized water according to the proportion of the materials, namely the balls and the water, of 1:1.5:0.9 to perform secondary wet ball milling for 20 hours.
6. Granulating
And (5) drying and granulating the slurry obtained in the step (5), and adding a binder during granulation, wherein the binder is a polyvinyl alcohol aqueous solution with the concentration of 5 wt%.
7. Shaping of
And (3) putting the granules obtained in the step (6) into a die for compression molding, wherein the sizes are as follows: 8mm, 15mm in height and 500kg/cm in molding pressure2。
8. Sintering
And (4) placing the product blank formed by pressing in the step (7) into a high-temperature electric furnace for oxygenation and sintering, wherein the sintering temperature is 1390 ℃, and the temperature is kept for 10 hours.
9. Cylindrical grinder
And (3) cylindrical grinding is carried out on the cylindrical product sintered in the step (8) by using a centerless grinder, and the outer diameter size is as follows: 6.6 ± 0.01mm, height: 13 mm.
(II) preparing a microwave ceramic tube:
1. weighing the raw materials according to the mass ratio of the formula and mixing.
2. Mixing
Mixing by using a horizontal ball mill, and feeding according to the weight ratio of powder, deionized water, a dispersing agent and zirconia balls of 190:140:1:1040 for 6 hours.
The dispersant used was ammonia water, and the zirconia balls had a diameter of 5 mm.
3. Drying
And drying the mixed slurry at 200 ℃ for 20 hours.
4. Calcination of
And (3) putting the dried powder into an air sintering furnace for calcining at 1260 ℃ for 7 hours.
5. Fine grinding
And (3) placing the calcined powder into a ball mill for fine grinding, wherein the powder is fed according to the weight ratio of the deionized water to the dispersant to the zirconia balls of 190:150:1:1180, the dispersant is ammonia water, and the ball milling time is 12 hours.
6. Spray granulation
Uniformly stirring 200kg of powder, 157kg of powder, 1.0kg of powder, 10.5kg of powder, 11.3kg of powder and 1.9kg of powder, deionized water, a dispersing agent, glue, a plasticizer and a release agent in a weight ratio, and then carrying out spray granulation. The used dispersing agent is ammonia water, glue PVA217(15), plasticizer PEG20K (20) and release agent LU 6418.
7. Shaping of
The molded product was formed into a circular ring shape by using a 100 ton press, and had an inner diameter of 7mm, an outer diameter of 11.5mm and a height of 15.2 mm.
8. Sintering
And (3) sintering the formed ceramic tube at high temperature of 1350 ℃ for 5 hours.
9. Internal grinding mill
And (3) carrying out internal grinding on the sintered ceramic tube to reduce the internal roughness of the ceramic tube, wherein the internal diameter size is 6.62mm, and the internal diameter size precision reaches +/-0.01 mm.
10. Cylindrical grinder
And (3) performing external grinding on the ceramic tube after internal grinding to reduce the external roughness of the ceramic tube, wherein the external diameter size is 9.3mm, and the external diameter size precision reaches +/-0.01 mm.
The microwave ceramic tube is prepared according to the steps, and the size of the ceramic tube is as follows: outer diameter: 9.3 plus or minus 0.01mm, 6.6 plus or minus 0.01mm in inner diameter and 13mm in height.
(III) preparing the composite magnetic sheet:
1. and uniformly coating glue (AB mixed glue) on the excircle of the cylindrical microwave ferrite.
2. And sleeving the microwave ferrite coated with the glue into a microwave ceramic tube.
3. And (3) drying the composite material obtained in the step (2) at the temperature of 150 ℃.
4. Slicing the composite material, wherein the slicing thickness is as follows: 0.72 mm.
5. Carrying out double-side grinding on the cut composite material wafer, wherein the thickness after grinding is as follows: 0.65mm, and reducing the surface roughness to prepare the composite microwave ferrite magnetic sheet.
Example 5
The embodiment provides a composite microwave ferrite magnetic sheet, which comprises a microwave ferrite magnetic sheet and a microwave ceramic dielectric sheet sleeved outside the microwave ferrite magnetic sheet, wherein the microwave ferrite magnetic sheet and the microwave ceramic dielectric sheet are mutually bonded and fixed through AB mixed glue. The composite microwave ferrite magnetic sheet is in a shape of a circular sheet, and the thickness of the composite microwave ferrite magnetic sheet is 0.65 mm.
In the composite microwave ferrite magnetic sheet provided in this embodiment, the microwave ferrite magnetic sheet comprises the following raw materials in parts by weight:
in the composite microwave ferrite magnetic sheet provided in this embodiment, the microwave ceramic dielectric sheet comprises the following raw materials in parts by weight:
the results of the performance tests of the composite microwave ferrite magnetic sheet provided in this example are shown in Table 1.
The embodiment also provides a preparation method of the composite microwave ferrite magnetic sheet, which comprises the following specific steps:
preparing microwave ferrite:
1. weighing the raw materials according to the mass ratio of the formula and mixing.
2. One-step ball milling
Mixing the raw materials weighed in the step 1, putting the mixture into a stainless steel ball milling tank, adding a steel ball and deionized water according to the proportion of the materials, namely the ball and the water, of 1:4.5:1, and carrying out wet ball milling for the first time: for 15 hours.
3. Drying by baking
And (3) passing the ball-milled materials through a 100-mesh screen, and drying for 15 hours at 180 ℃ to obtain dry materials.
4. Pre-sintering
And (3) sieving the dried powder through a 30-mesh screen, putting the powder into a bowl, putting the bowl into a high-temperature electric furnace, presintering at the presintering temperature of 1200 ℃, and preserving heat for 6 hours.
5. Secondary ball milling
And crushing the pre-sintered mixture, putting the crushed mixture into a stainless steel ball milling tank, and adding steel balls and deionized water according to the proportion of the materials to the balls to water of 1:4.5:1 to perform secondary wet ball milling for 30 hours.
6. Granulating
And (5) drying and granulating the slurry obtained in the step (5), and adding a binder during granulation, wherein the binder is a polyvinyl alcohol aqueous solution with the concentration of 5 wt%.
7. Shaping of
And (3) putting the granules obtained in the step (6) into a die for compression molding, wherein the sizes are as follows: 8mm, 15mm in height and 1000kg/cm in molding pressure2。
8. Sintering
And (4) placing the product blank formed by pressing in the step (7) into a high-temperature electric furnace for oxygenation and sintering, wherein the sintering temperature is 1460 ℃, and the heat preservation is carried out for 6 hours.
9. Cylindrical grinder
And (3) cylindrical grinding is carried out on the cylindrical product sintered in the step (8) by using a centerless grinder, and the outer diameter size is as follows: 6.6 ± 0.01mm, height: 13 mm.
(II) preparing a microwave ceramic tube:
1. weighing the raw materials according to the mass ratio of the formula and mixing.
2. Mixing
Mixing by using a horizontal ball mill, and feeding the powder, deionized water, a dispersing agent and zirconia balls according to the weight ratio of 210:160:1:106, wherein the ball milling time is 10 hours.
The dispersant used was ammonia water, and the zirconia balls had a diameter of 5 mm.
3. Drying
And drying the mixed slurry at 250 ℃ for 15 hours.
4. Calcination of
And (3) putting the dried powder into an air sintering furnace for calcining at 1260 ℃ for 7 hours.
5. Fine grinding
And (3) placing the calcined powder into a ball mill for fine grinding, wherein the powder is fed according to the weight ratio of deionized water to a dispersing agent to zirconia balls of 210:170:1:1220, the dispersing agent is ammonia water, and the ball milling time is 12 hours.
6. Spray granulation
Uniformly stirring 200kg of powder, 157kg of powder, 1.0kg of powder, 10.5kg of powder, 11.3kg of powder and 1.9kg of powder, deionized water, a dispersing agent, glue, a plasticizer and a release agent in a weight ratio, and then carrying out spray granulation. The used dispersing agent is ammonia water, glue PVA217(15), plasticizer PEG20K (20) and release agent LU 6418.
7. Shaping of
The molded product was formed into a circular ring shape by using a 100 ton press, and had an inner diameter of 7mm, an outer diameter of 11.5mm and a height of 15.2 mm.
8. Sintering
And (3) sintering the formed ceramic tube at high temperature of 1370 ℃ for 3 hours.
9. Internal grinding mill
And (3) carrying out internal grinding on the sintered ceramic tube to reduce the internal roughness of the ceramic tube, wherein the internal diameter size is 6.62mm, and the internal diameter size precision reaches +/-0.01 mm.
10. Cylindrical grinder
And (3) performing external grinding on the ceramic tube after internal grinding to reduce the external roughness of the ceramic tube, wherein the external diameter size is 9.3mm, and the external diameter size precision reaches +/-0.01 mm.
The microwave ceramic tube is prepared according to the steps, and the size of the ceramic tube is as follows: outer diameter: 9.3 plus or minus 0.01mm, 6.6 plus or minus 0.01mm in inner diameter and 13mm in height.
(III) preparing the composite magnetic sheet:
1. and uniformly coating glue (AB mixed glue) on the excircle of the cylindrical microwave ferrite.
2. And sleeving the microwave ferrite coated with the glue into a microwave ceramic tube.
3. And (3) drying the composite material obtained in the step (2) at the temperature of 150 ℃.
4. Slicing the composite material, wherein the slicing thickness is as follows: 0.72 mm.
5. Carrying out double-side grinding on the cut composite material wafer, wherein the thickness after grinding is as follows: 0.65mm, and reducing the surface roughness to prepare the composite microwave ferrite magnetic sheet.
Comparative example 1
This comparative example used only the microwave ferrite magnetic sheet of the composite microwave ferrite magnetic sheets provided in example 3 as a control, and the results of the performance tests are shown in Table 1.
Test method
The finally obtained material of the examples or the comparative examples was assembled into a separator, and the separator was tested for isolation and insertion loss, and the performance of the material was evaluated as the performance of the device.
Test conditions for isolation and insertion loss: frequency: 2.6-2.8GHZ, voltage: 0.03V, instrument: 5071C network analyzer.
The test results are given in the following table:
TABLE 1
It can be seen from the above examples and comparative examples that the composite microwave ferrite magnetic sheet provided by the examples has a wider isolation bandwidth and lower insertion loss. The composite microwave ferrite magnetic sheet provided by the embodiment adopts the mode that the microwave ceramic dielectric sheet is sleeved outside the microwave ferrite magnetic sheet, achieves the effect of improving the overall dielectric constant under the condition of not changing the dielectric constant of the microwave ferrite magnetic sheet, has extremely small size and meets the requirement of a 5G base station isolator.
The product provided in comparative example 1 has an insufficient dielectric constant as a whole because a microwave ceramic dielectric sheet is not sleeved outside a microwave ferrite magnetic sheet, and is not preferable in terms of isolation and insertion loss after being used for an isolator.
The applicant states that the present invention is illustrated by the above examples to show the detailed process equipment and process flow of the present invention, but the present invention is not limited to the above detailed process equipment and process flow, i.e. it does not mean that the present invention must rely on the above detailed process equipment and process flow to be implemented. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (10)
1. The composite microwave ferrite magnetic sheet is characterized by comprising a microwave ferrite magnetic sheet and a microwave ceramic dielectric sheet sleeved outside the microwave ferrite magnetic sheet.
2. A composite microwave ferrite magnetic sheet according to claim 1, wherein the microwave ferrite magnetic sheet and the microwave ceramic dielectric sheet are bonded and fixed to each other by an adhesive;
preferably, the adhesive is glue;
preferably, the microwave ferrite magnetic sheet comprises the following raw materials: fe2O3、Y2O3、CaCO3、ZrO2And MnCO3;
Preferably, the microwave ferrite magnetic sheet comprises the following raw materials in parts by weight:
preferably, the microwave ceramic dielectric sheet comprises the following raw materials: CaCO3、TiO2、Sm2O3、Al2O3And CeO2;
Preferably, the microwave ceramic dielectric sheet comprises the following raw materials in parts by weight:
3. a method of manufacturing a composite microwave ferrite magnetic sheet as claimed in claim 1 or 2, which comprises the steps of:
(1) preparing microwave ferrite;
(2) preparing microwave ceramics;
(3) and (3) compounding the microwave ferrite obtained in the step (1) with the microwave ceramic obtained in the step (2) to obtain the composite microwave ferrite magnetic sheet.
4. The method of claim 3, wherein the method of preparing a microwave ferrite according to the step (1) comprises:
mixing the raw materials according to the formula ratio, performing primary crushing, pre-sintering, secondary crushing, granulating, molding and sintering to obtain the microwave ferrite.
5. The preparation method according to the step 4, characterized in that the first crushing is ball milling;
preferably, the first crushing is wet ball milling;
preferably, in the wet ball milling, the mass ratio of the materials, the steel balls and the water is 1 (1.5-4.5) to 0.9-1;
preferably, the time for the first crushing is 15-20 h;
preferably, the first crushing is followed by sieving and drying at 200 ℃;
preferably, the temperature of the pre-sintering is 1050-;
preferably, the pre-sintering time is 6-10 h;
preferably, before the pre-sintering, the raw materials after the first crushing are sieved;
preferably, the second crushing is ball milling;
preferably, the second crushing is wet ball milling;
preferably, in the wet ball milling, the mass ratio of the materials, the steel balls and the water is 1 (1.5-4.5) to 0.9-1;
preferably, the time of the second crushing is 20-30 h;
preferably, the granulation is dry granulation;
preferably, a binder is added during the granulation;
preferably, the forming method is to place the granules in a mould for compression forming;
preferably, the pressure of the molding is 500-2;
Preferably, the forming forms the granules into a cylindrical blank;
preferably, the sintering temperature is 1390-;
preferably, the sintering time is 6-10 h;
preferably, the sintering is carried out in an oxygen-containing atmosphere;
preferably, the method for preparing microwave ferrite further comprises the step of performing external cylindrical grinding on the obtained product after sintering.
6. The method for preparing microwave ceramics according to any one of claims 3 to 5, wherein the method for preparing microwave ceramics according to step (2) comprises:
mixing the raw materials according to the formula ratio, performing primary crushing, calcining, secondary crushing, granulating, molding and sintering to obtain the microwave ceramic.
7. The preparation method according to the step 6, characterized in that the first crushing is wet ball milling;
preferably, in the wet ball milling, the mass ratio of the materials, water, the dispersing agent and the zirconia balls is (190-210): (140-160): 1: (1040-1060), and the dispersing agent comprises ammonia water;
preferably, the time for the first crushing is 6-10 h;
preferably, the first crushing is followed by drying at 250 ℃ and 200 ℃.;
preferably, the drying time is 15-20 h;
preferably, the temperature of the calcination is 1260-1300 ℃;
preferably, the calcination time is 5-7 h;
preferably, the second crushing is ball milling;
preferably, the second crushing is wet ball milling;
preferably, in the wet ball milling, the mass ratio of the materials, water, the dispersing agent and the zirconia balls is (190-210): 150-170): 1: (1180-1220), and the dispersing agent comprises ammonia water;
preferably, the time of the second crushing is 12-18 h;
preferably, the granulation method is spray granulation;
preferably, the feed liquid for spray granulation comprises materials, water, a dispersing agent, a binder, a plasticizer and a release agent;
preferably, the dispersant is ammonia;
preferably, the binder comprises glue, preferably polyvinyl alcohol;
preferably, the plasticizer comprises polyethylene glycol;
preferably, the forming is performed by a press;
preferably, the molding makes the granular materials into a circular ring shape;
preferably, the sintering temperature is 1350-;
preferably, the sintering time is 3-5 h;
preferably, the sintering is carried out in an oxygen-containing atmosphere;
preferably, the method for preparing microwave ceramics further comprises the step of carrying out internal grinding and external grinding on the obtained product after sintering.
8. The method for preparing a composite material according to any one of claims 3 to 7, wherein the method for compounding in step (3) comprises:
coating an adhesive on the microwave ferrite obtained in the step (1), sleeving the microwave ceramic obtained in the step (2) on the microwave ferrite coated with the adhesive, and drying to obtain the composite microwave ferrite magnetic sheet;
preferably, the preparation method of the composite microwave ferrite magnetic sheet further comprises the following steps: and slicing the composite microwave ferrite magnetic sheet and carrying out double-sided grinding.
9. The method for preparing according to any one of claims 3 to 8, characterized in that it comprises the steps of:
(1) mixing the raw materials according to the formula ratio, carrying out wet ball milling for 15-20h, then sieving, drying at the temperature of 150-2Pressing the obtained product into a cylindrical blank, sintering the cylindrical blank for 6 to 10 hours at the temperature of 1390-;
(2) mixing the raw materials according to the formula ratio, carrying out wet ball milling for 6-10h, drying for 15-20h, calcining for 5-7h at 1260-1300 ℃, carrying out wet ball milling for 12-18h for the second time, carrying out spray granulation, preparing the obtained granular material into a ring shape by using a press, sintering for 3-5h at 1370 ℃ in an oxygen-containing atmosphere, and carrying out inner circle grinding and outer circle grinding on the sintered product to obtain the microwave ceramic;
(3) and (3) coating an adhesive on the microwave ferrite obtained in the step (1), sleeving the microwave ceramic obtained in the step (2) on the microwave ferrite coated with the adhesive, drying, slicing and grinding the two sides to obtain the composite microwave ferrite magnetic sheet.
10. Use of a composite microwave ferrite magnetic sheet according to claim 1 or 2 in isolators of 5G base stations.
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CN112010665A (en) * | 2020-09-07 | 2020-12-01 | 中国振华集团云科电子有限公司 | Preparation method of embedded heterogeneous ceramic substrate |
CN112457040A (en) * | 2020-12-07 | 2021-03-09 | 北京无线电测量研究所 | Microwave ferrite sleeve sheet and preparation method thereof |
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Application publication date: 20200218 Assignee: Jinhua cimeng Intellectual Property Service Co.,Ltd. Assignor: HENGDIAN GROUP DMEGC MAGNETICS Co.,Ltd. Contract record no.: X2023330000883 Denomination of invention: A composite microwave ferrite magnetic sheet and its preparation method and application Granted publication date: 20210108 License type: Common License Record date: 20231128 |