CN115196955A - Y-type hexagonal ferrite material, preparation method thereof and microwave device - Google Patents
Y-type hexagonal ferrite material, preparation method thereof and microwave device Download PDFInfo
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Abstract
The invention discloses a Y-shaped hexagonal ferrite material, a preparation method thereof and a microwave device, wherein the Y-shaped hexagonal ferrite material has a chemical formula as follows: (Ba) x Sr 2‑x )(A 2 )Fe 12 O 22 Wherein A is any one of Co, mg, mn and Zn, and x is more than or equal to 0 and less than or equal to 2. The Y-type hexaferrite material has smaller coercive force, and the smaller coercive force can make the Y-type hexaferrite material more sensitive to the response of an external magnetic field, so that the Y-type hexaferrite material has higher magnetic conductivity.
Description
Technical Field
The invention relates to the field of electronic materials, in particular to a Y-type hexaferrite material, a preparation method thereof and a microwave device.
Background
With the development of 5G and millimeter wave communication, microwave devices are developing to higher frequency bands. This puts higher demands on the frequency of use of the magnetic material components in the device. For the magnetic component, part of the device is used for microwave signal transmission, but the other part is used for isolation and shielding of the microwave signal. For the material for the shielding function, the higher the initial permeability of the magnetic material needs to be, the better. While the material also needs to have suitable electrical properties.
Previous studies have shown that hexaferrites have uniaxial anisotropy at room temperature, with higher frequency of application compared to spinel ferrites. Therefore, the hexaferrite is more suitable to be used as a material of a microwave device (especially a phase shifter) working at GHz, and is also a good microwave absorbing material. However, the permeability of the currently common hexaferrite at room temperature is not high enough, which limits its performance in devices.
Disclosure of Invention
The invention aims to provide a Y-type hexaferrite material which has high magnetic permeability.
The invention also aims to provide a preparation method of the Y-shaped hexaferrite material and a microwave device.
In order to achieve the above object, an embodiment of the present invention provides a Y-type hexaferrite material, which has a chemical formula: (Ba) x Sr 2-x )(A 2 )Fe 12 O 22 Wherein A is any one of Co, mg, mn and Zn, and x is more than or equal to 0 and less than or equal to 2.
The embodiment of the invention also provides a preparation method of the Y-shaped hexagonal ferrite material, which comprises the following steps:
s1, mixing, grinding and drying the raw materials to obtain a premix;
s2, sintering the premix to obtain the Y-shaped hexagonal ferrite material;
the raw materials comprise a Ba source, a Sr source, an A source and a Fe source, wherein the A source is any one of a Co source, a Mg source, a Mn source and a Zn source.
In one or more embodiments of the present invention, the Ba source is barium carbonate; and/or the presence of a gas in the atmosphere,
the Sr source is strontium carbonate; and/or the presence of a gas in the gas,
the iron source is Fe 2 O 3 (ii) a And/or the presence of a gas in the gas,
the A source is any one of Co, mg, mn and Zn oxides.
In one or more embodiments of the present invention, in the raw material, a molar ratio of Ba element, sr element, a element, and Fe element is x: (2-x): 2:12, wherein x is more than or equal to 0 and less than or equal to 2.
In one or more embodiments of the present invention, in step S1, the grinding step includes: and performing ball milling treatment on the mixed raw materials.
In one or more embodiments of the present invention, the step of ball milling treatment comprises:
putting the mixed raw materials into a ball mill, and carrying out ball milling for 12-20h under the condition that the rotating speed is 100 r/min-350 r/min.
In one or more embodiments of the present invention, in step S1, the step of obtaining a premix includes:
and pre-burning the mixed, ground and dried raw materials to obtain the premix.
In one or more embodiments of the present invention, the step of burn-in processing includes:
mixing, grinding, drying in flowing oxygen atmosphere or air atmosphere, heating to 900-1000 deg.C at 2-4 deg.C/min, and pre-sintering at the temperature for 3-10 hr;
then the temperature is reduced to the room temperature at the cooling rate of 0.5-1 ℃/min.
In one or more embodiments of the present invention, in step S2, the step of sintering process includes:
the premix is in flowing oxygen atmosphere, and is heated to 1150-1300 ℃ at the heating rate of 2-4 ℃/min, and is sintered for 15-18h at the temperature;
then the temperature is reduced to the room temperature at the cooling rate of 1-2 ℃/min.
Embodiments of the present invention also provide a microwave device comprising a Y-type hexaferrite material as described above.
Compared with the prior art, the Y-type hexaferrite material has smaller coercive force, and the smaller coercive force can make the Y-type hexaferrite material more sensitive to response of an external magnetic field, so that the Y-type hexaferrite material has higher magnetic permeability.
Drawings
Fig. 1 is a flowchart of a method of preparing a Y-type hexaferrite material according to an embodiment of the present invention;
fig. 2 is an XRD pattern of the Y-type hexaferrite material obtained in example 1 according to the present invention;
fig. 3 is a room temperature magnetic effect test chart of the Y-type hexaferrite material obtained in example 1 according to the present invention.
Detailed Description
The following detailed description of the present invention is provided in conjunction with the accompanying drawings, but it should be understood that the scope of the present invention is not limited to the specific embodiments.
Throughout the specification and claims, unless explicitly stated otherwise, the word "comprise", or variations such as "comprises" or "comprising", will be understood to imply the inclusion of a stated element or component but not the exclusion of any other element or component.
According to a preferred embodiment of the invention, the Y-type hexaferrite material has a chemical formula: (Ba) x Sr 2-x )(A 2 )Fe 12 O 22 Wherein A is any one of Co, mg, mn and Zn, and x is more than or equal to 0 and less than or equal to 2.
As shown in fig. 1, an embodiment of the present invention further provides a preparation method of the Y-type hexaferrite material, including the following steps:
s1, mixing the raw materials, grinding and drying to obtain the premix.
In step S1, the raw materials include: ba source, sr source, A source and Fe source, wherein A source is any one of Co source, mg source, mn source and Zn source. When x is 0, it is considered that there is no Ba source in the raw material and the finally obtained product also has no Ba element. When x is 2, it is considered that there is no Sr source in the raw material and Sr element is not contained in the finally obtained product.
Specifically, the Ba source is barium carbonate; the Sr source is carbonStrontium acid; the source of Fe is Fe 2 O 3 (ii) a The A source is any one of Co, mg, mn and Zn oxides.
Specifically, in the raw materials, the molar ratio of the Ba element, the Sr element, the A element and the Fe element is x: (2-x): 2:12, wherein x is more than or equal to 0 and less than or equal to 2.
Specifically, the grinding step comprises: and performing ball milling treatment on the mixed raw materials. Preferably, the step of ball milling treatment may comprise:
putting the mixed raw materials into a ball mill, and ball-milling for 12-20h at the rotating speed of 100r/min to 350 r/min. The mixed raw materials can be placed into a ball milling tank of a ball milling machine in the ball milling process, absolute ethyl alcohol is added into the mixed raw materials to reach the position of two thirds of the height of the ball milling tank, and then ball milling is carried out.
The ball milling can grind and mix the components in the raw materials as uniformly as possible.
Specifically, the drying step may include: drying the ground raw materials in a dryer at 92-98 deg.C for 25-40min. The drying conditions may also be adjusted according to the amount of material actually dried.
Specifically, the step of obtaining the premix comprises:
and pre-burning the mixed, ground and dried raw materials to obtain the premix.
Preferably, the step of pre-firing treatment may include:
mixing, grinding, drying in flowing oxygen atmosphere or air atmosphere, heating to 900-1000 deg.C at 2-4 deg.C/min, and pre-sintering at the temperature for 3-10 hr;
then cooling to room temperature at a cooling rate of 0.5-1 deg.C/min to obtain the premix.
In order to facilitate the subsequent sintering treatment and prevent the premix from blocking in the pre-sintering treatment process and influencing the subsequent sintering treatment, the premix subjected to the pre-sintering treatment can be cleaned and ground for at least 20min. The grinding can be carried out by hand.
And S2, sintering the premix to obtain the Y-shaped hexagonal ferrite material.
Specifically, the sintering treatment comprises the following steps:
the premix is in flowing oxygen atmosphere, and is heated to 1150-1300 ℃ at the heating rate of 2-4 ℃/min, and is sintered for 15-18h at the temperature; and then cooling to room temperature at the cooling rate of 1-2 ℃/min to obtain the Y-type hexagonal ferrite material.
Embodiments of the present invention also provide a microwave device comprising a Y-type hexaferrite material as described above.
The Y-type hexaferrite material and the preparation method thereof according to the present invention will be described in detail with reference to specific examples.
Example 1
Respectively weighing 0.5 parts of barium carbonate, 1.5 parts of strontium carbonate, 2 parts of zinc oxide and 6 parts of Fe in parts by mole 2 O 3 。
Manually mixing the weighed raw materials, placing the mixture into a ball milling tank, adding ball milling beads, adding absolute alcohol to the position with two thirds height of the ball milling tank, and placing the ball milling tank into a ball mill. The rotating speed of the ball mill is 200r/min, and the ball milling time is 13h.
After the ball milling is finished, taking out the medicine in the ball milling tank, placing the medicine in a mortar, and placing the medicine in a dryer for drying, wherein the temperature of the dryer is set to be 95 ℃, and the drying time is 30min;
grinding the dried medicine, placing the ground medicine into a crucible, placing the crucible into a tube furnace, and pre-burning the medicine in a flowing oxygen atmosphere. Heating up to 1000 ℃ according to a certain temperature gradient with the heating rate of 2 ℃/min, and presintering for 5h at the temperature. The temperature is reduced to room temperature at the rate of 1 ℃/min.
After the completion of the pre-firing, the mixture was taken out and put into a cleaned mortar to be manually ground for 30 minutes, to obtain a premix.
The premix is put into a clean crucible and put into a tube furnace for sintering treatment in flowing oxygen atmosphere. Heating up to 1280 ℃ according to a certain temperature gradient with the heating rate of 2 ℃/min, and sintering for 17h at the temperature. Cooling to room temperature at a rate of 1.5 deg.C/min to obtain Y-type hexaferrite (Ba) 0.5 Sr 1.5 Zn 2 Fe 12 O 22 )。
The obtained Y-type hexaferrite material is subjected to XRD (X-ray diffraction) test and room temperature magnetic effect test, so as to obtain an XRD pattern as shown in fig. 2 and a room temperature magnetic effect test pattern as shown in fig. 3, respectively.
As can be seen from the XRD chart of fig. 2, the Y-type hexaferrite material (Ba) in the present example 0.5 Sr 1.5 Zn 2 Fe 12 O 22 ) Is single-phase hexaferrite.
As can be seen from the room temperature magnetic effect test chart shown in fig. 3, the Y-type hexaferrite material (Ba) in the present embodiment 0.5 Sr 1.5 Zn 2 Fe 12 O 22 ) Is less than 100Oe, is a typical soft magnetic material, and thus is a Y-type hexaferrite material (Ba) 0.5 Sr 1.5 Zn 2 Fe 12 O 22 ) Has high magnetic permeability.
Example 2
Respectively weighing 1.99 parts of barium carbonate, 0.01 part of strontium carbonate, 2 parts of zinc oxide and 6 parts of Fe in parts by mole 2 O 3 。
Manually mixing the weighed raw materials, placing the mixture into a ball milling tank, adding ball milling beads, adding absolute alcohol to the position with two thirds height of the ball milling tank, and placing the ball milling tank into a ball mill. The rotating speed of the ball mill is 100r/min, and the ball milling time is 20h.
After the ball milling is finished, taking out the medicine in the ball milling tank, placing the medicine in a mortar, and placing the mortar in a dryer for drying, wherein the temperature of the dryer is set to be 92 ℃, and the drying time is 40min;
and grinding the dried medicine, placing the ground medicine into a crucible, and placing the crucible into a tubular furnace to perform pre-burning treatment in a flowing oxygen atmosphere. Heating up to 900 ℃ according to a certain temperature gradient with the heating rate of 3 ℃/min, and presintering for 10h at the temperature. The temperature is reduced to room temperature at the rate of 1 ℃/min.
After the completion of the pre-firing, the mixture was taken out and put into a cleaned mortar to be manually ground for 30 minutes, to obtain a premix.
Placing the premix into a clean crucible, placing the crucible into a tube furnace, and flowingSintering treatment is carried out in an oxygen atmosphere. Heating up to 1150 ℃ according to a certain temperature gradient with the heating rate of 3 ℃/min, and sintering for 18h at the temperature. Cooling to room temperature at a rate of 1 deg.C/min to obtain Y-type hexaferrite (Ba) 1.99 Sr 0.01 Zn 2 Fe 12 O 22 )。
The Y-type hexaferrite material (Ba) obtained in this example 1.99 Sr 0.01 Zn 2 Fe 12 O 22 ) Various properties of (b) and the obtained Y-type hexaferrite material (Ba) in example 1 0.5 Sr 1.5 Zn 2 Fe 12 O 22 ) The performance of each aspect of (a) is substantially the same.
Example 3
Respectively weighing 0.01 part of barium carbonate, 1.99 parts of strontium carbonate, 2 parts of zinc oxide and 6 parts of Fe in parts by mole 2 O 3 。
Manually mixing the weighed raw materials, placing the mixture into a ball milling tank, adding ball milling beads, adding absolute alcohol to the position with two thirds height of the ball milling tank, and placing the ball milling tank into a ball mill. The rotating speed of the ball mill is 350r/min, and the ball milling time is 12h.
After the ball milling is finished, taking out the medicine in the ball milling tank, placing the medicine in a mortar, and placing the medicine in a dryer for drying, wherein the dryer is generally set at 98 ℃ and the drying time is 25min;
grinding the dried medicine, placing the ground medicine into a crucible, placing the crucible into a tube furnace, and pre-burning the medicine in a flowing oxygen atmosphere. Heating up to 950 ℃ according to a certain temperature gradient with the heating rate of 4 ℃/min, and presintering for 3h at the temperature. The temperature is reduced to the room temperature at the rate of 0.5 ℃/min.
After the completion of the pre-firing, the mixture was taken out and put into a cleaned mortar to be manually ground for 30 minutes, to obtain a premix.
The premix is put into a clean crucible and put into a tube furnace for sintering treatment in a flowing oxygen atmosphere. Heating up to 1300 ℃ according to a certain temperature gradient with the heating rate of 4 ℃/min, and sintering for 15h at the temperature. Cooling to room temperature at a rate of 2 deg.C/min to obtain Y-type hexagonal ferrite material (Ba) 0.01 Sr 1.99 Zn 2 Fe 12 O 22 )。
The Y-type hexaferrite material (Ba) obtained in this example 0.01 Sr 1.99 Zn 2 Fe 12 O 22 ) All aspects of the Properties and Y-type Hexahexaferrite Material (Ba) obtained in example 1 0.5 Sr 1.5 Zn 2 Fe 12 O 22 ) Are substantially identical in performance.
In conclusion, the Y-type hexaferrite material has high magnetic permeability.
The foregoing descriptions of specific exemplary embodiments of the present invention have been presented for purposes of illustration and description. It is not intended to limit the invention to the precise form disclosed, and obviously many modifications and variations are possible in light of the above teaching. The exemplary embodiments were chosen and described in order to explain certain principles of the invention and its practical application to enable one skilled in the art to make and use various exemplary embodiments of the invention and various alternatives and modifications as are suited to the particular use contemplated. It is intended that the scope of the invention be defined by the claims and their equivalents.
Claims (10)
1. A Y-type hexaferrite material is characterized in that the chemical formula is as follows: (Ba) x Sr 2-x )(A 2 )Fe 12 O 22 Wherein A is any one of Co, mg, mn and Zn, and x is more than or equal to 0 and less than or equal to 2.
2. The preparation method of the Y-type hexaferrite material as claimed in claim 1, characterized by comprising the following steps:
s1, mixing, grinding and drying the raw materials to obtain a premix;
s2, sintering the premix to obtain the Y-shaped hexagonal ferrite material;
the raw materials comprise a Ba source, a Sr source, an A source and a Fe source, wherein the A source is any one of a Co source, a Mg source, a Mn source and a Zn source.
3. The method for preparing a Y-hexaferrite material of claim 2, wherein the Ba source is barium carbonate; and/or the presence of a gas in the gas,
the Sr source is strontium carbonate; and/or the presence of a gas in the gas,
the iron source is Fe 2 O 3 (ii) a And/or the presence of a gas in the atmosphere,
the A source is any one of Co, mg, mn and Zn oxides.
4. The method for preparing a Y-type hexaferrite material as claimed in claim 2, wherein the molar ratio of Ba element, sr element, a element and Fe element in the raw material is x: (2-x): 2:12, wherein x is more than or equal to 0 and less than or equal to 2.
5. The method for preparing a Y-hexaferrite material as claimed in claim 2, wherein in step S1, the grinding step comprises: and performing ball milling treatment on the mixed raw materials.
6. The method for preparing a Y-type hexaferrite material as claimed in claim 5, wherein the step of ball milling treatment comprises:
putting the mixed raw materials into a ball mill, and ball-milling for 12-20h at the rotating speed of 100r/min to 350 r/min.
7. The method of preparing a Y-hexaferrite material of claim 2, wherein in step S1, the step of obtaining a premix comprises:
and pre-burning the mixed, ground and dried raw materials to obtain the premix.
8. The method for preparing a Y-type hexaferrite material as claimed in claim 7, wherein said pre-firing step comprises:
mixing, grinding, drying in flowing oxygen atmosphere or air atmosphere, heating to 900-1000 deg.C at 2-4 deg.C/min, and pre-sintering at the temperature for 3-10 hr;
then the temperature is reduced to the room temperature at the cooling rate of 0.5-1 ℃/min.
9. The method for preparing a Y-type hexaferrite material as claimed in claim 2, wherein in step S2, the step of sintering process comprises:
the premix is in flowing oxygen atmosphere, and is heated to 1150-1300 ℃ at the heating rate of 2-4 ℃/min, and is sintered for 15-18h at the temperature;
then the temperature is reduced to the room temperature at the speed of 1-2 ℃/min.
10. A microwave device comprising the Y-hexaferrite material of claim 1.
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| CN102173762A (en) * | 2010-12-13 | 2011-09-07 | 北矿磁材科技股份有限公司 | Ferrite wave-absorbing material used for injection moulding, preparation method thereof and magnetic wave-absorbing element |
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