CN104909740B - A kind of high second harmonic suppresses gyromagnetic material and preparation method thereof - Google Patents
A kind of high second harmonic suppresses gyromagnetic material and preparation method thereof Download PDFInfo
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Abstract
Suppress gyromagnetic material the invention discloses a kind of high second harmonic, the formula molecular formula of the material is Y2.8Ca0.1Gd0.1V0.05In0.32Fe（4.63‑n）O12, n=0.12~0.16；A kind of high second harmonic suppresses the preparation method of gyromagnetic material, comprises the following steps：S1. dispensing：Raw material Y is weighed in proportion2O3、CaCO3、Gd2O3、V2O5、In2O3And Fe2O3Carry out mixed preparing and obtain mixed dry material；S2. a ball milling；S3. discharging drying, the good slurry of ball milling is dried；S4. pre-burning, is put into pre-burning in chamber type electric resistance furnace；S5. secondary ball milling；S6. drying granulation：Add the granulation of PVA glue；S7. it is molded：Moisture content dries for 3.00 ~ 3.40% powder after sieving, and carries out sample compacting, and pressing pressure is 12 ~ 18MPa；S8. sinter：The sample suppressed is sintered, sintering temperature is 1300 ~ 1460 DEG C, soaking time is 6 ~ 10h.Gyromagnetic material insertion loss≤0.4dB of the present invention, isolation >=22dB, standing wave≤1.25, phase0± 5 °, consistent with previous level, second harmonic suppresses to bring up to more than 20dB by original below 18dB.
Description
Technical field
The present invention relates to a kind of gyromagnetic ferrite material containing elements such as Y, Ca, Gd, V, In and Fe and preparation method thereof,
Belong to magnetic composite field.
Background technology
Gyromagnetic ferrite is also known as microwave ferrite, and it has the characteristic of tensor permeability, i.e., mutually perpendicular steady at two
In the presence of Constant charge soil and electromagnetic wave magnetic field, when plane polarized electromagnetic wave is propagated in certain direction in gyromagnetic ferrite, partially
Face meeting of shaking constantly rotate around the direction of propagation, using this characteristic, waveguide or transmission line that gyromagnetic ferrite can be with conveying microwave
Deng the various microwave devices of composition.Gyromagnetic ferrite mainly has polymorphic and the major class of monocrystalline type two.Showing for monocrystalline type is of little use.Polycrystalline
Type, by structure point, mainly have：
(1) spinel-type, such as MgFe2O4System, NiFe2O4System, LiFe systems, Mg-Mn-Al systems, Nb-Co-A1 systems, Li-Zn-
Ti-Co systems etc.；
(2) carbuncle type, such as Y3F5O12, Y-Al systems, Y-Gd systems, Y-Gd-Al systems etc.；
(3) Magnetoplumbate-type, such as BaFe12O19Deng.
Gyromagnetic ferrite usually requires that its ferromagnetic resonance line width is small, spin wave resonance linewidth is big, dielectric loss is low, temperature is steady
Qualitative high, using electronic ceramic process, dry-pressing formed, oxygen atmosphere sintering is fabricated by, and is mainly used in making microwave ferrite
Device.
Chinese patent CN102603278B provides a kind of preparation method of nickel-zinc-ferrite material, using oxide legal system
It is standby, sinter under certain condition, crystal grain size is 20~30 μm after sintering, there is obvious crystal boundary, product, which has, is answering masterpiece
Change less feature with lower inductance, meet the needs of requirement of the power inductance of resin-encapsulated to Ferrite Material resistance to stress.In
State's patent 200910309272.9 discloses a kind of preparation method of Mg-Mn-Zn series ferrite materials, using MgZn ferrite and
Manganese-zinc ferrite is mixed, and has been obtained higher relaxation frequency, has also been obtained the frequency of use of wideband.
The saturation magnetization 4πms of gyromagnetic material determine the working frequency f of device0, ferromagnetic resonance line width Δ H resolvers
Bandwidth of operation Δ f, loss angle tangent the tg δ of partεThe insertion loss IL (insertion loss) of device is determined, in addition with width
Consistent property, harmonics restraint, intermodulation crosstalk etc..The performance indications of common circulator/isolator mainly have insertion loss, isolation,
Voltage standing wave ratio, but as modern communication technology develops, the second harmonic, triple-frequency harmonics or even higher order harmonics of device are suppressed
Ability, which is proposed, to be distinctly claimed.
The content of the invention
Do not change device design it is an object of the invention to overcome the deficiencies of the prior art and provide one kind and keep it to refer to
Mark improves its high second harmonic suppression gyromagnetic material and its preparation side to second harmonic rejection ability on the premise of meeting requirement
Method.
The purpose of the present invention is achieved through the following technical solutions：
A kind of high second harmonic suppresses gyromagnetic material, and the formula molecular formula of the material is
Y2.8Ca0.1Gd0.1V0.05In0.32Fe(4.63-n)O12, n=0.12~0.16.
Further, the formula molecular formula of the material is Y2.8Ca0.1Gd0.1V0.05In0.32Fe(4.63-n)O12, n=0.13
~0.15.
Further, the formula molecule of the material is Y2.8Ca0.1Gd0.1V0.05In0.32Fe(4.63-n)O12, n=0.14.
A kind of high second harmonic suppresses the preparation method of gyromagnetic material, comprises the following steps：
S1. dispensing：Raw material Y is weighed in proportion2O3、CaCO3、Gd2O3、V2O5、In2O3And Fe2O3Mixed preparing is carried out, is obtained
Mixed dry material；
S2. a ball milling：According to mixed dry material：Water：The weight ratio of steel ball is 1：1.0~1.4：4.3~4.7 carry out ball
Mill, drum's speed of rotation is 50~70r/min, and Ball-milling Time is 16~20h；
S3. discharging drying：By the slurry drying after ball milling, drying temperature is 160~200 DEG C, and drying time is 4~12h；
S4. pre-burning：Material after being dried in step S3 is pulverized, the quasi- sub-sieve of 60 targets is crossed, 150~200g circles are pressed into
Cake, is then placed in pre-burning in chamber type electric resistance furnace, and calcined temperature is 1000~1200 DEG C, is incubated 2~6h；
S5. secondary ball milling：Cake after pre-burning is smashed to pieces, the quasi- sub-sieve of 60 targets is crossed and powder is made, according to powder：Water：
The weight of steel ball compares 1：1.0~1.3：3.3~3.7 carry out secondary ball milling, and drum's speed of rotation is 87~93r/min, Ball-milling Time
For 18~24h；
S6. drying granulation：The slurry of secondary ball milled dry and obtains drying siccative, drying temperature is 100~140
DEG C, drying time is 8~12h, adds drying siccative quality 9~11%, and 120 mesh are crossed in the PVA glue granulation of concentration 9~11%
Standard sub-sieve；
S7. it is molded：It is 3.00~3.40% progress sample compactings, pressing pressure that a material after sieving, which is dried to moisture content,
For 12~18MPa；
S8. sinter：The sample suppressed is sintered, sintering temperature be 1300~1460 DEG C, soaking time be 6~
10h。
The water of a ball milling and secondary ball milling is distilled water in the step S2 and step S5.
The beneficial effects of the invention are as follows：(1) the usual iron deficiency amount in this area is between 0~0.12, and iron deficiency amount n of the present invention
Value is produced 0.12~0.16 primarily to suppressing ferrous iron, loss of the reduction gyromagnetic material to electromagnetic wave；
(2) gyromagnetic material insertion loss≤0.4dB that the present invention makes, isolation >=22dB, standing wave≤1.25, phase, consistent with previous level, second harmonic suppresses to bring up to more than 20dB by original below 18dB.
Embodiment
Technical scheme is described in further detail with reference to embodiment, but protection scope of the present invention is not limited to
In as described below.
First, embodiment is prepared：
【Embodiment 1】A kind of high second harmonic suppresses gyromagnetic material, and the gyromagnetic material formula is：Y2.8Ca0.1Gd0.1V0.05I
n0.32Fe(4.63-n)O12, n=0.12.
Gyromagnetic material 1000g is produced, the specific consumption of each component raw material is as follows：Y2O3For 419.7g, CaCO3For
13.3g, Gd2O3For 24g, V2O5For 6g, In2O3For 59g, Fe2O3For 478g.
A kind of high second harmonic suppresses the preparation method of gyromagnetic material, comprises the steps：
S1. dispensing：Raw material Y is weighed in proportion2O3、CaCO3、Gd2O3、V2O5、In2O3And Fe2O3Mixed preparing is carried out, is obtained
Mixed dry material；
S2. a ball milling：According to mixed dry material：Water：Steel ball weight ratio is 1：1.0：4.3 carry out ball milling, raw material, water and steel
Ball body consumption is respectively：Raw material 1000g, water 1200g, steel ball 4500g, drum's speed of rotation is 50r/min, and Ball-milling Time is
16h；
S3. discharging drying：Slurry after ball milling is dried, drying temperature is 160 DEG C, and drying time is 12h；
S4. the material after being dried in step S3 is pulverized, crosses the quasi- sub-sieve of 60 targets, be pressed into 150g or so cakes, then
Pre-burning in chamber type electric resistance furnace is put into, calcined temperature is 1000 DEG C, is incubated 6h；
S5. secondary ball milling：Cake after pre-burning is smashed to pieces, the quasi- sub-sieve of 60 targets is crossed and powder is made, according to powder：Water：
The weight of steel ball compares 1：1.0：3.3 carry out secondary ball milling, and raw material, water and the specific consumption of steel ball are respectively：1000g、1100g、
3500g, drum's speed of rotation is 87r/min, and Ball-milling Time is 18h；
S6. drying granulation：The slurry of secondary ball milled dry and obtains drying siccative, drying temperature is 100 DEG C, is dried
The dry time is 8h, adds drying siccative quality 9%, and concentration is 9% PVA glue granulation, crosses the quasi- sub-sieve of 120 targets；
S7. it is molded：It is 3.00% progress sample compacting that a material after sieving, which is dried to moisture content, and pressing pressure is
12MPa；
S8. sinter：The sample suppressed is sintered, sintering temperature is 1300 DEG C, and soaking time is 10h.
The water of a ball milling and secondary ball milling is distilled water in the step S2 and step S5.
【Embodiment 2】A kind of high second harmonic suppresses gyromagnetic material, and the gyromagnetic material formula is：
Y2.8Ca0.1Gd0.1V0.05In0.32Fe(4.63-n)O12, n=0.13.
Gyromagnetic material 1000g is produced, the specific consumption of each component is as follows：Y2O3For 420.1g, CaCO3For 13.3g,
Gd2O3For 24.1g, V2O5For 6g, In2O3For 59g, Fe2O3For 477.5g.
A kind of high second harmonic suppresses the preparation method of gyromagnetic material, comprises the following steps：
S1. dispensing：Raw material Y is weighed in proportion2O3、CaCO3、Gd2O3、V2O5、In2O3And Fe2O3Mixed preparing is carried out, is obtained
Mixed dry material；
S2. a ball milling：According to mixed dry material：Water：The weight ratio of steel ball is 1：1.2：4.5 carry out ball milling, and ball mill turns
Speed is 65r/min, and Ball-milling Time is 18h；
S3. discharging drying：Slurry after ball milling is dried, drying temperature is 180 DEG C, and drying time is 8h；
S4. the material after being dried in step S3 is pulverized, crosses the quasi- sub-sieve of 60 targets, be pressed into 160g or so cakes, then
Pre-burning in chamber type electric resistance furnace is put into, calcined temperature is 1150 DEG C, is incubated 5h；
S5. secondary ball milling：Cake after pre-burning is smashed to pieces, the quasi- sub-sieve of 60 targets is crossed and powder is made, according to powder：Water：
The weight of steel ball compares 1：1.2：3.6 carry out secondary ball milling, and drum's speed of rotation is 90r/min, and Ball-milling Time is 20h；
S6. drying granulation：The slurry of secondary ball milled dry and obtains drying siccative, drying temperature is 125 DEG C, is dried
The dry time is 11h, adds drying siccative quality 10%, and the quasi- sub-sieve of 120 targets is crossed in the PVA glue granulation of concentration 10%；
S7. it is molded：It is 3.30% progress sample compacting that a material after sieving, which is dried to moisture content, and pressing pressure is
13MPa；
S8. sinter：The sample suppressed is sintered, sintering temperature is 1350 DEG C, and soaking time is 8h.
The water of a ball milling and secondary ball milling is distilled water in the step S2 and step S5.
【Embodiment 3】A kind of high second harmonic suppresses gyromagnetic material, and the gyromagnetic material formula is：
Y2.8Ca0.1Gd0.1V0.05In0.32Fe(4.63-n)O12, n=0.14.
Production gyromagnetic material 1000g, the specific consumption of each component is as follows：Y2O3For 420.5g, CaCO3For 13.3g,
Gd2O3For 24.1g, V2O5For 6.1g, In2O3For 59.1g, Fe2O3For 476.9g.
A kind of high second harmonic suppresses the preparation method of gyromagnetic material, comprises the steps：
S1. dispensing：Raw material Y is weighed in proportion2O3、CaCO3、Gd2O3、V2O5、In2O3And Fe2O3Mixed preparing is carried out, is obtained
Mixed dry material；
S2. a ball milling：According to mixed dry material：Water：Steel ball weight ratio is 1：1：4.7, raw material, water and the specific consumption of steel ball
Respectively：1000g, 1000g, 4700g, drum's speed of rotation are 70r/min, and Ball-milling Time is 16h；
S3. discharging drying：Slurry after ball milling is dried, drying temperature is 160 DEG C, and drying time is 6h；
S4. the material after being dried in step S3 is pulverized, crosses the quasi- sub-sieve of 60 targets, be pressed into 170g or so cakes, then
Pre-burning in chamber type electric resistance furnace is put into, calcined temperature is 1100 DEG C, is incubated 6h；
S5. secondary ball milling：Cake after pre-burning is smashed to pieces, the quasi- sub-sieve of 60 targets is crossed and powder is made, according to powder：Water：
The weight of steel ball compares 1：1.3：3.3, raw material, water and the specific consumption of steel ball are respectively：1000g, 1300g, 3300g, ball mill turn
Speed is 93r/min, and Ball-milling Time is 24h；
S6. drying granulation：Will be equipped with secondary ball milled slurry carry out dry obtain dry siccative, drying temperature is 100
DEG C, drying time is 12h, adds drying siccative quality 11%, and concentration is 9% PVA glue granulation, crosses 120 mesh standard scores
Sample is sieved；
S7. it is molded：It is 3.10% progress sample compacting that a material after sieving, which is dried to moisture content, and pressing pressure is
15MPa；
S8. sinter：The sample suppressed is sintered, sintering temperature is 1400 DEG C, and soaking time is 8h.
The water of a ball milling and secondary ball milling is distilled water in the step S2 and step S5.
【Embodiment 4】A kind of high second harmonic suppresses gyromagnetic material, and the gyromagnetic material formula is：
Y2.8Ca0.1Gd0.1V0.05In0.32Fe(4.63-n)O12, n=0.15.
Gyromagnetic material 1000g is produced, the specific consumption of each component is as follows：Y2O3For 421g, CaCO3For 13.3g, Gd2O3
For 24.1g, V2O5For 6.1g, In2O3For 59.2g, Fe2O3For 476.3g.
A kind of high second harmonic suppresses the preparation method of gyromagnetic material, comprises the following steps：
S1. dispensing：Raw material Y is weighed in proportion2O3、CaCO3、Gd2O3、V2O5、In2O3And Fe2O3Mixed preparing is carried out, is obtained
Mixed dry material；
S2. a ball milling：According to mixed dry material：Water：The weight ratio of steel ball is 1：1.2：4.2 carry out ball milling, and ball mill turns
Speed is 55r/min, and Ball-milling Time is 17h；
S3. discharging drying：Slurry after ball milling is dried, drying temperature is 180 DEG C, and drying time is 9h；
S4. the material after being dried in step S3 is pulverized, crosses the quasi- sub-sieve of 60 targets, be pressed into 180g or so cakes, then
Pre-burning in chamber type electric resistance furnace is put into, calcined temperature is 1050 DEG C, is incubated 6h；
S5. secondary ball milling：Cake after pre-burning is smashed to pieces, the quasi- sub-sieve of 60 targets is crossed and powder is made, according to powder：Water：
The weight of steel ball compares 1：1.1：3.6 carry out secondary ball milling, and drum's speed of rotation is 88r/min, and Ball-milling Time is 21h；
S6. drying granulation：The slurry of secondary ball milled dry and obtains drying siccative, drying temperature is 125 DEG C, is dried
The dry time is 11h, adds drying siccative quality 9%, and the quasi- sub-sieve of 120 targets is crossed in the PVA glue granulation of concentration 10%；
S7. it is molded：It is 3.20% progress sample compacting that a material after sieving, which is dried to moisture content, and pressing pressure is
16MPa；
S8. sinter：The sample suppressed is sintered, sintering temperature is 1450 DEG C, and soaking time is 9h.
The water of a ball milling and secondary ball milling is distilled water in the step S2 and step S5.
【Embodiment 5】A kind of high second harmonic suppresses gyromagnetic material, and the gyromagnetic material formula is：
Y2.8Ca0.1Gd0.1V0.05In0.32Fe(4.63-n)O12, n=0.16.
Gyromagnetic material 1000g is produced, the specific consumption of each component raw material is as follows：Y2O3For 421.4g, CaCO3For
13.3g, Gd2O3For 24.2g, V2O5For 6.1g, In2O3For 59.2g, Fe2O3For 475.8g.
A kind of high second harmonic suppresses the preparation method of gyromagnetic material, comprises the steps：
S1. dispensing：Raw material Y is weighed in proportion2O3、CaCO3、Gd2O3、V2O5、In2O3And Fe2O3Mixed preparing is carried out, is obtained
Mixed dry material；
S2. a ball milling：According to mixed dry material：Water：The weight ratio of steel ball is 1：1.4：4.7 carry out ball milling, and ball mill turns
Speed is 70r/min, and Ball-milling Time is 20h；
S3. discharging drying：Slurry after ball milling is dried, drying temperature is 200 DEG C, and drying time is 4h；
S4. the material after being dried in step S3 is pulverized, crosses the quasi- sub-sieve of 60 targets, be pressed into 200g or so cakes, then
Pre-burning in chamber type electric resistance furnace is put into, calcined temperature is 1200 DEG C, is incubated 2h；
S5. secondary ball milling：Cake after pre-burning is smashed to pieces, the quasi- sub-sieve of 60 targets is crossed and powder is made, according to powder：Water：
The weight of steel ball compares 1：1.0~1.3：3.3~3.7 carry out secondary ball milling, and drum's speed of rotation is 93r/min, and Ball-milling Time is
24h；
S6. drying granulation：The slurry of secondary ball milled dry and obtains drying siccative, drying temperature is 140 DEG C, is dried
The dry time is 8h, adds drying siccative quality 11%, and the quasi- sub-sieve of 120 targets is crossed in the PVA glue granulation of concentration 11%；
S7. it is molded：By after sieving material dry to moisture content be 3.40% carry out sample compacting, pressing pressure be 12~
18MPa；
S8. sinter：The sample suppressed is sintered, sintering temperature is 1460 DEG C, and soaking time is 6h.
The water of a ball milling and secondary ball milling is distilled water in the step S2 and step S5.
2nd, experimental example：
1st, the high second harmonic of gained in embodiment 1~5 is suppressed into gyromagnetic material and carries out performance test, 4 π Ms of test, residence
In temperature Tc, test its line width △ H, permittivity εr, dielectric loss angle tangent tan δ.As a result such as table 1：
High second harmonic obtained by each embodiment of table 1 suppresses gyromagnetic material the performance test results
Find out that the change of the basic parameters such as saturation magnetization, Curie temperature, ferromagnetic resonance line width is little by table.
2nd, the high second harmonic of gained in embodiment 1~5 is suppressed into gyromagnetic material and ring is applied to by multi-disc assembling progress
In row device, parameter such as table 2 below：
Gyromagnetic material obtained by each embodiment of table 2 is applied to the canonical parameter test result in circulator
From table, in the range of the working frequency 1.2-1.4GHz of this circulator, lacking in being formulated with gyromagnetic material
Iron n values are changed from small to big, and second harmonic suppresses increasing, but insertion loss is also increasing, and listed index is equal in table
Meet device use requirement.But it can be seen from variation tendency when n values are bigger, second harmonic suppresses may be bigger, if
Without other control measure, the loss of device will be exceeded, but this is being applicable to the less demanding occasion of insertion loss.
Claims (2)
1. a kind of high second harmonic suppresses the preparation method of gyromagnetic material, it is characterised in that comprise the following steps：
S1. dispensing：Raw material Y is weighed in proportion2O3、CaCO3、Gd2O3、V2O5、In2O3And Fe2O3Mixed preparing is carried out, is mixed
Siccative；
S2. a ball milling：According to mixed dry material：Water：The weight ratio of steel ball is 1：1.0~1.4：4.3 ~ 4.7 carry out ball milling, ball milling
Machine rotating speed is 50 ~ 70r/min, and Ball-milling Time is 16 ~ 20h；
S3. discharging drying：By the slurry drying after ball milling, drying temperature is 160 ~ 200 DEG C, and drying time is 4 ~ 12h；
S4. pre-burning：Material after being dried in step S3 is pulverized, the quasi- sub-sieve of 60 targets is crossed, is pressed into 150 ~ 250g cakes, then
Pre-burning in chamber type electric resistance furnace is put into, calcined temperature is 1000 ~ 1200 DEG C, is incubated 2 ~ 6h；
S5. secondary ball milling：Cake after pre-burning is smashed to pieces, the quasi- sub-sieve of 60 targets is crossed and powder is made, according to powder：Water：Steel ball
Weight compare 1：1.0~1.3：3.3 ~ 3.7 carry out secondary ball millings, drum's speed of rotation be 87 ~ 93r/min, Ball-milling Time be 18 ~
24h；
S6. drying granulation：The slurry of secondary ball milled dry and obtains drying siccative, drying temperature is 100 ~ 140 DEG C, is dried
The dry time is 8 ~ 12h, adds drying siccative quality 9 ~ 11%, and the quasi- sub-sieve of 120 targets is crossed in the PVA glue granulation of concentration 9 ~ 11%；
S7. it is molded：By after sieving material dry to moisture content be 3.00 ~ 3.40% carry out sample compactings, pressing pressure be 12 ~
18MPa；
S8. sinter：The sample suppressed is sintered, sintering temperature is 1300 ~ 1460 DEG C, soaking time is 6 ~ 10h；Obtain
High second harmonic suppresses gyromagnetic material；
Wherein, the formula molecular formula that the high second harmonic suppresses gyromagnetic material is Y2.8Ca0.1Gd0.1V0.05In0.32Fe（4.63-n）
O12, n=0.14.
2. a kind of high second harmonic according to claim 1 suppresses the preparation method of gyromagnetic material, it is characterised in that described
The water of a ball milling and secondary ball milling is distilled water in step S2 and step S5.
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| CN108424135A (en) * | 2018-03-13 | 2018-08-21 | 海宁市天丰磁业有限公司 | A kind of preparation method of ferrite magnetic material |
| CN109836149B (en) * | 2019-03-26 | 2021-08-27 | 西南应用磁学研究所 | Garnet ferrite material with low magnetic moment, small loss and high temperature stability |
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