Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, provide a kind of and do not change device layout and under the prerequisite keeping its index to meet the demands, improve it to high second harmonic suppression gyromagnetic material of second harmonic rejection ability and preparation method thereof.
The object of the invention is to be achieved through the following technical solutions:
A kind of high second harmonic suppresses gyromagnetic material, and the formula molecular formula of this material is Y
2.8ca
0.1gd
0.1v
0.05in
0.32fe
(4.63-n)o
12, n=0.12 ~ 0.16.
Further, the formula molecular formula of described material is Y
2.8ca
0.1gd
0.1v
0.05in
0.32fe
(4.63-n)o
12, n=0.13 ~ 0.15.
Further, the formula molecule of described material is Y
2.8ca
0.1gd
0.1v
0.05in
0.32fe
(4.63-n)o
12, n=0.14.
High second harmonic suppresses a preparation method for gyromagnetic material, comprises the following steps:
S1. prepare burden: take raw material Y in proportion
2o
3, CaCO
3, Gd
2o
3, V
2o
5, In
2o
3and Fe
2o
3carry out mixed preparing, obtain mixed dry material;
S2. a ball milling: according to mixed dry material: water: the weight ratio of steel ball is that ball milling is carried out in 1:1.0 ~ 1.4:4.3 ~ 4.7, and drum's speed of rotation is 50 ~ 70r/min, and Ball-milling Time is 16 ~ 20h;
S3. discharging is dried: dried by the slip after ball milling, bake out temperature is 160 ~ 200 DEG C, and drying time is 4 ~ 12h;
S4. pre-burning: pulverized by the material after drying in step S3, cross the accurate sub-sieve of 60 target, be pressed into 150 ~ 200g cake, then put into chamber type electric resistance furnace pre-burning, calcined temperature is 1000 ~ 1200 DEG C, insulation 2 ~ 6h;
S5. secondary ball milling: the cake after pre-burning is smashed to pieces, cross the accurate sub-sieve of 60 target and make powder, according to powder: water: secondary ball milling is carried out in weight ratio 1:1.0 ~ 1.3:3.3 ~ 3.7 of steel ball, drum's speed of rotation is 87 ~ 93r/min, and Ball-milling Time is 18 ~ 24h;
S6. granulation is dried: the slip of secondary ball milled is carried out oven dry and obtain drying siccative, bake out temperature is 100 ~ 140 DEG C, and drying time is 8 ~ 12h, adds and dries siccative quality 9 ~ 11%, the PVA glue granulation of concentration 9 ~ 11%, crosses the accurate sub-sieve of 120 target;
S7. shaping: being dried by the material after sieving to water ratio is 3.00 ~ 3.40% carry out sample compacting, and pressing pressure is 12 ~ 18MPa;
S8. sinter: sintered by the sample suppressed, sintering temperature is 1300 ~ 1460 DEG C, and soaking time is 6 ~ 10h.
In described step S2 and step S5, the water of a ball milling and secondary ball milling is distilled water.
The invention has the beneficial effects as follows: the usual iron deficiency amount in (1) this area between 0 ~ 0.12, and iron deficiency amount n value of the present invention 0.12 ~ 0.16 mainly in order to suppress ferrous iron to produce, reduce gyromagnetic material to electromagnetic loss;
(2) the gyromagnetic material insertion loss≤0.4dB of the present invention's making, isolation>=22dB, standing wave≤1.25, phase place
, consistent with previous level, second harmonic suppresses to bring up to more than 20dB by original below 18dB.
Embodiment
Below in conjunction with embodiment, technical scheme of the present invention is described in further detail, but protection scope of the present invention is not limited to the following stated.
One, embodiment is prepared:
[embodiment 1] a kind of high second harmonic suppresses gyromagnetic material, and this gyromagnetic material formula is: Y
2.8ca
0.1gd
0.1v
0.05in
0.32fe
(4.63-n)o
12, n=0.12.
Produce this gyromagnetic material 1000g, the concrete consumption of each component raw material is as follows: Y
2o
3for 419.7g, CaCO
3for 13.3g, Gd
2o
3for 24g, V
2o
5for 6g, In
2o
3for 59g, Fe
2o
3for 478g.
High second harmonic suppresses a preparation method for gyromagnetic material, comprises the steps:
S1. prepare burden: take raw material Y in proportion
2o
3, CaCO
3, Gd
2o
3, V
2o
5, In
2o
3and Fe
2o
3carry out mixed preparing, obtain mixed dry material;
S2. a ball milling: according to mixed dry material: water: steel ball weight ratio is that 1:1.0:4.3 carries out ball milling, and the concrete consumption of raw material, water and steel ball is respectively: raw material 1000g, water 1200g, steel ball 4500g, and drum's speed of rotation is 50r/min, and Ball-milling Time is 16h;
S3. discharging is dried: dried by the slip after ball milling, bake out temperature is 160 DEG C, and drying time is 12h;
S4. pulverized by the material after oven dry in step S3, cross the accurate sub-sieve of 60 target, be pressed into about 150g cake, then put into chamber type electric resistance furnace pre-burning, calcined temperature is 1000 DEG C, insulation 6h;
S5. secondary ball milling: the cake after pre-burning is smashed to pieces, cross the accurate sub-sieve of 60 target and make powder, according to powder: water: the weight ratio 1:1.0:3.3 of steel ball carries out secondary ball milling, the concrete consumption of raw material, water and steel ball is respectively: 1000g, 1100g, 3500g, drum's speed of rotation is 87r/min, and Ball-milling Time is 18h;
S6. granulation is dried: the slip of secondary ball milled is carried out oven dry and obtain drying siccative, bake out temperature is 100 DEG C, and drying time is 8h, and add and dry siccative quality 9%, concentration is the glue granulation of the PVA of 9%, crosses the accurate sub-sieve of 120 target;
S7. shaping: being dried by the material after sieving to water ratio is 3.00% carry out sample compacting, and pressing pressure is 12MPa;
S8. sinter: sintered by the sample suppressed, sintering temperature is 1300 DEG C, and soaking time is 10h.
In described step S2 and step S5, the water of a ball milling and secondary ball milling is distilled water.
[embodiment 2] a kind of high second harmonic suppresses gyromagnetic material, and this gyromagnetic material formula is: Y
2.8ca
0.1gd
0.1v
0.05in
0.32fe
(4.63-n)o
12, n=0.13.
Produce this gyromagnetic material 1000g, the concrete consumption of each component is as follows: Y
2o
3for 420.1g, CaCO
3for 13.3g, Gd
2o
3for 24.1g, V
2o
5for 6g, In
2o
3for 59g, Fe
2o
3for 477.5g.
High second harmonic suppresses a preparation method for gyromagnetic material, comprises the following steps:
S1. prepare burden: take raw material Y in proportion
2o
3, CaCO
3, Gd
2o
3, V
2o
5, In
2o
3and Fe
2o
3carry out mixed preparing, obtain mixed dry material;
S2. a ball milling: according to mixed dry material: water: the weight ratio of steel ball is that 1:1.2:4.5 carries out ball milling, and drum's speed of rotation is 65r/min, and Ball-milling Time is 18h;
S3. discharging is dried: dried by the slip after ball milling, bake out temperature is 180 DEG C, and drying time is 8h;
S4. pulverized by the material after oven dry in step S3, cross the accurate sub-sieve of 60 target, be pressed into about 160g cake, then put into chamber type electric resistance furnace pre-burning, calcined temperature is 1150 DEG C, insulation 5h;
S5. secondary ball milling: the cake after pre-burning is smashed to pieces, cross the accurate sub-sieve of 60 target and make powder, according to powder: water: the weight ratio 1:1.2:3.6 of steel ball carries out secondary ball milling, drum's speed of rotation is 90r/min, and Ball-milling Time is 20h;
S6. granulation is dried: the slip of secondary ball milled is carried out oven dry and obtain drying siccative, bake out temperature is 125 DEG C, and drying time is 11h, adds and dries siccative quality 10%, the PVA glue granulation of concentration 10%, crosses the accurate sub-sieve of 120 target;
S7. shaping: being dried by the material after sieving to water ratio is 3.30% carry out sample compacting, and pressing pressure is 13MPa;
S8. sinter: sintered by the sample suppressed, sintering temperature is 1350 DEG C, and soaking time is 8h.
In described step S2 and step S5, the water of a ball milling and secondary ball milling is distilled water.
[embodiment 3] a kind of high second harmonic suppresses gyromagnetic material, and this gyromagnetic material formula is: Y
2.8ca
0.1gd
0.1v
0.05in
0.32fe
(4.63-n)o
12, n=0.14.
Produce this gyromagnetic material 1000g, the concrete consumption of each component is as follows: Y
2o
3for 420.5g, CaCO
3for 13.3g, Gd
2o
3for 24.1g, V
2o
5for 6.1g, In
2o
3for 59.1g, Fe
2o
3for 476.9g.
High second harmonic suppresses a preparation method for gyromagnetic material, comprises the steps:
S1. prepare burden: take raw material Y in proportion
2o
3, CaCO
3, Gd
2o
3, V
2o
5, In
2o
3and Fe
2o
3carry out mixed preparing, obtain mixed dry material;
S2. a ball milling: according to mixed dry material: water: steel ball weight ratio is 1:1:4.7, the concrete consumption of raw material, water and steel ball is respectively: 1000g, 1000g, 4700g, and drum's speed of rotation is 70r/min, and Ball-milling Time is 16h;
S3. discharging is dried: dried by the slip after ball milling, bake out temperature is 160 DEG C, and drying time is 6h;
S4. pulverized by the material after oven dry in step S3, cross the accurate sub-sieve of 60 target, be pressed into about 170g cake, then put into chamber type electric resistance furnace pre-burning, calcined temperature is 1100 DEG C, insulation 6h;
S5. secondary ball milling: smashed to pieces by the cake after pre-burning, crosses the accurate sub-sieve of 60 target and makes powder, according to powder: water: the weight ratio 1:1.3:3.3 of steel ball, the concrete consumption of raw material, water and steel ball is respectively: 1000g, 1300g, 3300g, drum's speed of rotation is 93r/min, and Ball-milling Time is 24h;
S6. granulation is dried: the slip that secondary ball milled is housed is carried out oven dry and obtain drying siccative, bake out temperature is 100 DEG C, and drying time is 12h, and add and dry siccative quality 11%, concentration is the glue granulation of the PVA of 9%, crosses the accurate sub-sieve of 120 target;
S7. shaping: being dried by the material after sieving to water ratio is 3.10% carry out sample compacting, and pressing pressure is 15MPa;
S8. sinter: sintered by the sample suppressed, sintering temperature is 1400 DEG C, and soaking time is 8h.
In described step S2 and step S5, the water of a ball milling and secondary ball milling is distilled water.
[embodiment 4] a kind of high second harmonic suppresses gyromagnetic material, and this gyromagnetic material formula is: Y
2.8ca
0.1gd
0.1v
0.05in
0.32fe
(4.63-n)o
12, n=0.15.
Produce this gyromagnetic material 1000g, the concrete consumption of each component is as follows: Y
2o
3for 421g, CaCO
3for 13.3g, Gd
2o
3for 24.1g, V
2o
5for 6.1g, In
2o
3for 59.2g, Fe
2o
3for 476.3g.
High second harmonic suppresses a preparation method for gyromagnetic material, comprises the following steps:
S1. prepare burden: take raw material Y in proportion
2o
3, CaCO
3, Gd
2o
3, V
2o
5, In
2o
3and Fe
2o
3carry out mixed preparing, obtain mixed dry material;
S2. a ball milling: according to mixed dry material: water: the weight ratio of steel ball is that 1:1.2:4.2 carries out ball milling, and drum's speed of rotation is 55r/min, and Ball-milling Time is 17h;
S3. discharging is dried: dried by the slip after ball milling, bake out temperature is 180 DEG C, and drying time is 9h;
S4. pulverized by the material after oven dry in step S3, cross the accurate sub-sieve of 60 target, be pressed into about 180g cake, then put into chamber type electric resistance furnace pre-burning, calcined temperature is 1050 DEG C, insulation 6h;
S5. secondary ball milling: the cake after pre-burning is smashed to pieces, cross the accurate sub-sieve of 60 target and make powder, according to powder: water: the weight ratio 1:1.1:3.6 of steel ball carries out secondary ball milling, drum's speed of rotation is 88r/min, and Ball-milling Time is 21h;
S6. granulation is dried: the slip of secondary ball milled is carried out oven dry and obtain drying siccative, bake out temperature is 125 DEG C, and drying time is 11h, adds and dries siccative quality 9%, the PVA glue granulation of concentration 10%, crosses the accurate sub-sieve of 120 target;
S7. shaping: being dried by the material after sieving to water ratio is 3.20% carry out sample compacting, and pressing pressure is 16MPa;
S8. sinter: sintered by the sample suppressed, sintering temperature is 1450 DEG C, and soaking time is 9h.
In described step S2 and step S5, the water of a ball milling and secondary ball milling is distilled water.
[embodiment 5] a kind of high second harmonic suppresses gyromagnetic material, and this gyromagnetic material formula is: Y
2.8ca
0.1gd
0.1v
0.05in
0.32fe
(4.63-n)o
12, n=0.16.
Produce this gyromagnetic material 1000g, the concrete consumption of each component raw material is as follows: Y
2o
3for 421.4g, CaCO
3for 13.3g, Gd
2o
3for 24.2g, V
2o
5for 6.1g, In
2o
3for 59.2g, Fe
2o
3for 475.8g.
High second harmonic suppresses a preparation method for gyromagnetic material, comprises the steps:
S1. prepare burden: take raw material Y in proportion
2o
3, CaCO
3, Gd
2o
3, V
2o
5, In
2o
3and Fe
2o
3carry out mixed preparing, obtain mixed dry material;
S2. a ball milling: according to mixed dry material: water: the weight ratio of steel ball is that 1:1.4:4.7 carries out ball milling, and drum's speed of rotation is 70r/min, and Ball-milling Time is 20h;
S3. discharging is dried: dried by the slip after ball milling, bake out temperature is 200 DEG C, and drying time is 4h;
S4. pulverized by the material after oven dry in step S3, cross the accurate sub-sieve of 60 target, be pressed into about 200g cake, then put into chamber type electric resistance furnace pre-burning, calcined temperature is 1200 DEG C, insulation 2h;
S5. secondary ball milling: the cake after pre-burning is smashed to pieces, cross the accurate sub-sieve of 60 target and make powder, according to powder: water: secondary ball milling is carried out in weight ratio 1:1.0 ~ 1.3:3.3 ~ 3.7 of steel ball, drum's speed of rotation is 93r/min, and Ball-milling Time is 24h;
S6. granulation is dried: the slip of secondary ball milled is carried out oven dry and obtain drying siccative, bake out temperature is 140 DEG C, and drying time is 8h, adds and dries siccative quality 11%, the PVA glue granulation of concentration 11%, crosses the accurate sub-sieve of 120 target;
S7. shaping: being dried by the material after sieving to water ratio is 3.40% carry out sample compacting, and pressing pressure is 12 ~ 18MPa;
S8. sinter: sintered by the sample suppressed, sintering temperature is 1460 DEG C, and soaking time is 6h.
In described step S2 and step S5, the water of a ball milling and secondary ball milling is distilled water.
Two, experimental example:
1, suppress gyromagnetic material to carry out performance test the high second harmonic of gained in embodiment 1 ~ 5, test 4 π Ms, Curie temperature T
c, test its live width △ H, DIELECTRIC CONSTANT ε
r, tangent of the dielectric loss angle tan δ.Result is as table 1:
The high second harmonic of table 1 each embodiment gained suppresses gyromagnetic material the performance test results
Found out that by table the basic parameter changes such as saturation magnetization, Curie temperature, ferromagnetic resonance line width are little.
2, suppress gyromagnetic material to be undertaken being applied in circulator by multi-disc assembling the high second harmonic of gained in embodiment 1 ~ 5, parameter is as following table 2:
The gyromagnetic material of each embodiment gained of table 2 is applied to the canonical parameter test result in circulator
From table, within the scope of the operating frequency 1.2-1.4GHz of this circulator, along with the iron deficiency amount n value in gyromagnetic material formula is changed from small to big, second harmonic suppresses increasing, but insertion loss is also increasing, index listed in table all meets device service requirements.But as can be seen from variation tendency, when n value is larger, second harmonic suppresses may be larger, if do not have other measure of control, the loss of device will exceed standard, but this is being applicable to the less demanding occasion of insertion loss.