CN105236949A - High squareness ratio LiZnTi ferrite material and preparation method thereof - Google Patents
High squareness ratio LiZnTi ferrite material and preparation method thereof Download PDFInfo
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Abstract
The present invention provides a high squareness ratio LiZnTi ferrite material and a preparation method thereof, and belongs to the technical field of magnetic materials. The high squareness ratio LiZnTi ferrite material comprises, by weight, 96-99.8% of a main material and 0.2-4% of a glass auxiliary burning agent, wherein the main material is Li0.27Zn0.23Ti0.23Fe2.27O4, and the glass auxiliary agent is prepared from raw materials according to a BaCO3 to CaCO3 to ZnO to B2O3 to SiO2 of 2:1:7:8:2. According to the present invention, the sintering and the preparation of the LiZnTi ferrite material at the low temperature (880-940 DEG C) are achieved, and the obtained LiZnTi ferrite material has characteristics of high squareness ratio, low coercive force, and high magnetic flux density.
Description
Technical field
The invention belongs to technical field of magnetic materials, be specifically related to a kind of low-temperature sintering LiZnTi Ferrite Material with high squareness ratio and preparation method thereof.
Background technology
In recent years, Li series ferrite material has been widely used in Ka wave band and with the ferrite microwave device of super band, LiZnTi gyromagnetic ferrite is the one of Li series ferrite material, it has the advantages such as low-coercivity, high saturated magnetic induction, high residual magnetic flux density, obtains and pay attention to widely in the preparation of microwave device.
In the various parameters of gyromagnetic material, squareness ratio weighs an important indicator of material property quality, and the material hysteresis loop line steeper of high squareness ratio, applies also more extensive.When magnet ring is applied in electric ballast, the magnet ring with high squareness ratio magnetic hysteresis loop can effectively reduce the temperature rise of transistor switch, prolongs life; High square ratio magnetic material is also widely used in magnetic recording field, effectively can improve the information record efficiency of magnetic recording, shortens record required time, also can reduce the self-demagnetization effect affecting magnetic recording material performance simultaneously.Therefore, the LiZnTi Ferrite Material finding a kind of high squareness ratio is necessary.
Summary of the invention
The object of this invention is to provide a kind of LiZnTi Ferrite Material with high squareness ratio and preparation method thereof.By optimizing sintering process and adding the low-temperature sintering that glass sintering agent achieves LiZnTi, obtain the LiZnTi Ferrite Material with high squareness ratio, also improve the saturation induction density of material simultaneously, reduce coercive force, optimize material property.
Technical scheme of the present invention is as follows:
One has high squareness ratio LiZnTi Ferrite Material, is made up of major ingredient and glassy phase sintering agent, and wherein the weight percent of major ingredient is 96% ~ 99.8%, and the weight percent of glassy phase sintering agent is 0.2% ~ 4%, and described major ingredient is Li
0.27zn
0.23ti
0.23fe
2.27o
4, described glassy phase sintering agent by raw material according to mass ratio BaCO
3: CaCO
3: ZnO:B
2o
3: SiO
2=2:1:7:8:2 prepares.
The above-mentioned preparation method with high squareness ratio LiZnTi Ferrite Material, comprises the following steps:
Step 1: with Fe
2o
3, ZnO, TiO
2, Li
2cO
3for raw material, according to Li
0.27zn
0.23ti
0.23fe
2.27o
4the ratio weighing of molecular formula, preparation obtains main powder;
Step 2: according to the main powder of mass ratio: water: iron ball=1:(1.2 ~ 1.4): the ratio of 3 carries out a ball milling, Ball-milling Time is 4 ~ 8h, dry at 100 ~ 120 DEG C after taking-up, sintering oven put into by the powder obtained after oven dry, 800 ~ 820 DEG C are risen to by room temperature with the temperature rise rate of 2 DEG C/min, insulation 1 ~ 3h, then with stove Temperature fall to room temperature, obtain LiZnTi major ingredient;
Step 3: with BaCO
3, CaCO
3, ZnO, B
2o
3, SiO
2for raw material, by raw material according to mass ratio BaCO
3: CaCO
3: ZnO:B
2o
3: SiO
2the ratio batching of=2:1:7:8:2, wet ball grinding 6h, dry at 100 ~ 120 DEG C after taking-up, powder after oven dry is put into crucible and is placed in sintering oven, rise to 1300 DEG C with the temperature rise rate of 5 DEG C/min by room temperature and be incubated 1h, then directly taking-up is poured rapid quenching in deionized water into and is obtained BCZBS transparent vitreous body, wears into micron particles, namely obtain glassy phase sintering agent after oven dry;
Step 4: glassy phase sintering agent step 3 obtained adds in the major ingredient that step 2 obtains, be made into powder, wherein the weight percent of major ingredient is 96% ~ 99.8%, the weight percent of glassy phase sintering agent is 0.2% ~ 4%, carry out secondary ball milling, wherein, the weight ratio of powder, water and iron ball is 1:1:3, Ball-milling Time is 4 ~ 8h, and rotational speed of ball-mill is 250r/min; Then secondary ball abrasive material taken out and dry, add polyvinyl alcohol (PVA) granulating and forming and be pressed into blank, again blank is put into sintering oven, 880 ~ 940 DEG C are risen to the temperature rise rate of 2 DEG C/min, insulation 2h, with stove Temperature fall to room temperature, namely obtain described LiZnTi Ferrite Material.
Further, when being pressed into blank described in step 4, pressure is 8 ~ 10MPa.
Beneficial effect of the present invention is: the invention provides a kind of LiZnTi Ferrite Material with high squareness ratio and preparation method thereof, and in LiZnTi major ingredient, adding BCZBS, (concrete composition is BaCO
3, CaCO
3, ZnO, B
2o
3, SiO
2) glass sintering agent, not only achieve low-temperature sintering (880 ~ 940 DEG C), and improve the squareness ratio of material; The fusing point of BCZBS glassy phase sintering agent is lower, also nucleation and the grain growing of LiZnTi ferrite crystal grains effectively can be promoted under 880 ~ 940 DEG C of low-temperature sintering conditions, and obtained Ferrite Material homogeneity and compactness are all better, have high squareness ratio, high saturated magnetic induction.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph (SEM) of the Ferrite Material that the embodiment of the present invention 3 obtains with comparative example.Wherein, the SEM figure of (a) Ferrite Material of obtaining for embodiment 3; The SEM figure of b Ferrite Material that () obtains for comparative example.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is described further.
Embodiment 1
There is a preparation method for high squareness ratio LiZnTi Ferrite Material, comprise the following steps:
Step 1: with Fe
2o
3, ZnO, TiO
2, Li
2cO
3for raw material, according to Li
0.27zn
0.23ti
0.23fe
2.27o
4the ratio weighing of molecular formula, preparation obtains main powder;
Step 2: according to the main powder of mass ratio: water: the ratio of iron ball=1:1.2:3 carries out a ball milling, Ball-milling Time is 4h, dry at 100 DEG C after taking-up, sintering oven put into by the powder obtained after oven dry, 800 DEG C are risen to by room temperature with the temperature rise rate of 2 DEG C/min, insulation 3h, then with stove Temperature fall to room temperature, obtain LiZnTi major ingredient;
Step 3: with BaCO
3, CaCO
3, ZnO, B
2o
3, SiO
2for raw material, by raw material according to mass ratio BaCO
3: CaCO
3: ZnO:B
2o
3: SiO
2the ratio batching of=2:1:7:8:2, wet ball grinding 6h, dry at 100 DEG C after taking-up, powder after oven dry is put into crucible and is placed in sintering oven, rise to 1300 DEG C with the temperature rise rate of 5 DEG C/min by room temperature and be incubated 1h, then directly taking-up is poured rapid quenching in deionized water into and is obtained BCZBS transparent vitreous body, wears into micron particles, namely obtain glassy phase sintering agent after oven dry;
Step 4: glassy phase sintering agent step 3 obtained adds in the major ingredient that step 2 obtains, be made into powder, wherein the weight percent of major ingredient is 99.5%, the weight percent of glassy phase sintering agent is 0.5%, carry out secondary ball milling, wherein, the weight ratio of powder, water and iron ball is 1:1:3, Ball-milling Time is 6h, and rotational speed of ball-mill is 250r/min; Then secondary ball abrasive material taken out and dry, add polyvinyl alcohol (PVA) granulating and forming and be pressed into blank, forming pressure is 10MPa, again blank is put into sintering oven, rise to 920 DEG C with the temperature rise rate of 2 DEG C/min, insulation 2h, with stove Temperature fall to room temperature, namely obtain described LiZnTi Ferrite Material.
The performance of the LiZnTi Ferrite Material that embodiment 1 prepares is: sample rate: 4.14g/cm
3, saturation induction density: 268mT, coercive force: 315.2A/m, squareness ratio: 0.84.
Embodiment 2
There is a preparation method for high squareness ratio LiZnTi Ferrite Material, comprise the following steps:
Step 1: with Fe
2o
3, ZnO, TiO
2, Li
2cO
3for raw material, according to Li
0.27zn
0.23ti
0.23fe
2.27o
4the ratio weighing of molecular formula, preparation obtains main powder;
Step 2: according to the main powder of mass ratio: water: the ratio of iron ball=1:1.3:3 carries out a ball milling, Ball-milling Time is 6h, dry at 100 DEG C after taking-up, sintering oven put into by the powder obtained after oven dry, 820 DEG C are risen to by room temperature with the temperature rise rate of 2 DEG C/min, insulation 1h, then with stove Temperature fall to room temperature, obtain LiZnTi major ingredient;
Step 3: with BaCO
3, CaCO
3, ZnO, B
2o
3, SiO
2for raw material, by raw material according to mass ratio BaCO
3: CaCO
3: ZnO:B
2o
3: SiO
2the ratio batching of=2:1:7:8:2, wet ball grinding 6h, dry at 100 DEG C after taking-up, powder after oven dry is put into crucible and is placed in sintering oven, rise to 1300 DEG C with the temperature rise rate of 5 DEG C/min by room temperature and be incubated 1h, then directly taking-up is poured rapid quenching in deionized water into and is obtained BCZBS transparent vitreous body, wears into micron particles, namely obtain glassy phase sintering agent after oven dry;
Step 4: glassy phase sintering agent step 3 obtained adds in the major ingredient that step 2 obtains, be made into powder, wherein the weight percent of major ingredient is 98%, the weight percent of glassy phase sintering agent is 2%, carry out secondary ball milling, wherein, the weight ratio of powder, water and iron ball is 1:1:3, Ball-milling Time is 4h, and rotational speed of ball-mill is 250r/min; Then secondary ball abrasive material taken out and dry, add polyvinyl alcohol (PVA) granulating and forming and be pressed into blank, forming pressure is 9MPa, again blank is put into sintering oven, rise to 900 DEG C with the temperature rise rate of 2 DEG C/min, insulation 2h, with stove Temperature fall to room temperature, namely obtain described LiZnTi Ferrite Material.
The performance of the LiZnTi Ferrite Material that embodiment 2 prepares is: sample rate: 4.25g/cm
3, saturation induction density: 278.5mT, coercive force: 300A/m, squareness ratio: 0.86.
Embodiment 3
There is a preparation method for high squareness ratio LiZnTi Ferrite Material, comprise the following steps:
Step 1: with Fe
2o
3, ZnO, TiO
2, Li
2cO
3for raw material, according to Li
0.27zn
0.23ti
0.23fe
2.27o
4the ratio weighing of molecular formula, preparation obtains main powder;
Step 2: according to the main powder of mass ratio: water: the ratio of iron ball=1:1.4:3 carries out a ball milling, Ball-milling Time is 8h, dry at 100 DEG C after taking-up, sintering oven put into by the powder obtained after oven dry, 800 DEG C are risen to by room temperature with the temperature rise rate of 2 DEG C/min, insulation 1h, then with stove Temperature fall to room temperature, obtain LiZnTi major ingredient;
Step 3: with BaCO
3, CaCO
3, ZnO, B
2o
3, SiO
2for raw material, by raw material according to mass ratio BaCO
3: CaCO
3: ZnO:B
2o
3: SiO
2the ratio batching of=2:1:7:8:2, wet ball grinding 6h, dry at 100 DEG C after taking-up, powder after oven dry is put into crucible and is placed in sintering oven, rise to 1300 DEG C with the temperature rise rate of 5 DEG C/min by room temperature and be incubated 1h, then directly taking-up is poured rapid quenching in deionized water into and is obtained BCZBS transparent vitreous body, wears into micron particles, namely obtain glassy phase sintering agent after oven dry;
Step 4: glassy phase sintering agent step 3 obtained adds in the major ingredient that step 2 obtains, be made into powder, wherein the weight percent of major ingredient is 99%, the weight percent of glassy phase sintering agent is 1%, carry out secondary ball milling, wherein, the weight ratio of powder, water and iron ball is 1:1:3, Ball-milling Time is 6h, and rotational speed of ball-mill is 250r/min; Then secondary ball abrasive material taken out and dry, add polyvinyl alcohol (PVA) granulating and forming and be pressed into blank, forming pressure is 10MPa, again blank is put into sintering oven, rise to 920 DEG C with the temperature rise rate of 2 DEG C/min, insulation 2h, with stove Temperature fall to room temperature, namely obtain described LiZnTi Ferrite Material.
The performance of the LiZnTi Ferrite Material that embodiment 3 prepares is: sample rate: 4.19g/cm
3, saturation induction density: 280mT, coercive force: 271.4A/m, squareness ratio: 0.87.
Embodiment 4
There is a preparation method for high squareness ratio LiZnTi Ferrite Material, comprise the following steps:
Step 1: with Fe
2o
3, ZnO, TiO
2, Li
2cO
3for raw material, according to Li
0.27zn
0.23ti
0.23fe
2.27o
4the ratio weighing of molecular formula, preparation obtains main powder;
Step 2: according to the main powder of mass ratio: water: the ratio of iron ball=1:1.2:3 carries out a ball milling, Ball-milling Time is 4h, dry at 100 DEG C after taking-up, sintering oven put into by the powder obtained after oven dry, 800 DEG C are risen to by room temperature with the temperature rise rate of 2 DEG C/min, insulation 2h, then with stove Temperature fall to room temperature, obtain LiZnTi major ingredient;
Step 3: with BaCO
3, CaCO
3, ZnO, B
2o
3, SiO
2for raw material, by raw material according to mass ratio BaCO
3: CaCO
3: ZnO:B
2o
3: SiO
2the ratio batching of=2:1:7:8:2, wet ball grinding 6h, dry at 100 DEG C after taking-up, powder after oven dry is put into crucible and is placed in sintering oven, rise to 1300 DEG C with the temperature rise rate of 5 DEG C/min by room temperature and be incubated 1h, then directly taking-up is poured rapid quenching in deionized water into and is obtained BCZBS transparent vitreous body, wears into micron particles, namely obtain glassy phase sintering agent after oven dry;
Step 4: glassy phase sintering agent step 3 obtained adds in the major ingredient that step 2 obtains, be made into powder, wherein the weight percent of major ingredient is 97%, the weight percent of glassy phase sintering agent is 3%, carry out secondary ball milling, wherein, the weight ratio of powder, water and iron ball is 1:1:3, Ball-milling Time is 8h, and rotational speed of ball-mill is 250r/min; Then secondary ball abrasive material taken out and dry, add polyvinyl alcohol (PVA) granulating and forming and be pressed into blank, forming pressure is 10MPa, again blank is put into sintering oven, rise to 880 DEG C with the temperature rise rate of 2 DEG C/min, insulation 2h, with stove Temperature fall to room temperature, namely obtain described LiZnTi Ferrite Material.
The performance of the LiZnTi Ferrite Material that embodiment 4 prepares is: sample rate: 4.18g/cm
3, saturation induction density: 240mT, coercive force: 348.5A/m, squareness ratio: 0.82.
Comparative example
A preparation method for LiZnTi Ferrite Material, comprises the following steps:
Step 1: with Fe
2o
3, ZnO, TiO
2, Li
2cO
3for raw material, according to Li
0.27zn
0.23ti
0.23fe
2.27o
4the ratio weighing of molecular formula, preparation obtains powder;
Step 2: according to quality than powder: water: the ratio of iron ball=1:1.3:3 carries out a ball milling, Ball-milling Time is 6h, dry at 100 DEG C after taking-up, sintering oven put into by the powder obtained after oven dry, 820 DEG C are risen to by room temperature with the temperature rise rate of 2 DEG C/min, insulation 1h, then with stove Temperature fall to room temperature;
Step 3: add polyvinyl alcohol (PVA) granulating and forming in the powder obtained after step 2 processes and be pressed into blank, forming pressure is 9MPa, again blank is put into sintering oven, 900 DEG C are risen to the temperature rise rate of 2 DEG C/min, insulation 2h, with stove Temperature fall to room temperature, namely obtains LiZnTi Ferrite Material.
The performance of the LiZnTi Ferrite Material that comparative example prepares is: sample rate: 4.0g/cm
3, saturation induction density: 100mT, coercive force: 620.4A/m, squareness ratio: 0.72.
Fig. 1 is the surface topography map of LiZnTi Ferrite Material (b) that high squareness ratio LiZnTi Ferrite Material (a) that obtains of embodiment 3 obtains with comparative example.As shown in Figure 1, the present invention is by after the sintering agent of interpolation 1% (weight ratio), and LiZnTi crystal grain is obviously grown up, and crystal boundary is clear, obtains the LiZnTi Ferrite Material even, density is high, squareness ratio is high.To sum up, the LiZnTi Ferrite Material that the present invention obtains each all more excellent to gyromagnet parameter, particularly squareness ratio is greatly improved, and has vital role in the Application Areas such as electric ballast, magnetic recording.
Claims (3)
1. have a high squareness ratio LiZnTi Ferrite Material, be made up of major ingredient and glassy phase sintering agent, wherein the weight percent of major ingredient is 96% ~ 99.8%, and the weight percent of glassy phase sintering agent is 0.2% ~ 4%, and described major ingredient is Li
0.27zn
0.23ti
0.23fe
2.27o
4, described glassy phase sintering agent by raw material according to mass ratio BaCO
3: CaCO
3: ZnO:B
2o
3: SiO
2=2:1:7:8:2 prepares.
2. there is a preparation method for high squareness ratio LiZnTi Ferrite Material, comprise the following steps:
Step 1: with Fe
2o
3, ZnO, TiO
2, Li
2cO
3for raw material, according to Li
0.27zn
0.23ti
0.23fe
2.27o
4the ratio weighing of molecular formula, preparation obtains main powder;
Step 2: according to the main powder of mass ratio: water: iron ball=1:(1.2 ~ 1.4): the ratio of 3 carries out a ball milling, Ball-milling Time is 4 ~ 8h, dry at 100 ~ 120 DEG C after taking-up, sintering oven put into by the powder obtained after oven dry, 800 ~ 820 DEG C are risen to by room temperature with the temperature rise rate of 2 DEG C/min, insulation 1 ~ 3h, then with stove Temperature fall to room temperature, obtain LiZnTi major ingredient;
Step 3: with BaCO
3, CaCO
3, ZnO, B
2o
3, SiO
2for raw material, by raw material according to mass ratio BaCO
3: CaCO
3: ZnO:B
2o
3: SiO
2the ratio batching of=2:1:7:8:2, wet ball grinding 6h, dry at 100 ~ 120 DEG C after taking-up, powder after oven dry is put into crucible and is placed in sintering oven, rise to 1300 DEG C with the temperature rise rate of 5 DEG C/min by room temperature and be incubated 1h, then directly taking-up is poured rapid quenching in deionized water into and is obtained BCZBS transparent vitreous body, wears into micron particles, namely obtain glassy phase sintering agent after oven dry;
Step 4: glassy phase sintering agent step 3 obtained adds in the major ingredient that step 2 obtains, be made into powder, wherein the weight percent of major ingredient is 96% ~ 99.8%, the weight percent of glassy phase sintering agent is 0.2% ~ 4%, carry out secondary ball milling, wherein, the weight ratio of powder, water and iron ball is 1:1:3, Ball-milling Time is 4 ~ 8h, and rotational speed of ball-mill is 250r/min; Then secondary ball abrasive material taken out and dry, add polyvinyl alcohol granulating and forming and be pressed into blank, then blank is put into sintering oven, 880 ~ 940 DEG C are risen to the temperature rise rate of 2 DEG C/min, insulation 2h, with stove Temperature fall to room temperature, namely obtains described LiZnTi Ferrite Material.
3. the preparation method with high squareness ratio LiZnTi Ferrite Material according to claim 2, is characterized in that, when being pressed into blank described in step 4, pressure is 8 ~ 10MPa.
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|---|---|---|---|
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110526298A (en) * | 2019-09-30 | 2019-12-03 | 北京无线电测量研究所 | A kind of ferritic method of magnetic field auxiliary glass crystallization method low temperature preparation |
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|---|---|---|---|---|
| CN103467099A (en) * | 2013-10-08 | 2013-12-25 | 云南云天化股份有限公司 | LTCC material and preparation method thereof |
| CN104030671A (en) * | 2014-06-09 | 2014-09-10 | 电子科技大学 | LiZnTi ferrite material for LTCC phase shifter and preparation method of material |
| CN104496448A (en) * | 2014-11-27 | 2015-04-08 | 电子科技大学 | LiZnTi gyromagnetic ferrite material and preparation method thereof |
-
2015
- 2015-09-14 CN CN201510584979.6A patent/CN105236949B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103467099A (en) * | 2013-10-08 | 2013-12-25 | 云南云天化股份有限公司 | LTCC material and preparation method thereof |
| CN104030671A (en) * | 2014-06-09 | 2014-09-10 | 电子科技大学 | LiZnTi ferrite material for LTCC phase shifter and preparation method of material |
| CN104496448A (en) * | 2014-11-27 | 2015-04-08 | 电子科技大学 | LiZnTi gyromagnetic ferrite material and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110526298A (en) * | 2019-09-30 | 2019-12-03 | 北京无线电测量研究所 | A kind of ferritic method of magnetic field auxiliary glass crystallization method low temperature preparation |
| CN110526298B (en) * | 2019-09-30 | 2022-07-15 | 北京无线电测量研究所 | Method for preparing ferrite at low temperature by magnetic field assisted glass crystallization method |
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