CN105884342A - Preparation method for Bi-substituted LiZnTiMn gyromagnetic ferrite baseplate material - Google Patents
Preparation method for Bi-substituted LiZnTiMn gyromagnetic ferrite baseplate material Download PDFInfo
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- CN105884342A CN105884342A CN201610098871.0A CN201610098871A CN105884342A CN 105884342 A CN105884342 A CN 105884342A CN 201610098871 A CN201610098871 A CN 201610098871A CN 105884342 A CN105884342 A CN 105884342A
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- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 68
- 239000000463 material Substances 0.000 title claims abstract description 59
- 238000002360 preparation method Methods 0.000 title claims abstract description 46
- 238000000498 ball milling Methods 0.000 claims abstract description 54
- 238000005245 sintering Methods 0.000 claims abstract description 28
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 12
- 239000001301 oxygen Substances 0.000 claims abstract description 12
- 239000000843 powder Substances 0.000 claims description 76
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 26
- 238000001035 drying Methods 0.000 claims description 26
- 229910000831 Steel Inorganic materials 0.000 claims description 22
- 239000008367 deionised water Substances 0.000 claims description 22
- 229910021641 deionized water Inorganic materials 0.000 claims description 22
- 239000010959 steel Substances 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 13
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 13
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 13
- AMWRITDGCCNYAT-UHFFFAOYSA-L manganese oxide Inorganic materials [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 13
- 239000002994 raw material Substances 0.000 claims description 13
- 238000005303 weighing Methods 0.000 claims description 13
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 11
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 11
- 229940068984 polyvinyl alcohol Drugs 0.000 claims description 11
- 235000019422 polyvinyl alcohol Nutrition 0.000 claims description 11
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims description 10
- 238000000227 grinding Methods 0.000 claims description 4
- 239000000758 substrate Substances 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 2
- 230000005350 ferromagnetic resonance Effects 0.000 abstract description 14
- 238000005516 engineering process Methods 0.000 abstract description 7
- 239000000696 magnetic material Substances 0.000 abstract description 2
- 238000002156 mixing Methods 0.000 abstract description 2
- 230000004907 flux Effects 0.000 abstract 1
- 238000000465 moulding Methods 0.000 abstract 1
- 230000006698 induction Effects 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 12
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 12
- 238000007710 freezing Methods 0.000 description 9
- 230000008014 freezing Effects 0.000 description 9
- 239000011521 glass Substances 0.000 description 4
- 230000005291 magnetic effect Effects 0.000 description 4
- 229920006395 saturated elastomer Polymers 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 238000009766 low-temperature sintering Methods 0.000 description 3
- 230000004913 activation Effects 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000003475 lamination Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- 229910008656 Li2O—SiO2 Inorganic materials 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/26—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on ferrites
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3201—Alkali metal oxides or oxide-forming salts thereof
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3298—Bismuth oxides, bismuthates or oxide forming salts thereof, e.g. zinc bismuthate
Abstract
The invention discloses a preparation method for a Bi-substituted LiZnTiMn gyromagnetic ferrite baseplate material and belongs to the technical field of magnetic material preparation. The oxide sintering preparation technology is adopted in the gyromagnetic ferrite baseplate material, material blending, ball milling, oxygen atmosphere presintering, secondary ball milling, prilling, molding and sintering are carried out, grains are controlled to evenly and compactly grow, and Bi-substituted LiZnTiMn gyromagnetic ferrite can be sintered at the low temperature ranging from 880 DEG C to 920 DEG C. The Bi-substituted LiZnTiMn gyromagnetic ferrite obtained through the preparation method has the advantages of being low in sintering temperature and dielectric loss, small in ferromagnetic resonance line width and high in saturation flux density and squareness ratio.
Description
Technical field
The invention belongs to magnetic material preparing technical field, be specifically related to the narrow line of a kind of LTCC technology application
The Bi of squareness ratio wide, high is for the preparation method of LiZnTiMn gyromagnetic ferrite baseplate material.
Background technology
In recent years, send out to miniaturization, high frequency, the quick of integrated modular along with microwave technology and electronic device
Exhibition, utilizes LTCC (LTCC) technology prepare surface encapsulation laminated microwave/millimetric wave device and realize
System integration becomes important developing direction.Due to have low dielectric loss, narrow ferromagnetic resonance line width,
High saturation induction density and squareness ratio, the LiZnTi gyromagnetic ferrite mixing Mn is micro-at X and Ka wave band
The preparation of ripple ferrite device comes into one's own, and the low temperature sintering technology compatible with LTCC technology (< 950 DEG C)
Improvement with gyromagnet performance becomes problem demanding prompt solution.
Research to LiZnTi system gyromagnetic ferrite low-temperature sintering method at present is concentrated mainly on low-melting glass and helps
Agent doping aspect.Application No. 201410252398.8, invention entitled " LTCC phase shifter LiZnTi
Ferrite Material and preparation method " Chinese patent, disclose a kind of at a temperature of 900～940 DEG C sintering
The ferritic preparation method of LiZnTi, this invention is with LBSCA glass (Li2O-B2O3-SiO2-CaO-Al2O3)
For sintering aid, it is provided that a kind of saturation induction density Bs:340～360mT, ferromagnetic resonance line width △ H:
161～200Oe, squareness ratio Br/Bs0.81～the ferritic preparation method of LiZnTi of 0.83.Application No.
201410705112.7, the China of invention entitled " a kind of LiZnTi gyromagnetic ferrite material and preparation method thereof "
Patent, discloses a kind of ferritic preparation method of LiZnTi of sintering at a temperature of 900～940 DEG C, this
Bright with BBBLS glass (BaO-Bi2O3-B2O3-Li2O-SiO2) it is sintering aid, it is provided that a kind of saturated magnetic strength
Answer intensity Bs:242～410mT, squareness ratio Br/Bs0.78～the ferritic preparation method of LiZnTi of 0.84.On
State the low-melting glass building-up process in prepared by LiZnTi ferrite complicated, it is easy to component segregation occurs,
Thus affect the uniformity of crystal structure and the gyromagnet performance of Ferrite Material.
Summary of the invention
It is an object of the invention to application based on lamination gyromagnetic device, it is provided that a kind of formula and simple to operate and have concurrently
Low-temperature sintering Bi of premium properties, the preparation method of Mn codope LiZnTi gyromagnetic ferrite baseplate material.
Technical scheme is as follows:
A kind of Bi, for the preparation method of LiZnTiMn gyromagnetic ferrite baseplate material, comprises the following steps:
Step 1: with Li2CO3、ZnO、TiO2、Mn3O4、Fe2O3And Bi2O3For raw material, according to
Li0.42Zn0.27Ti0.11Mn0.1Fe2.1-xBixO4The ratio weighing of (0 < x < 0.01) molecular formula, preparation obtains initial
Powder；
Step 2: initial powder wet ball grinding step 1 obtained, Ball-milling Time is 4～6h, the powder after drying
Material carries out pre-burning in sintering furnace, and calcined temperature is 840～860 DEG C, and burn-in time is 1～3h, then with stove certainly
So it is cooled to room temperature, obtains pre-burning powder；
Step 3: pre-burning powder step 2 obtained carries out secondary ball milling, Ball-milling Time is 4～8h, and ball milling turns
Speed is 200～250r/min；Slip after secondary ball milling takes out post-drying, adds the poly-second that concentration is 8～10wt%
Enolate solution granulating and forming is also pressed into blank；Then the blank after compacting is put in sintering furnace,
Sinter 2～3h at a temperature of 880～920 DEG C, cool to room temperature with the furnace and i.e. obtain described Bi for LiZnTiMn gyromagnet
Ferrite substrate material.
A kind of Bi, for the preparation method of LiZnTiMn gyromagnetic ferrite baseplate material, specifically includes following steps:
Step 1: with Li2CO3、ZnO、TiO2、Mn3O4、Fe2O3And Bi2O3For raw material, according to
Li0.42Zn0.27Ti0.11Mn0.1Fe2.1-xBixO4The ratio weighing of (0 < x < 0.01) molecular formula, preparation obtains initial
Powder；
Step 2: according to weight ratio initial powder: deionized water: steel ball=1:(1.3～1.5): (2.5～3)
Ratio carries out wet ball grinding 4～6h, and the slip obtained is dried after taking out at 90～100 DEG C, the powder after drying
Put into the sintering furnace of oxygen atmosphere, risen to 840～860 DEG C with the heating rate of 2～3 DEG C/min by room temperature and protect
Temperature 1～3h, is then naturally cooling to room temperature with stove, obtains pre-burning powder；
Step 3: pre-burning powder step 2 obtained carries out secondary ball milling, wherein, powder: deionized water:
The weight ratio of steel ball is 1:1:(2.5～3), Ball-milling Time is 4～8h, and rotational speed of ball-mill is 200～250r/min；Two
Slip after secondary ball milling takes out post-drying, adds poly-vinyl alcohol solution granulating and forming that concentration is 8～10wt% also
It is pressed into blank；Then, the blank after compacting is put in sintering furnace, sinters at a temperature of 880～920 DEG C
2～3h, cool to room temperature with the furnace and i.e. obtain described Bi for LiZnTiMn gyromagnetic ferrite baseplate material.
Further, when being pressed into blank described in step 3, pressure is 8～10MPa.
The invention have the benefit that and the invention provides a kind of lamination gyromagnetic device Bi for LiZnTiMn
The preparation method of ferrite substrate material, introduces Bi, Mn codope in LiZnTi ferrite structure, promotees
Make distortion of lattice and activation thus realize LiZnTiMn ferrite (880～920 DEG C) at low temperatures sintering and
Preparation；And the Bi that the present invention prepares has sintering temperature and low, low Jie for LiZnTiMn gyromagnetic ferrite
Electrical loss, narrow ferromagnetic resonance line width, high saturated magnetic induction and high squareness ratio.
Accompanying drawing explanation
The X-ray diffracting spectrum (XRD) of the Ferrite Material that Fig. 1 is the embodiment of the present invention and comparative example obtains.
Fig. 2 is the scanning electron microscope (SEM) photograph (SEM) of the Ferrite Material that the embodiment of the present invention obtains with comparative example；Its
In, (a) is the SEM figure of the Ferrite Material that comparative example 1 obtains；B () is the iron oxygen that embodiment 3 obtains
The SEM figure of body material.
Detailed description of the invention
The present invention provides the Bi of a kind of narrow linewidth, high saturated magnetic induction and squareness ratio to revolve for LiZnTiMn
The preparation method of magnetic ferrites baseplate material, does the present invention below in conjunction with embodiment and accompanying drawing and says further
Bright.
Embodiment 1
A kind of Bi, for the preparation method of LiZnTiMn gyromagnetic ferrite baseplate material, comprises the following steps:
Step 1: with Li2CO3、ZnO、TiO2、Mn3O4、Fe2O3And Bi2O3For raw material, according to
Li0.42Zn0.27Ti0.11Mn0.1Fe2.1-xBixO4(x=0.002) the ratio weighing of molecular formula, preparation obtains initial powder
Body；
Step 2: according to weight ratio initial powder: deionized water: the ratio of steel ball=1:1.5:2.5 carries out wet
Method ball milling 4h, dries after the slip obtained taking-up at 90 DEG C, and the burning of oxygen atmosphere put into by the powder after drying
In freezing of a furnace, risen to 840 DEG C with the heating rate of 2 DEG C/min by room temperature and be incubated 2h, then with stove Temperature fall
To room temperature, obtain pre-burning powder；
Step 3: pre-burning powder step 2 obtained carries out secondary ball milling, wherein, powder: deionized water:
The weight ratio of steel ball is 1:1:2.5, and Ball-milling Time is 6h, and rotational speed of ball-mill is 250r/min；After secondary ball milling
Slip takes out post-drying, adds concentration and is the poly-vinyl alcohol solution granulating and forming of 10wt% and is pressed into blank；So
After, the blank after compacting is put in sintering furnace, at a temperature of 920 DEG C, sinters 2h, be cooled to room temperature i.e. with stove
Obtain described Bi for LiZnTiMn gyromagnetic ferrite baseplate material.
The Bi that embodiment 1 prepares for the performance of LiZnTiMn gyromagnetic ferrite baseplate material is: sample
Density 4.67g/cm3；Ferromagnetic resonance line width: 192Oe；Saturation induction density: 362mT；Coercivity:
296A/m；Squareness ratio: 0.90.
Embodiment 2
A kind of Bi, for the preparation method of LiZnTiMn gyromagnetic ferrite baseplate material, comprises the following steps:
Step 1: with Li2CO3、ZnO、TiO2、Mn3O4、Fe2O3And Bi2O3For raw material, according to
Li0.42Zn0.27Ti0.11Mn0.1Fe2.1-xBixO4(x=0.003) the ratio weighing of molecular formula, preparation obtains initial powder
Body；
Step 2: according to weight ratio initial powder: deionized water: the ratio of steel ball=1:1.5:2.5 carries out wet
Method ball milling 4h, dries after the slip obtained taking-up at 100 DEG C, and the burning of oxygen atmosphere put into by the powder after drying
In freezing of a furnace, risen to 860 DEG C with the heating rate of 2 DEG C/min by room temperature and be incubated 2h, then with stove Temperature fall
To room temperature, obtain pre-burning powder；
Step 3: pre-burning powder step 2 obtained carries out secondary ball milling, wherein, powder: deionized water:
The weight ratio of steel ball is 1:1:2.5, and Ball-milling Time is 6h, and rotational speed of ball-mill is 250r/min；After secondary ball milling
Slip takes out post-drying, adds concentration and is the poly-vinyl alcohol solution granulating and forming of 10wt% and is pressed into blank；So
After, the blank after compacting is put in sintering furnace, at a temperature of 920 DEG C, sinters 2h, be cooled to room temperature i.e. with stove
Obtain described Bi for LiZnTiMn gyromagnetic ferrite baseplate material.
The Bi that embodiment 2 prepares for the performance of LiZnTiMn gyromagnetic ferrite baseplate material is: sample
Density 4.65g/cm3；Ferromagnetic resonance line width: 188Oe；Saturation induction density: 350mT；Coercivity:
94A/m；Squareness ratio: 0.80.
Embodiment 3
A kind of Bi, for the preparation method of LiZnTiMn gyromagnetic ferrite baseplate material, comprises the following steps:
Step 1: with Li2CO3、ZnO、TiO2、Mn3O4、Fe2O3And Bi2O3For raw material, according to
Li0.42Zn0.27Ti0.11Mn0.1Fe2.1-xBixO4(x=0.003) the ratio weighing of molecular formula, preparation obtains initial powder
Body；
Step 2: according to weight ratio initial powder: deionized water: the ratio of steel ball=1:1.5:2.5 carries out wet
Method ball milling 4h, dries after the slip obtained taking-up at 100 DEG C, and the burning of oxygen atmosphere put into by the powder after drying
In freezing of a furnace, risen to 860 DEG C with the heating rate of 2 DEG C/min by room temperature and be incubated 2h, then with stove Temperature fall
To room temperature, obtain pre-burning powder；
Step 3: pre-burning powder step 2 obtained carries out secondary ball milling, wherein, powder: deionized water:
The weight ratio of steel ball is 1:1:2.5, and Ball-milling Time is 6h, and rotational speed of ball-mill is 250r/min；After secondary ball milling
Slip takes out post-drying, adds concentration and is the poly-vinyl alcohol solution granulating and forming of 10wt% and is pressed into blank；So
After, the blank after compacting is put in sintering furnace, at a temperature of 880 DEG C, sinters 2h, be cooled to room temperature i.e. with stove
Obtain described Bi for LiZnTiMn gyromagnetic ferrite baseplate material.
The Bi that embodiment 3 prepares for the performance of LiZnTiMn gyromagnetic ferrite baseplate material is: sample
Density 4.60g/cm3；Ferromagnetic resonance line width: 154Oe；Saturation induction density: 350mT；Coercivity:
474A/m；Squareness ratio: 0.91.
Embodiment 4
A kind of Bi, for the preparation method of LiZnTiMn gyromagnetic ferrite baseplate material, comprises the following steps:
Step 1: with Li2CO3、ZnO、TiO2、Mn3O4、Fe2O3And Bi2O3For raw material, according to
Li0.42Zn0.27Ti0.11Mn0.1Fe2.1-xBixO4(x=0.004) the ratio weighing of molecular formula, preparation obtains initial powder
Body；
Step 2: according to weight ratio initial powder: deionized water: the ratio of steel ball=1:1.5:2.5 carries out wet
Method ball milling 4h, dries after the slip obtained taking-up at 100 DEG C, and the burning of oxygen atmosphere put into by the powder after drying
In freezing of a furnace, risen to 860 DEG C with the heating rate of 2 DEG C/min by room temperature and be incubated 2h, then with stove Temperature fall
To room temperature, obtain pre-burning powder；
Step 3: pre-burning powder step 2 obtained carries out secondary ball milling, wherein, powder: deionized water:
The weight ratio of steel ball is 1:1:2.5, and Ball-milling Time is 6h, and rotational speed of ball-mill is 250r/min；After secondary ball milling
Slip takes out post-drying, adds concentration and is the poly-vinyl alcohol solution granulating and forming of 10wt% and is pressed into blank；So
After, the blank after compacting is put in sintering furnace, at a temperature of 880 DEG C, sinters 2h, be cooled to room temperature i.e. with stove
Obtain described Bi for LiZnTiMn gyromagnetic ferrite baseplate material.
The Bi that embodiment 4 prepares for the performance of LiZnTiMn gyromagnetic ferrite baseplate material is: sample
Density 4.67g/cm3；Ferromagnetic resonance line width: 198Oe；Saturation induction density: 353mT；Coercivity:
132A/m；Squareness ratio: 0.86.
Embodiment 5
A kind of Bi, for the preparation method of LiZnTiMn gyromagnetic ferrite baseplate material, comprises the following steps:
Step 1: with Li2CO3、ZnO、TiO2、Mn3O4、Fe2O3And Bi2O3For raw material, according to
Li0.42Zn0.27Ti0.11Mn0.1Fe2.1-xBixO4(x=0.002) the ratio weighing of molecular formula, preparation obtains initial powder
Body；
Step 2: according to weight ratio initial powder: deionized water: the ratio of steel ball=1:1.5:2.5 carries out wet
Method ball milling 4h, dries after the slip obtained taking-up at 100 DEG C, and the burning of oxygen atmosphere put into by the powder after drying
In freezing of a furnace, risen to 860 DEG C with the heating rate of 2 DEG C/min by room temperature and be incubated 2h, then with stove Temperature fall
To room temperature, obtain pre-burning powder；
Step 3: pre-burning powder step 2 obtained carries out secondary ball milling, wherein, powder: deionized water:
The weight ratio of steel ball is 1:1:2.5, and Ball-milling Time is 6h, and rotational speed of ball-mill is 250r/min；After secondary ball milling
Slip takes out post-drying, adds concentration and is the poly-vinyl alcohol solution granulating and forming of 10wt% and is pressed into blank；So
After, the blank after compacting is put in sintering furnace, at a temperature of 900 DEG C, sinters 2h, be cooled to room temperature i.e. with stove
Obtain described Bi for LiZnTiMn gyromagnetic ferrite baseplate material.
The Bi that embodiment 5 prepares for the performance of LiZnTiMn gyromagnetic ferrite baseplate material is: sample
Density 4.61g/cm3；Ferromagnetic resonance line width: 212Oe；Saturation induction density: 344mT；Coercivity:
391A/m；Squareness ratio: 0.91.
Embodiment 6
A kind of Bi, for the preparation method of LiZnTiMn gyromagnetic ferrite baseplate material, comprises the following steps:
Step 1: with Li2CO3、ZnO、TiO2、Mn3O4、Fe2O3And Bi2O3For raw material, according to
Li0.42Zn0.27Ti0.11Mn0.1Fe2.1-xBixO4(x=0.003) the ratio weighing of molecular formula, preparation obtains initial powder
Body；
Step 2: according to weight ratio initial powder: deionized water: the ratio of steel ball=1:1.5:2.5 carries out wet
Method ball milling 4h, dries after the slip obtained taking-up at 100 DEG C, and the burning of oxygen atmosphere put into by the powder after drying
In freezing of a furnace, risen to 860 DEG C with the heating rate of 2 DEG C/min by room temperature and be incubated 2h, then with stove Temperature fall
To room temperature, obtain pre-burning powder；
Step 3: pre-burning powder step 2 obtained carries out secondary ball milling, wherein, powder: deionized water:
The weight ratio of steel ball is 1:1:2.5, and Ball-milling Time is 6h, and rotational speed of ball-mill is 250r/min；After secondary ball milling
Slip takes out post-drying, adds concentration and is the poly-vinyl alcohol solution granulating and forming of 10wt% and is pressed into blank；So
After, the blank after compacting is put in sintering furnace, at a temperature of 900 DEG C, sinters 2h, be cooled to room temperature i.e. with stove
Obtain described Bi for LiZnTiMn gyromagnetic ferrite baseplate material.
The Bi that embodiment 6 prepares for the performance of LiZnTiMn gyromagnetic ferrite baseplate material is: sample
Density 4.65g/cm3；Ferromagnetic resonance line width: 170Oe；Saturation induction density: 352mT；Coercivity:
115A/m；Squareness ratio: 0.83.
Comparative example 1:
The preparation method of a kind of LiZnTiMn gyromagnetic ferrite, comprises the following steps:
Step 1: with Li2CO3、ZnO、TiO2、Mn3O4And Fe2O3For raw material, according to
Li0.42Zn0.27Ti0.11Mn0.1Fe2.1O4The ratio weighing of molecular formula, preparation obtains initial powder；
Step 2: according to weight ratio initial powder: deionized water: the ratio of steel ball=1:1.5:2.5 carries out wet
Method ball milling 4h, dries after the slip obtained taking-up at 100 DEG C, and the burning of oxygen atmosphere put into by the powder after drying
In freezing of a furnace, risen to 860 DEG C with the heating rate of 2 DEG C/min by room temperature and be incubated 2h, then with stove Temperature fall
To room temperature, obtain pre-burning powder；
Step 3: pre-burning powder step 2 obtained carries out secondary ball milling, wherein, powder: deionized water:
The weight ratio of steel ball is 1:1:2.5, and Ball-milling Time is 6h, and rotational speed of ball-mill is 250r/min；After secondary ball milling
Slip takes out post-drying, adds concentration and is the poly-vinyl alcohol solution granulating and forming of 10wt% and is pressed into blank；So
After, the blank after compacting is put in sintering furnace, at a temperature of 880 DEG C, sinters 2h, be cooled to room temperature i.e. with stove
Obtain described LiZnTiMn gyromagnetic ferrite material.
The performance of the LiZnTiMn gyromagnetic ferrite material that comparative example 1 prepares is: sample rate
3.38g/cm3；Ferromagnetic resonance line width: 1507Oe；Saturation induction density: 151mT；Coercivity: 648A/m；
Squareness ratio: 0.66.
Comparative example 2:
The preparation method of a kind of LiZnTiMn gyromagnetic ferrite, comprises the following steps:
Step 1: with Li2CO3、ZnO、TiO2、Mn3O4And Fe2O3For raw material, according to
Li0.42Zn0.27Ti0.11Mn0.1Fe2.1O4The ratio weighing of molecular formula, preparation obtains initial powder；
Step 2: according to weight ratio initial powder: deionized water: the ratio of steel ball=1:1.5:2.5 carries out wet
Method ball milling 4h, dries after the slip obtained taking-up at 100 DEG C, and the burning of oxygen atmosphere put into by the powder after drying
In freezing of a furnace, risen to 860 DEG C with the heating rate of 2 DEG C/min by room temperature and be incubated 2h, then with stove Temperature fall
To room temperature, obtain pre-burning powder；
Step 3: pre-burning powder step 2 obtained carries out secondary ball milling, wherein, powder: deionized water:
The weight ratio of steel ball is 1:1:2.5, and Ball-milling Time is 6h, and rotational speed of ball-mill is 250r/min；After secondary ball milling
Slip takes out post-drying, adds concentration and is the poly-vinyl alcohol solution granulating and forming of 10wt% and is pressed into blank；So
After, the blank after compacting is put in sintering furnace, at a temperature of 900 DEG C, sinters 2h, be cooled to room temperature i.e. with stove
Obtain described LiZnTiMn gyromagnetic ferrite material.
The performance of the LiZnTiMn gyromagnetic ferrite material that comparative example 2 prepares is: sample rate
3.54g/cm3；Ferromagnetic resonance line width: 1132Oe；Saturation induction density: 186mT；Coercivity: 590A/m；
Squareness ratio: 0.73.
Comparative example 3:
The preparation method of a kind of LiZnTiMn gyromagnetic ferrite, comprises the following steps:
Step 1: with Li2CO3、ZnO、TiO2、Mn3O4And Fe2O3For raw material, according to
Li0.42Zn0.27Ti0.11Mn0.1Fe2.1O4The ratio weighing of molecular formula, preparation obtains initial powder；
Step 2: according to weight ratio initial powder: deionized water: the ratio of steel ball=1:1.5:2.5 carries out wet
Method ball milling 4h, dries after the slip obtained taking-up at 100 DEG C, and the burning of oxygen atmosphere put into by the powder after drying
In freezing of a furnace, risen to 860 DEG C with the heating rate of 2 DEG C/min by room temperature and be incubated 2h, then with stove Temperature fall
To room temperature, obtain pre-burning powder；
Step 3: pre-burning powder step 2 obtained carries out secondary ball milling, wherein, powder: deionized water:
The weight ratio of steel ball is 1:1:2.5, and Ball-milling Time is 6h, and rotational speed of ball-mill is 250r/min；After secondary ball milling
Slip takes out post-drying, adds concentration and is the poly-vinyl alcohol solution granulating and forming of 10wt% and is pressed into blank；So
After, the blank after compacting is put in sintering furnace, at a temperature of 920 DEG C, sinters 2h, be cooled to room temperature i.e. with stove
Obtain described LiZnTiMn gyromagnetic ferrite material.
The performance of the LiZnTiMn gyromagnetic ferrite material that comparative example 3 prepares is: sample rate
3.67g/cm3；Ferromagnetic resonance line width: 790Oe；Saturation induction density: 217mT；Coercivity: 534A/m；
Squareness ratio: 0.77.
The X-ray diffracting spectrum (XRD) of the Ferrite Material that Fig. 1 is the embodiment of the present invention and comparative example obtains,
Wherein, (a) is the XRD spectrum of 880 DEG C of sintered samples；B () is the XRD spectrum of 900 DEG C of sintered samples.
As shown in Figure 1, the Bi that the present invention prepares is spinel structure, part for LiZnTiMn Ferrite Material
The Bi ion mixed enter ferrite crystal structure cause distortion of lattice (diffraction maximum with the increase of incorporation to low
Angle end moves).Fig. 2 is the scanning electron microscope (SEM) photograph of the Ferrite Material that the embodiment of the present invention obtains with comparative example
(SEM)；Wherein, (a) is the SEM figure of the Ferrite Material that comparative example 1 obtains；B () is embodiment 3
The SEM figure of the Ferrite Material obtained.As shown in Figure 2, the present invention is by introducing trace in basic recipe
Bi ionic compartmentation Fe ion, causes ferrite lattice distortion and activation, promotes ferritic sintering and crystal grain
Growth, and it is expected to obtain the microstructure of dense uniform.
To sum up, the present invention provide a kind of Bi for the preparation method of LiZnTiMn gyromagnetic ferrite baseplate material,
Ferritic for LiZnTiMn sintering temperature is successfully reduced to about 900 DEG C by the method, and maintains
(ferromagnetic resonance line width significantly narrows the excellent gyromagnet performance of LiZnTiMn Ferrite Material, the most saturated
Magnetic induction intensity and squareness ratio are greatly improved) can be widely used for so that this material burns altogether with silver electrode
The manufacture of laminated microwave/millimetric wave device.
Claims (3)
1. Bi is for a preparation method for LiZnTiMn gyromagnetic ferrite baseplate material, comprises the following steps:
Step 1: with Li2CO3、ZnO、TiO2、Mn3O4、Fe2O3And Bi2O3For raw material, according to
Li0.42Zn0.27Ti0.11Mn0.1Fe2.1-xBixO4The ratio weighing of molecular formula, preparation obtains initial powder, wherein,
0<x<0.01；
Step 2: initial powder wet ball grinding step 1 obtained, Ball-milling Time is 4～6h, the powder after drying
Material carries out pre-burning in sintering furnace, and calcined temperature is 840～860 DEG C, and burn-in time is 1～3h, then with stove certainly
So it is cooled to room temperature, obtains pre-burning powder；
Step 3: pre-burning powder step 2 obtained carries out secondary ball milling, Ball-milling Time is 4～8h, and ball milling turns
Speed is 200～250r/min；Slip after secondary ball milling takes out post-drying, adds the poly-second that concentration is 8～10wt%
Enolate solution granulating and forming is also pressed into blank；Then the blank after compacting is put in sintering furnace,
Sinter 2～3h at a temperature of 880～920 DEG C, cool to room temperature with the furnace and i.e. obtain described Bi for LiZnTiMn gyromagnet
Ferrite substrate material.
2. Bi is for a preparation method for LiZnTiMn gyromagnetic ferrite baseplate material, comprises the following steps:
Step 1: with Li2CO3、ZnO、TiO2、Mn3O4、Fe2O3And Bi2O3For raw material, according to
Li0.42Zn0.27Ti0.11Mn0.1Fe2.1-xBixO4The ratio weighing of molecular formula, preparation obtains initial powder, wherein,
0<x<0.01；
Step 2: according to weight ratio initial powder: deionized water: steel ball=1:(1.3～1.5): (2.5～3)
Ratio carries out wet ball grinding 4～6h, and the slip obtained is dried after taking out at 90～100 DEG C, the powder after drying
Put into the sintering furnace of oxygen atmosphere, risen to 840～860 DEG C with the heating rate of 2～3 DEG C/min by room temperature and protect
Temperature 1～3h, is then naturally cooling to room temperature with stove, obtains pre-burning powder；
Step 3: pre-burning powder step 2 obtained carries out secondary ball milling, wherein, powder: deionized water:
The weight ratio of steel ball is 1:1:(2.5～3), Ball-milling Time is 4～8h, and rotational speed of ball-mill is 200～250r/min；Two
Slip after secondary ball milling takes out post-drying, adds poly-vinyl alcohol solution granulating and forming that concentration is 8～10wt% also
It is pressed into blank；Then, the blank after compacting is put in sintering furnace, sinters at a temperature of 880～920 DEG C
2～3h, cool to room temperature with the furnace and i.e. obtain described Bi for LiZnTiMn gyromagnetic ferrite baseplate material.
Bi the most according to claim 1 and 2 is for the preparation of LiZnTiMn gyromagnetic ferrite baseplate material
Method, it is characterised in that when being pressed into blank described in step 3, pressure is 8～10MPa.
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| CN108046790A (en) * | 2017-12-23 | 2018-05-18 | 雷笑天 | A kind of preparation method of high-performance gyromagnetic ferrite material |
| CN109053180A (en) * | 2018-10-15 | 2018-12-21 | 电子科技大学 | A kind of low-temperature sintering low-loss LiZn Ferrite Material and preparation method |
| CN112239358A (en) * | 2020-10-30 | 2021-01-19 | 成都子之源绿能科技有限公司 | Microwave LiZnTiMn gyromagnetic ferrite material and preparation method thereof |
| CN113213908A (en) * | 2021-04-25 | 2021-08-06 | 中国航天时代电子有限公司 | Microwave ferrite material for ferrite device and preparation method thereof |
| CN113511888A (en) * | 2021-04-07 | 2021-10-19 | 电子科技大学 | Narrow-linewidth LTCF gyromagnetic substrate material and preparation method thereof |
| CN113845359A (en) * | 2021-08-30 | 2021-12-28 | 电子科技大学 | Low-loss LiZnTiMn gyromagnetic ferrite material and preparation method thereof |
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| CN113845359A (en) * | 2021-08-30 | 2021-12-28 | 电子科技大学 | Low-loss LiZnTiMn gyromagnetic ferrite material and preparation method thereof |
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