CN104030671A - LiZnTi ferrite material for LTCC phase shifter and preparation method of material - Google Patents
LiZnTi ferrite material for LTCC phase shifter and preparation method of material Download PDFInfo
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- CN104030671A CN104030671A CN201410252398.8A CN201410252398A CN104030671A CN 104030671 A CN104030671 A CN 104030671A CN 201410252398 A CN201410252398 A CN 201410252398A CN 104030671 A CN104030671 A CN 104030671A
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Abstract
The invention aims at solving the technical problem of providing a LiZnTi ferrite material which is low in coercivity, low in ferromagnetic resonance linewidth and high in saturation magnetization intensity property under the circumstance of satisfying sintering at a low temperature below 950 DEG C; the LiZnTi ferrite material is used for an LTCC (Low Temperature Co-fired Ceramic) phase shifter. The ferrite material is composed of a main material and a glass phase sintering aid, wherein the percentage by weight of the main material is 99.3-99.85%, while the percentage by weight of the glass phase sintering aid is 0.15-0.7%; the main material is prepared from raw materials Li2CO3, ZnO, TiO2 and Fe2O3 according to a molecular formula Li0.43Zn0.27Ti0.13Fe2.17O4; the glass phase sintering aid is prepared by mixing 52.45mol% of Li2O, 31.06mol% of B2O3, 11.99mol% of SiO2, 2mol% of CaO and 2.5mol% of Al2O3 together, performing ball milling on the mixture for 12 hours, heating to 1150 DEG C and preserving heat for 1 hour, reducing to 1000 DEG C and carrying out quick quenching. The preparation method of the ferrite material has the advantages that the sintering temperature of the LiZnTi ferrite is successfully reduced to about 900 DEG C and the excellent gyromagnetism of the LiZnTi ferrite material is kept, and therefore, the material can be co-fired with a silver electrode and widely applied to manufacturing the LTCC phase shifters.
Description
Technical field
The gyromagnetic ferrite material and the glass-ceramic preparing technical field that the present invention relates to the application of LTCC technology, particularly a kind of low-temperature sintering has gyromagnetic ferrite material of low-coercivity, low ferromagnetic resonance line width and high saturated magnetic induction and preparation method thereof simultaneously.
Background technology
Phase shifter is widely used in phased array array antenna system and phase modulated communication system as key element.In recent years, electronic information technology is constantly to high frequency and digitizing future development, and components and parts comprise that phase shifter realizes miniaturization, integrated so that modularization seems more and more urgent.Utilize LTCC (LTCC) technology to realize the broad interest that phase shifter miniaturization more and more causes investigator.Wherein, the common burning temperature of LTCC is generally between 800 ℃～950 ℃.Yet, as phase shifter, mainly apply material, traditional method is prepared the ferritic sintering temperature of LiZnTi higher than the top temperature of burning altogether with silver electrode in LTCC technology (961 ℃).Therefore it is technical barrier urgently to be resolved hurrily that the sintering temperature that, reduces LiZnTi Ferrite Material keeps excellent gyromagnet performance simultaneously.
Summary of the invention
Technical problem to be solved by this invention is, meeting below 950 ℃ in low sintering situation, provides a kind of LiZnTi Ferrite Material with low-coercivity, low ferromagnetic resonance line width and high saturation and magnetic intensity characteristic, for LTCC phase shifter.Meanwhile, the present invention also provides the preparation method of this LiZnTi Ferrite Material.
Technical scheme of the present invention is: LTCC phase shifter LiZnTi Ferrite Material, by major ingredient and glassy phase sintering agent, formed, wherein major ingredient weight percent is 99.3～99.85%, glassy phase sintering agent weight percent is 0.15～0.7%, it is characterized in that, described major ingredient is with Li
2cO
3, ZnO, TiO
2and Fe
2o
3for raw material, according to molecular formula Li
0.43zn
0.27ti
0.13fe
2.17o
4preparation; Described glassy phase sintering agent is with Li
2o, B
2o
3, SiO
2, CaO and Al
2o
3for raw material, 52.45mol%Li in proportion
2o, 31.06mol%B
2o
3, 11.99mol%SiO
2, 2mol%CaO and 2.5mol%Al
2o
3preparation.
Preferably, described major ingredient Raw Li
2cO
3, ZnO, TiO
2and Fe
2o
3mol ratio is 43:54:26:217; Described glassy phase sintering agent batching, by 12h ball milling, is heated to 1150 ℃ of insulation 1h, is cooled to 1000 ℃ of rapid quenchings and makes.
The preparation method of LiZnTi Ferrite Material for above-mentioned LTCC phase shifter, comprises the following steps:
Step 1. is with Li
2cO
3, ZnO, TiO
2and Fe
2o
3for raw material, according to molecular formula Li
0.43zn
0.27ti
0.13fe
2.17o
4preparation winner powder;
Step 2. mixes step 1 preparation winner powder, according to the weight ratio of main powder and deionized water, be that 1:1.5 adds deionized water in main powder, adopt wet milling process to mix 4～5h, after taking-up, at 100～120 ℃, dry, cross 80 mesh sieves, main powder after sieving is warming up to 780～800 ℃ of insulation 2h with the temperature rise rate of 2 ℃/min by room temperature, is prepared into major ingredient;
Step 3. is with Li
2o, B
2o
3, SiO
2, CaO and Al
2o
3for raw material, 52.45mol%Li in proportion
2o, 31.06mol%B
2o
3, 11.99mol%SiO
2, 2mol%CaO and 2.5mol%Al
2o
3batching, with wet milling process ball milling 12h, after taking-up, at 100～120 ℃, dry, cross 80 mesh sieves, powder after sieving is put into crucible and by room temperature, is warming up to 1150 ℃ of insulation 1h with the temperature rise rate of 2 ℃/min, be cooled to 1000 ℃ of taking-ups and pour rapid quenching in deionized water into, after oven dry, wear into micron particles, be prepared into LBSCA glassy phase sintering agent;
Step 4. adds LBSCA glassy phase sintering agent in step 2 gained major ingredient, is made into powder, and wherein major ingredient weight percent is 99.3～99.85%, glassy phase sintering agent weight percent is 0.15～0.7%; According to the weight ratio of powder and deionized water, be that 1:1 adds deionized water in powder, after ball milling 6h, take out, put into baking oven dries at 100～120 ℃, after being added to 10% organic binder bond granulation by weight, gained powder is pressed into blank, again blank is put into atmosphere furnace, in oxygen atmosphere, at 900～920 ℃, sintering 2h is prepared into LiZnTi Ferrite Material.
The invention provides LiZnTi Ferrite Material and preparation method for a kind of LTCC phase shifter, this preparation method is successfully down to 900 ℃ of left and right by the ferritic sintering temperature of LiZnTi, and keep the gyromagnet performance of LiZnTi Ferrite Material excellence, thereby make this material to burn altogether the manufacture that can be widely used in LTCC phase shifter with silver electrode.
Accompanying drawing explanation
Fig. 1 is that the present invention is prepared into LiZnTi ferrite SEM figure for LTCC phase shifter,
As we can see from the figure, LTCC phase shifter is fine and close by LiZnTi ferrite microstructure, and void content is low, and median size is about 5.5 μ m.
Embodiment
The invention provides LiZnTi Ferrite Material and preparation method thereof for a kind of LTCC phase shifter, can obtain more clearly describing by following indefiniteness embodiment.
Embodiment 1:
(1) first by Li
2cO
3, ZnO, TiO
2and Fe
2o
3by molecular formula Li
0.43zn
0.27ti
0.13fe
2.17o
4be mixed with main powder;
(2) main powder step (1) being prepared mixes, according to the weight ratio of main powder and deionized water, be that 1:1.5 adds deionized water in main powder, adopt wet milling process to mix 4～5h, after taking-up, at 100～120 ℃, dry, with 80 object screen clothes, sieve, the main powder after sieving rises to 780～800 ℃ of insulation 2h left and right with the temperature rise rate of 2 ℃/min by room temperature;
(3) sintering agent LBSCA glass is with 52.45mol%Li
2o, 31.06mol%B
2o
3, 11.99mol%SiO
2, 2mol%CaO and 2.5mol%Al
2o
3batching, with wet milling process ball milling 12h, after taking-up, at 100～120 ℃, dry, with 80 object screen clothes, sieve, powder after sieving is put into crucible and by room temperature, is risen to 1150 ℃ of insulation 1h with the temperature rise rate of 2 ℃/min, be cooled to about 1000 ℃ taking-ups and pour rapid quenching in deionized water into, after oven dry, wear into micron particles;
(4) major ingredient of step (2) gained being added to weight percent is 0.3% LBSCA glass powder, be made into powder, according to the weight ratio of powder and deionized water, be that 1:1 adds deionized water in powder, after ball milling 6h, take out, put into baking oven and dry at 100～120 ℃, be pressed into blank after gained powder is added to 10% organic binder bond granulation by weight, then blank is put into atmosphere furnace, in oxygen atmosphere, at 900 ℃, sintering 2h gets final product to obtain gyromagnetic ferrite material.Saturation induction density, the rugged SY-8232B-H analyser test of Japanese rock for coercive force, row's kerosene method test for density, calculates porosity according to actual density and theoretical density, by the ferromagnetic resonance line width of IEC standard measure sample under 9.3GHz.
The gyromagnet performance of this LiZnTi Ferrite Material is: saturation induction density B
s: 358mT, ferromagnetic resonance line width Δ H:183Oe, coercive force H
c: 162A/m, squareness ratio B
r/ B
s: 0.81, porosity p:5.8%.
Embodiment 2:
(1) first by Li
2cO
3, ZnO, TiO
2and Fe
2o
3by molecular formula Li
0.43zn
0.27ti
0.13fe
2.17o
4be mixed with main powder;
(2) main powder step (1) being prepared mixes, according to the weight ratio of main powder and deionized water, be that 1:1.5 adds deionized water in main powder, adopt wet milling process to mix 4～5h, after taking-up, at 100～120 ℃, dry, with 80 object screen clothes, sieve, the main powder after sieving rises to 780～800 ℃ of insulation 2h left and right with the temperature rise rate of 2 ℃/min by room temperature;
(3) sintering agent LBSCA glass is with 52.45mol%Li
2o, 31.06mol%B
2o
3, 11.99mol%SiO
2, 2mol%CaO and 2.5mol%Al
2o
3batching, with wet milling process ball milling 12h, after taking-up, at 100～120 ℃, dry, with 80 object screen clothes, sieve, powder after sieving is put into crucible and by room temperature, is risen to 1150 ℃ of insulation 1h with the temperature rise rate of 2 ℃/min, be cooled to about 1000 ℃ taking-ups and pour rapid quenching in deionized water into, after oven dry, wear into micron particles;
(4) major ingredient of step (2) gained being added to weight percent is 0.4% LBSCA glass powder, be made into powder, according to the weight ratio of powder and deionized water, be that 1:1 adds deionized water in powder, after ball milling 6h, take out, put into baking oven and dry at 100～120 ℃, be pressed into blank after gained powder is added to 10% organic binder bond granulation by weight, then blank is put into atmosphere furnace, in oxygen atmosphere, at 900 ℃, sintering 2h gets final product to obtain microwave gyromagnetic ferrite material.
The gyromagnet performance of this LiZnTi Ferrite Material is: saturation induction density B
s: 350mT, ferromagnetic resonance line width Δ H:180Oe, coercive force H
c: 187A/m, squareness ratio B
r/ B
s: 0.81, porosity p:5.5%.
Embodiment 3:
(1) first by Li
2cO
3, ZnO, TiO
2and Fe
2o
3by molecular formula Li
0.43zn
0.27ti
0.13fe
2.17o
4be mixed with main powder;
(2) main powder step (1) being prepared mixes, according to the weight ratio of main powder and deionized water, be that 1:1.5 adds deionized water in main powder, adopt wet milling process to mix 4～5h, after taking-up, at 100～120 ℃, dry, with 80 object screen clothes, sieve, the main powder after sieving rises to 780～800 ℃ of insulation 2h left and right with the temperature rise rate of 2 ℃/min by room temperature;
(3) sintering agent LBSCA glass is with 52.45mol%Li
2o, 31.06mol%B
2o
3, 11.99mol%SiO
2, 2mol%CaO and 2.5mol%Al
2o
3batching, with wet milling process ball milling 12h, after taking-up, at 100～120 ℃, dry, with 80 object screen clothes, sieve, powder after sieving is put into crucible and by room temperature, is risen to 1150 ℃ of insulation 1h with the temperature rise rate of 2 ℃/min, be cooled to about 1000 ℃ taking-ups and pour rapid quenching in deionized water into, after oven dry, wear into micron particles;
(4) major ingredient of step (2) gained being added to weight percent is 0.55% LBSCA glass powder, be made into powder, according to the weight ratio of powder and deionized water, be that 1:1 adds deionized water in powder, after ball milling 6h, take out, put into baking oven and dry at 100～120 ℃, be pressed into blank after gained powder is added to 10% organic binder bond granulation by weight, then blank is put into atmosphere furnace, in oxygen atmosphere, at 900 ℃, sintering 2h gets final product to obtain microwave gyromagnetic ferrite material.
The gyromagnet performance of this LiZnTi Ferrite Material is: saturation induction density B
s: 345mT, ferromagnetic resonance line width Δ H:175Oe, coercive force H
c: 183A/m, squareness ratio B
r/ B
s: 0.82, porosity p:5.5%.
Embodiment 4:
(1) first by Li
2cO
3, ZnO, TiO
2and Fe
2o
3by molecular formula Li
0.43zn
0.27ti
0.13fe
2.17o
4be mixed with main powder;
(2) main powder step (1) being prepared mixes, according to the weight ratio of main powder and deionized water, be that 1:1.5 adds deionized water in main powder, adopt wet milling process to mix 4～5h, after taking-up, at 100～120 ℃, dry, with 80 object screen clothes, sieve, the main powder after sieving rises to 780～800 ℃ of insulation 2h left and right with the temperature rise rate of 2 ℃/min by room temperature;
(3) sintering agent LBSCA glass is with 52.45mol%Li
2o, 31.06mol%B
2o
3, 11.99mol%SiO
2, 2mol%CaO and 2.5mol%Al
2o
3batching, with wet milling process ball milling 12h, after taking-up, at 100～120 ℃, dry, with 80 object screen clothes, sieve, powder after sieving is put into crucible and by room temperature, is risen to 1150 ℃ of insulation 1h with the temperature rise rate of 2 ℃/min, be cooled to about 1000 ℃ taking-ups and pour rapid quenching in deionized water into, after oven dry, wear into micron particles;
(4) major ingredient of step (2) gained being added to weight percent is 0.7% LBSCA glass powder, be made into powder, according to the weight ratio of powder and deionized water, be that 1:1 adds deionized water in powder, after ball milling 6h, take out, put into baking oven and dry at 100～120 ℃, be pressed into blank after gained powder is added to 10% organic binder bond granulation by weight, then blank is put into atmosphere furnace, in oxygen atmosphere, at 900 ℃, sintering 2h gets final product to obtain microwave gyromagnetic ferrite material.
The gyromagnet performance of this LiZnTi Ferrite Material is: saturation induction density B
s: 338mT, ferromagnetic resonance line width Δ H:168Oe, coercive force H
c: 197A/m, squareness ratio B
r/ B
s: 0.82, porosity p:5.0%.
Embodiment 5:
(1) first by Li
2cO
3, ZnO, TiO
2and Fe
2o
3by molecular formula Li
0.43zn
0.27ti
0.13fe
2.17o
4be mixed with main powder;
(2) main powder step (1) being prepared mixes, according to the weight ratio of main powder and deionized water, be that 1:1.5 adds deionized water in main powder, adopt wet milling process to mix 4～5h, after taking-up, at 100～120 ℃, dry, with 80 object screen clothes, sieve, the main powder after sieving rises to 780～800 ℃ of insulation 2h left and right with the temperature rise rate of 2 ℃/min by room temperature;
(3) sintering agent LBSCA glass is with 52.45mol%Li
2o, 31.06mol%B
2o
3, 11.99mol%SiO
2, 2mol%CaO and 2.5mol%Al
2o
3batching, with wet milling process ball milling 12h, after taking-up, at 100～120 ℃, dry, with 80 object screen clothes, sieve, powder after sieving is put into crucible and by room temperature, is risen to 1150 ℃ of insulation 1h with the temperature rise rate of 2 ℃/min, be cooled to about 1000 ℃ taking-ups and pour rapid quenching in deionized water into, after oven dry, wear into micron particles;
(4) major ingredient of step (2) gained being added to weight percent is 0.15% LBSCA glass powder, be made into powder, according to the weight ratio of powder and deionized water, be that 1:1 adds deionized water in powder, after ball milling 6h, take out, put into baking oven and dry at 100～120 ℃, be pressed into blank after gained powder is added to 10% organic binder bond granulation by weight, then blank is put into atmosphere furnace, in oxygen atmosphere, at 920 ℃, sintering 2h gets final product to obtain microwave gyromagnetic ferrite material.
The gyromagnet performance of this LiZnTi Ferrite Material is: saturation induction density B
s: 366mT, ferromagnetic resonance line width Δ H:200Oe, coercive force H
c: 153A/m, squareness ratio B
r/ B
s: 0.82, porosity p:6.1%.
Embodiment 6:
(1) first by Li
2cO
3, ZnO, TiO
2and Fe
2o
3by molecular formula Li
0.43zn
0.27ti
0.13fe
2.17o
4be mixed with main powder;
(2) main powder step (1) being prepared mixes, according to the weight ratio of main powder and deionized water, be that 1:1.5 adds deionized water in main powder, adopt wet milling process to mix 4～5h, after taking-up, at 100～120 ℃, dry, with 80 object screen clothes, sieve, the main powder after sieving rises to 780～800 ℃ of insulation 2h left and right with the temperature rise rate of 2 ℃/min by room temperature;
(3) sintering agent LBSCA glass is with 52.45mol%Li
2o, 31.06mol%B
2o
3, 11.99mol%SiO
2, 2mol%CaO and 2.5mol%Al
2o
3batching, with wet milling process ball milling 12h, after taking-up, at 100～120 ℃, dry, with 80 object screen clothes, sieve, powder after sieving is put into crucible and by room temperature, is risen to 1150 ℃ of insulation 1h with the temperature rise rate of 2 ℃/min, be cooled to about 1000 ℃ taking-ups and pour rapid quenching in deionized water into, after oven dry, wear into micron particles;
(4) major ingredient of step (2) gained being added to weight percent is 0.3% LBSCA glass powder, be made into powder, according to the weight ratio of powder and deionized water, be that 1:1 adds deionized water in powder, after ball milling 6h, take out, put into baking oven and dry at 100～120 ℃, be pressed into blank after gained powder is added to 10% organic binder bond granulation by weight, then blank is put into atmosphere furnace, in oxygen atmosphere, at 920 ℃, sintering 2h gets final product to obtain microwave gyromagnetic ferrite material.
The gyromagnet performance of this LiZnTi Ferrite Material is: saturation induction density B
s: 360mT, ferromagnetic resonance line width Δ H:182Oe, coercive force H
c: 168A/m, squareness ratio B
r/ B
s: 0.82, porosity p:5.3%.
Embodiment 7:
(1) first by Li
2cO
3, ZnO, TiO
2and Fe
2o
3by molecular formula Li
0.43zn
0.27ti
0.13fe
2.17o
4be mixed with main powder;
(2) main powder step (1) being prepared mixes, according to the weight ratio of main powder and deionized water, be that 1:1.5 adds deionized water in main powder, adopt wet milling process to mix 4～5h, after taking-up, at 100～120 ℃, dry, with 80 object screen clothes, sieve, the main powder after sieving rises to 780～800 ℃ of insulation 2h left and right with the temperature rise rate of 2 ℃/min by room temperature;
(3) sintering agent LBSCA glass is with 52.45mol%Li
2o, 31.06mol%B
2o
3, 11.99mol%SiO
2, 2mol%CaO and 2.5mol%Al
2o
3batching, with wet milling process ball milling 12h, after taking-up, at 100～120 ℃, dry, with 80 object screen clothes, sieve, powder after sieving is put into crucible and by room temperature, is risen to 1150 ℃ of insulation 1h with the temperature rise rate of 2 ℃/min, be cooled to about 1000 ℃ taking-ups and pour rapid quenching in deionized water into, after oven dry, wear into micron particles;
(4) major ingredient of step (2) gained being added to weight percent is 0.4% LBSCA glass powder, be made into powder, according to the weight ratio of powder and deionized water, be that 1:1 adds deionized water in powder, after ball milling 6h, take out, put into baking oven and dry at 100～120 ℃, be pressed into blank after gained powder is added to 10% organic binder bond granulation by weight, then blank is put into atmosphere furnace, in oxygen atmosphere, at 920 ℃, sintering 2h gets final product to obtain microwave gyromagnetic ferrite material.
The gyromagnet performance of this LiZnTi Ferrite Material is: saturation induction density B
s: 347mT, ferromagnetic resonance line width Δ H:161Oe, coercive force H
c: 174A/m, squareness ratio B
r/ B
s: 0.82, porosity p:4.8%.
Embodiment 8:
(1) first by Li
2cO
3, ZnO, TiO
2and Fe
2o
3by molecular formula Li
0.43zn
0.27ti
0.13fe
2.17o
4be mixed with main powder;
(2) main powder step (1) being prepared mixes, according to the weight ratio of main powder and deionized water, be that 1:1.5 adds deionized water in main powder, adopt wet milling process to mix 4～5h, after taking-up, at 100～120 ℃, dry, with 80 object screen clothes, sieve, the main powder after sieving rises to 780～800 ℃ of insulation 2h left and right with the temperature rise rate of 2 ℃/min by room temperature;
(3) sintering agent LBSCA glass is with 52.45mol%Li
2o, 31.06mol%B
2o
3, 11.99mol%SiO
2, 2mol%CaO and 2.5mol%Al
2o
3batching, with wet milling process ball milling 12h, after taking-up, at 100～120 ℃, dry, with 80 object screen clothes, sieve, powder after sieving is put into crucible and by room temperature, is risen to 1150 ℃ of insulation 1h with the temperature rise rate of 2 ℃/min, be cooled to about 1000 ℃ taking-ups and pour rapid quenching in deionized water into, after oven dry, wear into micron particles;
(4) major ingredient of step (2) gained being added to weight percent is 0.55% LBSCA glass powder, be made into powder, according to the weight ratio of powder and deionized water, be that 1:1 adds deionized water in powder, after ball milling 6h, take out, put into baking oven and dry at 100～120 ℃, be pressed into blank after gained powder is added to 10% organic binder bond granulation by weight, then blank is put into atmosphere furnace, in oxygen atmosphere, at 920 ℃, sintering 2h gets final product to obtain microwave gyromagnetic ferrite material.
The gyromagnet performance of this LiZnTi Ferrite Material is: saturation induction density B
s: 340mT, ferromagnetic resonance line width Δ H:138Oe, coercive force H
c: 188A/m, squareness ratio B
r/ B
s: 0.83, porosity p:4.5%.
To sum up, the invention provides LiZnTi Ferrite Material and preparation method for a kind of LTCC phase shifter, this preparation method is successfully down to 900 ℃ of left and right by the ferritic sintering temperature of LiZnTi, and keep the gyromagnet performance of LiZnTi Ferrite Material excellence, thereby make this material to burn altogether the manufacture that can be widely used in LTCC phase shifter with silver electrode.
Claims (4)
1.LTCC phase shifter LiZnTi Ferrite Material, consists of major ingredient and glassy phase sintering agent, and wherein major ingredient weight percent is 99.3～99.85%, glassy phase sintering agent weight percent is 0.15～0.7%, it is characterized in that, described major ingredient is with Li
2cO
3, ZnO, TiO
2and Fe
2o
3for raw material, according to molecular formula Li
0.43zn
0.27ti
0.13fe
2.17o
4preparation; Described glassy phase sintering agent is with Li
2o, B
2o
3, SiO
2, CaO and Al
2o
3for raw material, 52.45mol%Li in proportion
2o, 31.06mol%B
2o
3, 11.99mol%SiO
2, 2mol%CaO and 2.5mol%Al
2o
3preparation.
2. by LTCC phase shifter LiZnTi Ferrite Material described in claim 1, it is characterized in that described major ingredient Raw Li
2cO
3, ZnO, TiO
2and Fe
2o
3mol ratio is 43:54:26:217.
3. by LTCC phase shifter LiZnTi Ferrite Material described in claim 1, it is characterized in that, described glassy phase sintering agent batching, by 12h ball milling, is heated to 1150 ℃ of insulation 1h, is cooled to 1000 ℃ of rapid quenchings and makes.
The preparation method of LiZnTi Ferrite Material for 4.LTCC phase shifter, comprises the following steps:
Step 1. is with Li
2cO
3, ZnO, TiO
2and Fe
2o
3for raw material, according to molecular formula Li
0.43zn
0.27ti
0.13fe
2.17o
4preparation winner powder;
Step 2. mixes step 1 preparation winner powder, according to the weight ratio of main powder and deionized water, be that 1:1.5 adds deionized water in main powder, adopt wet milling process to mix 4～5h, after taking-up, at 100～120 ℃, dry, cross 80 mesh sieves, main powder after sieving is warming up to 780～800 ℃ of insulation 2h with the temperature rise rate of 2 ℃/min by room temperature, is prepared into major ingredient;
Step 3. is with Li
2o, B
2o
3, SiO
2, CaO and Al
2o
3for raw material, 52.45mol%Li in proportion
2o, 31.06mol%B
2o
3, 11.99mol%SiO
2, 2mol%CaO and 2.5mol%Al
2o
3batching, with wet milling process ball milling 12h, after taking-up, at 100～120 ℃, dry, cross 80 mesh sieves, powder after sieving is put into crucible and by room temperature, is warming up to 1150 ℃ of insulation 1h with the temperature rise rate of 2 ℃/min, be cooled to 1000 ℃ of taking-ups and pour rapid quenching in deionized water into, after oven dry, wear into micron particles, be prepared into LBSCA glassy phase sintering agent;
Step 4. adds LBSCA glassy phase sintering agent in step 2 gained major ingredient, is made into powder, and wherein major ingredient weight percent is 99.3～99.85%, glassy phase sintering agent weight percent is 0.15～0.7%; According to the weight ratio of powder and deionized water, be that 1:1 adds deionized water in powder, after ball milling 6h, take out, put into baking oven dries at 100～120 ℃, after being added to 10% organic binder bond granulation by weight, gained powder is pressed into blank, again blank is put into atmosphere furnace, in oxygen atmosphere, at 900～920 ℃, sintering 2h is prepared into LiZnTi Ferrite Material.
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|---|---|---|---|
| CN201410252398.8A CN104030671B (en) | 2014-06-09 | 2014-06-09 | LTCC phase shifter LiZnTi Ferrite Material and preparation method |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104402427A (en) * | 2014-11-27 | 2015-03-11 | 电子科技大学 | Low-coercivity LiZnTi gyromagnetic ferrite material and preparation method thereof |
| CN104496448A (en) * | 2014-11-27 | 2015-04-08 | 电子科技大学 | LiZnTi gyromagnetic ferrite material and preparation method thereof |
| CN104944947A (en) * | 2015-05-20 | 2015-09-30 | 电子科技大学 | Microwave rotating magnetic-dielectric composite ceramic material and preparation method thereof |
| CN105236949A (en) * | 2015-09-14 | 2016-01-13 | 电子科技大学 | High squareness ratio LiZnTi ferrite material and preparation method thereof |
| CN108774005A (en) * | 2018-05-24 | 2018-11-09 | 成都锦钛精工科技有限公司 | Vitreum formula additive and preparation method and the application in ferrite permanent-magnet materials preparation |
| CN113321497A (en) * | 2021-06-30 | 2021-08-31 | 西南科技大学 | LiZnTi ferrite with large grain size and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103771842A (en) * | 2014-01-10 | 2014-05-07 | 电子科技大学 | LTCC (Low Temperature Co-fired Ceramics) microwave ceramic material with low cost, low dielectric constant and low loss and preparation method thereof |
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| CN103771842A (en) * | 2014-01-10 | 2014-05-07 | 电子科技大学 | LTCC (Low Temperature Co-fired Ceramics) microwave ceramic material with low cost, low dielectric constant and low loss and preparation method thereof |
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| TINGCHUAN ZHOU ET AL.: "Grain,growth,densification, and gyromagnetic properties of LiZnTi ferrites with H3BO3－Bi2O3-SiO2-ZnO glass additon", 《JOURNAL OF APPLIED PHYSICS》, vol. 115, 3 February 2014 (2014-02-03) * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104402427A (en) * | 2014-11-27 | 2015-03-11 | 电子科技大学 | Low-coercivity LiZnTi gyromagnetic ferrite material and preparation method thereof |
| CN104496448A (en) * | 2014-11-27 | 2015-04-08 | 电子科技大学 | LiZnTi gyromagnetic ferrite material and preparation method thereof |
| CN104496448B (en) * | 2014-11-27 | 2016-08-24 | 电子科技大学 | A kind of LiZnTi gyromagnetic ferrite material and preparation method thereof |
| CN104944947A (en) * | 2015-05-20 | 2015-09-30 | 电子科技大学 | Microwave rotating magnetic-dielectric composite ceramic material and preparation method thereof |
| CN104944947B (en) * | 2015-05-20 | 2017-07-11 | 电子科技大学 | A kind of microwave gyromagnet dielectric composite ceramic material and preparation method thereof |
| CN105236949A (en) * | 2015-09-14 | 2016-01-13 | 电子科技大学 | High squareness ratio LiZnTi ferrite material and preparation method thereof |
| CN108774005A (en) * | 2018-05-24 | 2018-11-09 | 成都锦钛精工科技有限公司 | Vitreum formula additive and preparation method and the application in ferrite permanent-magnet materials preparation |
| CN108774005B (en) * | 2018-05-24 | 2021-08-24 | 成都锦钛精工科技有限公司 | Vitreous additive, preparation method and application in preparation of ferrite permanent magnet material |
| CN113321497A (en) * | 2021-06-30 | 2021-08-31 | 西南科技大学 | LiZnTi ferrite with large grain size and preparation method thereof |
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