CN104030671B - LTCC phase shifter LiZnTi Ferrite Material and preparation method - Google Patents

LTCC phase shifter LiZnTi Ferrite Material and preparation method Download PDF

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CN104030671B
CN104030671B CN201410252398.8A CN201410252398A CN104030671B CN 104030671 B CN104030671 B CN 104030671B CN 201410252398 A CN201410252398 A CN 201410252398A CN 104030671 B CN104030671 B CN 104030671B
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ferrite material
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deionized water
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张怀武
周廷川
廖宇龙
贾利军
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University of Electronic Science and Technology of China
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Abstract

Technical problem to be solved by this invention is, meeting in less than 950 DEG C low sintering situations, 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.This Ferrite Material is made up 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%; 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 52.45mol%Li in proportion 2o, 31.06mol%B 2o 3, 11.99mol%SiO 2, 2mol%CaO and 2.5mol%Al 2o 3through 12h ball milling after batching, be heated to 1150 DEG C of insulation 1h, be cooled to 1000 DEG C of rapid quenchings and make.Ferritic for LiZnTi sintering temperature is successfully down to about 900 DEG C by this ferrite material preparation method for material, and keeps the gyromagnet performance of LiZnTi Ferrite Material excellence, thus makes this material can burn the manufacture that can be widely used in LTCC phase shifter altogether with silver electrode.

Description

LTCC phase shifter LiZnTi Ferrite Material and preparation method
Technical field
The present invention relates to gyromagnetic ferrite material and the glass-ceramic preparing technical field of LTCC technology application, 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 phase shifter and realize miniaturization, integrated so that modularization seems more and more urgent.LTCC (LTCC) technology is utilized 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 DEG C ~ 950 DEG C.But mainly apply material as phase shifter, traditional method prepares the ferritic sintering temperature of LiZnTi higher than the top temperature of burning altogether with silver electrode in LTCC technology (961 DEG C).Therefore, the sintering temperature reducing LiZnTi Ferrite Material keeps excellent gyromagnet performance to be technical barrier urgently to be resolved hurrily simultaneously.
Summary of the invention
Technical problem to be solved by this invention is, meeting in less than 950 DEG C low sintering situations, 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, be made up of major ingredient and glassy phase sintering agent, wherein major ingredient weight percent is 99.3 ~ 99.85%, glassy phase sintering agent weight percent is 0.15 ~ 0.7%, and 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; Through 12h ball milling after described glassy phase sintering agent batching, be heated to 1150 DEG C of insulation 1h, be cooled to 1000 DEG C of rapid quenchings and make.
The preparation method of above-mentioned LTCC phase shifter LiZnTi Ferrite Material, 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 1 is prepared winner's powder and is mixed by step 2., be that 1:1.5 adds deionized water in main powder according to the weight ratio of main powder and deionized water, adopt wet milling process mixing 4 ~ 5h, dry at 100 ~ 120 DEG C after taking-up, cross 80 mesh sieves, main powder after sieving by room temperature to 780 ~ 800 DEG C insulation 2h, is namely prepared into major ingredient with the temperature rise rate of 2 DEG C/min;
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, dry at 100 ~ 120 DEG C after taking-up, cross 80 mesh sieves, powder after sieving puts into crucible with the temperature rise rate of 2 DEG C/min by room temperature to 1150 DEG C insulation 1h, be cooled to 1000 DEG C of taking-ups and pour rapid quenching in deionized water into, wear into micron particles after oven dry, be namely 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%; Be that 1:1 adds deionized water in powder according to the weight ratio of powder and deionized water, take out after ball milling 6h, put into baking oven to dry at 100 ~ 120 DEG C, blank is pressed into after gained powder being added by weight 10% organic binder bond granulation, again blank is put into atmosphere furnace, in oxygen atmosphere, at 900 ~ 920 DEG C, sinter 2h be namely prepared into LiZnTi Ferrite Material.
The invention provides a kind of LTCC phase shifter LiZnTi Ferrite Material and preparation method, ferritic for LiZnTi sintering temperature is successfully down to about 900 DEG C by this preparation method, and keep the gyromagnet performance of LiZnTi Ferrite Material excellence, thus make this material can burn the manufacture that can be widely used in LTCC phase shifter altogether with silver electrode.
Accompanying drawing explanation
Fig. 1 is that the present invention is prepared into LTCC phase shifter LiZnTi ferrite SEM and schemes,
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 μm.
Embodiment
The invention provides a kind of LTCC phase shifter LiZnTi Ferrite Material and preparation method thereof, the description obtaining clearly by following nonlimiting examples.
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) the main powder that step (1) prepares is mixed, be that 1:1.5 adds deionized water in main powder according to the weight ratio of main powder and deionized water, adopt wet milling process mixing 4 ~ 5h, dry at 100 ~ 120 DEG C after taking-up, sieve with 80 object screen clothes, the main powder after sieving rises to 780 ~ 800 DEG C of insulation about 2h with the temperature rise rate of 2 DEG C/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, dry at 100 ~ 120 DEG C after taking-up, sieve with 80 object screen clothes, powder after sieving is put into crucible and is risen to 1150 DEG C of insulation 1h with the temperature rise rate of 2 DEG C/min by room temperature, be cooled to about 1000 DEG C taking-ups and pour rapid quenching in deionized water into, after oven dry, wear into micron particles;
(4) major ingredient of step (2) gained is added the LBSCA glass powder that weight percent is 0.3%, be made into powder, be that 1:1 adds deionized water in powder according to the weight ratio of powder and deionized water, take out after ball milling 6h, put into baking oven to dry at 100 ~ 120 DEG C, be pressed into blank after gained powder being added by weight 10% organic binder bond granulation, then blank is put into atmosphere furnace, in oxygen atmosphere, sinter at 900 DEG C 2h gyromagnetic ferrite material.The rugged SY-8232B-H analyser test of Japanese rock of saturation induction density, coercive force, density row's kerosene method test, calculates porosity, by the ferromagnetic resonance line width of IEC standard measure sample under 9.3GHz according to actual density and theoretical density.
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) the main powder that step (1) prepares is mixed, be that 1:1.5 adds deionized water in main powder according to the weight ratio of main powder and deionized water, adopt wet milling process mixing 4 ~ 5h, dry at 100 ~ 120 DEG C after taking-up, sieve with 80 object screen clothes, the main powder after sieving rises to 780 ~ 800 DEG C of insulation about 2h with the temperature rise rate of 2 DEG C/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, dry at 100 ~ 120 DEG C after taking-up, sieve with 80 object screen clothes, powder after sieving is put into crucible and is risen to 1150 DEG C of insulation 1h with the temperature rise rate of 2 DEG C/min by room temperature, be cooled to about 1000 DEG C taking-ups and pour rapid quenching in deionized water into, after oven dry, wear into micron particles;
(4) major ingredient of step (2) gained is added the LBSCA glass powder that weight percent is 0.4%, be made into powder, be that 1:1 adds deionized water in powder according to the weight ratio of powder and deionized water, take out after ball milling 6h, put into baking oven to dry at 100 ~ 120 DEG C, be pressed into blank after gained powder being added by weight 10% organic binder bond granulation, then blank is put into atmosphere furnace, in oxygen atmosphere, sinter at 900 DEG C 2h 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) the main powder that step (1) prepares is mixed, be that 1:1.5 adds deionized water in main powder according to the weight ratio of main powder and deionized water, adopt wet milling process mixing 4 ~ 5h, dry at 100 ~ 120 DEG C after taking-up, sieve with 80 object screen clothes, the main powder after sieving rises to 780 ~ 800 DEG C of insulation about 2h with the temperature rise rate of 2 DEG C/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, dry at 100 ~ 120 DEG C after taking-up, sieve with 80 object screen clothes, powder after sieving is put into crucible and is risen to 1150 DEG C of insulation 1h with the temperature rise rate of 2 DEG C/min by room temperature, be cooled to about 1000 DEG C taking-ups and pour rapid quenching in deionized water into, after oven dry, wear into micron particles;
(4) major ingredient of step (2) gained is added the LBSCA glass powder that weight percent is 0.55%, be made into powder, be that 1:1 adds deionized water in powder according to the weight ratio of powder and deionized water, take out after ball milling 6h, put into baking oven to dry at 100 ~ 120 DEG C, blank is pressed into after gained powder being added by weight 10% organic binder bond granulation, again blank is put into atmosphere furnace, in oxygen atmosphere, sinter at 900 DEG C 2h 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) the main powder that step (1) prepares is mixed, be that 1:1.5 adds deionized water in main powder according to the weight ratio of main powder and deionized water, adopt wet milling process mixing 4 ~ 5h, dry at 100 ~ 120 DEG C after taking-up, sieve with 80 object screen clothes, the main powder after sieving rises to 780 ~ 800 DEG C of insulation about 2h with the temperature rise rate of 2 DEG C/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, dry at 100 ~ 120 DEG C after taking-up, sieve with 80 object screen clothes, powder after sieving is put into crucible and is risen to 1150 DEG C of insulation 1h with the temperature rise rate of 2 DEG C/min by room temperature, be cooled to about 1000 DEG C taking-ups and pour rapid quenching in deionized water into, after oven dry, wear into micron particles;
(4) major ingredient of step (2) gained is added the LBSCA glass powder that weight percent is 0.7%, be made into powder, be that 1:1 adds deionized water in powder according to the weight ratio of powder and deionized water, take out after ball milling 6h, put into baking oven to dry at 100 ~ 120 DEG C, be pressed into blank after gained powder being added by weight 10% organic binder bond granulation, then blank is put into atmosphere furnace, in oxygen atmosphere, sinter at 900 DEG C 2h 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) the main powder that step (1) prepares is mixed, be that 1:1.5 adds deionized water in main powder according to the weight ratio of main powder and deionized water, adopt wet milling process mixing 4 ~ 5h, dry at 100 ~ 120 DEG C after taking-up, sieve with 80 object screen clothes, the main powder after sieving rises to 780 ~ 800 DEG C of insulation about 2h with the temperature rise rate of 2 DEG C/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, dry at 100 ~ 120 DEG C after taking-up, sieve with 80 object screen clothes, powder after sieving is put into crucible and is risen to 1150 DEG C of insulation 1h with the temperature rise rate of 2 DEG C/min by room temperature, be cooled to about 1000 DEG C taking-ups and pour rapid quenching in deionized water into, after oven dry, wear into micron particles;
(4) major ingredient of step (2) gained is added the LBSCA glass powder that weight percent is 0.15%, be made into powder, be that 1:1 adds deionized water in powder according to the weight ratio of powder and deionized water, take out after ball milling 6h, put into baking oven to dry at 100 ~ 120 DEG C, blank is pressed into after gained powder being added by weight 10% organic binder bond granulation, again blank is put into atmosphere furnace, in oxygen atmosphere, sinter at 920 DEG C 2h 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) the main powder that step (1) prepares is mixed, be that 1:1.5 adds deionized water in main powder according to the weight ratio of main powder and deionized water, adopt wet milling process mixing 4 ~ 5h, dry at 100 ~ 120 DEG C after taking-up, sieve with 80 object screen clothes, the main powder after sieving rises to 780 ~ 800 DEG C of insulation about 2h with the temperature rise rate of 2 DEG C/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, dry at 100 ~ 120 DEG C after taking-up, sieve with 80 object screen clothes, powder after sieving is put into crucible and is risen to 1150 DEG C of insulation 1h with the temperature rise rate of 2 DEG C/min by room temperature, be cooled to about 1000 DEG C taking-ups and pour rapid quenching in deionized water into, after oven dry, wear into micron particles;
(4) major ingredient of step (2) gained is added the LBSCA glass powder that weight percent is 0.3%, be made into powder, be that 1:1 adds deionized water in powder according to the weight ratio of powder and deionized water, take out after ball milling 6h, put into baking oven to dry at 100 ~ 120 DEG C, be pressed into blank after gained powder being added by weight 10% organic binder bond granulation, then blank is put into atmosphere furnace, in oxygen atmosphere, sinter at 920 DEG C 2h 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) the main powder that step (1) prepares is mixed, be that 1:1.5 adds deionized water in main powder according to the weight ratio of main powder and deionized water, adopt wet milling process mixing 4 ~ 5h, dry at 100 ~ 120 DEG C after taking-up, sieve with 80 object screen clothes, the main powder after sieving rises to 780 ~ 800 DEG C of insulation about 2h with the temperature rise rate of 2 DEG C/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, dry at 100 ~ 120 DEG C after taking-up, sieve with 80 object screen clothes, powder after sieving is put into crucible and is risen to 1150 DEG C of insulation 1h with the temperature rise rate of 2 DEG C/min by room temperature, be cooled to about 1000 DEG C taking-ups and pour rapid quenching in deionized water into, after oven dry, wear into micron particles;
(4) major ingredient of step (2) gained is added the LBSCA glass powder that weight percent is 0.4%, be made into powder, be that 1:1 adds deionized water in powder according to the weight ratio of powder and deionized water, take out after ball milling 6h, put into baking oven to dry at 100 ~ 120 DEG C, be pressed into blank after gained powder being added by weight 10% organic binder bond granulation, then blank is put into atmosphere furnace, in oxygen atmosphere, sinter at 920 DEG C 2h 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) the main powder that step (1) prepares is mixed, be that 1:1.5 adds deionized water in main powder according to the weight ratio of main powder and deionized water, adopt wet milling process mixing 4 ~ 5h, dry at 100 ~ 120 DEG C after taking-up, sieve with 80 object screen clothes, the main powder after sieving rises to 780 ~ 800 DEG C of insulation about 2h with the temperature rise rate of 2 DEG C/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, dry at 100 ~ 120 DEG C after taking-up, sieve with 80 object screen clothes, powder after sieving is put into crucible and is risen to 1150 DEG C of insulation 1h with the temperature rise rate of 2 DEG C/min by room temperature, be cooled to about 1000 DEG C taking-ups and pour rapid quenching in deionized water into, after oven dry, wear into micron particles;
(4) major ingredient of step (2) gained is added the LBSCA glass powder that weight percent is 0.55%, be made into powder, be that 1:1 adds deionized water in powder according to the weight ratio of powder and deionized water, take out after ball milling 6h, put into baking oven to dry at 100 ~ 120 DEG C, blank is pressed into after gained powder being added by weight 10% organic binder bond granulation, again blank is put into atmosphere furnace, in oxygen atmosphere, sinter at 920 DEG C 2h 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 a kind of LTCC phase shifter LiZnTi Ferrite Material and preparation method, ferritic for LiZnTi sintering temperature is successfully down to about 900 DEG C by this preparation method, and keep the gyromagnet performance of LiZnTi Ferrite Material excellence, thus make this material can burn the manufacture that can be widely used in LTCC phase shifter altogether with silver electrode.

Claims (4)

1.LTCC phase shifter LiZnTi Ferrite Material, is made up 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%, and 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, through 12h ball milling after described glassy phase sintering agent batching, be heated to 1150 DEG C of insulation 1h, be cooled to 1000 DEG C of rapid quenchings and make.
The 4.LTCC phase shifter preparation method of LiZnTi Ferrite Material, 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 1 is prepared winner's powder and is mixed by step 2., be that 1:1.5 adds deionized water in main powder according to the weight ratio of main powder and deionized water, adopt wet milling process mixing 4 ~ 5h, dry at 100 ~ 120 DEG C after taking-up, cross 80 mesh sieves, main powder after sieving by room temperature to 780 ~ 800 DEG C insulation 2h, is namely prepared into major ingredient with the temperature rise rate of 2 DEG C/min;
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, dry at 100 ~ 120 DEG C after taking-up, cross 80 mesh sieves, powder after sieving puts into crucible with the temperature rise rate of 2 DEG C/min by room temperature to 1150 DEG C insulation 1h, be cooled to 1000 DEG C of taking-ups and pour rapid quenching in deionized water into, wear into micron particles after oven dry, be namely 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%; Be that 1:1 adds deionized water in powder according to the weight ratio of powder and deionized water, take out after ball milling 6h, put into baking oven to dry at 100 ~ 120 DEG C, blank is pressed into after gained powder being added by weight 10% organic binder bond granulation, again blank is put into atmosphere furnace, in oxygen atmosphere, at 900 ~ 920 DEG C, sinter 2h be namely prepared into LiZnTi Ferrite Material.
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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
CN105236949B (en) * 2015-09-14 2017-06-09 电子科技大学 One kind has squareness ratio LiZnTi Ferrite Materials high and preparation method thereof
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
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