CN108383515A - A kind of preparation method of the texturing M-type strontium ferrite substrate material of high-orientation - Google Patents
A kind of preparation method of the texturing M-type strontium ferrite substrate material of high-orientation Download PDFInfo
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Abstract
A kind of preparation method of the texturing M-type strontium ferrite substrate material of high-orientation provided by the invention, belongs to magnetic material preparing technical field.First, using the raw material powder after low temperature calcination as base stock, template that the congruent platelet that is obtained using hydro-thermal reaction is grown as induced crystal texturing；Then, curtain coating laminated process is introduced, is uniformly distributed with ensureing that crystallite thin slice is parallel to surface in ceramic chips；Finally, by controlling calcination temperature and soaking time, the single-phase oriented growth of M type hexad ferrites is further ensured.The present invention by it is above-mentioned three aspect synergistic effect, obtain texturing M-type strontium ferrite substrate material, calculated according to X-ray diffraction intensity, the baseplate material the direction (0 0 l) the degree of orientation up to 96%.
Description
Technical field
The invention belongs to magnetic material preparing technical fields, and in particular to a kind of texturing M-type strontium iron oxygen of high-orientation
The preparation method of structure base board material.
Background technology
M-type strontium ferrite (SrFe12O19) there is higher saturation magnetization, high magnetocrystalline anisotropy field, higher
The advantages that coercivity, good chemical stability, has in miniaturization microwave device, magneto-optic, high-density magnetic recording media etc.
It and is widely applied.Currently, the preparation method of M-type strontium ferrite powder mainly has：Solid reaction process and wet chemistry method are (such as coprecipitated
Shallow lake method, sol-gel method, hydro-thermal method etc.).Wherein, hydro-thermal method is in control product form, raising anisotropic growth and crystal
Dispersion etc. there is apparent advantage, compared to solid reaction process, M phase powder can be obtained by needing not move through high-temperature calcination
Body.Since strontium ferrite has prodigious magnetocrystalline anisotropy field, generally use dry method or wet method pressing under magnetic field, magnetic field is utilized
Regulate and control induced orientation, to obtain anisotropy magnet.However, complicated pressing under magnetic field process is difficult to adapt to microwave with state modulator
The application demand of device and circuit integration technique.
Application No. is 200610019606.5, it is entitled " a kind of textured single phase hexagonal ferrite it is quick
The Chinese invention patent of preparation method " discloses a kind of preparation method of textured single phase hexagonal ferrite, will be co-precipitated
Presoma is fitted into high-strength graphite grinding tool and is positioned in discharge plasma sintering system, makes co-precipitation forerunner with the mode vacuumized
Body vacuum-densified at 5~20MPa is molded, and is 100~300 DEG C/min, 850~1000 DEG C of sintering temperature, is pressed in heating rate
Discharge plasma sintering is carried out under 5~20MPa of power, 10~40min of time, obtains texturing hexgonal screw, it still, should
Procedure is complicated, and the obtained ferrite degree of orientation is not also high.It is entitled " a kind of application No. is 201611001717.3
The Chinese invention patent of the preparation method of highly oriented strontium ferrite " discloses a kind of preparation method of highly oriented strontium ferrite, first
First with SrCl2·6H2O, FeCl3·6H2O and NaOH is raw material, obtains hexagonal plate strontium ferrite particle using hydro-thermal method, so
Afterwards by obtained strontium ferrite particle and epoxy resin pressing under magnetic field after evenly mixing, orientation texture is generated；However, in this method
Contain Fe in hexagonal plate strontium ferrite particle2O3、SrCO3Equal dephasigns so that the degree of orientation of product is affected, and is still
Magnetic anisotropy is obtained using pressing under magnetic field, complicated pressing under magnetic field process is difficult to adapt to Microwave Devices ＆ Circuits with state modulator
The application demand of integrated technology.
Invention content
The purpose of the present invention is to provide a kind of preparation sides of the texturing M-type strontium ferrite substrate material of high-orientation
Method.
To achieve the above object, the technical solution adopted by the present invention is as follows：
A kind of preparation method of the texturing M-type strontium ferrite substrate material of high-orientation, specifically includes following steps：
The preparation of step 1, hexagonal platelet powder：
1.1 ferric nitrate, strontium nitrate are added in deionized water, are uniformly mixed, obtain mixed liquor A；Wherein, in mixed liquor A
The molar ratio of a concentration of 1.2~1.5mol/L of ferric nitrate, ferric nitrate and strontium nitrate is 12：(1.5~2)；
1.2 compound concentrations are the strong base solution of 4.6~6mol/L；
1.3 strong base solutions for obtaining the mixed liquor A that step 1.1 obtains and step 1.2 mix, and obtain mixed liquid B,
In, the volume ratio of mixed liquor A and strong base solution is 3：4；
1.4 are transferred to the mixed liquid B that step 1.3 obtains in reaction kettle, at a temperature of 215~220 DEG C hydro-thermal reaction 1~
4h is detached after reaction, dry, obtains hexagonal platelet powder；
The preparation of step 2, raw material powder：
With Fe2O3、SrCO3For raw material, according to molar ratio Fe2O3：SrCO3=(5~7)：1 ratio dispensing, wet ball grinding 4
~6h is dried, sieving, and the powder after sieving keeps the temperature 2~4h in Muffle furnace at 600~800 DEG C, with stove cooled to room temperature
Afterwards, raw material powder is obtained；
The preparation of step 3, ferrite substrate：
3.1 mix the hexagonal platelet powder that step 1 obtains and raw material powder that step 2 obtains, obtain mixed powder；Its
In, the mass percent of hexagonal platelet powder is 15wt%~30wt%, the mass percent of raw material powder be 70wt%~
85wt%；
3.2 in the mixed powder that step 3.1 obtains be added be equivalent to the organic molten of mixed powder 40wt%~60wt%
Agent, the organic binder for being equivalent to mixed powder 25wt%~35wt% and the dispersion for being equivalent to mixed powder 2wt%~4wt%
Agent, 14~16h of ball milling, obtained slurry obtain ceramic chips through curtain coating, lamination, hot pressing；
3.3 are placed in the ceramic chips that step 3.2 obtains in Muffle furnace, at a temperature of 1175 DEG C~1185 DEG C keep the temperature 10~
20h takes out, you can obtain the ferrite substrate material after stove cooled to room temperature.
Further, highly basic described in step 1.2 is sodium hydroxide, potassium hydroxide etc..
Further, organic solvent described in step 3.2 is dimethylbenzene, n-butanol, propyl acetate or isobutanol etc.；It is described
Organic binder is B-76, vinyl or acrylic resin etc. in polyvinyl butyral system；The dispersant is X-
100, S-80 or fish oil etc..
Beneficial effects of the present invention are：
A kind of preparation method of the texturing M-type strontium ferrite substrate material of high-orientation provided by the invention is adopted first
Use the raw material powder after low temperature calcination as base stock, the congruent platelet obtained using hydro-thermal reaction is knitted as induced crystal
The template of structure metaplasia length；Then, curtain coating laminated process is introduced, is uniformly divided with ensureing that crystallite thin slice is parallel to surface in ceramic chips
Cloth；Finally, by controlling calcination temperature and soaking time, the single-phase oriented growth of M type hexad ferrites is further ensured.This
Invention obtains texturing M-type strontium ferrite substrate material by the synergistic effect of above-mentioned three aspect, strong according to X-ray diffraction
Degree calculate, the baseplate material the direction (0 0l) the degree of orientation up to 96%.
Description of the drawings
Fig. 1 is the XRD spectrum for the hexagonal platelet powder that 3 step 1 of embodiment obtains；
Fig. 2 is the XRD spectrum for the baseplate material that comparative example 5 (a) and embodiment 3 (b) obtain；
Fig. 3 is VSM magnetic of the obtained baseplate material of embodiment 3 under the perpendicular and parallel external magnetic field in substrate surface that hangs down
Hysteresis curves curve.
Specific implementation mode
With reference to the accompanying drawings and examples, technical scheme of the present invention is described in detail.
A kind of preparation method of the texturing M-type strontium ferrite substrate material of high-orientation, specifically includes following steps：
The preparation of step 1, hexagonal platelet powder：
1.1 ferric nitrate, strontium nitrate are added in deionized water, are uniformly mixed, obtain mixed liquor A；Wherein, in mixed liquor A
The molar ratio of a concentration of 1.2~1.5mol/L of ferric nitrate, ferric nitrate and strontium nitrate is 12：(1.5~2)；
1.2 compound concentrations are the strong base solution of 4.6~6mol/L；
1.3 strong base solutions for obtaining the mixed liquor A that step 1.1 obtains and step 1.2 mix, and obtain mixed liquid B,
In, the volume ratio of mixed liquor A and strong base solution is 3：4；
1.4 are transferred to the mixed liquid B that step 1.3 obtains in reaction kettle, and nitrogen is filled with after sealing so that in reaction kettle just
Beginning air pressure is 1~2MPa, reaction kettle is run, in stir speed (S.S.)<Hydro-thermal is anti-under conditions of 120r/min, temperature are 215~220 DEG C
1~4h is answered, after reaction, by the mixed liquor after reaction after filtering, washing, 80 DEG C of dry 2h, obtain hexagonal in an oven
Platelet powder；
The preparation of step 2, raw material powder：
With Fe2O3、SrCO3For raw material, according to molar ratio Fe2O3：SrCO3=(5~7)：1 ratio dispensing, wet ball grinding 4
It dries, be sieved at 90~100 DEG C after~6h, the powder after sieving is put into corundum crucible in Muffle furnace at 600~800 DEG C
2~4h of heat preservation obtains raw material powder after stove cooled to room temperature；
The preparation of step 3, ferrite substrate：
3.1 mix the hexagonal platelet powder that step 1 obtains and raw material powder that step 2 obtains, obtain mixed powder；Its
In, the mass percent of hexagonal platelet powder is 15wt%~30wt%, the mass percent of raw material powder be 70wt%~
85wt%；
3.2 in the mixed powder that step 3.1 obtains be added be equivalent to the organic molten of mixed powder 40wt%~60wt%
Agent, the organic binder for being equivalent to mixed powder 25wt%~35wt% and the dispersion for being equivalent to mixed powder 2wt%~4wt%
Agent, 14~16h of ball milling, obtained slurry obtain ceramic chips through curtain coating, lamination, hot pressing；
3.3 are placed in the ceramic chips that step 3.2 obtains in Muffle furnace, at a temperature of 1175 DEG C~1185 DEG C keep the temperature 10~
20h after cooling to room temperature with the furnace, takes out, you can obtain the ferrite substrate material.
Further, highly basic described in step 1.2 is sodium hydroxide, potassium hydroxide etc..
Further, diameter~1 μm for the hexagonal platelet powder that step 1 obtains, thickness<100nm.
Further, organic solvent described in step 3.2 is dimethylbenzene, n-butanol, propyl acetate or isobutanol etc.；It is described
Organic binder is B-76, vinyl or acrylic resin etc. in polyvinyl butyral system；The dispersant is X-
100, S-80 or fish oil etc..
Embodiment
A kind of preparation method of the texturing M-type strontium ferrite substrate material of high-orientation, specifically includes following steps：
The preparation of step 1, hexagonal platelet powder：
1.1 weigh 82.0304g ferric nitrates (Fe (NO3)3·9H2O), 5.3173g strontium nitrates (Sr (NO3)2) 150mL is added
It in deionized water, is uniformly mixed, obtains mixed liquor A；
1.2, which weigh 42.4489g NaOH, is added in 200mL deionized waters, and stirring and dissolving obtains strong base solution；
1.3 strong base solutions for obtaining the mixed liquor A that step 1.1 obtains and step 1.2 mix, and stir to get mixed liquid B；
1.4 are transferred to the mixed liquid B that step 1.3 obtains in reaction kettle, and nitrogen is filled with after sealing so that in reaction kettle just
Beginning air pressure is 1.5MPa, runs reaction kettle, hydro-thermal reaction 2h under conditions of stir speed (S.S.) 100r/min, temperature are 220 DEG C, instead
After answering, by the mixed liquor after reaction after being filtered, washed, obtained product 80 DEG C of dry 2h in an oven obtain hexagonal
Platelet powder；
The preparation of step 2, raw material powder：
With Fe2O3、SrCO3For raw material, 60.655g Fe are weighed2O3With 9.345g SrCO3, at 100 DEG C after wet ball grinding 6h
Lower drying, sieving, the powder after sieving are put into corundum crucible and keep the temperature 4h at 600 DEG C in Muffle furnace, naturally cooled to stove
After room temperature, raw material powder is obtained；
The preparation of step 3, ferrite substrate：
3.1 mix the hexagonal platelet powder that step 1 obtains and raw material powder that step 2 obtains, obtain mixed powder；Its
In, the mass percent of hexagonal platelet powder is 15wt%~30wt% (mass percent of hexagonal platelet powder is shown in Table 1), raw
The mass percent of feed powder body is 70wt%~85wt%；
3.2 in the mixed powder that step 3.1 obtains be added be equivalent to mixed powder 40wt% dimethylbenzene, be equivalent to it is mixed
It closes the B-76 in the polyvinyl butyral system of powder 30wt% and is equivalent to the dispersant X-100 of mixed powder 3wt%, ball milling
16h, obtained stream of slurry extend thickness as 30 μm or so of film strips, and hot pressing is given birth to for 20 minutes at 80 DEG C, 10Mpa after lamination
Tile；
3.3 are placed in the ceramic chips that step 3.2 obtains in Muffle furnace, at a temperature of 1175 DEG C~1185 DEG C keep the temperature 10~
20h (calcination temperature and soaking time are shown in Table 1) after cooling to room temperature with the furnace, takes out, you can obtain the ferrite substrate material
(performance indicator is shown in Table 2).
Comparative example
A kind of preparation method of the texturing M-type strontium ferrite substrate material of high-orientation, specifically includes following steps：
The preparation of step 1, hexagonal platelet powder：
1.1 weigh 82.0304g ferric nitrates (Fe (NO3)3·9H2O), 5.3173g strontium nitrates (Sr (NO3)2) 150mL is added
It in deionized water, is uniformly mixed, obtains mixed liquor A；
1.2, which weigh 42.4489g NaOH, is added in 200mL deionized waters, and stirring and dissolving obtains strong base solution；
1.3 strong base solutions for obtaining the mixed liquor A that step 1.1 obtains and step 1.2 mix, and stir to get mixed liquid B；
1.4 are transferred to the mixed liquid B that step 1.3 obtains in reaction kettle, and nitrogen is filled with after sealing so that in reaction kettle just
Beginning air pressure is 1.5MPa, runs reaction kettle, hydro-thermal reaction 2h under conditions of stir speed (S.S.) 100r/min, temperature are 220 DEG C, instead
After answering, by the mixed liquor after reaction after being filtered, washed, obtained product 80 DEG C of dry 2h in an oven obtain hexagonal
Platelet powder；
The preparation of step 2, raw material powder：
With Fe2O3、SrCO3For raw material, 60.655g Fe are weighed2O3With 9.345g SrCO3, at 100 DEG C after wet ball grinding 6h
Lower drying, sieving, the powder after sieving are put into corundum crucible and keep the temperature 4h at 600 DEG C in Muffle furnace, naturally cooled to stove
After room temperature, raw material powder is obtained；
The preparation of step 3, ferrite substrate：
3.1 mix the hexagonal platelet powder that step 1 obtains and raw material powder that step 2 obtains, obtain mixed powder；Its
In, the mass percent of hexagonal platelet powder is 15wt%~30wt% (mass percent of hexagonal platelet powder is shown in Table 1), raw
The mass percent of feed powder body is 70wt%~85wt%；
3.2 in the mixed powder that step 3.1 obtains be added be equivalent to mixed powder 40wt% dimethylbenzene, be equivalent to it is mixed
It closes the B-76 in the polyvinyl butyral system of powder 30wt% and is equivalent to the dispersant X-100 of mixed powder 3wt%, ball milling
16h, obtained stream of slurry extend thickness as 30 μm or so of film strips, and hot pressing is given birth to for 20 minutes at 80 DEG C, 10Mpa after lamination
Tile；
3.3 are placed in the ceramic chips that step 3.2 obtains in Muffle furnace, at a set temperature held for some time (calcining temperature
Degree and soaking time are shown in Table 1, and wherein comparative example 5 does not include step 1), after cooling to room temperature with the furnace, take out, you can obtain described
Ferrite substrate material (performance indicator is shown in Table 2).
The process conditions of 1 embodiment and comparative example of table
| Project | Calcination temperature Ts (DEG C) | Soaking time t (h) | Hexagonal platelet powder quality percentage (wt%) |
| Embodiment 1 | 1180 | 10 | 15 |
| Embodiment 2 | 1180 | 20 | 15 |
| Embodiment 3 | 1185 | 10 | 30 |
| Embodiment 4 | 1175 | 20 | 30 |
| Comparative example 1 | 1150 | 10 | 15 |
| Comparative example 2 | 1150 | 20 | 15 |
| Comparative example 3 | 1200 | 10 | 30 |
| Comparative example 4 | 1200 | 20 | 30 |
| Comparative example 5 | 1185 | 10 | 0 |
Note：Ts is calcination temperature, and t is soaking time
The performance evaluation of 2 embodiment and comparative example of table
Table 2 is the degree of orientation and magnetic property assessment result for the baseplate material that embodiment and comparative example obtains, wherein does not reach and refers to
Mark desired mark " # ".From table 2 it can be seen that the baseplate material that the method for the present invention obtains has the texturing knot of high-orientation
Structure can not only meet the needs of microwave magnetic material is to high-performance baseplate material, and its potential magnetoelectric effect is deposited in information
There is huge development prospect in storage field, sensor field.
Fig. 1 is the XRD spectrum for the hexagonal platelet powder that 3 step 1 of embodiment obtains；As shown in Figure 1, the hexagonal platelet obtained
Powder is single M phases, has no the diffraction maximum of other dephasigns.Fig. 2 is the baseplate material that comparative example 5 (a) and embodiment 3 (b) obtain
XRD spectrum；As shown in Figure 2, after self template-mediated growing method using the present invention, obtained baseplate material is at (0 0l)
The diffraction peak intensity in direction is greatly enhanced, and the diffraction maximum of other crystal faces is greatly weakened, and shows that the method for the present invention is made
Texturing baseplate material have the higher degree of orientation.Fig. 3 be the obtained baseplate material of embodiment 3 hang down it is perpendicular and parallel in substrate
VSM Curve of Magnetic Hysteresis Loop under the external magnetic field on surface；From the figure 3, it may be seen that the baseplate material that embodiment 3 obtains is in different directions
Magnetic field under be magnetized that degree is significantly different, and when magnetic field is perpendicular to substrate surface, material is magnetized into saturation state quickly, shows
The direction is direction of easy axis；And when magnetic field is parallel to substrate surface, saturation still cannot be magnetized at 15000Oe, it should
Direction shows difficult magnetization characteristic.
Claims (3)
1. a kind of preparation method of the texturing M-type strontium ferrite substrate material of high-orientation, includes the following steps：
The preparation of step 1, hexagonal platelet powder：
1.1 ferric nitrate, strontium nitrate are added in deionized water, are uniformly mixed, obtain mixed liquor A；Wherein, nitric acid in mixed liquor A
The molar ratio of a concentration of 1.2~1.5mol/L of iron, ferric nitrate and strontium nitrate is 12：(1.5~2)；
1.2 compound concentrations are the strong base solution of 4.6~6mol/L；
1.3 strong base solutions for obtaining the mixed liquor A that step 1.1 obtains and step 1.2 mix, and obtain mixed liquid B, wherein mixed
The volume ratio for closing liquid A and strong base solution is 3：4；
1.4 are transferred to the mixed liquid B that step 1.3 obtains in reaction kettle, 1~4h of hydro-thermal reaction at a temperature of 215~220 DEG C,
After reaction, it detaches, it is dry, obtain hexagonal platelet powder；
The preparation of step 2, raw material powder：
With Fe2O3、SrCO3For raw material, according to molar ratio Fe2O3：SrCO3=(5~7)：1 ratio dispensing, wet ball grinding 4~
6h is dried, sieving, and the powder after sieving keeps the temperature 2~4h in Muffle furnace at 600~800 DEG C, with stove cooled to room temperature
Afterwards, raw material powder is obtained；
The preparation of step 3, ferrite substrate：
3.1 mix the hexagonal platelet powder that step 1 obtains and raw material powder that step 2 obtains, obtain mixed powder；Wherein,
The mass percent of hexagonal platelet powder is 15wt%~30wt%, the mass percent of raw material powder be 70wt%~
85wt%；
3.2 in the mixed powder that step 3.1 obtains be added be equivalent to mixed powder 40wt%~60wt% organic solvent,
The organic binder of 25wt%~35wt% and the dispersant of 2wt%~4wt%, 14~16h of ball milling, obtained slurry is through stream
Prolong, lamination, hot pressing, obtain ceramic chips；
3.3 are placed in the ceramic chips that step 3.2 obtains in Muffle furnace, and 10~20h is kept the temperature at a temperature of 1175 DEG C~1185 DEG C, with
After stove cooled to room temperature, take out, you can obtain the ferrite substrate material.
2. the preparation method of the texturing M-type strontium ferrite substrate material of high-orientation according to claim 1, feature
It is, highly basic described in step 1.2 is sodium hydroxide or potassium hydroxide.
3. the preparation method of the texturing M-type strontium ferrite substrate material of high-orientation according to claim 1, feature
It is, organic solvent described in step 3.2 is dimethylbenzene, n-butanol, propyl acetate or isobutanol；The organic binder is poly-
B-76, vinyl in vinyl butyral system or acrylic resin；The dispersant is X-100, S-80 or fish oil.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810256251.4A CN108383515B (en) | 2018-03-27 | 2018-03-27 | Preparation method of textured M-type strontium ferrite substrate material with high orientation degree |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810256251.4A CN108383515B (en) | 2018-03-27 | 2018-03-27 | Preparation method of textured M-type strontium ferrite substrate material with high orientation degree |
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| CN108383515A true CN108383515A (en) | 2018-08-10 |
| CN108383515B CN108383515B (en) | 2021-02-05 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02133324A (en) * | 1988-11-11 | 1990-05-22 | Toda Kogyo Corp | Production of sr ferrite particles |
| CN101973764A (en) * | 2010-10-15 | 2011-02-16 | 同济大学 | Textured calcium bismuth niobate ceramic material and preparation method thereof |
| CN106745296A (en) * | 2016-11-15 | 2017-05-31 | 彭晓领 | A kind of preparation method of highly oriented strontium ferrite |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02133324A (en) * | 1988-11-11 | 1990-05-22 | Toda Kogyo Corp | Production of sr ferrite particles |
| CN101973764A (en) * | 2010-10-15 | 2011-02-16 | 同济大学 | Textured calcium bismuth niobate ceramic material and preparation method thereof |
| CN106745296A (en) * | 2016-11-15 | 2017-05-31 | 彭晓领 | A kind of preparation method of highly oriented strontium ferrite |
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