CN108383515B - Preparation method of textured M-type strontium ferrite substrate material with high orientation degree - Google Patents
Preparation method of textured M-type strontium ferrite substrate material with high orientation degree Download PDFInfo
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Abstract
The invention provides a preparation method of a textured M-type strontium ferrite substrate material with high orientation degree, belonging to the technical field of magnetic material preparation. Firstly, raw material powder calcined at low temperature is used as a basic raw material, and a flaky crystal with the same components obtained by hydrothermal reaction is used as a template for inducing crystal texture growth; then, introducing a tape casting lamination process to ensure that the microcrystalline thin slices are uniformly distributed in the green ceramic chip in parallel with the surface; and finally, the single-phase directional growth of the M-type hexagonal ferrite is further ensured by controlling the calcination temperature and the heat preservation time. According to the invention, the textured M-type strontium ferrite substrate material is obtained through the synergistic effect of the three aspects, and the orientation degree of the substrate material in the (00 l) direction can reach 96% according to the calculation of X-ray diffraction intensity.
Description
Technical Field
The invention belongs to the technical field of magnetic material preparation, and particularly relates to a preparation method of a textured M-type strontium ferrite substrate material with high orientation degree.
Background
M type strontium ferrite (SrFe)12O19) The magnetic material has the advantages of higher saturation magnetization, high magnetocrystalline anisotropy field, higher coercive force, good chemical stability and the like, and is widely applied to the aspects of miniaturized microwave devices, magneto-optical, high-density magnetic recording media and the like. At present, the preparation method of the M-type strontium ferrite powder mainly comprises the following steps: solid phase reaction methods and wet chemical methods (e.g., coprecipitation methods, sol-gel methods, hydrothermal methods, etc.). Among them, the hydrothermal method has obvious advantages in controlling the product morphology, improving the anisotropic growth and the crystal dispersion, and compared with the solid phase reaction method, the hydrothermal method can be used for controlling the product morphology, improving the anisotropic growth and the crystal dispersion without high-temperature calcinationObtaining M-phase powder. Because the strontium ferrite has a large magnetocrystalline anisotropy field, dry or wet magnetic field forming is usually adopted, and magnetic field regulation and control are utilized to induce orientation so as to obtain an anisotropic magnet. However, the complicated magnetic field forming process and parameter control are difficult to adapt to the application requirements of microwave devices and circuit integration technologies.
The invention discloses a method for preparing a textured single-phase hexagonal ferrite, which is characterized in that a coprecipitation precursor is loaded into a high-strength graphite grinding tool and placed in a discharge plasma sintering system, the coprecipitation precursor is subjected to vacuum dense forming at the pressure of 5-20 MPa in a vacuumizing mode, and discharge plasma sintering is carried out at the temperature rise rate of 100-300 ℃/min, the sintering temperature of 850-1000 ℃, the pressure of 5-20 MPa and the time of 10-40 min to obtain the textured hexagonal ferrite, but the method has a complex process and the orientation degree of the obtained ferrite is not high. The Chinese patent with the application number of 201611001717.3 and the invention name of 'a preparation method of high-orientation strontium ferrite' discloses a preparation method of high-orientation strontium ferrite, which firstly uses SrCl2·6H2O，FeCl3·6H2Taking O and NaOH as raw materials, obtaining hexagonal sheet strontium ferrite particles by a hydrothermal method, uniformly mixing the obtained strontium ferrite particles with epoxy resin, and then forming in a magnetic field to generate an oriented structure; however, in the method, the hexagonal flaky strontium ferrite particles contain Fe2O3、SrCO3The orientation degree of the product is influenced by the impurities, magnetic anisotropy is still obtained by adopting magnetic field forming, and the complex magnetic field forming process and parameter control are difficult to adapt to the application requirements of microwave devices and circuit integration technologies.
Disclosure of Invention
The invention aims to provide a preparation method of a textured M-type strontium ferrite substrate material with high orientation degree.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of a textured M-type strontium ferrite substrate material with high orientation degree specifically comprises the following steps:
step 1, preparing hexagonal platelet powder:
1.1 adding ferric nitrate and strontium nitrate into deionized water, and uniformly mixing to obtain a mixed solution A; wherein the concentration of ferric nitrate in the mixed solution A is 1.2-1.5 mol/L, and the molar ratio of ferric nitrate to strontium nitrate is 12: (1.5-2);
1.2 preparing a strong base solution with the concentration of 4.6-6 mol/L;
1.3 mixing the mixed solution A obtained in the step 1.1 with the strong base solution obtained in the step 1.2 to obtain a mixed solution B, wherein the volume ratio of the mixed solution A to the strong base solution is 3: 4;
1.4 transferring the mixed solution B obtained in the step 1.3 into a reaction kettle, carrying out hydrothermal reaction for 1-4 h at the temperature of 215-220 ℃, separating and drying after the reaction is finished, so as to obtain hexagonal platelet powder;
step 2, preparation of raw material powder:
with Fe2O3、SrCO3As raw material, according to the mol ratio of Fe2O3：SrCO3(5-7): 1, ball-milling for 4-6 h by a wet method, drying, sieving, preserving the heat of the sieved powder in a muffle furnace at 600-800 ℃ for 2-4 h, and naturally cooling to room temperature along with the furnace to obtain raw powder;
step 3, preparation of the ferrite substrate:
3.1 mixing the hexagonal platelet powder obtained in the step 1 with the raw material powder obtained in the step 2 to obtain mixed powder; wherein, the mass percent of the hexagonal platelet powder is 15 wt% -30 wt%, and the mass percent of the raw material powder is 70 wt% -85 wt%;
3.2 adding an organic solvent which is equivalent to 40-60 wt% of the mixed powder, an organic binder which is equivalent to 25-35 wt% of the mixed powder and a dispersing agent which is equivalent to 2-4 wt% of the mixed powder into the mixed powder obtained in the step 3.1, ball-milling for 14-16 h, and carrying out tape casting, laminating and hot pressing on the obtained slurry to obtain a green ceramic chip;
3.3, placing the green ceramic chip obtained in the step 3.2 in a muffle furnace, preserving the heat for 10-20 h at the temperature of 1175-1185 ℃, naturally cooling to room temperature along with the furnace, and taking out to obtain the ferrite substrate material.
Further, in step 1.2, the strong base is sodium hydroxide, potassium hydroxide and the like.
Further, in step 3.2, the organic solvent is xylene, n-butanol, propyl acetate or isobutanol, etc.; the organic binder is B-76 in polyvinyl butyral, vinyl resin, acrylic resin or the like; the dispersant is X-100, S-80 or fish oil, etc.
The invention has the beneficial effects that:
the invention provides a preparation method of a textured M-type strontium ferrite substrate material with high orientation degree, which comprises the following steps of firstly, adopting raw material powder calcined at low temperature as a basic raw material, and taking a plate crystal with the same components obtained by hydrothermal reaction as a template for inducing crystal textured growth; then, introducing a tape casting lamination process to ensure that the microcrystalline thin slices are uniformly distributed in the green ceramic chip in parallel with the surface; and finally, the single-phase directional growth of the M-type hexagonal ferrite is further ensured by controlling the calcination temperature and the heat preservation time. According to the invention, the textured M-type strontium ferrite substrate material is obtained through the synergistic effect of the three aspects, and the orientation degree of the substrate material in the (00 l) direction can reach 96% according to the calculation of X-ray diffraction intensity.
Drawings
FIG. 1 is an XRD pattern of hexagonal platelet powder obtained in step 1 of example 3;
FIG. 2 is an XRD spectrum of the substrate materials obtained in comparative example 5(a) and example 3 (b);
FIG. 3 is a VSM hysteresis loop curve of the substrate material obtained in example 3 under the action of external magnetic fields perpendicular and parallel to the substrate surface.
Detailed Description
The technical scheme of the invention is detailed below by combining the accompanying drawings and the embodiment.
A preparation method of a textured M-type strontium ferrite substrate material with high orientation degree specifically comprises the following steps:
step 1, preparing hexagonal platelet powder:
1.1 adding ferric nitrate and strontium nitrate into deionized water, and uniformly mixing to obtain a mixed solution A; wherein the concentration of ferric nitrate in the mixed solution A is 1.2-1.5 mol/L, and the molar ratio of ferric nitrate to strontium nitrate is 12: (1.5-2);
1.2 preparing a strong base solution with the concentration of 4.6-6 mol/L;
1.3 mixing the mixed solution A obtained in the step 1.1 with the strong base solution obtained in the step 1.2 to obtain a mixed solution B, wherein the volume ratio of the mixed solution A to the strong base solution is 3: 4;
1.4 transferring the mixed solution B obtained in the step 1.3 into a reaction kettle, sealing, and then filling nitrogen gas to ensure that the initial air pressure in the reaction kettle is 1-2 MPa, operating the reaction kettle, carrying out hydrothermal reaction for 1-4 h under the conditions that the stirring speed is less than 120r/min and the temperature is 215-220 ℃, after the reaction is finished, carrying out suction filtration and washing on the reacted mixed solution, and drying for 2h at 80 ℃ in an oven to obtain hexagonal platelet powder;
step 2, preparation of raw material powder:
with Fe2O3、SrCO3As raw material, according to the mol ratio of Fe2O3：SrCO3(5-7): 1, performing wet ball milling for 4-6 hours, drying at 90-100 ℃, sieving, putting the sieved powder into a corundum crucible, keeping the temperature of the corundum crucible in a muffle furnace at 600-800 ℃ for 2-4 hours, and naturally cooling to room temperature along with the furnace to obtain raw material powder;
step 3, preparation of the ferrite substrate:
3.1 mixing the hexagonal platelet powder obtained in the step 1 with the raw material powder obtained in the step 2 to obtain mixed powder; wherein, the mass percent of the hexagonal platelet powder is 15 wt% -30 wt%, and the mass percent of the raw material powder is 70 wt% -85 wt%;
3.2 adding an organic solvent which is equivalent to 40-60 wt% of the mixed powder, an organic binder which is equivalent to 25-35 wt% of the mixed powder and a dispersing agent which is equivalent to 2-4 wt% of the mixed powder into the mixed powder obtained in the step 3.1, ball-milling for 14-16 h, and carrying out tape casting, laminating and hot pressing on the obtained slurry to obtain a green ceramic chip;
3.3, placing the green ceramic chip obtained in the step 3.2 in a muffle furnace, preserving heat for 10-20 h at the temperature of 1175-1185 ℃, cooling to room temperature along with the furnace, and taking out to obtain the ferrite substrate material.
Further, in step 1.2, the strong base is sodium hydroxide, potassium hydroxide and the like.
Furthermore, the diameter of the hexagonal platelet powder obtained in the step 1 is 1 μm, and the thickness is less than 100 nm.
Further, in step 3.2, the organic solvent is xylene, n-butanol, propyl acetate or isobutanol, etc.; the organic binder is B-76 in polyvinyl butyral, vinyl resin, acrylic resin or the like; the dispersant is X-100, S-80 or fish oil, etc.
Examples
A preparation method of a textured M-type strontium ferrite substrate material with high orientation degree specifically comprises the following steps:
step 1, preparing hexagonal platelet powder:
1.1 82.0304g of iron nitrate (Fe (NO)3)3·9H2O), 5.3173g strontium nitrate (Sr (NO)3)2) Adding the mixture into 150mL of deionized water, and stirring and mixing the mixture uniformly to obtain a mixed solution A;
1.2 weighing 42.4489g of NaOH, adding into 200mL of deionized water, and stirring for dissolving to obtain a strong alkali solution;
1.3, mixing the mixed solution A obtained in the step 1.1 with the strong base solution obtained in the step 1.2, and stirring to obtain a mixed solution B;
1.4 transferring the mixed solution B obtained in the step 1.3 into a reaction kettle, sealing, and filling nitrogen gas to ensure that the initial air pressure in the reaction kettle is 1.5MPa, operating the reaction kettle, carrying out hydrothermal reaction for 2 hours under the conditions of a stirring speed of 100r/min and a temperature of 220 ℃, filtering and washing the reacted mixed solution after the reaction is finished, and drying the obtained product in an oven at 80 ℃ for 2 hours to obtain hexagonal platelet powder;
step 2, preparation of raw material powder:
with Fe2O3、SrCO360.655g of Fe are weighed as raw materials2O3And 9.345g SrCO3Wet ball milling for 6h at 1Drying and sieving at 00 ℃, putting the sieved powder into a corundum crucible, preserving the heat for 4 hours at 600 ℃ in a muffle furnace, and naturally cooling to room temperature along with the furnace to obtain raw material powder;
step 3, preparation of the ferrite substrate:
3.1 mixing the hexagonal platelet powder obtained in the step 1 with the raw material powder obtained in the step 2 to obtain mixed powder; wherein, the mass percentage of the hexagonal platelet powder is 15 wt% -30 wt% (the mass percentage of the hexagonal platelet powder is shown in table 1), and the mass percentage of the raw material powder is 70 wt% -85 wt%;
3.2 adding xylene which is equivalent to 40 weight percent of the mixed powder, B-76 in a polyvinyl butyral system which is equivalent to 30 weight percent of the mixed powder and a dispersing agent X-100 which is equivalent to 3 weight percent of the mixed powder into the mixed powder obtained in the step 3.1, carrying out ball milling for 16 hours, casting a film belt with the thickness of about 30 mu m from the obtained slurry, laminating, and carrying out hot pressing at 80 ℃ and 10Mpa for 20 minutes to obtain a green ceramic chip;
3.3, placing the green ceramic chip obtained in the step 3.2 in a muffle furnace, preserving heat for 10-20 h at the temperature of 1175-1185 ℃ (the calcining temperature and the heat preservation time are shown in the table 1), cooling to room temperature along with the furnace, and taking out to obtain the ferrite substrate material (the performance index is shown in the table 2).
Comparative example
A preparation method of a textured M-type strontium ferrite substrate material with high orientation degree specifically comprises the following steps:
step 1, preparing hexagonal platelet powder:
1.1 82.0304g of iron nitrate (Fe (NO)3)3·9H2O), 5.3173g strontium nitrate (Sr (NO)3)2) Adding the mixture into 150mL of deionized water, and stirring and mixing the mixture uniformly to obtain a mixed solution A;
1.2 weighing 42.4489g of NaOH, adding into 200mL of deionized water, and stirring for dissolving to obtain a strong alkali solution;
1.3, mixing the mixed solution A obtained in the step 1.1 with the strong base solution obtained in the step 1.2, and stirring to obtain a mixed solution B;
1.4 transferring the mixed solution B obtained in the step 1.3 into a reaction kettle, sealing, and filling nitrogen gas to ensure that the initial air pressure in the reaction kettle is 1.5MPa, operating the reaction kettle, carrying out hydrothermal reaction for 2 hours under the conditions of a stirring speed of 100r/min and a temperature of 220 ℃, filtering and washing the reacted mixed solution after the reaction is finished, and drying the obtained product in an oven at 80 ℃ for 2 hours to obtain hexagonal platelet powder;
step 2, preparation of raw material powder:
with Fe2O3、SrCO360.655g of Fe are weighed as raw materials2O3And 9.345g SrCO3Wet ball milling for 6 hr, stoving at 100 deg.c, sieving, setting the sieved powder inside corundum crucible and inside muffle furnace at 600 deg.c for 4 hr, and cooling naturally to room temperature to obtain raw material powder;
step 3, preparation of the ferrite substrate:
3.1 mixing the hexagonal platelet powder obtained in the step 1 with the raw material powder obtained in the step 2 to obtain mixed powder; wherein, the mass percentage of the hexagonal platelet powder is 15 wt% -30 wt% (the mass percentage of the hexagonal platelet powder is shown in table 1), and the mass percentage of the raw material powder is 70 wt% -85 wt%;
3.2 adding xylene which is equivalent to 40 weight percent of the mixed powder, B-76 in a polyvinyl butyral system which is equivalent to 30 weight percent of the mixed powder and a dispersing agent X-100 which is equivalent to 3 weight percent of the mixed powder into the mixed powder obtained in the step 3.1, carrying out ball milling for 16 hours, casting a film belt with the thickness of about 30 mu m from the obtained slurry, laminating, and carrying out hot pressing at 80 ℃ and 10Mpa for 20 minutes to obtain a green ceramic chip;
3.3 placing the green ceramic chip obtained in the step 3.2 in a muffle furnace, preserving the heat for a certain time at a set temperature (the calcining temperature and the heat preservation time are shown in the table 1, wherein the step 1 is not included in the comparative example 5), cooling the green ceramic chip to room temperature along with the furnace, and taking out the green ceramic chip to obtain the ferrite substrate material (the performance index is shown in the table 2).
TABLE 1 Process conditions for the examples and comparative examples
| Item | Calcination temperature Ts (. degree. C.) | Holding time t (h) | Hexagonal platelet powder mass percent (wt%) |
| Example 1 | 1180 | 10 | 15 |
| Example 2 | 1180 | 20 | 15 |
| Example 3 | 1185 | 10 | 30 |
| Example 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, t is holding time
TABLE 2 evaluation of the properties of the examples and comparative examples
Table 2 shows the results of evaluation of the degree of orientation and magnetic properties of the substrate materials obtained in examples and comparative examples, in which "#" is a mark that does not meet the index requirements. As can be seen from Table 2, the substrate material obtained by the method has a textured structure with high orientation degree, and not only can meet the requirements of microwave magnetic devices on high-performance substrate materials, but also has a huge development prospect in the fields of information storage and sensors due to the potential magnetoelectric effect.
FIG. 1 is an XRD pattern of hexagonal platelet powder obtained in step 1 of example 3; as can be seen from fig. 1, the hexagonal platelet powder obtained was a single M phase, and no diffraction peak of other impurity phases was observed. FIG. 2 is an XRD spectrum of the substrate materials obtained in comparative example 5(a) and example 3 (b); as can be seen from FIG. 2, after the self-template induced growth method of the present invention is adopted, the diffraction peak intensity of the obtained substrate material in the (00 l) direction is greatly enhanced, and the diffraction peaks of other crystal faces are greatly weakened, which indicates that the textured substrate material prepared by the method of the present invention has a high degree of orientation. FIG. 3 is a VSM hysteresis loop curve of the substrate material obtained in example 3 under the action of external magnetic fields perpendicular and parallel to the substrate surface; as can be seen from fig. 3, the substrate material obtained in example 3 has significantly different degrees of magnetization under magnetic fields in different directions, and when the magnetic field is perpendicular to the substrate surface, the material is quickly magnetized to a saturated state, indicating that the direction is an easy magnetization direction; and when the magnetic field is parallel to the substrate surface, it still cannot be magnetized to saturation at 15000Oe, and the direction shows hard magnetization characteristic.
Claims (3)
1. A preparation method of a textured M-type strontium ferrite substrate material with high orientation degree comprises the following steps:
step 1, preparing hexagonal platelet powder:
1.1 adding ferric nitrate and strontium nitrate into deionized water, and uniformly mixing to obtain a mixed solution A; wherein the concentration of ferric nitrate in the mixed solution A is 1.2-1.5 mol/L, and the molar ratio of ferric nitrate to strontium nitrate is 12: (1.5-2);
1.2 preparing a strong base solution with the concentration of 4.6-6 mol/L;
1.3 mixing the mixed solution A obtained in the step 1.1 with the strong base solution obtained in the step 1.2 to obtain a mixed solution B, wherein the volume ratio of the mixed solution A to the strong base solution is 3: 4;
1.4 transferring the mixed solution B obtained in the step 1.3 into a reaction kettle, sealing, filling nitrogen gas to ensure that the initial air pressure in the reaction kettle is 1-2 MPa, operating the reaction kettle, carrying out hydrothermal reaction for 1-4 h under the conditions that the stirring speed is less than 120r/min and the temperature is 215-220 ℃, and after the reaction is finished, separating and drying to obtain hexagonal platelet powder;
step 2, preparation of raw material powder:
with Fe2O3、SrCO3As raw material, according to the mol ratio of Fe2O3：SrCO3(5-7): 1, ball-milling for 4-6 h by a wet method, drying, sieving, and keeping the sieved powder at 600-800 ℃ in a muffle furnace to be 2-to-eNaturally cooling to room temperature along with the furnace for 4h to obtain raw material powder;
step 3, preparation of the ferrite substrate:
3.1 mixing the hexagonal platelet powder obtained in the step 1 with the raw material powder obtained in the step 2 to obtain mixed powder; wherein, the mass percent of the hexagonal platelet powder is 15 wt% -30 wt%, and the mass percent of the raw material powder is 70 wt% -85 wt%;
3.2 adding 40-60 wt% of organic solvent, 25-35 wt% of organic binder and 2-4 wt% of dispersant into the mixed powder obtained in the step 3.1, ball milling for 14-16 h, casting and laminating the obtained slurry, and hot pressing at 80 ℃ and 10Mpa to obtain a green ceramic chip;
3.3, placing the green ceramic chip obtained in the step 3.2 in a muffle furnace, preserving the heat for 10-20 h at the temperature of 1175-1185 ℃, naturally cooling to room temperature along with the furnace, and taking out to obtain the ferrite substrate material.
2. The method for preparing a textured M-type strontium ferrite substrate material with high degree of orientation according to claim 1, wherein the strong base in step 1.2 is sodium hydroxide or potassium hydroxide.
3. The method for preparing a textured M-type strontium ferrite substrate material with high degree of orientation according to claim 1, wherein the organic solvent in step 3.2 is xylene, n-butanol, propyl acetate or isobutanol; the organic binder is B-76 in polyvinyl butyral, vinyl resin or acrylic resin; the dispersant is X-100, S-80 or fish oil.
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|---|---|---|---|---|
| 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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2018
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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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