CN112341180A - Preparation method of ferrite material for mobile OLED display power supply - Google Patents
Preparation method of ferrite material for mobile OLED display power supply Download PDFInfo
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- CN112341180A CN112341180A CN202011278617.1A CN202011278617A CN112341180A CN 112341180 A CN112341180 A CN 112341180A CN 202011278617 A CN202011278617 A CN 202011278617A CN 112341180 A CN112341180 A CN 112341180A
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- 239000000463 material Substances 0.000 title claims abstract description 112
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 238000000227 grinding Methods 0.000 claims abstract description 44
- 239000000654 additive Substances 0.000 claims abstract description 41
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000007689 inspection Methods 0.000 claims abstract description 19
- 238000002156 mixing Methods 0.000 claims abstract description 19
- 238000005245 sintering Methods 0.000 claims abstract description 19
- 238000012545 processing Methods 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 14
- 238000005469 granulation Methods 0.000 claims abstract description 14
- 230000003179 granulation Effects 0.000 claims abstract description 14
- 239000007921 spray Substances 0.000 claims abstract description 14
- 238000004806 packaging method and process Methods 0.000 claims abstract description 7
- 238000005453 pelletization Methods 0.000 claims abstract description 7
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 48
- 230000000996 additive effect Effects 0.000 claims description 34
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 33
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 24
- UPWOEMHINGJHOB-UHFFFAOYSA-N oxo(oxocobaltiooxy)cobalt Chemical compound O=[Co]O[Co]=O UPWOEMHINGJHOB-UHFFFAOYSA-N 0.000 claims description 24
- 239000011787 zinc oxide Substances 0.000 claims description 24
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 20
- 238000001816 cooling Methods 0.000 claims description 19
- 238000005070 sampling Methods 0.000 claims description 18
- 239000002002 slurry Substances 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 18
- 239000004576 sand Substances 0.000 claims description 17
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 16
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 14
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 13
- GEYXPJBPASPPLI-UHFFFAOYSA-N manganese(III) oxide Inorganic materials O=[Mn]O[Mn]=O GEYXPJBPASPPLI-UHFFFAOYSA-N 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 13
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 12
- 239000008187 granular material Substances 0.000 claims description 12
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical group O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims description 12
- 229910052681 coesite Inorganic materials 0.000 claims description 11
- 229910052906 cristobalite Inorganic materials 0.000 claims description 11
- 239000000377 silicon dioxide Substances 0.000 claims description 11
- 229910052682 stishovite Inorganic materials 0.000 claims description 11
- 229910052905 tridymite Inorganic materials 0.000 claims description 11
- 238000003801 milling Methods 0.000 claims description 10
- 238000004321 preservation Methods 0.000 claims description 10
- 230000004907 flux Effects 0.000 claims description 7
- 238000005520 cutting process Methods 0.000 claims description 6
- 238000011049 filling Methods 0.000 claims description 6
- 230000005389 magnetism Effects 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 238000003825 pressing Methods 0.000 claims description 6
- 238000004537 pulping Methods 0.000 claims description 6
- 238000012360 testing method Methods 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- GNRSAWUEBMWBQH-UHFFFAOYSA-N nickel(II) oxide Inorganic materials [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims description 5
- 230000000630 rising effect Effects 0.000 claims description 5
- 238000002425 crystallisation Methods 0.000 abstract description 8
- 230000008025 crystallization Effects 0.000 abstract description 8
- 239000013078 crystal Substances 0.000 abstract description 5
- 238000010438 heat treatment Methods 0.000 abstract description 2
- 238000000748 compression moulding Methods 0.000 abstract 1
- -1 sanding Substances 0.000 abstract 1
- 239000008188 pellet Substances 0.000 description 15
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 5
- YOBAEOGBNPPUQV-UHFFFAOYSA-N iron;trihydrate Chemical compound O.O.O.[Fe].[Fe] YOBAEOGBNPPUQV-UHFFFAOYSA-N 0.000 description 5
- PPNAOCWZXJOHFK-UHFFFAOYSA-N manganese(2+);oxygen(2-) Chemical compound [O-2].[Mn+2] PPNAOCWZXJOHFK-UHFFFAOYSA-N 0.000 description 5
- VASIZKWUTCETSD-UHFFFAOYSA-N manganese(II) oxide Inorganic materials [Mn]=O VASIZKWUTCETSD-UHFFFAOYSA-N 0.000 description 5
- 229910010413 TiO 2 Inorganic materials 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000004973 liquid crystal related substance Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
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- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
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Abstract
The invention discloses a preparation method of a ferrite material for a mobile OLED display power supply, which belongs to the technical field of material preparation and comprises the steps of mixing materials, pelletizing, presintering, vibromilling, slurrying, adding additives, sanding, spray granulation, compression molding, sintering, grinding processing, inspection and packaging. According to the invention, the highest sintering temperature and the stable temperature rise rate are reduced, so that the crystallization stability of sintering can be effectively improved, fine and uniform crystal grains are obtained, the quality of the magnetic core is improved, the condition of unstable crystallization caused by the influence of water vapor during preheating and heating can be prevented through drying treatment of the ball material, and the crystallization stability is further improved by matching with secondary stable temperature reduction after sintering.
Description
Technical Field
The invention relates to the technical field of material preparation, in particular to a preparation method of a ferrite material for a mobile OLED display power supply.
Background
In recent years, the development of OLEDs in the display area can be said to be wind-driven and water-borne. The OLED has the advantages of self-luminescence, no need of a backlight plate, high contrast, uniform image quality, wide viewing angle, small injury to human eyes, high response speed, thin body, flexibility and folding, capability of even generating sound through screen vibration without depending on a sound generating unit and the like, is very suitable for being applied to small and medium-sized display panels, and is widely accepted in the fields of mobile phones, wearable products, VR (Virtual reality) and the like at present. As OLED technology matures, its market share will rise, and the potential of the technology for applications in cell phones, digital cameras, and pocket computer screens is great, and there is a possibility of replacing LCD in the future. Many believe that there is a necessary connection between an OLED and an LED, but not. Although the LED and the OLED only differ by one letter, the imaging technologies of the LED and the OLED are completely different. LCDs (Liquid Crystal display) can be classified into CCFLs and LEDs according to the backlight source. OLED (Organic Light-EmitTIng Diode) is literally understood as "Organic Light-EmitTIng Diode", and the largest difference from LCD is that it has self-luminous property, and the element of Organic Light-EmitTIng semiconductor can emit Light by itself without the support of backlight. The OLED is a current-driven type device, unlike the LCD liquid crystal display. The OLED display driving assembly has also become more advanced, and the OLED bias power supply circuit has started to be miniaturized and specialized.
For power supply assembly technology, the main challenge is how to provide a solution with high efficiency and minimal volume at the same time. The magnetic core in the OLED bias power supply circuit is also required to be efficient and miniaturized, the sintering crystallization stability of the existing preparation method of the magnetic core is not high, the preparation efficiency and the quality of crystal grains are low, and the higher and higher performance requirements of the magnetic core cannot be met.
Disclosure of Invention
The invention aims to provide a preparation method of a ferrite material for a mobile OLED display power supply, which aims to solve the problems that the sintering crystallization stability is low, the preparation efficiency and the crystal grain quality are low, and the higher and higher performance requirements of a magnetic core cannot be met in the existing preparation method of the magnetic core of an OLED bias power supply circuit.
In order to solve the technical problems, the invention provides the following technical scheme: the preparation method of the ferrite material for the mobile OLED display power supply comprises the following steps of iron sesquioxide, manganous manganic oxide, zinc oxide and an additive:
s1, mixing materials:
weighing corresponding mass of ferric oxide, manganic oxide and zinc oxide respectively by using a high-precision electronic scale in proportion, mixing for 10-15 minutes by using a cone mixer, and uniformly mixing and grinding in a pass-through vibrating mill;
s2, pelletizing:
putting the vibro-milled material into a pelletizer, adding 5-15 wt% of pure water, making into pellets, and drying with a dryer to prevent internal moisture;
s3, pre-burning:
after the ball material is dried, the temperature is raised to 930-;
s4, vibromilling:
after the pre-sintered ball material is cooled, the pre-sintered ball material is subjected to vibration grinding again through a vibration grinding machine to form powdery vibration grinding materials;
s5, pulping:
injecting pure water into the slurry pool, adding a vibration grinding material, and stirring by using stirring equipment;
s6, adding an additive:
adding Nb in turn while stirring2O5、CaCO3、Co2O3、SnO2、SiO 20, NiO, ZrO2, TiO2 and other additives;
s7, sanding:
after the additive is added into the slurry, putting the slurry into a sand mill for sand milling;
s8, spray granulation;
adding 0.5-1.2% PVA into the ground material, and preparing into 0.05-0.5mm granules by adopting a spray granulation drying tower;
s9, profiling:
pressing the granular materials into required product blanks by using a powder press, and controlling the density of the blanks to be 3.0-3.1g/cm 3;
s10, sintering:
and (3) increasing the temperature of the pressed blank to 1280-1350 ℃ at the temperature rising speed of 60-80 ℃/min by using a bell jar furnace, and continuously preserving the heat for 180-270 minutes. After the heat preservation is finished, filling a proper amount of nitrogen into the furnace body, cooling to 150 ℃, opening the furnace, and then transferring to a cooling chamber for natural cooling to normal temperature;
s11, grinding:
after the sintered blank is cooled, processing the blank into a magnetic core with a specific size or shape by using a cutting machine or a grinding machine;
s12, checking:
after the processing is finished, performing sampling inspection according to a sampling inspection rate of five percent, firstly detecting the saturation magnetic flux density, the residual magnetism and the coercive force of the magnetic core by adopting a SY-8219 instrument, then testing the magnetic conductivity of the magnetic core by adopting a 4284A type LCR instrument, finally detecting the power consumption of the magnetic core by adopting a CH2335 power consumption instrument, and after the sampling inspection is finished, packaging according to specifications.
Preferably, the material formula comprises the following components in the ratio of the mass of Fe2O 3: 51-56 mol%, Mn3O 4: 38-42 mol%, ZnO: 6-10mol percent.
Preferably, the formula of the additive is Nb2O5：200-300ppm、CaCO3：200-500ppm、Co2O3：3000-5000ppm、SnO2：0-500ppm、SiO2：0-200ppm、NiO：0-10000ppm、ZrO2：0-200ppm、TiO2：0-3000ppm。
Preferably, the purity grade of the additive is electronic purity.
Preferably, the purity of the ferric oxide is more than or equal to 99 percent, the purity of the manganic manganous oxide is more than or equal to 98.5 percent, and the purity of the zinc oxide is more than or equal to 99.7 percent.
Preferably, in the second step, the pellet material of the pelletizer is prepared into a pellet material with the standard diameter of 2-10 mm.
Preferably, in the third step, the temperature rise speed of the rotary kiln is 120 ℃/min at 100-.
Preferably, in the fourth step, the material is vibrated and ground by a through type vibration grinding machine until the average particle diameter is 1.8-2.5 microns.
Preferably, in the fifth step, the ratio of the vibration grinding material to the pure water is 1: 0.4-0.55.
Preferably, in the seventh step, the average grain size standard of the sand grinding is 0.8-1.1 microns, so that the effect of spray granulation is improved.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention can effectively improve the crystallization stability of sintering by reducing the highest sintering temperature and stabilizing the temperature rise rate so as to obtain fine and uniform crystal grains and improve the quality of the magnetic core.
2. According to the invention, through drying treatment of the ball material, unstable crystallization caused by the influence of water vapor during preheating and heating can be prevented, and crystallization stability is further improved by matching with secondary stable cooling after sintering, so that the practicability of the invention is enhanced.
3. The invention effectively improves the preparation efficiency and the crystal grain quality, reduces the reconstruction cost and improves the practicability under the condition of not changing the production line in a large range.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
FIG. 1 is a characteristic diagram of initial permeability of ferrite material for mobile OLED display power supply according to the present invention;
FIG. 2 is a characteristic diagram of saturation magnetic flux density of ferrite material for mobile OLED display power supply according to the present invention;
FIG. 3 is a power loss characteristic diagram of the ferrite material for mobile OLED display power supply according to the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The first embodiment is as follows:
referring to fig. 1-3, the present invention provides the following technical solutions: the preparation method of the ferrite material for the mobile OLED display power supply comprises the following steps of iron sesquioxide, manganous manganic oxide, zinc oxide and an additive:
s1, mixing materials:
weighing corresponding mass of ferric oxide, manganic oxide and zinc oxide respectively by using a high-precision electronic scale in proportion, mixing for 10 minutes by using a cone mixer, and uniformly mixing and grinding in a pass-through vibrating mill;
s2, pelletizing:
putting the vibro-milled material into a pelletizer, adding 5 wt% of pure water, making into pellets, making the pellets into pellets with the standard diameter of 2mm, and drying by using a dryer after making into pellets;
s3, pre-burning:
after the ball material is dried, the temperature is raised to 930 ℃ by using a rotary kiln, and is kept for a certain time, pre-sintering is carried out, wherein the temperature rise speed of the rotary kiln is 120 ℃/min, and the heat preservation time is 10 min;
s4, vibromilling:
after the pre-sintered ball material is cooled, the pre-sintered ball material is vibrated and ground again through a vibrating grinder until the average grain diameter is 1.8-2.5 microns, and a powdery vibrating grinding material is formed;
s5, pulping:
injecting pure water into the slurry pond, adding a vibration grinding material, and stirring by using stirring equipment, wherein the ratio of the vibration grinding material to the pure water is 1: 0.55;
s6, adding an additive:
adding Nb in turn while stirring2O5、CaCO3、Co2O3、SnO2、SiO 20, NiO, ZrO2, TiO2 and other additives;
s7, sanding:
after the additive is added into the slurry, putting the slurry into a sand mill for sand milling, wherein the average grain diameter standard of the sand milling is 1.1 micron;
s8, spray granulation;
adding 0.5% PVA into the ground material, and preparing into 0.05-0.5mm granules by adopting a spray granulation drying tower;
s9, profiling:
pressing the granular material into required product blank by using a powder press, and controlling the density of the blank to be 3.0-3.1g/cm3；
S10, sintering:
and (3) raising the temperature of the pressed blank to 1280 ℃ by using a bell jar furnace at the temperature rise speed of 80 ℃/min, and keeping the temperature for 180 minutes. After the heat preservation is finished, filling a proper amount of nitrogen into the furnace body, cooling to 150 ℃, opening the furnace, and then transferring to a cooling chamber for natural cooling to normal temperature;
s11, grinding:
after the sintered blank is cooled, processing the blank into a magnetic core with a specific size or shape by using a cutting machine or a grinding machine;
s12, checking:
after the processing is finished, performing sampling inspection according to a sampling inspection rate of five percent, firstly detecting the saturation magnetic flux density, the residual magnetism and the coercive force of the magnetic core by adopting a SY-8219 instrument, then testing the magnetic conductivity of the magnetic core by adopting a 4284A type LCR instrument, finally detecting the power consumption of the magnetic core by adopting a CH2335 power consumption instrument, and after the sampling inspection is finished, packaging according to specifications.
The material formula comprises the following components in percentage by mass: 53 mol%, Mn3O 4: 38 mol%, ZnO: 9mol percent of additive, and the formula of the additive is Nb2O5：200ppm、CaCO3：200ppm、Co2O3：5000ppm、SnO2：500ppm、SiO2: 200ppm, NiO: 10000ppm, ZrO 2: 200ppm, TiO 2: 3000ppm, the purity grade of the additive is electronic purity, the purity of ferric oxide is more than or equal to 99 percent, the purity of manganous oxide is more than or equal to 98.5 percent, the purity of zinc oxide is more than or equal to 99.7 percent, and the processing time is shortened under the condition of ensuring the basic performance.
Example two:
the difference between the present embodiment and the first embodiment is: the preparation method of the ferrite material for the mobile OLED display power supply comprises the following steps of iron sesquioxide, manganous manganic oxide, zinc oxide and an additive:
s1, mixing materials:
weighing corresponding mass of ferric oxide, manganic oxide and zinc oxide respectively by using a high-precision electronic scale in proportion, mixing for 15 minutes by using a cone mixer, and uniformly mixing and grinding in a pass-through vibrating mill;
s2, pelletizing:
putting the vibro-milled material into a pelletizer, adding 15 wt% of pure water, making into pellets, making the pellets into pellets with the standard diameter of 10mm, and drying by using a dryer after making into pellets;
s3, pre-burning:
after the ball material is dried, the temperature is raised to 1020 ℃ by using a rotary kiln, and is kept for a certain time, pre-sintering is carried out, wherein the temperature rise speed of the rotary kiln is 100 ℃/min, and the heat preservation time is 15 min;
s4, vibromilling:
after the pre-sintered ball material is cooled, the pre-sintered ball material is vibrated and ground again through a vibrating grinder until the average grain diameter is 1.8-2.5 microns, and a powdery vibrating grinding material is formed;
s5, pulping:
injecting pure water into the slurry pond, adding a vibration grinding material, and stirring by using stirring equipment, wherein the ratio of the vibration grinding material to the pure water is 1: 0.4;
s6, adding an additive:
adding Nb in turn while stirring2O5、CaCO3、Co2O3、SnO2、SiO 20, NiO, ZrO2, TiO2 and other additives;
s7, sanding:
after the additive is added into the slurry, putting the slurry into a sand mill for sand milling, wherein the average grain diameter standard of the sand milling is 0.8-1.1 micron;
s8, spray granulation;
adding the ground material into 1.2% PVA, and preparing into 0.05-0.5mm granules by adopting a spray granulation drying tower;
s9, profiling:
pressing the granular material into required product blank by using a powder press, and controlling the density of the blank to be 3.0-3.1g/cm3；
S10, sintering:
and (3) increasing the temperature of the pressed blank to 1350 ℃ at the temperature rising speed of 60 ℃/min by using a bell jar furnace, and keeping the temperature for 270 minutes. After the heat preservation is finished, filling a proper amount of nitrogen into the furnace body, cooling to 150 ℃, opening the furnace, and then transferring to a cooling chamber for natural cooling to normal temperature;
s11, grinding:
after the sintered blank is cooled, processing the blank into a magnetic core with a specific size or shape by using a cutting machine or a grinding machine;
s12, checking:
after the processing is finished, performing sampling inspection according to a sampling inspection rate of five percent, firstly detecting the saturation magnetic flux density, the residual magnetism and the coercive force of the magnetic core by adopting a SY-8219 instrument, then testing the magnetic conductivity of the magnetic core by adopting a 4284A type LCR instrument, finally detecting the power consumption of the magnetic core by adopting a CH2335 power consumption instrument, and after the sampling inspection is finished, packaging according to specifications.
The material formula comprises the following components in percentage by mass: 56 mol%, Mn3O 4: 38 mol%, ZnO: 6mol percent of additive, and the formula of the additive is Nb2O5：200ppm、CaCO3：200-ppm、Co2O3：3000ppm、SnO2：500ppm、SiO2: 200ppm, NiO: 10000ppm, ZrO 2: 200ppm, TiO 2: 3000ppm, the purity grade of the additive is electronic purity, the purity of ferric oxide is more than or equal to 99 percent, the purity of manganous oxide is more than or equal to 98.5 percent, and the purity of zinc oxide is more than or equal to 99.7 percent, thereby improving the material performance, but increasing the preparation time.
Example three:
the present embodiment is different from the first and second embodiments in that: the preparation method of the ferrite material for the mobile OLED display power supply comprises the following steps of iron sesquioxide, manganous manganic oxide, zinc oxide and an additive:
s1, mixing materials:
weighing corresponding mass of ferric oxide, manganic oxide and zinc oxide respectively by using a high-precision electronic scale in proportion, mixing for 10-15 minutes by using a cone mixer, and uniformly mixing and grinding in a pass-through vibrating mill;
s2, pelletizing:
putting the vibro-milled material into a pelletizer, adding 5-15 wt% of pure water to prepare a ball material, preparing the ball material of the pelletizer into a ball material with the standard diameter of 2-10mm, and drying by using a dryer after preparing the ball material;
s3, pre-burning:
after the ball material is dried, the temperature is raised to 1020 ℃ by using a rotary kiln, and is kept for a certain time, pre-sintering is carried out, wherein the temperature rise speed of the rotary kiln is 120 ℃/min, and the heat preservation time is 15 min;
s4, vibromilling:
after the pre-sintered ball material is cooled, the pre-sintered ball material is vibrated and ground again through a vibrating grinder until the average grain diameter is 1.8-2.5 microns, and a powdery vibrating grinding material is formed;
s5, pulping:
injecting pure water into the slurry pond, adding a vibration grinding material, and stirring by using stirring equipment, wherein the ratio of the vibration grinding material to the pure water is 1: 0.55;
s6, adding an additive:
adding Nb in turn while stirring2O5、CaCO3、Co2O3、SiO 20, NiO, TiO2 and other additives;
s7, sanding:
after the additive is added into the slurry, putting the slurry into a sand mill for sand milling, wherein the average grain diameter standard of the sand milling is 0.8-1.1 micron;
s8, spray granulation;
adding the ground material into 1.2% PVA, and preparing into 0.05-0.5mm granules by adopting a spray granulation drying tower;
s9, profiling:
pressing the granular material into required product blank by using a powder press, and controlling the density of the blank to be 3.0-3.1g/cm3；
S10, sintering:
and (3) increasing the temperature of the pressed blank to 1350 ℃ at the temperature rising speed of 60 ℃/min by using a bell jar furnace, and keeping the temperature for 270 minutes. After the heat preservation is finished, filling a proper amount of nitrogen into the furnace body, cooling to 150 ℃, opening the furnace, and then transferring to a cooling chamber for natural cooling to normal temperature;
s11, grinding:
after the sintered blank is cooled, processing the blank into a magnetic core with a specific size or shape by using a cutting machine or a grinding machine;
s12, checking:
after the processing is finished, performing sampling inspection according to a sampling inspection rate of five percent, firstly detecting the saturation magnetic flux density, the residual magnetism and the coercive force of the magnetic core by adopting a SY-8219 instrument, then testing the magnetic conductivity of the magnetic core by adopting a 4284A type LCR instrument, finally detecting the power consumption of the magnetic core by adopting a CH2335 power consumption instrument, and after the sampling inspection is finished, packaging according to specifications.
The material formula comprises the following components in percentage by mass: 53 mol%, Mn3O 4: 38 mol%, ZnO: 9mol percent of additive, and the formula of the additive is Nb2O5：300ppm、CaCO3：500ppm、Co2O3：3000ppm、SiO2: 200ppm, NiO: 10000ppm, TiO 2: 3000ppm, the purity grade of the additive is electronic purity, the purity of ferric oxide is more than or equal to 99 percent, the purity of manganous oxide is more than or equal to 98.5 percent, the purity of zinc oxide is more than or equal to 99.7 percent, and certain material cost and preparation time are reduced under the condition of ensuring basic performance.
Example four:
the present embodiment differs from the above embodiments in that: the preparation method of the ferrite material for the mobile OLED display power supply comprises the following steps of iron sesquioxide, manganous manganic oxide, zinc oxide and an additive:
s1, mixing materials:
weighing corresponding mass of ferric oxide, manganic oxide and zinc oxide respectively by using a high-precision electronic scale in proportion, mixing for 15 minutes by using a cone mixer, and uniformly mixing and grinding in a pass-through vibrating mill;
s2, pelletizing:
putting the vibro-milled material into a pelletizer, adding 5 wt% of pure water, making into pellets, making the pellets into pellets with the standard diameter of 10mm, and drying by using a dryer after making into pellets;
s3, pre-burning:
after the ball material is dried, the temperature is raised to 1020 ℃ by using a rotary kiln, and is kept for a certain time, pre-sintering is carried out, wherein the temperature rise speed of the rotary kiln is 120 ℃/min, and the heat preservation time is 15 min;
s4, vibromilling:
after the pre-sintered ball material is cooled, the pre-sintered ball material is vibrated and ground again through a vibrating grinder until the average grain diameter is 1.8-2.5 microns, and a powdery vibrating grinding material is formed;
s5, pulping:
injecting pure water into the slurry pond, adding a vibration grinding material, and stirring by using stirring equipment, wherein the ratio of the vibration grinding material to the pure water is 1: 0.55;
s6, adding an additive:
adding Nb in turn while stirring2O5、CaCO3、Co2O3、SnO2、SiO 20, NiO, ZrO2, TiO2 and other additives;
s7, sanding:
after the additive is added into the slurry, putting the slurry into a sand mill for sand milling, wherein the average grain diameter standard of the sand milling is 0.8-1.1 micron;
s8, spray granulation;
adding 0.5-1.2% PVA into the ground material, and preparing into 0.05-0.5mm granules by adopting a spray granulation drying tower;
s9, profiling:
pressing the granular material into required product blank by using a powder press, and controlling the density of the blank to be 3.0-3.1g/cm3；
S10, sintering:
and (3) raising the temperature of the pressed blank to 1280 ℃ by using a bell jar furnace at the temperature rise speed of 60 ℃/min, and keeping the temperature for 180 minutes. After the heat preservation is finished, filling a proper amount of nitrogen into the furnace body, cooling to 150 ℃, opening the furnace, and then transferring to a cooling chamber for natural cooling to normal temperature;
s11, grinding:
after the sintered blank is cooled, processing the blank into a magnetic core with a specific size or shape by using a cutting machine or a grinding machine;
s12, checking:
after the processing is finished, performing sampling inspection according to a sampling inspection rate of five percent, firstly detecting the saturation magnetic flux density, the residual magnetism and the coercive force of the magnetic core by adopting a SY-8219 instrument, then testing the magnetic conductivity of the magnetic core by adopting a 4284A type LCR instrument, finally detecting the power consumption of the magnetic core by adopting a CH2335 power consumption instrument, and after the sampling inspection is finished, packaging according to specifications.
The material formula comprises the following components in percentage by mass: 56 mol%, Mn3O 4: 38 mol%, ZnO: 6mol percent of additive, and the formula of the additive is Nb2O5：300ppm、CaCO3：500ppm、Co2O3：3000ppm、SnO2: 500ppm, NiO: 10000ppm, ZrO 2: 100ppm, TiO 2: 1000ppm, the purity grade of the additive is electronic purity, the purity of ferric oxide is more than or equal to 99 percent, the purity of manganous oxide is more than or equal to 98.5 percent, the purity of zinc oxide is more than or equal to 99.7 percent, and the performance of medium products is enhanced, but the processing time and the cost are effectively reduced.
The material properties described above are listed below:
it is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The preparation method of the ferrite material for the mobile OLED display power supply comprises ferric oxide, manganic oxide, zinc oxide and an additive, and is characterized in that: the preparation steps are as follows:
s1, mixing materials:
weighing corresponding mass of ferric oxide, manganic oxide and zinc oxide respectively by using a high-precision electronic scale in proportion, mixing for 10-15 minutes by using a cone mixer, and uniformly mixing and grinding in a pass-through vibrating mill;
s2, pelletizing:
putting the vibro-milled material into a pelletizer, adding 5-15 wt% of pure water, making a ball material, and drying by using a dryer after the ball material is prepared;
s3, pre-burning:
after the ball material is dried, the temperature is raised to 930-;
s4, vibromilling:
after the pre-sintered ball material is cooled, the pre-sintered ball material is subjected to vibration grinding again through a vibration grinding machine to form powdery vibration grinding materials;
s5, pulping:
injecting pure water into the slurry pool, adding a vibration grinding material, and stirring by using stirring equipment;
s6, adding an additive:
adding Nb in turn while stirring2O5、CaCO3、Co2O3、SnO2、SiO20, NiO, ZrO2, TiO2 and other additives;
s7, sanding:
after the additive is added into the slurry, putting the slurry into a sand mill for sand milling;
s8, spray granulation;
adding 0.5-1.2% PVA into the ground material, and preparing into 0.05-0.5mm granules by adopting a spray granulation drying tower;
s9, profiling:
pressing the granular material into required product blank by using a powder press, and controlling the density of the blank to be 3.0-3.1g/cm3；
S10, sintering:
and (3) increasing the temperature of the pressed blank to 1280-1350 ℃ at the temperature rising speed of 60-80 ℃/min by using a bell jar furnace, and continuously preserving the heat for 180-270 minutes. After the heat preservation is finished, filling a proper amount of nitrogen into the furnace body, cooling to 150 ℃, opening the furnace, and then transferring to a cooling chamber for natural cooling to normal temperature;
s11, grinding:
after the sintered blank is cooled, processing the blank into a magnetic core with a specific size or shape by using a cutting machine or a grinding machine;
s12, checking:
after the processing is finished, performing sampling inspection according to a sampling inspection rate of five percent, firstly detecting the saturation magnetic flux density, the residual magnetism and the coercive force of the magnetic core by adopting a SY-8219 instrument, then testing the magnetic conductivity of the magnetic core by adopting a 4284A type LCR instrument, finally detecting the power consumption of the magnetic core by adopting a CH2335 power consumption instrument, and after the sampling inspection is finished, packaging according to specifications.
2. The method for preparing the ferrite material for the mobile OLED display power supply according to claim 1, wherein the ferrite material comprises the following steps: the material formula comprises the following components in percentage by mass: 51-56 mol%, Mn3O 4: 38-42 mol%, ZnO: 6-10mol percent.
3. The method for preparing the ferrite material for the mobile OLED display power supply according to claim 1, wherein the ferrite material comprises the following steps: the formula of the additive is Nb2O5：200-300ppm、CaCO3：200-500ppm、Co2O3：3000-5000ppm、SnO2：0-500ppm、SiO2：0-200ppm、NiO：0-10000ppm、ZrO2：0-200ppm、TiO2：0-3000ppm。
4. The method for preparing the ferrite material for the mobile OLED display power supply according to claim 1, wherein the ferrite material comprises the following steps: the purity grade of the additive is electronic purity.
5. The method for preparing the ferrite material for the mobile OLED display power supply according to claim 1, wherein the ferrite material comprises the following steps: the purity of the ferric oxide is more than or equal to 99 percent, the purity of the manganic oxide is more than or equal to 98.5 percent, and the purity of the zinc oxide is more than or equal to 99.7 percent.
6. The method for preparing the ferrite material for the mobile OLED display power supply according to claim 1, wherein the ferrite material comprises the following steps: in the second step, the ball material of the pelletizer is made into the ball material with the standard diameter of 2-10 mm.
7. The method for preparing the ferrite material for the mobile OLED display power supply according to claim 1, wherein the ferrite material comprises the following steps: in the third step, the temperature rising speed of the rotary kiln is 100-.
8. The method for preparing the ferrite material for the mobile OLED display power supply according to claim 1, wherein the ferrite material comprises the following steps: in the fourth step, the materials are vibrated and ground by a pass type vibration grinding machine until the average grain diameter is 1.8-2.5 microns.
9. The method for preparing the ferrite material for the mobile OLED display power supply according to claim 1, wherein the ferrite material comprises the following steps: in the fifth step, the ratio of the vibration grinding material to the pure water is 1: 0.4-0.55.
10. The method for preparing the ferrite material for the mobile OLED display power supply according to claim 1, wherein the ferrite material comprises the following steps: in the seventh step, the average grain size standard of sanding is 0.8-1.1 microns.
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