阅读说明：本技术 一种锰锌铁氧体磁性材料的生产工艺 (A kind of production technology of manganese-zinc ferrite magnetic material ) 是由 严华军 于 2019-08-26 设计创作，主要内容包括：本发明公开了一种锰锌铁氧体磁性材料的生产工艺,包括以下步骤：(1)按摩尔百分含量取如下组分的主料：Fe<Sub>2</Sub>O<Sub>3</Sub>、MnO<Sub>2</Sub>、Mn<Sub>3</Sub>O<Sub>4</Sub>,余量为ZnO,将主料加入容器中,再加入蒸馏水、Bi<Sub>2</Sub>O<Sub>3</Sub>、P<Sub>2</Sub>O<Sub>5</Sub>、TiO<Sub>2</Sub>,并充分混合搅拌均匀得到混合物；(2)将经步骤(1)烧结得到的物料加入容器中搅拌,充分混合,送入烧结炉内在氮气气氛保护下进行烧结；(3)将经步骤(2)烧结后的物料压制成块状,在氮气气氛保护下进行烧结；(4)按重量百分含量向经步骤(3)三次烧结后的物料中添加Co<Sub>2</Sub>O<Sub>3</Sub>、CuO和SiO<Sub>2</Sub>,并进行充分混合,在氮气气氛保护下进行烧结,得到锰锌铁氧体磁性材料,本发明优点是：提高了锰锌铁氧体磁性材料粒度分布的均匀程度,有效提升了锰锌铁氧体磁性材料的电阻率,并且降低了材料的损耗。(The invention discloses a kind of production technologies of manganese-zinc ferrite magnetic material, comprising the following steps: (1) major ingredient of following component: Fe is taken by molar content 2 O 3 、MnO 2 、Mn 3 O 4 , major ingredient is added to the container by surplus ZnO, adds distilled water, Bi 2 O 3 、P 2 O 5 、TiO 2 , and be sufficiently mixed and be uniformly mixing to obtain mixture；(2) material obtained through step (1) sintering is added to the container stirring, be sufficiently mixed, be sent into sintering furnace under nitrogen atmosphere protection and be sintered；(3) it will be pressed into bulk through step (2) sintered material, will be sintered under nitrogen atmosphere protection；(4) percentage composition adds Co in through step (3) three times sintered material by weight 2 O 3 , CuO and SiO 2 , and be sufficiently mixed, it is sintered under nitrogen atmosphere protection; obtain manganese-zinc ferrite magnetic material; the invention has the advantages that: the uniformity coefficient of manganese-zinc ferrite magnetic material particle size distribution is improved, effectively improves the resistivity of manganese-zinc ferrite magnetic material, and reduce the loss of material.)

1. a kind of production technology of manganese-zinc ferrite magnetic material, it is characterised in that the following steps are included:

(1) major ingredient of following component: 48~52mol%Fe is taken by molar content₂O₃, 9~16mol%MnO₂, 23~ 25mol%Mn₃O₄, major ingredient is added to the container by surplus ZnO, then 40 ~ 50wt% steaming is added into container for percentage composition by weight Distilled water, 330 ~ 400ppmBi₂O₃、340~450ppm P₂O₅、400~480ppm TiO₂, and be sufficiently mixed and be uniformly mixing to obtain mixing Object, it is 80~86um that mixture, which is added into ball mill, and be ground to for the first time partial size, and the material after first grinding is sent into It is sintered under nitrogen atmosphere protection in sintering furnace, is 0.5 ~ 0.8% by the oxygen volumetric concentration control in sintering furnace, will burn Initial temperature control in freezing of a furnace is 30 ~ 35 DEG C, and the temperature in sintering furnace is risen to 950 by the heating rate of 3~3.5 DEG C/min ~ 1000 DEG C, and keep the temperature 2 ~ 2.1 hours, then, the temperature in sintering furnace is down to 870 by the rate of temperature fall of 4~4.5 DEG C/min ~ 900 DEG C, and keep the temperature 1.6 ~ 1.8 hours, then the temperature in sintering furnace risen to 1200 by the heating rate of 5.2~5.4 DEG C/min ~ 1250 DEG C, and 1.2 ~ 1.5 hours are kept the temperature, the temperature in sintering furnace is finally down to room by the rate of temperature fall of 2.5~3.1 DEG C/min Temperature；

(2) material obtained through step (1) sintering is added to the container, 52 ~ 60wt% is added into container for percentage composition by weight Distilled water, and carry out ultrasonic wave and stir 25 ~ 32 minutes, it is 56 ~ 72% that mass concentration is added dropwise into container while agitating The pH of mixed liquor in container is adjusted to 10.5 ~ 11.3, and is 54 ~ 62 DEG C by the control of the temperature of mixed liquor by NaOH solution, then, Sediment is obtained by filtration in mixed liquor after standing 3.8 ~ 4.1 hours, percentage composition by weight takes 260 ~ 320ppm CaCO₃、280~ 330ppm Nb₂O₅With 340 ~ 370ppm SnO₂It is added in sediment, and is sufficiently mixed, mixed material is added Carried out in ball mill it is secondary be ground to 50~54um of partial size, by after secondary grinding material be sent into sintering furnace in nitrogen atmosphere It is sintered under protection, is 0.6 ~ 0.9% by the oxygen volumetric concentration control in sintering furnace, by the initial temperature control in sintering furnace 30 ~ 35 DEG C are made as, the temperature in sintering furnace is risen to 1020 ~ 1045 DEG C by the heating rate of 4.1~4.3 DEG C/min, and keep the temperature 3.8 ~ 4.2 hours, then, the temperature in sintering furnace is risen to 1100 ~ 1150 DEG C by the heating rate of 3.5~3.9 DEG C/min, and Heat preservation 2.4 ~ 2.7 hours, then the temperature in sintering furnace is down to 980 ~ 990 DEG C by the rate of temperature fall of 3.6~3.8 DEG C/min, and Heat preservation 2.3 ~ 2.5 hours, is finally down to room temperature for the temperature in sintering furnace by the rate of temperature fall of 4.2~4.5 DEG C/min；

(3) it will be pressed into bulk through step (2) sintered material, block material will be placed in autoclave, led into autoclave Enter nitrogen, and be 8.6 ~ 9.3Mpa by the pressure control in autoclave, is lighted block material energization by tungsten wire, through self- propagating Reaction generates blank block, and being ground to partial size three times to blank block using ball mill is 14~18um, after grinding three times Material is sent into sintering furnace under nitrogen atmosphere protection and is sintered, by the oxygen volumetric concentration control in sintering furnace for 0.4 ~ 0.7%, it is 30 ~ 35 DEG C by the initial temperature control in sintering furnace, it will be in sintering furnace by the heating rate of 2.8~3.1 DEG C/min Temperature rises to 940 ~ 950 DEG C, and keeps the temperature 2.9 ~ 3.4 hours, then, will be in sintering furnace by the heating rate of 3.2~3.5 DEG C/min Temperature rise to 1030 ~ 1070 DEG C, and keep the temperature 3.3 ~ 3.6 hours, then by 2.9~3.2 DEG C/min rate of temperature fall by sintering furnace Interior temperature is down to 910 ~ 930 DEG C, and keeps the temperature 3.7 ~ 4 hours, finally will be in sintering furnace by the rate of temperature fall of 2.8~3 DEG C/min Temperature be down to room temperature；

(4) percentage composition by weight is to through adding 340 ~ 380ppm Co in step (3) three times sintered material₂O₃、410~ 470ppm CuO and 380 ~ 420ppm SiO₂, and be sufficiently mixed, mixed material is added in ball mill and carries out four The secondary partial size that is ground to is 0.8~1.3um, and it is poly- that 1.5 ~ 1.8wt% is added into the material after four grindings for percentage composition by weight Vinyl alcohol is crossed 80~100 meshes, is obtained particulate material after drying, particulate material is pressed into base by mold using manual granulation Green body is sent into sintering furnace under nitrogen atmosphere protection and is sintered by body, is by the oxygen volumetric concentration control in sintering furnace 1.3 ~ 1.5%, it is 30 ~ 35 DEG C by the initial temperature control in sintering furnace, by the heating rate of 4.6~4.8 DEG C/min by sintering furnace Interior temperature rises to 1200 ~ 1280 DEG C, and keeps the temperature 3.1 ~ 3.5 hours, then, will burn by the rate of temperature fall of 3.6~3.9 DEG C/min Temperature in freezing of a furnace is down to 1000 ~ 1100 DEG C, and keeps the temperature 2.5 ~ 2.8 hours, then will burn by the heating rate of 2.7~3 DEG C/min Temperature in freezing of a furnace rises to 1130 ~ 1200 DEG C, and keeps the temperature 2.5 ~ 2.7 hours, finally presses the rate of temperature fall of 4.2~4.5 DEG C/min Temperature in sintering furnace is down to room temperature, obtains manganese-zinc ferrite magnetic material.

2. a kind of production technology of manganese-zinc ferrite magnetic material according to claim 1, it is characterised in that: ground secondary Material after mill is sent into sintering furnace under nitrogen atmosphere protection and is sintered, and is by the oxygen volumetric concentration control in sintering furnace 0.8%, it is 32 DEG C by the initial temperature control in sintering furnace, rises to the temperature in sintering furnace by the heating rate of 4.2 DEG C/min 1030 DEG C, and 4 hours are kept the temperature, then, the temperature in sintering furnace is risen to 1130 DEG C by the heating rate of 3.7 DEG C/min, and protect Temperature 2.5 hours, then the temperature in sintering furnace is down to 985 DEG C by the rate of temperature fall of 3.7 DEG C/min, and keep the temperature 2.4 hours, finally The temperature in sintering furnace is down to room temperature by the rate of temperature fall of 4.3 DEG C/min.

3. a kind of production technology of manganese-zinc ferrite magnetic material according to claim 1 or 2, it is characterised in that: by three Material after secondary grinding is sent into sintering furnace under nitrogen atmosphere protection and is sintered, by the oxygen volumetric concentration control in sintering furnace It is made as 0.5%, is 32 DEG C by the initial temperature control in sintering furnace, by the heating rate of 3 DEG C/min by the temperature liter in sintering furnace To 945 DEG C, and 3.1 hours are kept the temperature, then, the temperature in sintering furnace is risen to 1040 DEG C by the heating rate of 3.3 DEG C/min, and Heat preservation 3.4 hours, then the temperature in sintering furnace is down to 920 DEG C by the rate of temperature fall of 3 DEG C/min, and keep the temperature 3.9 hours, finally The temperature in sintering furnace is down to room temperature by the rate of temperature fall of 2.9 DEG C/min.

Technical field

The present invention relates to the technical fields of ferrite magnetic material production technology, more particularly to manganese-zinc ferrite The technical field of magnetic materials production technique.

Background technique

Manganese-zinc ferrite magnetic material is a kind of composite oxide sintered body nonmetal magnetic material, very as one kind Important basic function material, manganese-zinc ferrite magnetic material have high saturated magnetic induction, high initial permeability, low-loss Etc. characteristics, be widely used in produce power transformer, pulse broadband transformer, magnetic deflection arrangement, sensor, lighting transformer In the calutrons such as electric ballast, application range is related to communication, broadcast, TV, automatic control, space flight and aviation, calculating The fields such as mechanical, electrical sub- equipment, it is inseparable with the production and living of people.Currently, the production that manganese-zinc ferrite magnetic material is common Method is broadly divided into dry process and wet processing, however use manganese-zinc ferrite magnetic material made from these production methods its Not the defects of uniformity of crystal grain is not very unanimously that density is smaller, is easy to appear stomata, powder reuniting, thus to manganese-zinc ferrite The performances such as the initial permeability and resistivity of body magnetic material cause not small influence.

Summary of the invention

The object of the invention is to provide a kind of uniformity and density that crystal grain can be improved to solve above-mentioned deficiency, The defects of reducing the porosity, improves the manganese-zinc ferrite magnetic of the performances such as manganese-zinc ferrite magnetic material initial permeability and resistivity The production technology of property material.

In order to solve the above-mentioned technical problem technical solution that the present invention uses is as follows:

A kind of production technology of manganese-zinc ferrite magnetic material, comprising the following steps:

(1) major ingredient of following component: 48~52mol%Fe is taken by molar content₂O₃, 9~16mol%MnO₂, 23~ 25mol%Mn₃O₄, major ingredient is added to the container by surplus ZnO, then 40 ~ 50wt% steaming is added into container for percentage composition by weight Distilled water, 330 ~ 400ppmBi₂O₃、340~450ppm P₂O₅、400~480ppm TiO₂, and be sufficiently mixed and be uniformly mixing to obtain mixing Object, it is 80~86um that mixture, which is added into ball mill, and be ground to for the first time partial size, and the material after first grinding is sent into It is sintered under nitrogen atmosphere protection in sintering furnace, is 0.5 ~ 0.8% by the oxygen volumetric concentration control in sintering furnace, will burn Initial temperature control in freezing of a furnace is 30 ~ 35 DEG C, and the temperature in sintering furnace is risen to 950 by the heating rate of 3~3.5 DEG C/min ~ 1000 DEG C, and keep the temperature 2 ~ 2.1 hours, then, the temperature in sintering furnace is down to 870 by the rate of temperature fall of 4~4.5 DEG C/min ~ 900 DEG C, and keep the temperature 1.6 ~ 1.8 hours, then the temperature in sintering furnace risen to 1200 by the heating rate of 5.2~5.4 DEG C/min ~ 1250 DEG C, and 1.2 ~ 1.5 hours are kept the temperature, the temperature in sintering furnace is finally down to room by the rate of temperature fall of 2.5~3.1 DEG C/min Temperature；

(2) material obtained through step (1) sintering is added to the container, 52 ~ 60wt% is added into container for percentage composition by weight Distilled water, and carry out ultrasonic wave and stir 25 ~ 32 minutes, it is 56 ~ 72% that mass concentration is added dropwise into container while agitating The pH of mixed liquor in container is adjusted to 10.5 ~ 11.3, and is 54 ~ 62 DEG C by the control of the temperature of mixed liquor by NaOH solution, then, Sediment is obtained by filtration in mixed liquor after standing 3.8 ~ 4.1 hours, percentage composition by weight takes 260 ~ 320ppm CaCO₃、280~ 330ppm Nb₂O₅With 340 ~ 370ppm SnO₂It is added in sediment, and is sufficiently mixed, mixed material is added Carried out in ball mill it is secondary be ground to 50~54um of partial size, by after secondary grinding material be sent into sintering furnace in nitrogen atmosphere It is sintered under protection, is 0.6 ~ 0.9% by the oxygen volumetric concentration control in sintering furnace, by the initial temperature control in sintering furnace 30 ~ 35 DEG C are made as, the temperature in sintering furnace is risen to 1020 ~ 1045 DEG C by the heating rate of 4.1~4.3 DEG C/min, and keep the temperature 3.8 ~ 4.2 hours, then, the temperature in sintering furnace is risen to 1100 ~ 1150 DEG C by the heating rate of 3.5~3.9 DEG C/min, and Heat preservation 2.4 ~ 2.7 hours, then the temperature in sintering furnace is down to 980 ~ 990 DEG C by the rate of temperature fall of 3.6~3.8 DEG C/min, and Heat preservation 2.3 ~ 2.5 hours, is finally down to room temperature for the temperature in sintering furnace by the rate of temperature fall of 4.2~4.5 DEG C/min；

(3) it will be pressed into bulk through step (2) sintered material, block material will be placed in autoclave, led into autoclave Enter nitrogen, and be 8.6 ~ 9.3Mpa by the pressure control in autoclave, is lighted block material energization by tungsten wire, through self- propagating Reaction generates blank block, and being ground to partial size three times to blank block using ball mill is 14~18um, after grinding three times Material is sent into sintering furnace under nitrogen atmosphere protection and is sintered, by the oxygen volumetric concentration control in sintering furnace for 0.4 ~ 0.7%, it is 30 ~ 35 DEG C by the initial temperature control in sintering furnace, it will be in sintering furnace by the heating rate of 2.8~3.1 DEG C/min Temperature rises to 940 ~ 950 DEG C, and keeps the temperature 2.9 ~ 3.4 hours, then, will be in sintering furnace by the heating rate of 3.2~3.5 DEG C/min Temperature rise to 1030 ~ 1070 DEG C, and keep the temperature 3.3 ~ 3.6 hours, then by 2.9~3.2 DEG C/min rate of temperature fall by sintering furnace Interior temperature is down to 910 ~ 930 DEG C, and keeps the temperature 3.7 ~ 4 hours, finally will be in sintering furnace by the rate of temperature fall of 2.8~3 DEG C/min Temperature be down to room temperature；

(4) percentage composition by weight is to through adding 340 ~ 380ppm Co in step (3) three times sintered material₂O₃、410~ 470ppm CuO and 380 ~ 420ppm SiO₂, and be sufficiently mixed, mixed material is added in ball mill and carries out four The secondary partial size that is ground to is 0.8~1.3um, and it is poly- that 1.5 ~ 1.8wt% is added into the material after four grindings for percentage composition by weight Vinyl alcohol is crossed 80~100 meshes, is obtained particulate material after drying, particulate material is pressed into base by mold using manual granulation Green body is sent into sintering furnace under nitrogen atmosphere protection and is sintered by body, is by the oxygen volumetric concentration control in sintering furnace 1.3 ~ 1.5%, it is 30 ~ 35 DEG C by the initial temperature control in sintering furnace, by the heating rate of 4.6~4.8 DEG C/min by sintering furnace Interior temperature rises to 1200 ~ 1280 DEG C, and keeps the temperature 3.1 ~ 3.5 hours, then, will burn by the rate of temperature fall of 3.6~3.9 DEG C/min Temperature in freezing of a furnace is down to 1000 ~ 1100 DEG C, and keeps the temperature 2.5 ~ 2.8 hours, then will burn by the heating rate of 2.7~3 DEG C/min Temperature in freezing of a furnace rises to 1130 ~ 1200 DEG C, and keeps the temperature 2.5 ~ 2.7 hours, finally presses the rate of temperature fall of 4.2~4.5 DEG C/min Temperature in sintering furnace is down to room temperature, obtains manganese-zinc ferrite magnetic material.

Preferably, the material after secondary grinding is sent into sintering furnace under nitrogen atmosphere protection and is sintered, will be sintered Oxygen volumetric concentration control in furnace is 0.8%, is 32 DEG C by the initial temperature control in sintering furnace, by the heating of 4.2 DEG C/min Temperature in sintering furnace is risen to 1030 DEG C by rate, and keeps the temperature 4 hours, then, by the heating rate of 3.7 DEG C/min by sintering furnace Interior temperature rises to 1130 DEG C, and keeps the temperature 2.5 hours, then be down to the temperature in sintering furnace by the rate of temperature fall of 3.7 DEG C/min 985 DEG C, and 2.4 hours are kept the temperature, the temperature in sintering furnace is finally down to room temperature by the rate of temperature fall of 4.3 DEG C/min.

Preferably, the material after grinding three times is sent into sintering furnace under nitrogen atmosphere protection and is sintered, will be sintered Oxygen volumetric concentration control in furnace is 0.5%, is 32 DEG C by the initial temperature control in sintering furnace, by the heating speed of 3 DEG C/min Temperature in sintering furnace is risen to 945 DEG C by rate, and keeps the temperature 3.1 hours, then, by the heating rate of 3.3 DEG C/min by sintering furnace Interior temperature rises to 1040 DEG C, and keeps the temperature 3.4 hours, then the temperature in sintering furnace is down to 920 by the rate of temperature fall of 3 DEG C/min DEG C, and 3.9 hours are kept the temperature, the temperature in sintering furnace is finally down to room temperature by the rate of temperature fall of 2.9 DEG C/min.

The present invention is using the above-mentioned attainable beneficial effect of technical solution:

1, this production technology passes through four grindings and sintering respectively, and precipitates manganese, zinc, iron metal ion by NaOH solution, Block material energization is lighted by carry out self-propagating reaction by tungsten wire simultaneously, so that the polycrystalline structure of high density fine grain is obtained, Manganese-zinc ferrite magnetic material obtained has even particle size distribution, purity is high, activity big, good dispersion, ingredient segregation-free etc. Advantage.

2, in four sintering processes, different sintering temperature curves has been respectively adopted, which is basis The characteristic progress of different times material is well-designed to be obtained, and is not only increased sintered density, has been refined crystal grain, and reduce and grind The reunion degree of milling body, greatly improved the uniformity coefficient of manganese-zinc ferrite magnetic material particle size distribution, effectively improves manganese The resistivity of zinc ferrite magnetic material, and reduce the loss of material.

3, by the way that Bi is added in step (1)₂O₃、P₂O₅And TiO₂, to reduce the gas of manganese-zinc ferrite magnetic material Porosity increases density, makes initial permeability, quality factor, resistivity and the Curie temperature value of manganese-zinc ferrite magnetic material Obtain a degree of raising.By the way that CaCO is added in step (2)₃、Nb₂O₅And SnO₂, to improve manganese-zinc ferrite magnetic The uniformity of property material grains, reduces the porosity and eddy-current loss, improves initial permeability and resistivity.By in step (4) Co is added in₂O₃, CuO and SiO₂, to promote uniformly growing up for crystal grain, increase lattice constant.

Specific embodiment