CN106045494B - A kind of Mn-Zn soft magnetic ferrite and preparation method thereof - Google Patents

A kind of Mn-Zn soft magnetic ferrite and preparation method thereof Download PDF

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CN106045494B
CN106045494B CN201610379003.XA CN201610379003A CN106045494B CN 106045494 B CN106045494 B CN 106045494B CN 201610379003 A CN201610379003 A CN 201610379003A CN 106045494 B CN106045494 B CN 106045494B
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lithium chloride
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soft magnetic
water
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CN106045494A (en
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王传伟
王传礼
张晓东
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SHANDONG JIANUO ELECTRONICS Co Ltd
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Abstract

The present invention provides a kind of Mn-Zn soft magnetic ferrite preparation method, and Mn-Zn soft magnetic ferrite of the present invention introduces secondary plus miscellaneous process during the preparation process, in addition to once adding the miscellaneous mass percent being added in the process to be CaCO in material preparation30.03~0.05%, Co2O30.35~0.45%, Nb2O50.03~0.05%, except the additive of ZrO 0.02~0.05%, it also joined the lithium chloride for being dissolvable in water water during secondary plus miscellaneous, additive amount is 200~300PPM.Mn-Zn soft magnetic ferrite of the invention has wide temperature, ultra-low loss characteristic.

Description

A kind of Mn-Zn soft magnetic ferrite and preparation method thereof
Technical field
It is the present invention relates to a kind of Mn-Zn soft magnetic ferrite, in particular to a kind of with wide warm, ultra-low loss characteristic Mn-Zn soft magnetic ferrite and preparation method thereof.
Background technique
Currently, Mn-Zn soft magnetic ferrite in field of power electronics using more and more extensive, especially in communication electricity In terms of source, in recent years, with advancing by leaps and bounds for mechanics of communication, also its matched basic material is put forward higher requirements.
With popularizing for 4G technology, all stepping up to build 4G communication base station, the need of matched communication power supply all over the world The amount of asking is also more and more.Since communication base station is mostly built in field, in some remote districts, base station generally all construction are in spaciousness Place, these regional temperature difference are larger, and bad environments, our matched materials are also required to adapt to various environment, so This blank has just been filled up in the exploitation of wide temperature, low-loss material.
Summary of the invention
In view of the above-mentioned problems, the object of the present invention is to provide a kind of low-loss Mn-Zn soft magnetic ferrite and its preparations Method.
The present invention is achieved through the following technical solutions:
A kind of Mn-Zn soft magnetic ferrite (JNP96), principal component are di-iron trioxide 53.0 ± 0.3%, manganese oxide 36.5 ± 0.2%, zinc oxide 10.5 ± 0.2% (percentage composition is all using molal quantity as units of percent).
The preparation method of above-mentioned Mn-Zn soft magnetic ferrite (JNP96), which is characterized in that comprise the following steps:
(1) by mixing raw materials: above-mentioned di-iron trioxide, mangano-manganic oxide and zinc oxide are mixed, further, above-mentioned raw materials It may be selected to be technical grade;
(2) it is granulated: three kinds of raw material being uniformly mixed in pure water, is added adhesive (PVA), is then dried by spray tower Particulate material is formed after dry;
(3) pre-burning: pre-burning is carried out by rotary kiln, temperature is controlled at 850~950 DEG C;
(4) be sanded: in this process, sand mill is added in additive required for being formulated, i.e., once plus miscellaneous, with raw material It is mixed together grinding;The additive and mole percent level of addition are CaCO30.03~0.05%, Co2O30.35~ 0.45%, Nb2O50.03~0.05%, ZrO 0.02~0.05%;
(5) mist projection granulating: it is identical as step (2), it can obtain being conducive to be pressed by adjusting the size of spray orifice and swirl plate The powder particle material of type;
(6) secondary plus miscellaneous: lithium chloride to be added, lithium chloride is dissolved in water;Aqueous solution is made in lithium chloride, is prepared in step (5) Powder particle material carry out damping when be sprayed among material by damping machine,
(7) it forms
(8) it is sintered
(9) finished product is made in attrition process.
The concentration of above-mentioned lithium chloride is 200~500PPM, preferably 300-400PPM.
The utility model has the advantages that
Invention introduces secondary plus miscellaneous concept, it is more accurate controllable to make the content of its additive, and can reduce material The sintering temperature of material improves the sintered density of finished product.Secondary plus miscellaneous lithium chloride be added is soluble in water, in this way can be more It is conveniently added into material.Secondary plus miscellaneous lithium chloride be added is dissolved in water and solution is made, and carries out damping in material powder When be sprayed among material by damping machine, additive can in this way mixed with material more uniform.It is secondary plus miscellaneous added The lithium chloride entered can play the role of reducing material sintering temperature, improve finished product sintered density.
Mn-Zn soft magnetic ferrite of the present invention introduces secondary plus miscellaneous process during the preparation process, in addition in material system The standby mass percent once plus during miscellaneous being added is CaCO30.03~0.05%, Co2O3
0.35~0.45%, Nb2O50.03~0.05%, except the additive of ZrO 0.02~0.05%, also secondary Add it is miscellaneous during joined the lithium chloride for being dissolvable in water water, additive amount is 200~500PPM, the quality percentage that additive respectively forms Than be with respect to principal component gross mass calculate and obtain.Mn-Zn soft magnetic ferrite of the invention has wide temperature, ultra-low loss special Property.
In general technical process, it can be carried out in the sand milling process of MnZn manufacturing process once plus miscellaneous, it will be needed for formula Sand mill is added in the additive wanted, and is mixed together grinding with raw material;And manufacturing process of the invention is not only in sand grinding process Carry out once plus miscellaneous, also after spray process, carried out again before molding it is once plus miscellaneous, will be secondary plus miscellaneous required by damping machine Additive be added among finished product powder.
Due to it is secondary plus it is miscellaneous be directly to be added in finished product powder dry powder, in order to ensure additive can mix with powder Even, we have chosen the lithium chloride that can be dissolved in deionized water, and the water jet using damping machine will be sprayed to after solution atomization Among powder, while damping machine is rotated with given pace, enable additive and water be evenly distributed on together powder dry powder it In.
The content of microelement in secondary plus miscellaneous control manganese-zinc ferrite powder that can not only be more accurate, while also can It enough avoids some impurity from once adding the miscellaneous some agglomerations generated in the process, each component part of powder can be made more equal It is even.
It, can be with by the content and uniformity of important microelement in secondary plus miscellaneous accurate control manganese-zinc ferrite powder Improve the microstructure of manganese-zinc ferrite product, reduces the power loss of material at various temperatures, apply in the various ministrys of electronics industry It can play the role of improving efficiency among part, energy-saving and emission-reduction.
The lithium chloride being added by such method can make the sintering temperature of manganese-zinc ferrite product from original 1350 DEG C Left and right is reduced to existing 1280 DEG C or so (according to the shape and size of product, sintering temperature has ± 20 DEG C of deviation), together When product performance can also be better than original product.Exploitation Mn-Zn soft magnetic ferrite is secondary to add general labourer's skill, not only saves the energy, but also Improve the performance of product.
Detailed description of the invention
Fig. 1 is the curve graph of power loss and temperature;
Fig. 2 is conventional Mn-Zn soft magnetic ferrite production process figure;
Fig. 3 is the loss temperature comparisons figure of material of the present invention and other materials.
Specific embodiment
Below with reference to embodiment the present invention is described in detail, but embodiment should not limit the scope of the invention.
Embodiment 1:
A kind of preparation method of Mn-Zn soft magnetic ferrite (JNP96), comprises the following steps:
(1) by mixing raw materials: di-iron trioxide 53.0 ± 0.3%, manganese oxide 36.5 ± 0.2%, zinc oxide 10.5 ± 0.2% (percentage composition is all using molal quantity as units of percent)
(2) it is granulated: three kinds of raw material being uniformly mixed in pure water, a certain amount of adhesive (PVA) is added, then passes through Particulate material is formed after spray tower drying,
(3) pre-burning: pre-burning is carried out by rotary kiln, temperature is controlled at 850~950 DEG C
(4) be sanded: in this process, sand mill is added in additive required for being formulated, i.e., once plus miscellaneous, with raw material It is mixed together grinding;The additive and content of addition are CaCO30.03%, Co2O30.35%, Nb2O50.03%, ZrO 0.02%;The mass percent that additive respectively forms is the gross mass calculating with respect to principal component and obtains.
(5) mist projection granulating: by adjusting the size of spray orifice and swirl plate, the powder particle material conducive to compression moulding is obtained
(6) secondary plus miscellaneous: lithium chloride is added, aqueous solution is made in lithium chloride, step (5) preparation powder particle material into It is sprayed among material when row damping by damping machine, the concentration of lithium chloride is 300PPM.
(7) it forms: being pressed into the shape of customer requirement.
(8) be sintered: sintering process can be adjusted according to different product, different weight etc.
(9) finished product is made in attrition process
Embodiment 2:
A kind of preparation method of Mn-Zn soft magnetic ferrite (JNP96), comprises the following steps:
(1) by mixing raw materials: di-iron trioxide 53.0 ± 0.3%, manganese oxide 36.5 ± 0.2%, zinc oxide 10.5 ± 0.2% (percentage composition is all using molal quantity as units of percent)
(2) it is granulated: three kinds of raw material being uniformly mixed in pure water, a certain amount of adhesive (PVA) is added, then passes through Particulate material is formed after spray tower drying,
(3) pre-burning: pre-burning is carried out by rotary kiln, temperature is controlled at 850~950 DEG C
(4) be sanded: in this process, sand mill is added in additive required for being formulated, i.e., once plus miscellaneous, with raw material It is mixed together grinding;The additive and content of addition are CaCO30.03%, Co2O30.35%, Nb2O50.03%, ZrO 0.02%;The mass percent that additive respectively forms is the gross mass calculating with respect to principal component and obtains.
(5) mist projection granulating: by adjusting the size of spray orifice and swirl plate, the powder particle material conducive to compression moulding is obtained
(6) secondary plus miscellaneous: lithium chloride is added, aqueous solution is made in lithium chloride, step (5) preparation powder particle material into It is sprayed among material when row damping by damping machine, the concentration of lithium chloride is 400PPM.
(7) it forms: being pressed into the shape of customer requirement.
(8) be sintered: sintering process can be adjusted according to different product, different weight etc.
(9) finished product is made in attrition process
Embodiment 3:
A kind of preparation method of Mn-Zn soft magnetic ferrite (JNP96), comprises the following steps:
(1) by mixing raw materials: di-iron trioxide 53.0 ± 0.3%, manganese oxide 36.5 ± 0.2%, zinc oxide 10.5 ± 0.2% (percentage composition is all using molal quantity as units of percent)
(2) it is granulated: three kinds of raw material being uniformly mixed in pure water, a certain amount of adhesive (PVA) is added, then passes through Particulate material is formed after spray tower drying,
(3) pre-burning: pre-burning is carried out by rotary kiln, temperature is controlled at 850~950 DEG C
(4) be sanded: in this process, sand mill is added in additive required for being formulated, i.e., once plus miscellaneous, with raw material It is mixed together grinding;The additive and content of addition are CaCO30.05%, Co2O30.45%, Nb2O50.05%, ZrO 0.05%;The mass percent that additive respectively forms is the gross mass calculating with respect to principal component and obtains.
(5) mist projection granulating: by adjusting the size of spray orifice and swirl plate, the powder particle material conducive to compression moulding is obtained
(6) secondary plus miscellaneous: lithium chloride is added, aqueous solution is made in lithium chloride, step (5) preparation powder particle material into It is sprayed among material when row damping by damping machine, the concentration of lithium chloride is 400PPM.
(7) it forms: being pressed into the shape of customer requirement.
(8) be sintered: sintering process can be adjusted according to different product, different weight etc.
(9) finished product is made in attrition process
Embodiment 4
A kind of preparation method of Mn-Zn soft magnetic ferrite (JNP96), comprises the following steps:
(1) by mixing raw materials: di-iron trioxide 53.0 ± 0.3%, manganese oxide 36.5 ± 0.2%, zinc oxide 10.5 ± 0.2% (percentage composition is all using molal quantity as units of percent)
(2) it is granulated: three kinds of raw material being uniformly mixed in pure water, a certain amount of adhesive (PVA) is added, then passes through Particulate material is formed after spray tower drying,
(3) pre-burning: pre-burning is carried out by rotary kiln, temperature is controlled at 850~950 DEG C
(4) be sanded: in this process, sand mill is added in additive required for being formulated, i.e., once plus miscellaneous, with raw material It is mixed together grinding;The additive and content of addition are CaCO30.035%, Co2O30.45%, Nb2O50.04%, ZrO 0.03%;The mass percent that additive respectively forms is the gross mass calculating with respect to principal component and obtains.
(5) mist projection granulating: by adjusting the size of spray orifice and swirl plate, the powder particle material conducive to compression moulding is obtained
(6) secondary plus miscellaneous: lithium chloride is added, aqueous solution is made in lithium chloride, step (5) preparation powder particle material into It is sprayed among material when row damping by damping machine, the concentration of lithium chloride is 500PPM.
(7) it forms: being pressed into the shape of customer requirement.
(8) be sintered: sintering process can be adjusted according to different product, different weight etc.
(9) finished product is made in attrition process
Mn-Zn soft magnetic ferrite (JNP96) prepared by the present invention can make the sintering temperature of manganese-zinc ferrite product from 1350 DEG C or so originally are reduced to existing 1280 DEG C or so, and (according to the shape and size of product, sintering temperature has ± 20 DEG C deviation), while the performance of product can also be better than original product.Exploitation Mn-Zn soft magnetic ferrite is secondary to add general labourer's skill, both The energy is saved, and improves the performance of product.
Present invention JNP96 material newly developed reduces by 10% or so than traditional 95 material overall losses of wide-temperature and low-consumption, The efficiency of power supply can further be promoted, the curve of specific power loss and temperature is as shown in Figure 1.
Following table and Fig. 3 be JNP96 material with 95 materials before simultaneously made of EE70 manganese-zinc ferrite core and its Loss temperature comparisons' data of his 96 material of company:
Temperature comparisons' data are lost in table 1
From the point of view of upper table 1 and Fig. 3, the product that JNP96 material is fabricated obviously is better than other materials in loss.
Embodiment described above only describe the preferred embodiments of the invention, not to model of the invention It encloses and is defined, without departing from the spirit of the design of the present invention, those of ordinary skill in the art are to technical side of the invention The various changes and improvements that case is made should all be fallen into the protection scope that claims of the present invention determines.

Claims (4)

1. a kind of preparation method of Mn-Zn soft magnetic ferrite, includes the following steps:
(1) by mixing raw materials: di-iron trioxide, mangano-manganic oxide and zinc oxide being mixed, are calculated as three with mole percent level Aoxidize two iron 53.0 ± 0.3%, mangano-manganic oxide 36.5 ± 0.2%, zinc oxide 10.5 ± 0.2%;
(2) it is granulated: three kinds of raw material being uniformly mixed in pure water, adhesive is added, is formed after then being dried by spray tower Particulate material;
(3) pre-burning: pre-burning is carried out by rotary kiln, temperature is controlled at 850 ~ 950 DEG C;
(4) be sanded: in this process, sand mill is added in additive required for being formulated, i.e., once plus miscellaneous, together with raw material Mixed grinding;The additive and mole percent level of addition are CaCO3 0.03~0.05%、Co2O3 0.35~0.45%、Nb2O5 0.03~0.05%,ZrO 0.02~0.05%;
(5) mist projection granulating: by adjusting the size of spray orifice and swirl plate, the powder particle material conducive to compression moulding is obtained;
(6) secondary plus miscellaneous: lithium chloride to be added, lithium chloride is dissolved in water;Aqueous solution is made in lithium chloride, in the powder of step (5) preparation Last particulate material be sprayed among material when damping by damping machine, wherein aqueous solution is atomized by the water jet using damping machine After be sprayed among powder particle material, while damping machine is rotated with given pace, is evenly distributed on water lithium chloride solution Among powder particle material dry powder;
(7) it forms;
(8) it is sintered;
(9) finished product is made in attrition process;
The sintering temperature of the finished product is reduced to 1280 DEG C.
2. preparation method according to claim 1, it is characterised in that: described adhesive PVA.
3. preparation method according to claim 1, it is characterised in that: the concentration of water lithium chloride solution is 200-500PPM.
4. preparation method according to claim 3, it is characterised in that: the concentration of the water lithium chloride solution is 300- 500PPM。
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