Background technology
So-called soft magnetic materials refers in particular to those coercive forces magneticsubstance little, that magnetize and demagnetize easily.So-called soft, refer to that these materials magnetize easily, performance " soft " on magnetic.The purposes of soft magnetic materials is very extensive.Because they are magnetization and demagnetization easily, and has a very high permeability, can play the effect of good gathering magnetic line of force, so soft magnetic materials is widely used for the path as magnetic line of force, promptly as magnetically permeable material, the iron core of transformer, transmitter for example, magnetic shielding cover, the yoke of special magnetic circuit etc.The invention of soft magnetic ferrite and practicability, existing half a century so far.Because it has high magnetic permeability, high resistivity, low-loss and Standpoint of Ceramic Wear-resisting Function, thereby the deflector coil of making of soft magnetic ferrite, kickback transformer, rotating transformer, in all transformers, pulse transformer, switch power supply, wave filter, reactance coil, inducer, anti-electromagnetic interference transformer, electric ballasts etc. (broad sense is called electronic transformer) are at computer, micro-cells, communication, office automation, indicating meter, remote monitoring, colour receiver, audio-visual apparatus, household electrical appliance, electromagnetic compatibility, green illumination, play filtering in environmental protection and energy saving and the electronic information, the impedance conversion, effect such as energy storage and energy transformation is widely used.Soft magnetic ferrite can be divided into spinel type and flush type hexaplanar two classes such as MnZn, NiZn, MgZn, MnMgZn by composition.MgZn, MgMnZn series ferrite material have good high frequency characteristics, do not need strategic material nickel, and cost is low, can partly substitute the NiZn based material aspect the product for civilian use.High resistivity (ρ=10
5Ω .cm~10
8Ω .cm) MgZn, MgMnZn series ferrite material can improve the electrical insulative property of televisor, indicating meter as the television picture tube deflecting core, can make color monitor avoid high-voltage breakdown, improve its line-scanning frequency.Relate to a kind of manganese-zinc power soft ferrite material powder and preparation method thereof as Chinese patent application (03115906.0).With Fe
2O
3, Mn
3O
4, ZnO is main raw material, by mixing, pre-burning, coarse reduction, sand milling, five operations of mist projection granulating are made manganese-zinc power soft ferrite material powder, though it is lower that the finish mix powder has power consumption, saturation induction density Bs height, superior performance, characteristics such as with low cost.But owing to lack the existence of flux, make sintering temperature need reach 1320 ℃, kiln is not long work-ing life, has increased cost.And the qualification rate of product is lower, and substandard products are many.
Summary of the invention
Main purpose of the present invention is to realize the reduction of sintering temperature by adding solubility promoter, prolongs the life-span of kiln, reduces cost.
Another object of the present invention is by the interpolation solubility promoter, realizes improving the stability of product quality, and the qualification rate of product is greatly enhanced.
Above-mentioned technical problem of the present invention is mainly solved by following technical proposals: a kind of Mg-Zn soft magnetic ferrite, and by Fe
2O
3, MgO, ZnO, Mn
3O
4, CuO forms, and it is characterized in that each composition and consumption thereof are as follows:
Fe
2O
3 47.5-48.7wt%
MgO 25.5-30.0wt%
ZnO 18.0-21.4wt%
Mn
3O
4 0.5-1.2wt%
Flux 3.0-4.2wt%
Auxiliary material 0-5wt%
Total satisfied amount: 100%.
As preferably, described flux is CuO or Bi
2O
3In one or both, wherein must contain CuO.
Those of ordinary skill is thought added CuO, Bi in main formula
2O
3Increased the content of impurity in the prescription Deng the solubility promoter result, influenced the characteristic of product, appeared to the quality that has reduced product, this is a technology barrier, so they can not walk this mistaken ideas all the time.
The inventor once also entered into such mistaken ideas, but by discoverys that study for a long period of time: as long as, just can overcome the influence of the interpolation of solubility promoter to product quality to the adjusting slightly of main formula, but owing to adding CuO, Bi
2O
3Deng solubility promoter, greatly reduce sintering temperature, make originally from 1320 ℃ and be reduced to 1220 ℃, furnace service life extends to 2 years (originally 8 months life-spans).Improve 2~3 times the work-ing life of auxiliary refractory materials such as push pedal, saggar.
As preferably, described flux is CuO or Bi
2O
3In one or both, wherein must contain CuO.
As preferably, described auxiliary material is one or more in defoamer, dispersion agent, cementing agent, the lubricant.
As preferably, described defoamer is a n-Octanol.
As preferably, described dispersion agent is a gum arabic.
As preferably, described for cementing agent be PVA.
As preferably, described lubricant is a Zinic stearas.
In the above-mentioned prescription, auxiliary material comprises one or more in defoamer, dispersion agent, cementing agent, the lubricant etc.Auxiliary material can induce spinel to shift to an earlier date rapid crystallization mutually, can reduce the needed intensity of activation of solid state reaction; Thereby solve problems such as iron oxide red raw material poor activity.
The preparation method of a kind of Mg-Zn soft magnetic ferrite that the present invention proposes is as follows:
(1) batching: by claim 1 proportioning raw materials batching, wherein said flux is CuO, and through the strong machine uniform mixing that mixes, blended time 20~30min mixes back material powder and directly is controlled at below the 1.8 μ m.
(2) make ball: above-mentioned mixed uniformly material powder is added the ball material that 10%~20% moisture content is made diameter phi 3~φ 6mm intensity 〉=40N through making ball.
(3) pre-burning: above-mentioned ball material by certain inlet amount, is used the rotary kiln pre-burning under 900~1080 ℃ temperature.
(4) pulverize: it is that 1.2~1.5 μ m, viscosity are 600~1500mpa.s, proportion 1.9~2.2g/cm that the ball material after the above-mentioned pre-burning is become to have granularity through one-level, secondary sand milling by 100: 30 material-water ratio examples
3Water content is 30~37% slip; Stir after the pulverizing.
(5) mist projection granulating: with above-mentioned pulverizing and the spray-dried tower of slip after stirring make that to have loose specific weight be 1.25~1.45g/cm
3, water content is that 0.2~0.4% particle diameter is the runny spherical particle that 0.1~0.3mm distributes.
(6) batch mixing: the particulate material after the above-mentioned spraying is mixed through mixer; Time 10~the 30min of batch mixing.
(7) moulding and sintering: the particulate material behind the above-mentioned batch mixing is pressed into desired shape, size through the moulding mouldenpress, the blank of compact density, described blank after being 1220 ℃ of sintering, kiln temperature is generated size, the FERRITE CORE of characteristic conforms product requirement.
As preferably, also has Bi the ball material in the described crushing process after adding pre-burning
2O
3, the ratio of interpolation is 0.1~0.3%.
As preferably, described pulverizing is a kind of wet pulverization, utilizes tap water as solvent, adds defoamer when pulverizing fast the end, and the ratio that adds is 0.1~0.2%.
As preferably, to remove the slurry that adds after pulverizing in the whipping process after the described pulverizing and also have cementing agent, the ratio of interpolation is: 0.5~1.2%.
As preferably, also have lubricant except that the particulate material behind the adding mist projection granulating in the described batch mixing process, the ratio of interpolation is: 0.3~0.7%.
The present invention has added the CuO flux with the speed of response of raising ferrite in the solid state reaction process in the starting material main formula, thereby reaches the purpose that reduces sintering temperature.And in the pre-burning process, the material through pre-burning is added Bi
2O
3Help and melted active material, improve the formation speed of ferrite crystallisation process, reduce sintering temperature.
The present invention adjusts main formula in blending process, has overcome because of CuO and Bi
2O
3Interpolation to the influence of product performance, the present invention has also adjusted calcined temperature in the pre-burning process, reduce because of CuO and Bi
2O
3Interpolation to the characteristic of material contracts.
The Mg-Zn soft magnetic ferrite that the present invention proposes has good performance, presses GB9623-88 through appropriate authority, SJ2876-88, and SJ2877-88 detects, and material property is as follows:
Initial permeability μ i=350
Saturation induction density Bs 〉=210mT (23 ℃)
Remanent magnetism Br≤150mT (23 ℃)
Coercivity H≤40A/m (23 ℃)
Curie temperature Tc 〉=150 ℃
Electricalresistivity 〉=10
5Ω .m
Therefore, the present invention has the following advantages and 1. greatly reduces sintering temperature, makes originally from 1320 ℃ and is reduced to 1220 ℃, and furnace service life extends to 2 years (originally 8 months life-spans).Improve 2~3 times the work-ing life of auxiliary refractory materials such as push pedal, saggar.2. improved the stability of product quality, yield rate is brought up to 94%~96% (being 90%~92% before the application), and 3. raw material supply is convenient, domestic aboundresources, and cost is lower, can satisfy the demands for a long time.4. the product saturation induction density height of Sheng Chaning, superior performance.
Embodiment
Below by embodiment, technical scheme of the present invention is done further specific description.
Embodiment 1
Take by weighing 47.5wt%Fe
2O
3, 30.0wt%MgO, 18.5wt%ZnO 0.6wt%Mn
3O
4, 3.0wt%CuO is through the strong machine uniform mixing that mixes, blended time 20min mixes back material powder and directly is controlled at 1.75 μ m.Above-mentioned mixed uniformly material powder is added the ball material that 10% moisture content is made diameter 6mm intensity 70N through making ball.To burn till in advance in the rotary kiln of above-mentioned ball material under 900 ℃ temperature, it is that 1.5 μ m, viscosity are that 600mpa.s, proportion are 2.20g/cm that the ball material after the above-mentioned pre-burning is become to have granularity through one-level, secondary sand milling by 110:40 material-water ratio example
3Water content is 30% slip; The time one-level 50min that pulverizes, secondary 50min.The PVA of the interpolation of the slurry after the above-mentioned pulverizing 9.5% is made the slip that can spray through a mixing bowl stirring; The time 2h that stirs.The spray-dried tower of slip after the above-mentioned stirring made to have loose specific weight be 1.45g/cm
3, water content is that 0.2% particle diameter is 0.1~0.3 equally distributed runny spherical particle.The Zinic stearas of the particulate material after the above-mentioned spraying and 0.4% is mixed through mixer; The particulate material of the time 10min of batch mixing after with above-mentioned batch mixing is pressed into desired shape through the moulding mouldenpress, compact density 2.80g/cm
3Blank, be to generate the FERRITE CORE that every performance parameters conformance with standard requires after 1220 ℃ and soaking time are the 4h sintering with described blank through kiln temperature.
Embodiment 2
Take by weighing 48.0wt%Fe
2O
3, 29.5wt%MgO, 18.0wt%ZnO 0.5wt%Mn
3O
4, 3.5wt%CuO is through the strong machine uniform mixing that mixes, blended time 25min mixes back material powder and directly is controlled at 1.7 μ m.Above-mentioned mixed uniformly material powder is added the ball material that 15% moisture content is made diameter 6mm intensity 70N through making ball.To burn till in advance in the rotary kiln of above-mentioned ball material under 1050 ℃ temperature, it is that 1.3 μ m, viscosity are that 900mpa.s, proportion are 2.10g/cm that the ball material after the above-mentioned pre-burning is become to have granularity through one-level, secondary sand milling by 90: 30 material-water ratio examples
3Water content is 34% slip; The time one-level 50min that pulverizes, secondary 50min.The PVA of the interpolation of the slurry after the above-mentioned pulverizing 9.5% is made the slip that can spray through a mixing bowl stirring; The time 2h that stirs.The spray-dried tower of slip after the above-mentioned stirring made to have loose specific weight be 1.40g/cm
3, water content is that 0.25% particle diameter is 0.1~0.3 equally distributed runny spherical particle.The Zinic stearas of the particulate material after the above-mentioned spraying and 0.4% is mixed through mixer; The particulate material of the time 25min of batch mixing after with above-mentioned batch mixing is pressed into desired shape through the moulding mouldenpress, compact density 2.80g/cm
3Blank, be to generate the FERRITE CORE that every performance parameters conformance with standard requires after 1020 ℃ and soaking time are the 4h sintering with described blank through kiln temperature.
Embodiment 3
Take by weighing 48.2wt%Fe
2O
3, 26.0wt%MgO, 20.9wt%ZnO 0.6wt%Mn
3O
4, 3.7wt%CuO is through the strong machine uniform mixing that mixes, blended time 30min mixes back material powder and directly is controlled at 1.7 μ m.Above-mentioned mixed uniformly material powder is added the ball material that 20% moisture content is made diameter 6mm intensity 70N through making ball.To burn till in advance in the rotary kiln of above-mentioned ball material under 1050 ℃ temperature, it is that 1.2 μ m, viscosity are that 1500mpa.s, proportion are 1.90g/cm that the ball material after the above-mentioned pre-burning is become to have granularity through one-level, secondary sand milling by 80: 20 material-water ratio examples
3Water content is 37% slip; The time one-level 50min that pulverizes, secondary 50min.The PVA of the interpolation of the slurry after the above-mentioned pulverizing 9.5% is made the slip that can spray through a mixing bowl stirring; The time 2h that stirs.The spray-dried tower of slip after the above-mentioned stirring made to have loose specific weight be 1.25g/cm
3, water content is that 0.40% particle diameter is 0.1~0.3 equally distributed runny spherical particle.The Zinic stearas of the particulate material after the above-mentioned spraying and 0.4% is mixed through mixer; The particulate material of the time 20min of batch mixing after with above-mentioned batch mixing is pressed into desired shape through the moulding mouldenpress, compact density 2.80g/cm
3Blank, be to generate the FERRITE CORE that every performance parameters conformance with standard requires after 1020 ℃ and soaking time are the 4h sintering with described blank through kiln temperature.
Embodiment 4
Take by weighing 48.7wt%Fe
2O
3, 25.5wt%MgO, 20.9wt%ZnO 0.5wt%Mn
3O
4, 4.2wt%CuO is through the strong machine uniform mixing that mixes, blended time 30min mixes back material powder and directly is controlled at 1.65 μ m.Above-mentioned mixed uniformly material powder is added the ball material that 14% moisture content is made diameter 6mm intensity 70N through making ball.To burn till in advance in the rotary kiln of above-mentioned ball material under 1050 ℃ temperature, it is that 1.4 μ m, viscosity are that 800mpa.s, proportion are 2.00g/cm that the ball material after the above-mentioned pre-burning is become to have granularity through one-level, secondary sand milling by 400: 120 material-water ratio examples
3Water content is 33% slip; The time one-level 50min that pulverizes, secondary 50min.The PVA of the interpolation of the slurry after the above-mentioned pulverizing 9.5% is made the slip that can spray through a mixing bowl stirring; The time 2h that stirs.The spray-dried tower of slip after the above-mentioned stirring made to have loose specific weight be 1.28g/cm
3, water content is that 0.28% particle diameter is 0.1~0.3 equally distributed runny spherical particle.The Zinic stearas of the particulate material after the above-mentioned spraying and 0.4% is mixed through mixer; The particulate material of the time 18min of batch mixing after with above-mentioned batch mixing is pressed into desired shape through the moulding mouldenpress, compact density 2.80g/cm
3Blank, be to generate the FERRITE CORE that every performance parameters conformance with standard requires after 1220 ℃ and soaking time are the 4h sintering with described blank through kiln temperature.
Embodiment 5
Take by weighing 49.2wt%Fe
2O
3, 26.0wt%MgO, 20wt%ZnO 1.2wt%Mn
3O
4, 3.6wt%CuO is through the strong machine uniform mixing that mixes, blended time 30min mixes back material powder and directly is controlled at 1.60 μ m.Above-mentioned mixed uniformly material powder is added the ball material that 18% moisture content is made diameter 6mm intensity 70N through making ball.To burn till in advance in the rotary kiln of above-mentioned ball material under 1050 ℃ temperature, it is that 1.3 μ m, viscosity are that 1100mpa.s, proportion are 1.95g/cm that the ball material after the above-mentioned pre-burning is become to have granularity through one-level, secondary sand milling by 80: 25 material-water ratio examples
3Water content is 34% slip; The time one-level 50min that pulverizes, secondary 50min.The PVA of the interpolation of the slurry after the above-mentioned pulverizing 9.5% is made the slip that can spray through a mixing bowl stirring; The time 2h that stirs.The spray-dried tower of slip after the above-mentioned stirring made to have loose specific weight be 1.32g/cm
3, water content is that 0.32% particle diameter is 0.1~0.3 equally distributed runny spherical particle.The Zinic stearas of the particulate material after the above-mentioned spraying and 0.4% is mixed through mixer; The particulate material of the time 22min of batch mixing after with above-mentioned batch mixing is pressed into desired shape through the moulding mouldenpress, compact density 2.80g/cm
3Blank, be to generate the FERRITE CORE that every performance parameters conformance with standard requires after 1220 ℃ and soaking time are the 4h sintering with described blank through kiln temperature.