CN102173767A - Magnetic material for photovoltaic inverter - Google Patents

Magnetic material for photovoltaic inverter Download PDF

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Publication number
CN102173767A
CN102173767A CN2011100086367A CN201110008636A CN102173767A CN 102173767 A CN102173767 A CN 102173767A CN 2011100086367 A CN2011100086367 A CN 2011100086367A CN 201110008636 A CN201110008636 A CN 201110008636A CN 102173767 A CN102173767 A CN 102173767A
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ferrite
principal constituent
photovoltaic
magneticsubstance
converter
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CN102173767B (en
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陆明岳
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Shandong Zhongrui Electronics Co ltd
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LINYI ZHONGRUI ELECTRONICS CO Ltd
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Priority to CN201110008636.7A priority Critical patent/CN102173767B/en
Priority to PCT/CN2011/000804 priority patent/WO2012097482A1/en
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Abstract

The invention discloses a magnetic material for a photovoltaic inverter. The magnetic material is characterized by being a MnZn ferrite material and comprising 51.5 to 57.5 molar percent of Fe2O3, 4.5 to 15.5 molar percent of ZnO and the balance of MnO which serve as main components and 0.05 to 0.15 weight percent of Eu2O3 and 0.008 to 0.10 weight percent of Al2O3 which serve as auxiliary components, and one or more of 0 to 0.15 weight percent of CaO, 0 to 0.035 weight percent of SiO2, 0 to 0.50 weight percent of MgO, 0 to 0.06 weight percent of Nb2O5 and 0 to 0.055 weight percent of ZrO2 which also serve as auxiliary components. The magnetic material is characterized in that: the thermal expansion coefficient is less than 8*10<-6>; the magnetostrictive coefficient is less than -0.3*10<-6>; the magnetic conductivity at the temperature of 25 DEG C is 2,100+/-25 percent; the saturation magnetic flux density at the temperature of 25 DEG C is more than 530mT and the saturation magnetic flux density at the temperature of 100 DEG C is more than 430mT; and at the temperature of 100 DEG C, under the conditions of 25KHz*200mT and 100KHz*200mT, the energy consumption is less than 65mW/cm<3> and 320mW/cm<3> respectively.

Description

A kind of photovoltaic DC-to-AC converter magneticsubstance
Technical field
The present invention relates to a kind of photovoltaic DC-to-AC converter magneticsubstance and preparation method thereof.
Background technology
In recent years, along with the enhancing of people's environmental consciousness, more and more for the concern of renewable energy source.In all kinds of renewable energy sources such as sun power, wind energy, tidal energy, sun power becomes people's first-selection.Solar photovoltaic generation system is made of jointly solar panel, charge controller, invertor and store battery etc.In the solar photovoltaic generation system, photovoltaic DC-to-AC converter is the key component of whole solar energy system, is the core of photovoltaic system, and sun power transforms by cell panel and produces electric energy.But, the electric power that cell panel transformed is direct current, will really become a just bound special equipment---the invertor of the spendable alternating-current of most occasions, the function of invertor is that direct current is converted to alternating-current, and photovoltaic DC-to-AC converter is the photovoltaic system core devices.The improvement of invertor performance is for the reliability, the efficient that improve system, improve system life-span, reduce cost most important.
Inverter can be divided into power frequency conversion and high frequency conversion by mapping mode, but any mapping mode all needs to use magneticsubstance.Adopt in the main power circuit of Industrial Frequency Transformer at invertor, the electromagnetic component that plays isolation and power change action is an Industrial Frequency Transformer, because operating frequency is lower, have only 50 or 60Hz, the most cold-rolled orientation silicon steel sheet closed assemblies that adopt of magneticsubstance form, therefore, the Industrial Frequency Transformer volume is big, Heavy Weight; Adopt in the high-frequency transformer insulating main power circuit at invertor, the electromagnetic component that plays isolation and power change action is a high-frequency transformer, early stage circuit work frequency is between 15～20KHz, because cold-rolled orientation silicon steel sheet power loss (abbreviation power consumption) under this frequency is excessive, can not use, and adopt magnetic materials such as the Fe-Si-Al magnetic heart or MnZn soft magnetic ferrite to manufacture magnetic core; But along with the invertor inversion transformation technique just develops towards the direction that frequency is higher, more powerful, efficient is higher, volume is littler, circuit work frequency improves constantly, the power consumption of the Fe-Si-Al magnetic heart increases along with the raising of operating frequency is rapid and can't use, can only adopt the MnZn ferrite material in this case, this is that another outstanding advantage of MnZn Ferrite Material is that its cost will be significantly less than the Fe-Si-Al magnetic heart because the MnZn ferrite has a lower power consumption under high frequency.
Because the singularity of photovoltaic generating system, DC stacked composition is more in the invertor pull up circuit, and the magneticstrength of working simultaneously is bigger, is not that common MnZn ferrite material can both meet the demands therefore.The MnZn ferrite material that works in the photovoltaic DC-to-AC converter must have electromagnetic performance preferably, i.e. high-frequency and low-consumption, and its dc superposition characteristic is good simultaneously.
In addition, for the high-power photovoltaic generating system more than the 1KW,, often need to use large-sized MnZn Ferrite Material magnetic core because transfer power is bigger, the weight of these magnetic cores is all more than 1Kg, even reach 16Kg, owing to be operated under the high frequency high field, the magnetic core temperature is higher, for guaranteeing the safe and reliable work of invertor, require magnetic core to have lower thermal expansivity, otherwise be easy to winding or skeleton are burst during large-sized ferrite core expanded by heating, thus can't works better; Another aspect that can't ignore is, it is more obvious that large-sized ferrite core is operated under the high frequency high field its magnetostriction storage effect, can influence the reliability and stability of invertor work greatly, simultaneously electrical equipment is on every side produced tangible electromagnetic interference, influence the works better of other electronics.Therefore, require the magnetostriction coefficient of Ferrite Material low as much as possible.
In sum, the MnZn Ferrite Material that is used for photovoltaic generating system, the characteristic that must have following two aspects simultaneously: be that thermal expansivity and magnetostriction coefficient are low as much as possible on the one hand, require on the other hand that power consumption is lower under the high frequency high field, dc superposition characteristic is good.This be higher than far away general electronic circuit transformer (for example: switching mode power supply transformer) and reactance coil to the requirement of MnZn ferrite material, this is because general electronic circuit transformer general size is less, transfer power is lower, usually arrive between several hectowatts at several watts, therefore, general electronic circuit transformer has only the requirement of above-mentioned second aspect usually to the MnZn ferrite material.
People are reducing the power consumption of material, are improving aspect such as dc superposition characteristic and done a large amount of work, in Chinese invention patent ZL 01112082.7, announced content by control P element, and the improvement sintering process, obtain the method for Switch Power Transformer with the reduce power consumption Ferrite Material;
In Chinese invention patent ZL 00126316.1, announced by introducing SiO 2, CaO, NiO and ZrO 2Deng, thereby obtained to be used for the Ferrite Material with reduce power consumption and high saturation magnetic flux density of supply transformer.
Above-mentioned these patents mainly are in order to reduce switching mode power supply transformer or reactance coil with MnZn Ferrite Material power consumption and improve its saturation magnetic flux density, and to how reducing magnetic core thermal expansivity and magnetostriction coefficient do not have substantially to consider, this is because general electronic circuit transformer general size is less, transfer power is lower, usually arrive between several hectowatts at several watts, therefore, general electronic circuit transformer is not considered usually to the thermal expansivity and the magnetostriction coefficient of MnZn ferrite material.
Be used at present photovoltaic DC-to-AC converter the MnZn Ferrite Material its roughly performance be: thermal expansivity is about 12 * 10 -6Magnetostriction coefficient is about-0.6 * 10 -6Magnetic permeability under 25 ℃ is 2300 ± 25%; Saturation magnetic flux density under 25 ℃ and 100 ℃ of conditions is respectively 510mT and 400mT; Power consumption under 100 ℃, 25KHz * 200mT and 100KHz * 200mT condition is respectively 70mW/cm 3And 420mW/cm 3It still is proper that this material is worked below 25KHz in frequency, but along with inversion transformation technique develops towards the direction that frequency is higher, more powerful, efficient is higher, volume is littler, invertor needs the better MnZn Ferrite Material of over-all properties.
The present invention just is being based on this present situation and is proposing, and its purpose is, provide had low thermal coefficient of expansion and low magnetostriction coefficient and high-frequency and low-consumption simultaneously, the magneticsubstance and the manufacture method thereof of the excellent performance of high saturation magnetic flux density.
Summary of the invention
The present invention seeks to: the magneticsubstance and the preparation method of the excellent performance of a kind of photovoltaic DC-to-AC converter usefulness low thermal coefficient of expansion and low magnetostriction coefficient, high-frequency and low-consumption, high saturation magnetic flux density are proposed.
Technical scheme of the present invention is: a kind of photovoltaic DC-to-AC converter magneticsubstance is characterized in that: this magneticsubstance is a kind of MnZn ferrite, comprises principal constituent and ancillary component, and principal constituent comprises and is scaled (mol ratio): Fe 2O 3: 51.5～57.5mol%, ZnO:4.5～15.5mol%, surplus is MnO; Ancillary component comprises Eu 2O 3, Al 2O 3Also comprise other ancillary components CaO, SiO in addition 2, MgO, Nb 2O 5And ZrO 2In more than a kind or a kind, described ancillary component is with respect to principal constituent total amount content following (weight ratio): Eu 2O 3: 0.05～0.15wt%, Al 2O 3: 0.008～0.10wt%, CaO:0～0.15wt%, SiO 2: 0～0.035wt%, MgO:0～0.50wt%, Nb 2O 5: 0～0.06wt%, ZrO 2: 0～0.055wt%.
Below, the qualification reason of the numerical range of principal constituent of the present invention and ancillary component is described.
Work as Fe 2O 3Composition less than 51.5mol%, or the composition of ZnO is difficult to obtain higher saturation magnetic flux density during greater than 15.5mol%.Work as Fe 2O 3Composition greater than 57.5mol%, although can obtain higher saturation magnetic flux density, power consumption obviously strengthens.In addition, when the composition of ZnO during less than 4.5mol%, the product power consumption also obviously strengthens.
The ferrite that the present invention relates to as ancillary component, adds the Eu of 0.01～0.15wt% 2O 3Al with 0.008～0.10wt% 2O 3Be in order to obtain lower thermal expansivity and lower magnetostriction coefficient.Work as Eu 2O 3Amount less than 0.05wt%, or Al 2O 3Amount during less than 0.008wt%, to reducing material coefficient of thermal expansion coefficient and magnetostriction coefficient DeGrain.And work as Eu 2O 3Amount greater than 0.15wt%, or Al 2O 3Amount during greater than 0.10wt%, can cause the ferrite power consumption obviously to rise, saturation magnetic flux density descends simultaneously.In addition, Eu 2O 3And Al 2O 3Need to add simultaneously, add Al separately 2O 3The time, the ferrite power consumption is obviously risen, and saturation magnetic flux density descend; Add Eu separately 2O 3The time, although saturation magnetic flux density is obviously risen, the ferrite power consumption descends, and reduces material coefficient of thermal expansion coefficient and magnetostriction coefficient effect not clearly.
The ferrite that the present invention relates to is as other ancillary components CaO, SiO 2, MgO, Nb 2O 5And ZrO 2, the needs adding wherein more than at least a kind or a kind, adds the SiO of 0～0.15wt%CaO, 0～0.035wt% 2, mainly be for when ferrite sintered, on ferritic grain boundary, form resistive formation, thereby reach the purpose that reduces the ferrite power consumption.When the amount of CaO during greater than 0.15wt%, or SiO 2Amount during greater than 0.035wt%, will make ferrite when sintering, produce discontinuous grain growth, thereby ferritic power consumption is sharply risen; The MgO, the Nb of 0～0.06wt% that add 0～0.50wt% 2O 5, 0～0.055wt% ZrO 2, can reduce ferritic sintering temperature, reduce ferritic power consumption, and improve ferritic saturation magnetic flux density.When the amount of MgO greater than 0.5wt%, Nb 2O 5Amount greater than 0.06wt%, ZrO 2Amount during greater than 0.055wt%, cause ferrite crystal grains misgrowth easily, thereby the tendency that worsens ferrite performance arranged.
A kind of photovoltaic DC-to-AC converter of the present invention is characterized in that may further comprise the steps: 1) with principal constituent Fe with magneticsubstance and preparation method 2O 3, Mn 3O 4, ZnO adds and to grind in the sand mill be added with deionized water in advance or the ball mill and then through spray drying granulation, 850～950 ℃ of pre-burnings in rotary kiln or box-type furnace, obtain ferrite prefiring material; 2) ferrite prefiring material is added in the sand mill that is added with deionized water in advance or the ball mill with ancillary component grind, obtain ferrite slurry, add 10% PVA solution (concentration is 10%) subsequently and carry out spray drying granulation, obtain ferrite powder; 3) ferrite powder being obtained density through the press compacting is 3.0 ± 0.2g/cm 3The ferrite blank, the ferrite blank can be a different shape.With blank at vacuum sintering furnace or bell jar stove or N 2In the protection pushed bat kiln, in oxygen partial pressure is 1～10% balanced atmosphere, 1280～1380 ℃ of sintering temperatures 2～5 hours.
By such manufacture method, just can easily make magneticsubstance of the present invention.
The invention has the beneficial effects as follows: obtained the magneticsubstance of a kind of photovoltaic DC-to-AC converter with the excellent performance of high-frequency and low-consumption, high saturation magnetic flux density, low thermal coefficient of expansion and low magnetostriction coefficient.Satisfied the active demand that invertor further develops towards the direction that frequency is higher, more powerful, efficient is higher, volume is littler.
Utilize the feature of the magneticsubstance of the inventive method preparation to be: thermal expansivity is less than 8 * 10 -6Magnetostriction coefficient is less than-0.3 * 10 -6Magnetic permeability under 25 ℃ is 2100 ± 25%; Saturation magnetic flux density under 25 ℃ and 100 ℃ of conditions is respectively greater than 530mT and 430mT; Power consumption under 100 ℃, 25KHz * 200mT and 100KHz * 200mT condition is respectively less than 65mW/cm 3And 320mW/cm 3
Embodiment
Below, based on embodiment explanation the present invention.
1) starting material weighing: take by weighing starting material by the principal constituent prescription, starting material are Fe 2O 3, ZnO and Mn 3O4.The principal constituent prescription comprises and is scaled (mol ratio): Fe 2O 3: 51.5～57.5mol%, ZnO:4.5～15.5mol%, surplus is MnO.
2) sand milling: load weighted starting material are put into sand mill, carry out the wet type sand milling, slip water content 30%～50%, 0.5～1.0 hour sand milling time;
3) spray drying granulation: in the starting material slip, add about 10%PVA solution (concentration is 10%), carry out spray drying granulation one time;
4) pre-burning: a spray drying granulation powder is carried out pre-burning by rotary kiln, and burning temperature is 850～950 ℃;
5) ancillary component adds: add following ancillary component, ancillary component is with respect to principal constituent total amount content following (weight percent): Eu 2O 3: 0.05～0.15wt%, Al 2O 3: 0.008～0.10wt%, in addition, also need add CaO:0～0.15wt%, SiO again 2: 0～0.035wt%, MgO:0～0.50wt%, Nb 2O 5: 0～0.06wt%, ZrO 2: among 0～0.055wt% more than a kind or a kind.
6) secondary sand milling: ferrite prefiring material and above-mentioned ancillary component are put into sand mill, carry out the wet type sand milling, slip water content 30%～50%, 1.5～2.5 hours sand milling time;
7) secondary spray drying granulation:
In ferrite slurry, add about 10%PVA solution (concentration is 10%), carry out the secondary spray drying granulation;
8) moulding: it is 3.0 ± 0.2g/cm that secondary spray drying granulation ferrite powder is pressed into density 3The ferrite blank;
9) sintering: with blank at vacuum sintering furnace or bell jar stove or N 2In the protection pushed bat kiln, by the control of following sintering temperature curve and atmosphere: from room temperature to 600 ℃, this is the binder removal stage, and it is comparatively mild to heat up, and it is abundant that this helps binder removal, 50～150 ℃/hr of temperature rise rate, air atmosphere; After binder removal finished, temperature rise rate was brought up to 150～300 ℃/hr, air atmosphere; 1280～1380 ℃ of sintering temperatures are incubated 2～5 hours, and the sintering equilibrium oxygen partial pres-sure is 1～10%; Insulation finishes to about 1100 ℃ temperature-fall period, and Control for Oxygen Content is 0.05～2%, 100～150 ℃/hr of rate of temperature fall; Since 1100 ℃, fast cooling arrives room temperature, 150～250 ℃/h of rate of temperature fall, and Control for Oxygen Content is below 0.01%.
Above-mentioned prescription and preparation method can make magneticsubstance reach performance perameter of the present invention fully.The present invention will be further described below in conjunction with specific embodiment, yet the present invention is not limited to these facility examples.For further specifying beneficial effect of the present invention, comparative example 1 and comparative example 2 have been enumerated.
Wherein: the MnZn Ferrite Material of comparative example 1 correspondence is mainly used in switching mode power supply transformer or reactance coil is used relevant field, although the ferrite power consumption is less, its thermal expansivity and magnetostriction coefficient are bigger, and thermal expansivity is 15.5 * 10 -6, magnetostriction coefficient is about-1.0 * 10 -6, but, be not suitable for making large size superpower ferrite core because thermal expansivity and magnetostriction coefficient are bigger, in addition, its saturation magnetic flux density is not high enough, thereby its dc superposition characteristic is good inadequately;
The MnZn Ferrite Material of comparative example 2 correspondences, because of thermal expansivity and magnetostriction coefficient reduce to some extent, although still can be as the photovoltaic DC-to-AC converter Ferrite Material at present, but because its power consumption is higher, saturation magnetic flux density is not high enough, its dc superposition characteristic is good inadequately, thereby can not satisfy the demand that photovoltaic DC-to-AC converter further develops towards the direction that frequency is higher, more powerful, efficient is higher, volume is littler.
Table 1 is listed the maximum current that the ferrite core size, weight, through-put power and the permission that are used for photovoltaic DC-to-AC converter in embodiment 1 and the comparative example 2 passed through.Although both inductance values are identical, inductance value is about 1.00mH, but core size and weight are significantly less than comparative example 2 among the embodiment 1, wherein, embodiment 1 core size is: UU120 * 160 * 20, long 160mm, wide 120mm, thick 20mm, weight is 1.24Kg, core size is in the comparative example 2: UU120 * 310 * 20mm, and long 310mm, wide 120mm, thick 20mm, weight is 2.11Kg.Because to have the high frequency power consumption lower and saturation magnetic flux density is higher for Ferrite Material among the embodiment 1, thereby its dc superposition characteristic obviously is better than comparative example 2, the maximum direct current that magnetic core allows to pass through among the embodiment 1 is that 23A is (when feeding direct current in the inducer, inductance value can descend, its inductance value descend 10% pairing galvanic current be called allow the maximum direct current passed through), and the maximum direct current that magnetic core allows to pass through in the comparative example 2 is 20A, thereby embodiment 1 magnetic core can be worked under higher magneticflux-density, under the situation that volume and weight reduces, can transmit essentially identical power, embodiment 1 peak power output 3.23KW wherein, comparative example 2 maximum transmission power 3.14KW.
Table 2 is listed two kinds of dc superposition characteristics that are used for the ferrite core of photovoltaic DC-to-AC converter in embodiment 1 and the comparative example 2, the magnetic core inductance is when feeding 23A among the embodiment 1, inductance value descends 10%, the magnetic core inductance is when feeding 20A in the comparative example 2, inductance value descends 10%, and obviously the magnetic core dc superposition characteristic is better among the embodiment 1.
A kind of photovoltaic DC-to-AC converter magneticsubstance of the present invention, be a kind of have more low thermal coefficient of expansion and more the low magnetostriction coefficient have the high-frequency and low-consumption and the MnZn Ferrite Material of the excellent performance of high saturation magnetic flux density more simultaneously, can satisfy the demand that photovoltaic DC-to-AC converter further develops towards the direction that frequency is higher, more powerful, efficient is higher, volume is littler fully.
Embodiment 1: by principal constituent prescription (mol ratio): Fe 2O 3: 54.6mol%, ZnO:10.8mol%, MnO:34.6mol% takes by weighing Fe 2O 3, Mn 3O 4And ZnO.Drop in the sand mill that is added with deionized water in advance and grind, slip water content 40%, 0.5 hour sand milling time, behind a mist projection granulating, electricity consumption heating revolving kiln carries out pre-burning under 850 degree with slip.Pre-subsequently imitation frosted glass input is added with the deionized water sand mill in advance and carries out the secondary sand milling, slip water content 30%, and described relatively principal constituent content in the sand grinding process adds Eu 2O 3: 0.06wt%, Al 2O 3: 0.09wt%, in addition, also add CaO:0.08wt%, SiO 2: 0.005wt%, MgO:0.03wt%, Nb 2O 5: 0.02wt%, 1.5 hours sand milling time, the median size of control sand milling is 1.1 ± 0.3 μ m.Carry out the secondary spraying at last and obtain MnZn ferrite particle material powder.Get this particulate material moulding compacting φ 25mm * φ 15mm * 7.5mm, density is approximately 3.0 ± 0.2g/cm 3Annulus.
In addition, for studying its practical situations on photovoltaic DC-to-AC converter, be pressed into U type large size magnetic core, two magnetic cores are spliced to form an approximate square toroidal core (keeping certain air gap) behind the sintering, be of a size of: UU120 * 160 * 20, long 160mm, wide 120mm, thick 20mm, weight is 1.24Kg.Two groups of each 60 circle diameters of coiling thereon are the insulated copper wire winding of 3mm, measure its inductance dc superposition characteristic, and output rating.Table 1 illustrates measuring result, and inductance value is 1.01mH, peak power output 3.23KW, and the maximum direct current that allows to pass through is 23A.
Sintering is by the control of following sintering temperature curve and atmosphere behind the sintering: from room temperature to 600 ℃, this is the binder removal stage, and it is comparatively mild to heat up, and it is abundant that this helps binder removal, 50～150 ℃/hr of temperature rise rate, air atmosphere; After binder removal finished, temperature rise rate was brought up to 150～300 ℃/hr, air atmosphere; 1335 ℃ of sintering temperatures are incubated 3 hours, and equilibrium oxygen partial pres-sure is 8%; Finish to about 1100 ℃ temperature-fall period from insulation, Control for Oxygen Content is 0.05～2%, 100～150 ℃/hr of rate of temperature fall; Since 1100 ℃, fast cooling arrives room temperature, 150～250 ℃/hr of rate of temperature fall, and Control for Oxygen Content is below 0.01%.
The magnet ring performance that obtains is: thermal expansivity is 7.9 * 10 -6Magnetostriction coefficient is about-0.29 * 10 -6Magnetic permeability under 25 ℃ is 2250; Saturation magnetic flux density under 25 ℃ and 100 ℃ of conditions is respectively 545mT and 445mT; Power consumption under 100 ℃, 25KHz * 200mT and 100KHz * 200mT condition is respectively 58mW/cm 3And 295mW/cm 3
Embodiment 2: by principal constituent prescription (mol ratio): Fe 2O 3: 53.5mol%, ZnO:12.5mol%, MnO:34.0mol% takes by weighing Fe 2O 3, Mn 3O 4And ZnO.Drop in the sand mill that is added with deionized water in advance and grind, slip water content 40%, 0.5 hour sand milling time, behind a mist projection granulating, electricity consumption heating revolving kiln carries out pre-burning under 900 degree with slip.Pre-subsequently imitation frosted glass input is added with the deionized water sand mill in advance and carries out the secondary sand milling, slip water content 30%, and described relatively principal constituent content in the sand grinding process adds Eu 2O 3: 0.10wt%, Al 2O 3: 0.05wt%, CaO:0.03wt%, SiO 2: 0.01wt%, in addition, also add CaO:0.03wt%, SiO 2: 0.01wt%, MgO:0.10wt%, Nb 2O 5: 0.03wt%, ZrO 2: 0.03wt%, 1.5 hours sand milling time, the median size of control sand milling is 1.1 ± 0.3 μ m.Carry out the secondary spraying at last and obtain MnZn ferrite particle material powder.Get this particulate material moulding compacting φ 25mm * φ 15mm * 7.5mm, density is approximately 3.0 ± 0.2g/cm 3Annulus, sintering is by the control of following sintering temperature curve and atmosphere: from room temperature to 600 ℃, this is the binder removal stage, and it is comparatively mild to heat up, and it is abundant that this helps binder removal, 50～150 ℃/hr of temperature rise rate, air atmosphere; After binder removal finished, temperature rise rate was brought up to 150～300 ℃/hr, air atmosphere; 1325 ℃ of sintering temperatures are incubated 3 hours, and equilibrium oxygen partial pres-sure is 5%; Finish to about 1100 ℃ temperature-fall period from insulation, Control for Oxygen Content is 0.05～2%, 100～150 ℃/hr of rate of temperature fall; Since 1100 ℃, fast cooling arrives room temperature, 150～250 ℃/h of rate of temperature fall, and Control for Oxygen Content is below 0.01%.
The magnet ring performance that obtains is: thermal expansivity is 7.5 * 10 -6Magnetostriction coefficient is about-0.24 * 10 -6Magnetic permeability under 25 ℃ is 2350; Saturation magnetic flux density under 25 ℃ and 100 ℃ of conditions is respectively 540mT and 438mT; Power consumption under 100 ℃, 25KHz * 200mT and 100KHz * 200mT condition is respectively 55mW/cm 3And 300mW/cm 3
Embodiment 3: by principal constituent prescription (mol ratio): Fe 2O 3: 51.9mol%, ZnO:15.1mol%, MnO:33.0mol% takes by weighing Fe 2O 3, Mn 3O 4And ZnO.Drop in the sand mill that is added with deionized water in advance and grind, slip water content 40%, 0.5 hour sand milling time, behind a mist projection granulating, electricity consumption heating revolving kiln carries out pre-burning under 870 degree with slip.Pre-subsequently imitation frosted glass input is added with the deionized water sand mill in advance and carries out the secondary sand milling, slip water content 30%, and described relatively principal constituent content in the sand grinding process adds Eu 2O 3: 0.15wt%, Al 2O 3: 0.03wt%, in addition, also add CaO:0.04wt%, SiO 2: 0.015wt%, Nb 2O 5: 0.02wt%, ZrO 2: 0.03wt%, 1.5 hours sand milling time, the median size of control sand milling is 1.1 ± 0.3 μ m.Carry out the secondary spraying at last and obtain MnZn ferrite particle material powder.Get this particulate material moulding compacting φ 25mm * φ 15mm * 7.5mm, density is approximately 3.0 ± 0.2g/cm 3Annulus, sintering is by the control of following sintering temperature curve and atmosphere: from room temperature to 600 ℃, this is the binder removal stage, and it is comparatively mild to heat up, and it is abundant that this helps binder removal, 50～150 ℃/hr of temperature rise rate, air atmosphere; After binder removal finished, temperature rise rate was brought up to 150～300 ℃/hr, air atmosphere; 1315 ℃ of sintering temperatures are incubated 3 hours, and equilibrium oxygen partial pres-sure is 3%; Finish to about 1100 ℃ temperature-fall period from insulation, Control for Oxygen Content is 0.05～1.5%, 100～150 ℃/hr of rate of temperature fall; Since 1100 ℃, fast cooling arrives room temperature, 150～250 ℃/h of rate of temperature fall, and Control for Oxygen Content is below 0.01%.
The magnet ring performance that obtains is: thermal expansivity is 7.0 * 10 -6Magnetostriction coefficient is about-0.20 * 10 -6Magnetic permeability under 25 ℃ is 2180; Saturation magnetic flux density under 25 ℃ and 100 ℃ of conditions is respectively 530mT and 430mT; Power consumption under 100 ℃, 25KHz * 200mT and 100KHz * 200mT condition is respectively 61mW/cm 3And 305mW/cm 3
Embodiment 4: by principal constituent prescription (mol ratio): Fe 2O 3: 55.3mol%, ZnO:9.5mol%, MnO:35.2mol% takes by weighing Fe 2O 3, Mn 3O 4And ZnO.Drop in the sand mill that is added with deionized water in advance and grind, slip water content 40%, 0.5 hour sand milling time, behind a mist projection granulating, electricity consumption heating revolving kiln carries out pre-burning under 920 degree with slip.Pre-subsequently imitation frosted glass input is added with the deionized water sand mill in advance and carries out the secondary sand milling, slip water content 30%, and described relatively principal constituent content in the sand grinding process adds Eu 2O 3: 0.10wt%, Al 2O 3: 0.06wt%, in addition, also add CaO:0.06wt%, SiO 2: 0.010wt%, MgO:0.30wt%, Nb 2O 5: 0.06wt%, 2.0 hours sand milling time, the median size of control sand milling is 1.1 ± 0.3 μ m.Carry out the secondary spraying at last and obtain MnZn ferrite particle material powder.Get this particulate material moulding compacting φ 25mm * φ 15mm * 7.5mm, density is approximately 3.0 ± 0.2g/cm 3Annulus, sintering is by the control of following sintering temperature curve and atmosphere: from room temperature to 600 ℃, this is the binder removal stage, and it is comparatively mild to heat up, and it is abundant that this helps binder removal, 50～150 ℃/hr of temperature rise rate, air atmosphere; After binder removal finished, temperature rise rate was brought up to 150～300 ℃/hr, air atmosphere; 1355 ℃ of sintering temperatures are incubated 4 hours, and equilibrium oxygen partial pres-sure is 2%; Finish to about 1100 ℃ temperature-fall period from insulation, Control for Oxygen Content is 0.05～1%, 100～150 ℃/hr of rate of temperature fall; Since 1100 ℃, fast cooling arrives room temperature, 150～250 ℃/h of rate of temperature fall, and Control for Oxygen Content is below 0.01%.
The magnet ring performance that obtains is: thermal expansivity is 7.6 * 10 -6Magnetostriction coefficient is about-0.25 * 10 -6Magnetic permeability under 25 ℃ is 2050; Saturation magnetic flux density under 25 ℃ and 100 ℃ of conditions is respectively 550mT and 435mT; Power consumption under 100 ℃, 25KHz * 200mT and 100KHz * 200mT condition is respectively 63mW/cm 3And 312mW/cm 3
Embodiment 5: by principal constituent prescription (mol ratio): Fe 2O 3: 57.0mol%, ZnO:5.0mol%, MnO:38.0mol% takes by weighing Fe 2O 3, Mn 3O 4And ZnO.Drop in the sand mill that is added with deionized water in advance and grind, slip water content 40%, 0.5 hour sand milling time, behind a mist projection granulating, electricity consumption heating revolving kiln carries out pre-burning under 950 degree with slip.Pre-subsequently imitation frosted glass input is added with the deionized water sand mill in advance and carries out the secondary sand milling, slip water content 30%, and described relatively principal constituent content in the sand grinding process adds Eu 2O 3: 0.15wt%, Al 2O 3: 0.08wt%, in addition, also add CaO:0.10wt%, SiO 2: 0.015wt%, MgO:0.50wt%, ZrO 2: 0.055wt%, 2.0 hours sand milling time, the median size of control sand milling is 1.1 ± 0.3 μ m.Carry out the secondary spraying at last and obtain MnZn ferrite particle material powder.Get this particulate material moulding compacting φ 25mm * φ 15mm * 7.5mm, density is approximately 3.0 ± 0.2g/cm 3Annulus, sintering is by the control of following sintering temperature curve and atmosphere: from room temperature to 600 ℃, this is the binder removal stage, and it is comparatively mild to heat up, and it is abundant that this helps binder removal, 50～150 ℃/hr of temperature rise rate, air atmosphere; After binder removal finished, temperature rise rate was brought up to 150～300 ℃/hr, air atmosphere; 1370 ℃ of sintering temperatures are incubated 5 hours, and equilibrium oxygen partial pres-sure is 1%; Finish to about 1100 ℃ temperature-fall period from insulation, Control for Oxygen Content is 0.05～2%, 100～150 ℃/hr of rate of temperature fall; Since 1100 ℃, fast cooling arrives room temperature, 150～250 ℃/h of rate of temperature fall, and Control for Oxygen Content is below 0.01%.
The magnet ring performance that obtains is: thermal expansivity is 7.4 * 10 -6Magnetostriction coefficient is about-0.24 * 10 -6Magnetic permeability under 25 ℃ is 1980; Saturation magnetic flux density under 25 ℃ and 100 ℃ of conditions is respectively 560mT and 460mT; Power consumption under 100 ℃, 25KHz * 200mT and 100KHz * 200mT condition is respectively 65mW/cm 3And 320mW/cm 3
Comparative example 1: by principal constituent prescription (mol ratio): Fe 2O 3: 53.5mol%, ZnO:12.5mol%, MnO:34.0mol% takes by weighing Fe 2O 3, Mn 3O 4And ZnO.Drop in the sand mill that is added with deionized water in advance and grind, slip water content 40%, 0.5 hour sand milling time, behind a mist projection granulating, electricity consumption heating revolving kiln carries out pre-burning under 900 degree with slip.Pre-subsequently imitation frosted glass input is added with the deionized water sand mill in advance and carries out the secondary sand milling, slip water content 30%, and described relatively principal constituent content in the sand grinding process adds CaO:0.03wt%, SiO 2: 0.01wt%, MgO:0.10wt%, Nb 2O 5: 0.03wt%, ZrO 2: 0.03wt%, 1.5 hours sand milling time, the median size of control sand milling is 1.1 ± 0.3 μ m.Carry out the secondary spraying at last and obtain MnZn ferrite particle material powder.Get this particulate material moulding compacting φ 25mm * φ 15mm * 7.5mm, density is approximately 3.0 ± 0.2g/cm 3Annulus, sintering is by by the control of following sintering temperature curve and atmosphere: from room temperature to 600 ℃, this is the binder removal stage, and it is comparatively mild to heat up, and it is abundant that this helps binder removal, 50～150 ℃/hr of temperature rise rate, air atmosphere; After binder removal finished, temperature rise rate was brought up to 150～300 ℃/hr, air atmosphere; 1325 ℃ of sintering temperatures are incubated 3 hours, and equilibrium oxygen partial pres-sure is 5%; Finish to about 1100 ℃ temperature-fall period from insulation, Control for Oxygen Content is 0.05～2%, 100～150 ℃/hr of rate of temperature fall; Since 1100 ℃, fast cooling arrives room temperature, 150～250 ℃/h of rate of temperature fall, and Control for Oxygen Content is below 0.01%.
The magnet ring performance that obtains is: thermal expansivity is 15.5 * 10 -6Magnetostriction coefficient is about-1.0 * 10 -6Magnetic permeability under 25 ℃ is 2450; Saturation magnetic flux density under 25 ℃ and 100 ℃ of conditions is respectively 530mT and 420mT; Power consumption under 100 ℃, 25KHz * 200mT and 100KHz * 200mT condition is respectively 55mW/cm 3And 285mW/cm 3
Comparative example 2: by principal constituent prescription (mol ratio): Fe 2O 3: 53.5mol%, ZnO:12.5mol%, MnO:34.0mol% takes by weighing Fe 2O 3, Mn 3O 4And ZnO.Drop in the sand mill that is added with deionized water in advance and grind, slip water content 40%, 0.5 hour sand milling time, behind a mist projection granulating, electricity consumption heating revolving kiln carries out pre-burning under 900 degree with slip.Pre-subsequently imitation frosted glass input is added with the deionized water sand mill in advance and carries out the secondary sand milling, slip water content 30%, and described relatively principal constituent content in the sand grinding process adds Al 2O 3: 0.05wt%, CaO:0.03wt%, SiO 2: 0.01wt%, MgO:0.10wt%, Nb 2O 5: 0.03wt%, ZrO 2: 0.03wt%, 1.5 hours sand milling time, the median size of control sand milling is 1.1 ± 0.3 μ m.Carry out the secondary spraying at last and obtain MnZn ferrite particle material powder.Get this particulate material moulding compacting φ 25mm * φ 15mm * 7.5mm, density is approximately 3.0 ± 0.2g/cm 3Annulus.
In addition, for studying its practical situations on photovoltaic DC-to-AC converter, be pressed into U type large size magnetic core, two magnetic cores are spliced to form an approximate square toroidal core (keeping certain air gap) behind the sintering, be of a size of: UU120 * 310 * 20, long 310mm, wide 120mm, thick 20mm, weight is 2.11Kg.Two groups of each 65 circle diameters of coiling thereon are the insulated copper wire winding of 3mm, measure its inductance dc superposition characteristic, and output rating.Table 1 illustrates measuring result, and inductance value is 1.02mH, peak power output 3.14KW, and the maximum direct current that allows to pass through is 20A.
Sintering is by by the control of following sintering temperature curve and atmosphere: from room temperature to 600 ℃, this is the binder removal stage, and it is comparatively mild to heat up, and it is abundant that this helps binder removal, 50～150 ℃/hr of temperature rise rate, air atmosphere; After binder removal finished, temperature rise rate was brought up to 150～300 ℃/hr, air atmosphere; 1325 ℃ of sintering temperatures are incubated 3 hours, and equilibrium oxygen partial pres-sure is 5%; Finish to about 1100 ℃ temperature-fall period from insulation, Control for Oxygen Content is 0.05～2%, 100～150 ℃/hr of rate of temperature fall; Since 1100 ℃, fast cooling arrives room temperature, 150～250 ℃/h of rate of temperature fall, and Control for Oxygen Content is below 0.01%.
The magnet ring performance that obtains is: thermal expansivity is 12 * 10 -6Magnetostriction coefficient is about-0.6 * 10 -6Magnetic permeability under 25 ℃ is 2500; Saturation magnetic flux density under 25 ℃ and 100 ℃ of conditions is respectively 510mT and 410mT; Power consumption under 100 ℃, 25KHz * 200mT and 100KHz * 200mT condition is respectively 70mW/cm 3And 420mW/cm 3
Table 1
Figure BSA00000419302900101
Table 2
Figure BSA00000419302900102

Claims (5)

1. photovoltaic DC-to-AC converter magneticsubstance, it is characterized in that: this material is a kind of MnZn Ferrite Material, comprises principal constituent Fe 2O 3, ZnO, MnO and ancillary component, principal constituent comprises and is scaled (mol ratio): Fe 2O 3: 51.5～57.5mol%, ZnO:4.5～15.5mol%, surplus is MnO; Described ancillary component comprises Eu 2O 3, Al 2O 3, described relatively principal constituent total amount, Eu 2O 3And Al 2O 3Total content be 0.05～0.25wt%.
The magneticsubstance of the inventive method preparation is characterized in that: thermal expansivity is less than 8 * 10 -6Magnetostriction coefficient is less than-0.3 * 10 -6Magnetic permeability under 25 ℃ is 2100 ± 25%; Saturation magnetic flux density under 25 ℃ and 100 ℃ of conditions is respectively greater than 530mT and 430mT; Power consumption under 100 ℃, 25KHz * 200mT and 100KHz * 200mT condition is respectively less than 65mW/cm 3And 320mW/cm 3
2. a kind of photovoltaic DC-to-AC converter magneticsubstance according to claim 1, it is characterized in that: described ancillary component with respect to the content of principal constituent is respectively: Eu 2O 3: 0.05～0.15wt%, Al 2O 3: 0.008～0.10wt%.
3. a kind of photovoltaic DC-to-AC converter magneticsubstance according to claim 1 and 2, it is characterized in that: described ancillary component further comprises CaO, SiO 2, MgO, Nb 2O 5And ZrO 2In more than a kind or a kind, described relatively principal constituent total amount, these ancillary component total contents are 0～0.80wt%.
4. a kind of photovoltaic DC-to-AC converter magneticsubstance according to claim 3, it is characterized in that: described ancillary component with respect to the content of principal constituent is respectively: CaO:0～0.15wt%, SiO 2: 0～0.035wt%, MgO:0～0.50wt%, Nb 2O 5: 0～0.06wt%, ZrO 2: 0～0.055wt%.
5. according to the preparation method of the described a kind of photovoltaic DC-to-AC converter of claim 1～4, it is characterized in that: may further comprise the steps: 1) with the main raw material Fe of corresponding each principal constituent with magneticsubstance 2O 3, Mn 3O 4, ZnO add in the sand mill be added with deionized water in advance or the ball mill grind, with slip in 850～950 ℃ of pre-burnings behind the mist projection granulating, in rotary kiln or box-type furnace, obtain ferrite prefiring material; 2) ferrite prefiring material is added in the sand mill that is added with deionized water in advance or the ball mill with ancillary component grind, obtain the ferrite slurry that median size is 1.1 ± 0.3 μ m, add 10% PVA solution (concentration is 10%) subsequently and carry out spray drying granulation, obtain ferrite powder; 3) ferrite powder being obtained density through the press compacting is 3.0 ± 0.2g/cm 3The ferrite blank, the ferrite blank can be a different shape.With blank at vacuum sintering furnace or bell jar stove or N 2In the protection pushed bat kiln, in oxygen partial pressure is 1～10% balanced atmosphere, 1280～1380 ℃ of sintering temperatures 2～5 hours.
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CN104217832A (en) * 2014-08-08 2014-12-17 萨瑞新能源技术（苏州）有限公司 Composite magnetic material for photovoltaic inverter and preparation method thereof
CN104217832B (en) * 2014-08-08 2017-01-18 江苏北斗绿迅新能源科技有限公司 Composite magnetic material for photovoltaic inverter and preparation method thereof
CN104882240A (en) * 2015-05-14 2015-09-02 江苏有能新能源有限公司 Magnetic material for photovoltaic inverter and preparation method thereof
CN107162581A (en) * 2017-06-08 2017-09-15 合肥华盖光伏科技有限公司 A kind of photovoltaic DC-to-AC converter high-performance manganese-zinc magnetic material and preparation method thereof
CN108164261A (en) * 2018-01-23 2018-06-15 合肥华盖光伏科技有限公司 A kind of photovoltaic transformer magnetic material and preparation method thereof
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