CN102390988B - Wide-temperature-range low-loss Mn-Zn ferrite specially used for solar energy inverter, and preparation method thereof - Google Patents
Wide-temperature-range low-loss Mn-Zn ferrite specially used for solar energy inverter, and preparation method thereof Download PDFInfo
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- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 51
- 239000011701 zinc Substances 0.000 claims abstract description 29
- 239000011787 zinc oxide Substances 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 20
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000000126 substance Substances 0.000 claims abstract description 19
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 18
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 9
- 238000000280 densification Methods 0.000 claims abstract description 9
- AMWRITDGCCNYAT-UHFFFAOYSA-L manganese oxide Inorganic materials [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims abstract description 9
- 239000000470 constituent Substances 0.000 claims description 35
- 238000005245 sintering Methods 0.000 claims description 29
- 239000010955 niobium Substances 0.000 claims description 23
- 239000002245 particle Substances 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 13
- 229910052758 niobium Inorganic materials 0.000 claims description 11
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 10
- 229910000428 cobalt oxide Inorganic materials 0.000 claims description 10
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- 229910052760 oxygen Inorganic materials 0.000 claims description 10
- 239000001301 oxygen Substances 0.000 claims description 10
- 238000010298 pulverizing process Methods 0.000 claims description 9
- 238000000227 grinding Methods 0.000 claims description 8
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 5
- 239000003595 mist Substances 0.000 claims description 5
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims description 5
- 238000005507 spraying Methods 0.000 claims description 5
- 238000005469 granulation Methods 0.000 claims description 4
- 230000003179 granulation Effects 0.000 claims description 4
- 239000011236 particulate material Substances 0.000 claims description 4
- 229910052720 vanadium Inorganic materials 0.000 claims description 4
- 239000004615 ingredient Substances 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 230000035699 permeability Effects 0.000 abstract description 34
- 230000005291 magnetic effect Effects 0.000 abstract description 22
- 238000005286 illumination Methods 0.000 abstract description 2
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 abstract 4
- UPWOEMHINGJHOB-UHFFFAOYSA-N oxo(oxocobaltiooxy)cobalt Chemical compound O=[Co]O[Co]=O UPWOEMHINGJHOB-UHFFFAOYSA-N 0.000 abstract 4
- 235000010216 calcium carbonate Nutrition 0.000 abstract 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 29
- 239000011162 core material Substances 0.000 description 19
- 239000004576 sand Substances 0.000 description 15
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 14
- 238000004519 manufacturing process Methods 0.000 description 9
- 238000011161 development Methods 0.000 description 6
- 238000003801 milling Methods 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 239000013078 crystal Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000011156 evaluation Methods 0.000 description 4
- 239000000654 additive Substances 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000013530 defoamer Substances 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 230000004907 flux Effects 0.000 description 3
- 230000005415 magnetization Effects 0.000 description 3
- 238000003825 pressing Methods 0.000 description 3
- 239000007921 spray Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 238000013461 design Methods 0.000 description 2
- 241001269238 Data Species 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 229910001308 Zinc ferrite Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000003203 everyday effect Effects 0.000 description 1
- 230000005308 ferrimagnetism Effects 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000002085 persistent effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- WGEATSXPYVGFCC-UHFFFAOYSA-N zinc ferrite Chemical compound O=[Zn].O=[Fe]O[Fe]=O WGEATSXPYVGFCC-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention relates to wide-temperature-range low-loss Mn-Zn ferrite specially used for a solar energy inverter, and a preparation method thereof. The Mn-Zn ferrite comprises main components of: 53.5mol%-54.5mol% of iron oxide calculated according to Fe2O3, 8.0mol%-10.0mol% of zinc oxide calculated according to ZnO, and balance of mangano-manganic oxide. The Mn-Zn ferrite also comprises minor components of, by weight: 0.03-0.04% of CaCO3, 0.005-0.01% of Nb2O5, 0.01-0.03% of V2O5, and 0.03-0.2% of Co2O3, calculated according to standard substances of CaCO3, Nb2O5, V2O5, and Co2O3. The Mn-Zn ferrite is prepared with an oxide method, and is sintered under an elevator furnace densification condition. The obtained product has relatively high initial magnetic permeability mui, and low power loss Pcv. With the Mn-Zn ferrite, the loss under a high-frequency transformer operation status is reduced, and the efficiency of the transformer is improved. With the Mn-Zn ferrite, miniature inverters can be produced with high frequency, small size, and intelligence. Also, a requirement of efficiency improving under a condition of illumination variation can be satisfied. The product is advantaged in high reliability and good stability. With the product, a miniature inverter can be used in environments with large temperature variations, such as deserts and islands.
Description
Technical field
The invention belongs to low-consumption Mn-Zn soft magnetic ferrite technical field, be specifically related to Mn-Zn ferrite of a kind of sintering temperature and low, wide temperature range, the little invertor special use of low-power consumption sun power and preparation method thereof.
Background technology
Solar energy resources cleaning, pollution-free, renewable, environmental protection is more and more paid attention at new energy field, and national governments launch respectively its development of policy support.Along with the development and progress of solar energy generation technology, combining inverter is development and progress thereupon also.
The efficiency of conversion of general solar cell is only the 10-20% left and right.High-level efficiency and have the key index that cost-benefit invertor becomes evaluation solar power system quality.On average export electric energy as 190kWh as example every day take a 20kWp erecting equipment, suppose that inverter efficiency brings up to 96% from 95%, if force rate for incorporation into the power network by 1.0 yuan/degree, and calculate with 10 years life cycles, the income that this improved efficiency of 1% is brought will be near half of invertor cost taken by themselves.The lifting of inverter efficiency becomes the rigid index of invertor development.MPPT maximum power point tracking (maximum power point tracking, MPPT) utilization of technology in little invertor, solved in centralized, string data and many string datas systems, the MPPT technology can't be taken into account each photovoltaic array in system, and single photovoltaic array utilization ratio is low, the persistent ailment of the anti-local shade ability of system.
In the little invertor of DC/AC, loss is more main with the loss of magnetics.The loss that reduces the ferrimagnetism element just seems extremely important.In the invertor that adopts the high-frequency transformer insulation mode, magnetic device be operated in the high frequency state (〉=20kHz).With respect to low-frequency transformer, volume and weight is less, and cost is lower, and efficient is higher.Applicable magneticsubstance is soft magnetic ferrite.As high-frequency transformer magnetic soft magnetic ferrite, technical requirements low-loss, high saturation magnetic flux density.Under its working order, electric current may reach 20-30A.At night, photovoltaic plant is because illumination is not enough and out of service, and invertor often is in holding state.In addition, photovoltaic plant is often built the places such as desert, island in, and day and night temperature is large, and is very high to the reliability requirement of magnetic elements.Consider these factors, design suitable production technique, produce high magnetic permeability, high saturation magnetic flux density, superimposed characteristics is good, and the Ferrite Material that power loss is low is significant to the efficient that improves invertor.
Summary of the invention
For the requirement of the little invertor of sun power to magnetic elements, the purpose of this invention is to provide a kind of wide-temperature and low-consumption Mn-Zn ferrite, this ferrite has following excellent comprehensive performance: sintering under cold condition, have high initial magnetoconductivity, low high-frequency loss, high saturation magnetic flux density, reasonably damage curve design, more be conducive to invertor to high frequency, miniaturization, lightweight, high power density, high-level efficiency, high reliability, intelligentized future development.
The cardinal principle of technical solution problem of the present invention is: adopt Fe
2O
3Molar content adds Co greater than 50% rich iron formula in minor component
2O
3Improve power consumption characteristics and the magnetic permeability characteristic of material, and dc superposition characteristic; Add CaCO in minor component
3With Nb
2O
5Combined dopants is optimized the crystal grain vesicular structure, reduces the high band relative loss factor factor; Add V in minor component
2O
5Reduce sintering temperature; Adjust material crystals structure and crystal boundary distribution by production technique, obtain good material behavior.
The technical solution used in the present invention is:
The special-purpose wide-temperature and low-consumption Mn-Zn ferrite of a kind of solar inverter has good power loss P at 25 ℃ ~ 100 ℃, 300kHz ~ 500kHz
cv, be used for little invertor high-frequency transformer, the loss in the high-frequency transformer working process is reduced, improve little inverter efficiency, satisfy the demand that is applied to severe environment, it comprises principal constituent and minor component, and principal constituent is: ferric oxide, trimanganese tetroxide, zinc oxide; Described principal constituent is as follows in the content of standard substance separately:
Fe
2O
3：53.5mol%~54.5mol%，
ZnO：8.0mol%~10.0mol%，
All the other are Mn
3O
4
Described minor component comprises calcium carbonate, Niobium Pentxoxide, Vanadium Pentoxide in FLAKES and cobalt oxide, relatively described principal constituent total amount, and described minor component is with its standard substance CaCO separately
3, Nb
2O
5, V
2O
5And Co
2O
3The total content of meter is 0.075wt% ~ 0.18wt%, and wherein cobalt oxide is with its standard substance Co
2O
3The content of meter is 0.03 wt% ~ 0.2 wt%.
As a kind of preferred, relatively described principal constituent total amount, described minor component calcium carbonate, Niobium Pentxoxide and Vanadium Pentoxide in FLAKES are with its standard substance CaCO separately
3, Nb
2O
5And V
2O
5The content of meter is respectively: CaCO
3: 0.03 wt% ~ 0.04 wt%, Nb
2O
5: 0.005 wt% ~ 0.01 wt%, V
2O
5: 0.01 wt% ~ 0.03 wt%.
The special-purpose wide-temperature and low-consumption Mn-Zn ferrite of described solar inverter, in the lower-most point of power loss under 300kHz ~ 500kHz, 50mT ~ 100mT range of condition in 0 ℃ ~ 60 ℃ scopes.
The preparation method of the special-purpose wide-temperature and low-consumption Mn-Zn ferrite of a kind of solar inverter is characterized in that, comprises successively mixing, pre-burning, pulverizing, granulation, compacting and sintering step, wherein:
⑴ mix: by the principal constituent proportion ingredient, carry out together wet-mixed, mixing time is 30 ~ 60 minutes; Described principal constituent is take the content of standard substance separately as Fe
2O
3: 53.5mol% ~ 54.5mol%, ZnO:8.0mol% ~ 10.0mol%, all the other are Mn
3O
4
⑵ pre-burning: carry out pre-burning in rotary kiln with adding after principal constituent slip spraying drying, calcined temperature is controlled at 850 ℃ ~ 950 ℃, and the pre-burning time is 30 ~ 60 minutes;
⑶ pulverize: carry out wet pulverization add minor component in the principal constituent Preburning material that upper step pre-burning obtains after, grinding time is 90 ~ 150 minutes, and after pulverizing, the slip particle diameter is controlled at 1.0 ~ 1.5 μ m; Described minor component is with its standard substance CaCO separately
3, Nb
2O
5, V
2O
5And Co
2O
3The total content of meter is 0.075wt% ~ 0.18wt%, and wherein cobalt oxide is with its standard substance Co
2O
3The content of meter is 0.03 wt% ~ 0.2 wt%;
⑷ granulation: added 1.5% the PVA that is equivalent to slip weight at the slip in upper step, adopt mist projection granulating, obtain particulate material;
⑸ compacting: adopt the powder former compacting to obtain blank the particulate material in upper step, the pressed density of blank is controlled at 3.0 ± 0.2g/cm
3
⑹ sintering: blank sintering in clock hood type furnace that the upper step is obtained, temperature rise rate is controlled at 1.25 ~ 3 ℃/minute, carrying out densification at 900 ℃ to sintering temperature controls, control the oxygen level volume ratio lower than 1%, sintering temperature is controlled at 1200 ℃ ~ 1220 ℃, holding-zone oxygen level volume ratio is controlled at 3.0% ~ 5.0%, is incubated 3 ~ 5 hours, and rate of temperature fall is controlled at 1.25 ~ 2 ℃/minute.
As a kind of preferred, in pulverising step ⑶, wherein said minor component calcium carbonate, Niobium Pentxoxide and Vanadium Pentoxide in FLAKES are with its standard substance CaCO separately
3, Nb
2O
5And V
2O
5The content of meter is respectively: CaCO
3: 0.03 wt% ~ 0.04 wt%, Nb
2O
5: 0.005 wt% ~ 0.01 wt%, V
2O
5: 0.01 wt% ~ 0.03 wt%.
In manufacture method of the present invention, sintering temperature is at 1200 ℃ ~ 1220 ℃, and the sintering temperature of 1280 ℃ ~ 1300 ℃ of the material of relatively conventional initial magnetic permeability 1000 ~ 3000 has reduced by 60 ~ 80 ℃.The production technique of the special-purpose wide temperature low-power consumption Mn-Zn ferrite of solar inverter of the present invention has low pre-burning and sintering temperature, effectively reduces the production energy consumption of product.
Mixing of the minor component of the present invention by rational principal constituent proportioning and optimization, be equipped with suitable processing condition, made the tiny homogeneous of microcosmic crystal grain, cavernous Mn-Zn ferrite under the condition of sintering temperature and low, this ferrite has 1000 ~ 3000 initial magnetic permeability, low high band power loss and high high temperature saturation magnetization.Specifically, the initial permeability μ of the Mn-Zn ferrite that makes of the present invention
iFor: 1000 ~ 3000(10kHz, 0.25mT, 25 ℃ ± 3 ℃), its power loss P
cvLess than 80kW/m
3(500kHz, 50mT, 25 ℃ ± 3 ℃) is less than 120kW/m
3(500kHz, 50mT, 100 ℃ ± 3 ℃) is less than 300kW/m
3(300kHz, 100mT, 25 ℃ ± 3 ℃) is less than 400kW/m
3(300kHz, 100mT, 100 ℃ ± 3 ℃), power loss P
cv0 ~ 60 ℃ of minimum point temperature scope.The special-purpose wide temperature low-power consumption Mn-Zn ferrite of solar inverter of the present invention is superior in the over-all properties of wide temperature section and high band, and the performances such as its initial permeability, power loss and saturation magnetization can be good at satisfying the service requirements of the little invertor medium/high frequency transformer of sun power.Particularly 25 ℃ ~ 100 ℃ have low power loss, can be good at reducing the loss of high-frequency transformer, improve stability and the reliability of equipment, improve the efficient of little invertor.
The present invention has following characteristics compared with prior art: adopt the special-purpose wide temperature low-power consumption Mn-Zn ferrite of the little invertor of sun power of the production method preparation of low temperature densification sintering to have low power loss, high high temperature saturation magnetization, high frequency of utilization scope, stable production technique and good performance, can be good at satisfying the little invertor of sun power with the service requirements of high-frequency transformer.
Description of drawings
Fig. 1 toroidal core exemplar.
Fig. 2 densification sintering atmosphere figure.
Embodiment
Below the invention will be further described by specific embodiment, but the present invention is not limited to these embodiment.
Embodiment 1:
Take the Fe of 53.7mol%
2O
3, 36.5 mol% Mn
3O
4ZnO with 9.8 mol%.After above-mentioned principal constituent is mixed, add in sand mill and mix, mixing time 30 minutes is sent into rotary kiln after spraying drying, pre-burning at 900 ℃ ± 10 ℃ temperature, 45 minutes pre-burning time.Add subsequently minor component to drop into sand mill in Preburning material and pulverize, grinding time 120 minutes, after pulverizing, the slip particle diameter is controlled at 1.0 ~ 1.5 μ m; Relatively described principal constituent total amount, described minor component in its separately the content of standard substance (wt%) be respectively: CaCO
3: 0.03, Nb
2O
5: 0.005, V
2O
5: 0.02, Co
2O
3: 0.10.Described mixing sand milling and pulverize the 35 wt % that need add pure water to be equivalent to the principal constituent total amount in sand grinding process, and dispersion agent and defoamer some (being as the criterion to obtain setting particle size range).Last 1.5% the PVA that is equivalent to slip weight that adds in the sand milling slip obtains Mn-Zn ferrite particles by the spray tower mist projection granulating.
Getting this particle adopts pressure forming to be as shown in Figure 1 toroidal core.Pressed density is controlled at 3.0 ± 0.2g/cm
3Sintering in clock hood type furnace, as shown in Fig. 2 curve, temperature rise rate is controlled at 1.25 ~ 3 ℃/minute, carries out densification at 900 ℃ to sintering temperature and controls, and controls the oxygen level volume ratio lower than 1%, sintering temperature is controlled at 1200 ℃ ~ 1220 ℃, holding-zone oxygen level volume ratio is controlled at 3.0% ~ 5.0%, is incubated 3 ~ 5 hours, and rate of temperature fall is controlled at 1.25 ~ 2 ℃/minute.Making described Mn-Zn ferrite toroidal core product size is Φ 25mm * Φ 15 mm * h7.5 mm.Through the magnetic core of said process preparation, test respectively normal temperature initial permeability μ with instruments such as HP4284A LCR tester, high cryostats
i, the power loss P that 500kHz, 50 mT and 300kHz, 100 mT conditions are lower 25 ℃, 100 ℃
cv, power loss P
cvMinimum point temperature.
Prepared magnetic core is estimated.Normal temperature initial permeability μ
iBe under 1000 ~ 3000,500kHz, 50 mT conditions, 25 ℃ of power loss P
cv＜80kW/m
3, 100 ℃ of power loss P
cv＜120kW/m
3, under 300kHz, 100mT condition, 25 ℃ of power loss P
cv＜300kW/m
3, 100 ℃ of power loss P
cv＜400kW/m
3, power loss P
cv0 ~ 60 ℃ of minimum point temperature scope.When above condition all meets the requirements, be evaluated as " √ ": good, as long as have one undesirable, be evaluated as " * ": bad.
Table 1 toroidal core material property of the present invention I
As shown in table 1, the initial permeability μ of embodiment 1
i: 1761, meet initial permeability μ
i1000 ~ 3000, requirement, and good power loss P is arranged under high frequency
cv, satisfy under 500kHz, 50 mT conditions 25 ℃ of power loss P
cv＜80kW/m
3(actual 42 kW/m
3), 100 ℃ of power loss P
cv＜120kW/m
3(actual 93 kW/m
3), under 300kHz, 100mT condition, 25 ℃ of power loss P
cv＜300kW/m
3(actual 220 kW/m
3), 100 ℃ of power loss P
cv＜400kW/m
3(actual 375kW/m
3), power loss P
cv0 ~ 60 ℃ of minimum point temperature scope (actual 30 ℃), evaluating characteristics all good (" √ ").
Embodiment 2 ~ 6:
As shown in table 1, except the Fe as principal constituent
2O
3Composition is outside the composition of 53.5mol% ~ 54.5mol% scope and ZnO changes in 8.0mol% ~ 10.0mol% scope, and all the other are trimanganese tetroxide.All the other techniques are all carried out similarly to Example 1, and above-mentioned principal constituent adds in sand mill and mixes after mixing, and mixing time 30 minutes is sent into rotary kiln after spraying drying, pre-burning at 900 ℃ ± 10 ℃ temperature, 45 minutes pre-burning time kind.Add subsequently minor component to drop into sand mill in Preburning material and pulverize, grinding time 120 minutes, after pulverizing, the slip particle diameter is controlled at 1.0 ~ 1.5 μ m; Relatively described principal constituent total amount, described minor component in its separately the content of standard substance (wt%) be respectively: CaCO
3: 0.03, Nb
2O
5: 0.005, V
2O
5: 0.02, Co
2O
3: 0.10.Described mixing sand milling and pulverize the 35wt% that need add pure water to be equivalent to the principal constituent total amount in sand grinding process, and dispersion agent and defoamer some (being as the criterion to obtain setting particle size range).Last 1.5% the PVA that is equivalent to slip weight that adds in the sand milling slip obtains Mn-Zn ferrite particles by the spray tower mist projection granulating.
Get this particle and adopt pressure forming to be as shown in Figure 1 toroidal core, pressed density is controlled at 3.0 ± 0.2g/cm
3Sintering in clock hood type furnace, as shown in Fig. 2 curve, temperature rise rate is controlled at 1.25 ~ 3 ℃/minute, carries out densification at 900 ℃ to sintering temperature and controls, and controls the oxygen level volume ratio lower than 1%, sintering temperature is controlled at 1200 ℃ ~ 1220 ℃, holding-zone oxygen level volume ratio is controlled at 3.0% ~ 5.0%, is incubated 3 ~ 5 hours, and rate of temperature fall is controlled at 1.25 ~ 2 ℃/minute.Making described Mn-Zn ferrite toroidal core product size is Φ 25mm * Φ 15 mm * h7.5 mm.Through the magnetic core of said process preparation, test respectively normal temperature initial permeability μ with instruments such as HP4284A LCR tester, high cryostats
i, the power loss P that 500kHz, 50mT and 300kHz, 100mT condition are lower 25 ℃, 100 ℃
cv, power loss P
cvMinimum point temperature.
Prepared magnetic core is estimated.Normal temperature initial permeability μ
iBe under 1000 ~ 3000,500kHz, 50mT condition, 25 ℃ of power loss P
cv＜80kW/m
3, 100 ℃ of power loss P
cv＜120kW/m
3, under 300kHz, 100mT condition, 25 ℃ of power loss P
cv＜300kW/m
3, 100 ℃ of power loss P
cv＜400kW/m
3, power loss P
cv0 ~ 60 ℃ of minimum point temperature scope.When above condition all meets the requirements, be evaluated as " √ ": good, as long as have one undesirable, be evaluated as " * ": bad.
As shown in table 1, the initial permeability μ of embodiment 2 ~ 6
i: 1061 ~ 2552, meet initial permeability μ
i1000 ~ 3000, requirement, and good power loss P is arranged under high frequency
cv, satisfy under 500kHz, 50mT condition 25 ℃ of power loss P
cv＜80kW/m
3(actual 32 ~ 75 kW/m
3), 100 ℃ of power loss P
cv＜120kW/m
3(actual 88 ~ 112 kW/m
3), under 300kHz, 100mT condition, 25 ℃ of power loss P
cv＜300kW/m
3(actual 198 ~ 260 kW/m
3), 100 ℃ of power loss P
cv＜400kW/m
3(actual 346 ~ 390kW/m
3), power loss P
cv0 ~ 60 ℃ of minimum point temperature scope (actual 5 ~ 55 ℃), evaluating characteristics all good (" √ ").
Comparative Examples 1 ~ 8:
As shown in table 1, except the Fe as principal constituent
2O
3Composition is outside the composition of 52.5mol% ~ 55.5mol% scope and ZnO changes in 7.0mol% ~ 11.0mol% scope, and all the other are trimanganese tetroxide.All the other techniques are all carried out equally with embodiment 1 ~ 6, and above-mentioned principal constituent adds in sand mill and mixes after mixing, and mixing time 30 minutes is sent into rotary kiln after spraying drying, pre-burning at 900 ℃ ± 10 ℃ temperature, 45 minutes pre-burning time kind.Add subsequently minor component to drop into sand mill in Preburning material and pulverize, grinding time 120 minutes, after pulverizing, the slip particle diameter is controlled at 1.0 ~ 1.5 μ m; Relatively described principal constituent total amount, described minor component in its separately the content of standard substance (wt%) be respectively: CaCO
3: 0.03, Nb
2O
5: 0.005, V
2O
5: 0.02, Co
2O
3: 0.1.Described mixing sand milling and pulverize the 35wt% that need add pure water to be equivalent to the principal constituent total amount in sand grinding process, and dispersion agent and defoamer some (being as the criterion to obtain setting particle size range).Last 1.5% the PVA that is equivalent to slip weight that adds in the sand milling slip obtains Mn-Zn ferrite particles by the spray tower mist projection granulating.
Get this particle and adopt pressure forming to be as shown in Figure 1 toroidal core, pressed density is controlled at 3.0 ± 0.2g/cm
3Sintering in clock hood type furnace, as shown in Fig. 2 curve, temperature rise rate is controlled at 1.25 ~ 3 ℃/minute, carries out densification at 900 ℃ to sintering temperature and controls, and controls the oxygen level volume ratio lower than 1%, sintering temperature is controlled at 1200 ℃ ~ 1220 ℃, holding-zone oxygen level volume ratio is controlled at 3.0% ~ 5.0%, is incubated 3 ~ 5 hours, and rate of temperature fall is controlled at 1.25 ~ 2 ℃/minute.Making described Mn-Zn ferrite toroidal core product size is Φ 25mm * Φ 15 mm * h7.5 mm.Through the magnetic core of said process preparation, test respectively normal temperature initial permeability μ with instruments such as HP4284A LCR tester, high cryostats
i, the power loss P that 500kHz, 50mT and 300kHz, 100mT condition are lower 25 ℃, 100 ℃
cv, power loss P
cvMinimum point temperature.
Prepared magnetic core is estimated.Normal temperature initial permeability μ
iBe under 1000 ~ 3000,500kHz, 50mT condition, 25 ℃ of power loss P
cv＜80kW/m
3, 100 ℃ of power loss P
cv＜120kW/m
3, under 300kHz, 100mT condition, 25 ℃ of power loss P
cv＜300kW/m
3, 100 ℃ of power loss P
cv＜400kW/m
3, power loss P
cv0 ~ 60 ℃ of minimum point temperature scope.When above condition all meets the requirements, be evaluated as " √ ": good, as long as have one undesirable, be evaluated as " * ": bad.
Comparative Examples 1 is that iron oxide content surpasses 53.5mol% ~ 54.5mol% upper limit (in column additional " ※ ").
Comparative Examples 2 is that iron oxide content surpasses 53.5mol% ~ 54.5mol% lower limit (in column additional " * ").
Comparative Examples 3 is that zinc oxide content surpasses 8.0mol% ~ 10.0mol% upper limit (in column additional " ※ ").
Comparative Examples 4 is that zinc oxide content surpasses 8.0mol% ~ 10.0mol% lower limit (in column additional " * ").
Comparative Examples 5 is that iron oxide content surpasses 53.5mol% ~ 54.5mol% upper limit (in column additional " ※ "), and zinc oxide content surpasses 8.0mol% ~ 10.0mol% upper limit (in column additional " ※ ").
Comparative Examples 6 is that iron oxide content surpasses 53.5mol% ~ 54.5mol% upper limit (in column additional " ※ "), and zinc oxide content surpasses 8.0mol% ~ 10.0mol% lower limit (in column additional " * ").
Comparative Examples 7 is that iron oxide content surpasses 53.5mol% ~ 54.5mol% lower limit (in column additional " * "), and zinc oxide content surpasses 8.0mol% ~ 10.0mol% upper limit (in column additional " ※ ").
Comparative Examples 8 is that iron oxide content surpasses 53.5mol% ~ 54.5mol% lower limit (in column additional " * "), and zinc oxide content surpasses 8.0mol% ~ 10.0mol% lower limit (in column additional " * ").
Its result shown in table 1 gives to surpass initial permeability μ
iAdditional " ※ " of 1000 ~ 3000 upper limits, additional " * " of lower limit, the power loss P that 500kHz, 50mT and 300kHz, 100mT condition are lower 25 ℃, 100 ℃
cvAdditional " ※ " that surpasses the upper limit, power loss P
cv0 ~ 60 ℃ of additional " ※ " that surpasses the upper limit of minimum point temperature scope is over additional " * " of lower limit.The evaluation of comparative example 1 ~ 8 is bad (" * ") all.
Estimate 1:
Above embodiment and the Comparative Examples of contrast can be found out, contains with Fe
2O
3The 53.50mol% ~ 54.5mol% ferric oxide of meter, in the 8.0mol% of ZnO ~ 10.0mol% zinc oxide, all the other are trimanganese tetroxides, relatively described principal constituent total amount, described minor component in its separately the content of standard substance (wt%) be respectively: CaCO
3: 0.03, Nb
2O
5: 0.005, V
2O
5: 0.02, Co
2O
3: 0.05, can confirm to meet initial permeability μ
i1000 ~ 3000; Under 500kHz, 50 mT conditions, 25 ℃ of power loss P
cv＜80kW/m
3, 100 ℃ of power loss P
cv＜120kW/m
3Under 300kHz, 100mT condition, 25 ℃ of power loss P
cv＜300kW/m
3, 100 ℃ of power loss P
cv＜400kW/m
3Requirement.
Embodiment 7 ~ 8:
As shown in table 2, as the Fe of principal constituent
2O
3, ZnO, Mn
3O
4Content is all identical with embodiment 1, changes the content as the minor component cobalt oxide of additive, to its normal temperature initial permeability μ
i, the power loss P that 500kHz, 50mT and 300kHz, 100mT condition are lower 25 ℃, 100 ℃
cvCharacteristic, power loss P
cvMinimum point temperature is studied.
Embodiment 7 is lower limits that cobalt oxide content is in 0.03 wt% ~ 0.2wt% scope.
Embodiment 8 is upper limits that cobalt oxide content is in 0.03 wt% ~ 0.2wt% scope.
Except pressing the listed composition of table 2, all adopt with embodiment 1 same process and obtain Mn-Zn ferrite goods exemplar, test respectively normal temperature initial permeability μ with instruments such as HP4284A LCR tester, high cryostats
i, the power loss P that 500kHz, 50mT and 300kHz, 100mT condition are lower 25 ℃, 100 ℃
cvCharacteristic, power loss P
cvMinimum point temperature.
Prepared magnetic core is estimated.Normal temperature initial permeability μ
i: 1000 ~ 3000; Under 500kHz, 50mT condition, 25 ℃ of power loss P
cv＜80kW/m
3, 100 ℃ of power loss P
cv＜120kW/m
3Under 300kHz, 100mT condition, 25 ℃ of power loss P
cv＜300kW/m
3, 100 ℃ of power loss P
cv＜400kW/m
3, power loss P
cv0 ~ 60 ℃ of minimum point temperature scope when above condition all meets the requirements, is evaluated as " √ ": good, as long as have one undesirable, be evaluated as " * ": bad.
As shown in table 2, the initial permeability μ of embodiment 7 ~ 8
i: 1711 ~ 2856, meet initial permeability μ
i25 ℃ of power loss P are satisfied under 500kHz, 50 mT conditions in 1000 ~ 3000 requirement simultaneously
cv＜80kW/m
3(actual 35 ~ 57 kW/m
3), 100 ℃ of power loss P
cv＜120kW/m
3(actual 77 ~ 108 kW/m
3), under 300kHz, 100mT condition, 25 ℃ of power loss P
cv＜300kW/m
3(actual 173 ~ 254 kW/m
3), 100 ℃ of power loss P
cv＜400kW/m
3(actual 317 ~ 382kW/m
3), power loss P
cv0 ~ 60 ℃ of minimum point temperature scope (actual 20 ~ 35 ℃), evaluating characteristics all good (" √ ").
Comparative Examples 9 ~ 10:
In Comparative Examples 9 ~ 10, change the content as the minor component cobalt oxide of additive, to its normal temperature initial permeability μ
i, the power loss P that 500kHz, 50mT and 300kHz, 100mT condition are lower 25 ℃, 100 ℃
cvCharacteristic, power loss P
cvMinimum point temperature is studied.
As shown in table 2, in Comparative Examples 9 ~ 10 as the Fe of principal constituent
2O
3, ZnO, Mn
3O
4Content is identical with embodiment 1.
Comparative Examples 9 is lower limits (in column additional " * ") that cobalt oxide content surpasses 0.03 wt% ~ 0.2wt% scope.
Comparative Examples 10 is upper limits (in column additional " ※ ") that cobalt oxide content surpasses 0.03 wt% ~ 0.2wt% scope.
Except pressing the listed composition of table 2, all adopt with embodiment 1 same process and obtain Mn-Zn ferrite goods exemplar.Test respectively normal temperature initial permeability μ with instruments such as HP4284A LCR tester, high cryostats
i, the power loss P that 500kHz, 50mT and 300kHz, 100mT condition are lower 25 ℃, 100 ℃
cvCharacteristic, power loss P
cvMinimum point temperature.
Prepared magnetic core is estimated.Normal temperature initial permeability μ
i1000 ~ 3000; Under 500kHz, 50mT condition, 25 ℃ of power loss P
cv＜80kW/m
3, 100 ℃ of power loss P
cv＜120kW/m
3Under 300kHz, 100mT condition, 25 ℃ of power loss P
cv＜300kW/m
3, 100 ℃ of power loss P
cv＜400kW/m
3, power loss P
cv0 ~ 60 ℃ of minimum point temperature scope when above condition all meets the requirements, is evaluated as " √ ": good, as long as have one undesirable, be evaluated as " * ": bad.
Table 2 toroidal core material property of the present invention II
Its result shown in table 2 gives to surpass initial permeability μ
iAdditional " ※ " of 1000 ~ 3000 upper limits, additional " * " of lower limit, the power loss P that 500kHz, 50mT and 300kHz, 100mT condition are lower 25 ℃, 100 ℃
cvAdditional " ※ " that surpasses the upper limit, power loss P
cvMinimum point temperature surpasses additional " ※ " of the upper limit, additional " * " of lower limit.The evaluation of Comparative Examples 9 ~ 10 is bad (" * ") all.
Estimate 2:
Above embodiment and the Comparative Examples of contrast can be found out, contains with Fe
2O
3The 53.5mol% ~ 54.5mol% ferric oxide of meter, in the 8.0mol% of ZnO ~ 10.0mol% zinc oxide, all the other are trimanganese tetroxides, relatively described principal constituent total amount, described minor component in its separately the content of standard substance be respectively (wt%): CaCO
3: 0.03, Nb
2O
5: 0.005, V
2O
5: 0.02, Co
2O
3: 0.03 ~ 0.2, can confirm to meet initial permeability μ
iUnder 1000 ~ 3000,500kHz, 50 mT conditions, 25 ℃ of power loss P
cv＜80kW/m
3, 100 ℃ of power loss P
cv＜120kW/m
3Under 300kHz, 100mT condition, 25 ℃ of power loss P
cv＜300kW/m
3, 100 ℃ of power loss P
cv＜400kW/m
3, the requirement that power loss Pcv minimum point temperature scope is 0 ~ 60 ℃.
Comparative Examples 11 ~ 16:
In Comparative Examples 11 ~ 16, change any minor component calcium carbonate, Niobium Pentxoxide as additive, the content of Vanadium Pentoxide in FLAKES is to its normal temperature initial permeability μ
i, the power loss P that 500kHz, 50 mT and 300kHz, 100 mT conditions are lower 25 ℃, 100 ℃
cvCharacteristic, power loss P
cvMinimum point temperature is studied.
As shown in table 3, in Comparative Examples 11 ~ 16 as the Fe of principal constituent
2O
3, ZnO, Mn
3O
4Content is identical with embodiment 1.
Comparative Examples 11 is lower limits (in column additional " * ") that calcium carbonate content surpasses 0.03wt% ~ 0.04wt% scope.
Comparative Examples 12 is upper limits (in column additional " ※ ") that calcium carbonate content surpasses 0.03wt% ~ 0.04wt% scope.
Comparative Examples 13 is lower limits (in column additional " * ") that Niobium Pentxoxide content surpasses 0.005wt% ~ 0.01wt% scope.
Comparative Examples 14 is upper limits (in column additional " ※ ") that Niobium Pentxoxide content surpasses 0.005wt% ~ 0.01wt% scope.
Comparative Examples 15 is lower limits (in column additional " * ") that pentoxide content surpasses 0.01wt% ~ 0.03wt% scope.
Comparative Examples 16 is upper limits (in column additional " ※ ") that pentoxide content surpasses 0.01wt% ~ 0.03wt% scope.
Except pressing the listed composition of table 3, all adopt with embodiment 1 same process and obtain Mn-Zn ferrite goods exemplar.Test respectively normal temperature initial permeability μ with instruments such as HP4284A LCR tester, high cryostats
i, the power loss P that 500kHz, 50mT and 300kHz, 100mT condition are lower 25 ℃, 100 ℃
cvCharacteristic, power loss P
cvMinimum point temperature.
Prepared magnetic core is estimated.Normal temperature initial permeability μ
i1000 ~ 3000; Under 500kHz, 50 mT conditions, 25 ℃ of power loss P
cv＜80kW/m
3, 100 ℃ of power loss P
cv＜120kW/m
3Under 300kHz, 100mT condition, 25 ℃ of power loss P
cv＜300kW/m
3, 100 ℃ of power loss P
cv＜400kW/m
3, power loss P
cv0 ~ 60 ℃ of minimum point temperature scope when above condition all meets the requirements, is evaluated as " √ ": good, as long as have one undesirable, be evaluated as " * ": bad.
Table 3 toroidal core material property of the present invention III
Its result shown in table 3 gives to surpass initial permeability μ
iAdditional " ※ " of 1000 ~ 3000 upper limits, additional " * " of lower limit, the power loss P that 500kHz, 50 mT and 300kHz, 100 mT conditions are lower 25 ℃, 100 ℃
cvAdditional " ※ " that surpasses the upper limit, power loss P
cvMinimum point temperature surpasses additional " ※ " of the upper limit, additional " * " of lower limit.The evaluation of Comparative Examples 11 ~ 16 is bad (" * ") all.
Estimate 3:
Above embodiment and the Comparative Examples of contrast can be found out, contains with Fe
2O
3The 53.5mol% ~ 54.5mol% ferric oxide of meter, in the 8.0mol% of ZnO ~ 10.0mol% zinc oxide, all the other are trimanganese tetroxides, relatively described principal constituent total amount, described minor component in its separately the content of standard substance be respectively (wt%): CaCO
3: 0.03 ~ 0.04, Nb
2O
5: 0.005 ~ 0.01, V
2O
5: 0.01 ~ 0.03, Co
2O
3: 0.05, can confirm to meet initial permeability μ
iUnder 1000 ~ 3000,500kHz, 50mT condition, 25 ℃ of power loss P
cv＜80kW/m
3, 100 ℃ of power loss P
cv＜120kW/m
3Under 300kHz, 100mT condition, 25 ℃ of power loss P
cv＜300kW/m
3, 100 ℃ of power loss P
cv＜400kW/m3, power loss P
cvThe requirement that the minimum point temperature scope is 0 ~ 60 ℃.
As mentioned above, adopt the wide-temperature low-distortion mangan zinc ferrite of the production method preparation of the densification sintering in the present invention, have high initial magnetoconductivity, low power loss, wide use temperature scope (25 ℃ ~ 100 ℃), stable production technique and good performance, can satisfy the ferritic demand for development of the little invertor high-frequency transformer of sun power, satisfy the user demand of the severe environment such as desert, island.
Claims (2)
1. the special-purpose wide-temperature and low-consumption Mn-Zn ferrite of a solar inverter, its under 500kHz, 50mT condition, 25 ℃ of power loss P
cv＜80kW/m
3, 100 ℃ of power loss P
cv＜120kW/m
3, under 300kHz, 100mT condition, 25 ℃ of power loss P
cv＜300kW/m
3, 100 ℃ of power loss P
cv＜400kW/m
3In the lower-most point of power loss under 300kHz ~ 500kHz, 50mT ~ 100mT range of condition in 0 ℃ ~ 60 ℃ scopes, be used for little invertor high-frequency transformer, loss in the high-frequency transformer working process is reduced, improve little inverter efficiency, satisfy the demand that is applied to severe environment, it comprises principal constituent and minor component, and principal constituent is: ferric oxide, trimanganese tetroxide, zinc oxide; It is characterized in that,
Described principal constituent is as follows in the content of standard substance separately: Fe
2O
3: 53.5mol% ~ 54.5mol%, ZnO:8.0mol% ~ 10.0mol%, all the other are Mn
3O
4
Described minor component comprises calcium carbonate, Niobium Pentxoxide, Vanadium Pentoxide in FLAKES and cobalt oxide, relatively described principal constituent total amount, described minor component in its separately the content of standard substance be respectively: CaCO
3: 0.03 wt% ~ 0.04 wt%, Nb
2O
5: 0.005 wt% ~ 0.01 wt%, V
2O
5: 0.01 wt% ~ 0.03 wt%, Co
2O
3: 0.03 wt% ~ 0.05 wt%.
2. the preparation method of the special-purpose wide-temperature and low-consumption Mn-Zn ferrite of a kind of solar inverter as claimed in claim 1, is characterized in that, comprises successively mixing, pre-burning, pulverizing, granulation, compacting and sintering step, wherein:
⑴ mix: by the principal constituent proportion ingredient, carry out together wet-mixed, mixing time is 30 ~ 60 minutes; Described principal constituent is take the content of standard substance separately as Fe
2O
3: 53.5mol% ~ 54.5mol%, ZnO:8.0mol% ~ 10.0mol%, all the other are Mn
3O
4
⑵ pre-burning: carry out pre-burning in rotary kiln with adding after principal constituent slip spraying drying, calcined temperature is controlled at 850 ℃ ~ 950 ℃, and the pre-burning time is 30 ~ 60 minutes;
⑶ pulverize: carry out wet pulverization add minor component in the principal constituent Preburning material that upper step pre-burning obtains after, grinding time is 90 ~ 150 minutes, and after pulverizing, the slip particle diameter is controlled at 1.0 ~ 1.5 μ m; Described minor component is with its standard substance CaCO separately
3, Nb
2O
5, V
2O
5And Co
2O
3The content of meter is respectively: CaCO
3: 0.03 wt% ~ 0.04 wt%, Nb
2O
5: 0.005 wt% ~ 0.01 wt%, V
2O
5: 0.01 wt% ~ 0.03 wt%, Co
2O
3: 0.03 wt% ~ 0.05 wt%;
⑷ granulation: added 1.5% the PVA that is equivalent to slip weight at the slip in upper step, adopt mist projection granulating, obtain particulate material;
⑸ compacting: adopt the powder former compacting to obtain blank the particulate material in upper step, the pressed density of blank is controlled at 3.0 ± 0.2g/cm
3
⑹ sintering: blank sintering in clock hood type furnace that the upper step is obtained, temperature rise rate is controlled at 1.25 ~ 3 ℃/minute, carrying out densification at 900 ℃ to sintering temperature controls, control oxygen level lower than 1%, sintering temperature is controlled at 1200 ℃ ~ 1220 ℃, the holding-zone Control for Oxygen Content is incubated 3 ~ 5 hours 3.0% ~ 5.0%, and rate of temperature fall is controlled at 1.25 ~ 2 ℃/minute.
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| CN103117146A (en) * | 2013-02-26 | 2013-05-22 | 苏州冠达磁业有限公司 | High-Curie-temperature low-loss high-strength ferrite magnetic block and preparation method thereof |
| CN103771849B (en) * | 2014-01-06 | 2015-07-01 | 苏州冠达磁业有限公司 | High-performance soft magnet for high-frequency low-loss switching mode power supply transformer |
| CN106747394A (en) * | 2016-11-24 | 2017-05-31 | 上海宝钢磁业有限公司 | A kind of high magnetic permeability lower losses ferrite material and preparation method thereof |
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| CN109896848A (en) * | 2019-04-22 | 2019-06-18 | 南通冠优达磁业有限公司 | A kind of preparation method of low-consumption Mn-Zn ferrite |
| CN110511015A (en) * | 2019-09-30 | 2019-11-29 | 山东凯通电子有限公司 | The preparation method of manganese-zinc ferrite |
| CN112382455B (en) * | 2020-11-12 | 2024-02-23 | 南通三优佳磁业有限公司 | Ferrite material for common-mode inductance choke coil |
| CN112382456B (en) * | 2020-11-12 | 2022-02-22 | 南通三优佳磁业有限公司 | Preparation method of soft magnetic ferrite material for power converter of hybrid electric vehicle |
| CN112456994A (en) * | 2020-11-27 | 2021-03-09 | 天通控股股份有限公司 | Low-temperature sintered high-frequency low-loss MnZn soft magnetic ferrite and preparation method thereof |
| CN116891378B (en) * | 2023-08-07 | 2024-09-27 | 广东肇庆微硕电子有限公司 | Bias-reduction-resistant lean iron-manganese-zinc ferrite material and preparation method thereof |
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Effective date of registration: 20210210 Address after: 314499 1st floor, East District, building 2, No. 306, Gushui Road, Haining Economic Development Zone, Haining City, Jiaxing City, Zhejiang Province Patentee after: Haining Ruisi Technology Co.,Ltd. Address before: 314400 Pioneer Building, No. 5, 128 Shuanglian Road, Haining Economic Development Zone, Jiaxing City, Zhejiang Province, 4th Floor Patentee before: TIANTONG RUIHONG TECHNOLOGY Co.,Ltd. |
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