CN101286397B - Initial magnetic-inductive capacity 40 (-8) (+8) nickel-zinc ferrite material and preparation method - Google Patents
Initial magnetic-inductive capacity 40 (-8) (+8) nickel-zinc ferrite material and preparation method Download PDFInfo
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- CN101286397B CN101286397B CN200810059671XA CN200810059671A CN101286397B CN 101286397 B CN101286397 B CN 101286397B CN 200810059671X A CN200810059671X A CN 200810059671XA CN 200810059671 A CN200810059671 A CN 200810059671A CN 101286397 B CN101286397 B CN 101286397B
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Abstract
The invention discloses an oxygen body material of nickel, zinc and ferrum with initial permeability being 40<-8><+8> and a preparation method thereof. The main phase of the material is spinel structure, and the material essentially consists of Fe2O3, ZnO, MnO, NiO and CoO, and the contents of composition calculated by oxide are: 46mol percent to 49mol percent of Fe2O3, 2mol percent to 8mol percent of ZnO, 0.1mol percent to 1.0mol percent of MnO, 41.7mol percent to 48mol percent of NiO and 0.3mol percent to 1.5mol percent of CoO; the oxygen body material of nickel, zinc and ferrum with initial permeability being 40<-8><+8> has broadband, low electromagnetic consumption and good stability in larger working current and can be used for producing various power couplers of high-frequency electrodeless lamps with the working frequency in 30MHz; the material has extremely low electromagnetic consumption in high frequency ranging from 2MHz to 30MHz; when the frequency is in the range of 2.5MHz to 3MHz, the quality factor Q is more than 200; when the frequency is 30MHz, the quality factor Q is more than 80; due to good electromagnetic consumption characteristic in such wide frequency range, the oxygen body material can be applied to any electrodeless lamp with the working frequency in 30MHz.
Description
Technical field
The present invention relates to a kind ofly can be used to make operating frequency at the nickel-zinc-ferrite material of 30MHz with interior various high-frequency non-polar lamp power couplers, particularly a kind of initial permeability is 40
-8 + 8Nickel-zinc-ferrite material and preparation method.
Background technology
HF lamp without electrodes (High Frequency Electronic Discharge Lamp) is the novel light source of high-tech that integrates up-to-date electronics power-saving technique and electric light source technology, it is without filament, adopt magnetic field to come energizing gas discharge, luminous, have plurality of advantages such as energy-efficient, environmental protection, long-life.HF lamp without electrodes is by excitation power supply, and power coupler and bulb three parts are formed, and driving source produces the above electricity of 2MHz electric current frequently, and it delivers to power coupler through feeder line.When high-frequency current passes through power coupler, produce an electromagnetic field of high frequency.The magnetic field that changes promptly produces an electric field perpendicular to changes of magnetic field, and the electronics in bulb internal discharge space is quickened by electric field, when energy reaches certain value, bumps with gas molecule in the container, and the gas avalanche ionization forms plasma in the bulb.When the plasma excited atom is returned ground state, spontaneous ejaculation ultraviolet light, it excites the phosphor powder on the bulb walls to send visible light.
The technological development of HF lamp without electrodes and application are attracting the scientific and technological development personnel and the enterpriser of the industry of electric light illumination both at home and abroad always.This is because HF lamp without electrodes has many unique distinctions, it integrates long-lived, energy-conservation and environmental protection, as a kind of novel green electric light source, its its resultant effect of comparing with the traditional electrical light source is far superior to the electric light source of other types, its technology and industry are in the fast-developing stage of growth at present, the same with led light source, HF lamp without electrodes is a kind of rising industry.
Road as from the foregoing, HF lamp without electrodes needs an electromagnetic field of high frequency to come activated plasma, and high frequency magnetic field is produced by power coupler, the power-conversion efficiencies of power coupler has also directly determined the Energy Efficiency Ratio of HF lamp without electrodes in addition, so the quality of power coupler is one of key problem in technology of HF lamp without electrodes.Power coupler itself is the inductor of high frequency oscillation circuit, both is made of lead institute on the soft magnetic ferrite.Hence one can see that, and the power-conversion efficiencies of power coupler mainly is subjected to the influence of soft magnetic ferrite electromagnetic property.
Current, external general employing 3F4 power manganese-zinc ferrite is applied to prepare the power coupler in the HF lamp without electrodes, but manganese-zinc ferrite is owing to exist
Such conduction is right, so its resistivity is lower usually, and because the operating frequency of HF lamp without electrodes is generally more than the 2MHz, this causes ferritic eddy current loss sharply to rise, thereby greatly reduces the efficient of light fixture.In addition, because the eddy current loss of manganese-zinc ferrite is very big, and eddy current loss mainly is converted into heat, this causes ferritic in the course of the work temperature can reach more than 100 ℃ unexpectedly, thereby make 3F4 power manganese-zinc ferrite in the assembling power coupler, just must will carry out special insulation processing and skeleton support, cause technology comparatively complicated, increased production cost.
Summary of the invention
The objective of the invention is provides a kind of higher electric resistivity that has for the deficiency that solves above-mentioned technology, under the big electric current of high frequency, have utmost point lower electromagnetic loss, solve effectively that high-frequency non-polar lamp power coupler efficient is lower, the big problem of caloric value be used to that to make operating frequency be 40 at 30MHz with the initial permeability of interior various high-frequency non-polar lamp power couplers
-8 + 8Nickel-zinc-ferrite material and preparation method.
In order to achieve the above object, the designed a kind of initial permeability of the present invention is 40
-8 + 8Nickel-zinc-ferrite material, its principal phase is a spinel structure, comprise Fe main the composition
2O
3, ZnO, MnO, NiO and CoO, it is characterized in that it forms content and be calculated as with oxide: Fe
2O
3Be 46mol%～49mol%; ZnO is 2mol%～8mol%; MnO is 0.1mol%～1.0mol%; NiO is 41.7mol%～48mol%; CoO is 0.3mol%～1.5mol%.For the ease of the acceleration of sintering solid phase reaction, thereby reduced sintering temperature effectively, it is characterized in that it also includes the nanoscale V as the sintering flux of the 0.3wt%～0.6wt% that accounts for total weight
2O
5In preparation process, can also add the polyvinyl alcohol (PVA) that accounts for total weight 9wt%～14wt%, polyvinyl alcohol is volatilized behind the final molding sintering fully.
A kind of initial permeability is 40
-8 + 8The preparation method of nickel-zinc-ferrite material, it is characterized in that the preparation method is:
1) ball milling:
With the 46mol%～49mol%Fe that weighs up
2O
3, 2mol%～8mol%ZnO, 0.1mol%～1.0mol%MnCO
3, 41.7mol%～48mol%NiO and 0.3mol%～1.5mol%CoO raw material put into sand mill, add deionized water, the weight of deionized water is 1.2 times of raw material total weight, the ball milling time is 1 hour～2 hours;
2) pre-burning:
With a good raw material oven dry of ball milling, to put into electric furnace and carry out pre-burning, calcined temperature is 950 ℃～1100 ℃, the pre-burning time is 1.5 hours～3.5 hours, cools off with stove after the pre-burning;
3) impurity adds:
Select nanometer V for use
2O
5As the sintering flux, its addition is the 0.3wt%～0.6wt% that accounts for total weight.
4) secondary ball milling:
The pre-imitation frosted glass that has added behind the impurity is put into sand mill, add deionized water, the weight of deionized water is 0.9 times of raw material total weight, and the ball milling time is 2 hours～4 hours, requires powder average particle size behind the ball milling between 1.00 μ m～1.60 μ m.
5) forming and sintering:
The pre-imitation frosted glass oven dry that secondary ball milling is good, add the polyvinyl alcohol (PVA) that accounts for total weight 9wt%～14wt%, evenly mix, the granulation of sieving, the box type furnace sintering is put in compression moulding, and sintering temperature is controlled within 1100 ℃～1250 ℃, temperature retention time is 1 hour～3 hours, gets final product with the stove cool to room temperature.
Initial permeability provided by the invention is 40
-8 + 8Nickel-zinc-ferrite material and preparation method, calcined temperature be 950 ℃～1100 ℃, sintering temperature be 1100 ℃～1250 ℃, in 2MHz～30MHz high-frequency range, have extremely low electromagnetic consumable, initial permeability is 40
-8 + 8, at-20 ℃～100 ℃ very wide temperature range internal ratio temperatures coefficient less than 8.0 * 10
-6Nickel-zinc-ferrite material in only have the spinelle phase, do not have other dephasigns, crystallite dimension is between 1.15 μ m～3.10 μ m.
Initial magnetic conductance 0 rate provided by the invention is 40
-8 + 8Nickel-zinc-ferrite material and preparation method, raw material are selected commercially pure Fe
2O
3, ZnO, MnCO
3, NiO and CoO.Take by weighing various raw material according to the component molecules formula and carry out ball milling one time, one time ball-grinding machine is selected sand mill for use.In mechanical milling process, add deionized water, the weight of deionized water is 1.2 times of raw material total weight, the ball milling time is 1 hour～2 hours, and raw material are mixed.
Temperature range during pre-burning is 950 ℃～1100 ℃, and calcined temperature is low excessively, will cause in the pre-burning process raw-material reaction incomplete, and this will be unfavorable for the follow-up sintering solid phase reaction of powder.And if sintering temperature is too high, will cause pre-burning to finish the rapid reduction of the pre-imitation frosted glass reactivity in back, this makes the follow-up sintering temperature raise, thereby will worsen ferritic electromagnetic consumable characteristic.
Select nano level V for use
2O
5As adding impurity.V
2O
5Fusing point be lower than 700 ℃, in sintering process, can under very low temperature, form liquid phase, the acceleration of sintering solid phase reaction, thereby reduced sintering temperature effectively.But too much V
2O
5The interpolation meeting on the crystal boundary of ferritic spinelle phase intergranule, form nonmagnetic glassy phase, this will produce a kind of magnetic dilution effect, cause the decline of saturation magnetization and magnetic permeability and the deterioration of electromagnetic consumable characteristic.Select other V of nanometer chi level for use
2O
5Powder is as the sintering flux, because nanometer powder has very big specific area and quite high surface energy, its fusing point will be lower, more help the acceleration of sintering solid phase reaction, thereby the amount of required interpolation will be still less, and this helps improving the magnetic property of nickel-zinc ferrite.
Pre-imitation frosted glass is carried out secondary ball milling, and requiring the particle mean size of the particle behind the ball milling is between 1.00 μ m～1.60 μ m, and this makes preburning powdered material have certain sintering reaction activity, helps follow-up sintering reaction.
A kind of initial permeability provided by the invention is 40
-8 + 8Nickel-zinc-ferrite material and preparation method, under big operating current, have the wideband lower electromagnetic loss and good wide temperature is stable, can be used to make operating frequency at the nickel-zinc-ferrite material of 30MHz with interior various high-frequency non-polar lamp power couplers.This material has extremely low electromagnetic consumable in 2MHz～30MHz high-frequency range, its quality factor Q is more than 200 when 2.5MHz～3MHz frequency, its quality factor Q is more than 80 when the 30MHz frequency, in so wide frequency range, all has good electromagnetic consumable characteristic, this can guarantee this material can be advantageously applied to operating frequency 30MHz with interior any electrodeless lamp in, enlarged application surface, the market demand is huge.In addition, by the nickel-zinc-ferrite material that the inventive method provides, initial permeability is 40
-8 + 8, under big operating current, have wideband lower electromagnetic loss and good temperature characteristics, in-20 ℃～100 ℃ very wide temperature ranges, its than temperature coefficient less than 8.0 * 10
-6, Curie temperature is greater than 300 ℃.This material has utmost point lower electromagnetic loss under the big electric current of high frequency, still can operate as normal under higher temperature, these help to reduce the electromagnetic consumable and the heating of high-frequency non-polar lamp power coupler, guarantee its normal steady operation, help miniaturization of devices, so this material has very vast market prospect in novel electrodeless lamp illuminating system.
A kind of initial permeability provided by the invention is 40
-8 + 8Nickel-zinc-ferrite material and preparation method owing to have the pre-burning and the sintering range of broad, and need not atmosphere protection, make process repeatability and consistency of product all fine.In the preparation method owing to adopted the V of Nano grade
2O
5As the sintering flux, this will cause reducing of sintering flux use amount, help to improve the electromagnetic consumable characteristic of nickel-zinc ferrite.
Embodiment
The invention will be further described in conjunction with subordinate list below by embodiment.
A kind of initial permeability that present embodiment provides is 40
-8 + 8Nickel-zinc-ferrite material and preparation method, can realize by following scheme:
Embodiment 1
1) raw-material selection: a kind of initial permeability that present embodiment provides is 46 nickel-zinc-ferrite material and preparation method, and its raw material are selected commercially pure Fe
2O
3, ZnO, MnCO
3, NiO and CoO.
2) composition design and weighing: according to Fe
2O
3For 49mol%, ZnO are 8mol%, MnCO
3For 1mol%, NiO are that 41.7mol% and CoO are 0.3mol%;
3) raw-material mixing: the raw material that weigh up are put into sand mill, add deionized water, the weight of deionized water is 1.2 times of raw material total weight, and the ball milling time is 2 hours;
4) pre-burning: with a good raw material oven dry of ball milling, put into electric furnace and carry out pre-burning, calcined temperature is 950 ℃, and the pre-burning time is 3.5 hours, cools off with stove after the pre-burning.After the pre-burning, pre-imitation frosted glass is carried out the XRD facies analysis, determine only to have spinel structure in the pre-imitation frosted glass, do not have other dephasigns;
5) impurity adds: select nanometer V
2O
5Powder adds as impurity, and its addition is the 0.6wt% that accounts for total weight.
6) secondary ball milling: the pre-imitation frosted glass that has added behind the impurity is put into sand mill, add deionized water, the weight of deionized water is 0.9 times of raw material total weight, and the ball milling time is 4 hours, requires powder average particle size behind the ball milling between 1.00 μ m～1.60 μ m.
7) forming and sintering: the pre-imitation frosted glass oven dry that secondary ball milling is good, add the polyvinyl alcohol (PVA) that accounts for total weight 9wt%, evenly mix, the granulation of sieving, the box type furnace sintering is put in compression moulding, sintering temperature is 1100 ℃, and temperature retention time is 3 hours, gets final product with the stove cool to room temperature.
The magnetism testing of the sample ring for preparing carries out on Hp4284A electric impedance analyzer and HF Q meter, and the density of sample adopts buoyancy method to measure.
The magnetic property of sample and density measurement result are as shown in table 1:
Table 1:
From table 1, can see, it is 46 that the nickel-zinc ferrite sample of preparing has initial permeability, under 2.65MHz, 3MHz and 30MHz frequency quality factor Q respectively up to 263,257 and 91 ,-20 ℃～100 ℃ very wide temperature range internal ratio temperature coefficient only be 7.3 * 10
-6, saturation flux density is the good electric magnetic characteristic of 327mT, and Curie temperature is up to 308 ℃.Therefore this material is applied to prepare the Ferrite Material of the power coupler of HF lamp without electrodes than existing 3F4 etc., has better electromagnetic consumable and temperature characterisitic, can meet the need of market better.
Embodiment 2
1) raw-material selection: a kind of initial permeability that present embodiment provides is 39 nickel-zinc-ferrite material and preparation method, and its raw material are selected commercially pure Fe
2O
3, ZnO, MnCO
3, NiO and CoO.
2) composition design and weighing: according to Fe
2O
3For 46mol%, ZnO are 4.4mol%, MnCO
3For 0.1mol%, NiO are that 48mol% and CoO are 1.5mol%.
3) raw-material mixing: the raw material that weigh up are put into sand mill, add deionized water, the weight of deionized water is 1.2 times of raw material total weight, and the ball milling time is 1 hour.
4) pre-burning: with a good raw material oven dry of ball milling, put into electric furnace and carry out pre-burning, calcined temperature is 1100 ℃, and the pre-burning time is 1.5 hours, cools off with stove after the pre-burning.After the pre-burning, pre-imitation frosted glass is carried out the XRD facies analysis, determine only to have spinel structure in the pre-imitation frosted glass, do not have other dephasigns.
5) impurity adds: select nanometer V
2O
5Powder adds as impurity, and its addition is the 0.3wt% that accounts for total weight.
6) secondary ball milling: the pre-imitation frosted glass that has added behind the impurity is put into sand mill, add deionized water, the weight of deionized water is 0.9 times of raw material total weight, and the ball milling time is 2 hours, requires powder average particle size behind the ball milling between 1.00 μ m～1.60 μ m.
7) forming and sintering: the pre-imitation frosted glass oven dry that secondary ball milling is good, add the polyvinyl alcohol (PVA) that accounts for total weight 14wt%, evenly mix, the granulation of sieving, the box type furnace sintering is put in compression moulding, sintering temperature is 1250 ℃, and temperature retention time is 1 hour, gets final product with the stove cool to room temperature.
The magnetism testing of the sample ring for preparing carries out on Hp4284A electric impedance analyzer and HF Q meter, and the density of sample adopts buoyancy method to measure.
The magnetic property of sample and density measurement result are as shown in table 2:
Table 2:
From table 2, can see, it is 39 that the nickel-zinc ferrite sample of preparing has initial permeability, under 2.65MHz, 3MHz and 30MHz frequency quality factor Q respectively up to 211,213 and 83 ,-20 ℃～100 ℃ very wide temperature range internal ratio temperature coefficient only be 7.9 * 10
-6, saturation flux density is the good electric magnetic characteristic of 312mT, and Curie temperature is up to 307 ℃.Therefore this material is applied to prepare the Ferrite Material of the power coupler of HF lamp without electrodes than existing 3F4 etc., has better electromagnetic consumable and temperature characterisitic, can meet the need of market better.
Embodiment 3
1) raw-material selection: a kind of initial permeability that present embodiment provides is 34 nickel-zinc-ferrite material and preparation method, and its raw material are selected commercially pure Fe
2O
3, ZnO, MnCO
3, NiO and CoO.
2) composition design and weighing: according to Fe
2O
3For 49mol%, ZnO are 2mol%, MnCO
3For 0.4mol%, NiO are that 48mol% and CoO are 0.6mol%.
3) raw-material mixing: the raw material that weigh up are put into sand mill, add deionized water, the weight of deionized water is 1.2 times of raw material total weight, and the ball milling time is 1.5 hours.
4) pre-burning: with a good raw material oven dry of ball milling, put into electric furnace and carry out pre-burning, calcined temperature is 1000 ℃, and the pre-burning time is 2 hours, cools off with stove after the pre-burning.After the pre-burning, pre-imitation frosted glass is carried out the XRD facies analysis, determine only to have spinel structure in the pre-imitation frosted glass, do not have other dephasigns.
5) impurity adds: select nanometer V
2O
5Powder adds as impurity, and its addition is the 0.4wt% that accounts for total weight.
6) secondary ball milling: the pre-imitation frosted glass that has added behind the impurity is put into sand mill, add deionized water, the weight of deionized water is 0.9 times of raw material total weight, and the ball milling time is 3 hours, requires powder average particle size behind the ball milling between 1.00 μ m～1.60 μ m.
7) forming and sintering: the pre-imitation frosted glass oven dry that secondary ball milling is good, add the polyvinyl alcohol (PVA) that accounts for total weight 12wt%, evenly mix, the granulation of sieving, the box type furnace sintering is put in compression moulding, sintering temperature is 1200 ℃, and temperature retention time is 2 hours, gets final product with the stove cool to room temperature.
The magnetism testing of the sample ring for preparing carries out on Hp4284A electric impedance analyzer and HF Q meter, and the density of sample adopts buoyancy method to measure.
The magnetic property of sample and density measurement result are as shown in table 3:
Table 3:
From table 3, can see, it is 34 that the nickel-zinc ferrite sample of preparing has initial permeability, under 2.65MHz, 3MHz and 30MHz frequency quality factor Q respectively up to 231,232 and 84 ,-20 ℃～100 ℃ very wide temperature range internal ratio temperature coefficient only be 7.6 * 10
-6, saturation flux density is the good electric magnetic characteristic of 301mT, and Curie temperature is up to 322 ℃.Therefore this material is applied to prepare the Ferrite Material of the power coupler of HF lamp without electrodes than existing 3F4 etc., has better electromagnetic consumable and temperature characterisitic, can meet the need of market better.
Claims (3)
1. an initial permeability is 40
-8 + 8Nickel-zinc-ferrite material, its principal phase is a spinel structure, comprise Fe main the composition
2O
3, ZnO, MnO, NiO and CoO, it is characterized in that it forms content and be calculated as with oxide: Fe
2O
3Be 46mol%～49mol%; ZnO is 2mol%～8mol%; MnO is 0.1mol%～1.0mol%; NiO is 41.7mol%～48mol%; CoO is 0.3mol%～1.5mol%.
2. a kind of initial permeability according to claim 1 is 40
-8 + 8Nickel-zinc-ferrite material, it is characterized in that it also includes the nanoscale V as the sintering flux of the 0.3wt%～0.6wt% that accounts for total weight
2O
5
3. an initial permeability is 40
-8 + 8The preparation method of nickel-zinc-ferrite material, it is characterized in that the preparation method is:
1) ball milling:
With the 46mol%～49mol%Fe that weighs up
2O
3, 2mol%～8mol%ZnO, 0.1mol%～1.0mol%MnCO
3, 41.7mol%～48mol%NiO and 0.3mol%～1.5mol%CoO raw material put into sand mill, add deionized water, the weight of deionized water is 1.2 times of raw material total weight, the ball milling time is 1 hour～2 hours;
2) pre-burning:
With a good raw material oven dry of ball milling, to put into electric furnace and carry out pre-burning, calcined temperature is 950 ℃～1100 ℃, the pre-burning time is 1.5 hours～3.5 hours, cools off with stove after the pre-burning;
3) impurity adds:
Select nanometer V for use
2O
5As the sintering flux, its addition is the 0.3wt%～0.6wt% of total weight;
4) secondary ball milling:
The pre-imitation frosted glass that has added behind the impurity is put into sand mill, add deionized water, the weight of deionized water is 0.9 times of raw material total weight, and the ball milling time is 2 hours～4 hours, requires powder average particle size behind the ball milling between 1.00 μ m～1.60 μ m;
5) forming and sintering:
The pre-imitation frosted glass oven dry that secondary ball milling is good, the polyvinyl alcohol that adds the 9wt%～14wt% of total weight, evenly mix, the granulation of sieving, the box type furnace sintering is put in compression moulding, and sintering temperature is controlled within 1100 ℃～1250 ℃, temperature retention time is 1 hour～3 hours, gets final product with the stove cool to room temperature.
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| CN102167572A (en) * | 2010-12-24 | 2011-08-31 | 嘉兴龙晴照明科技有限公司 | Nickel zinc ferrite material with initial permeability of 10+/-20 percent and preparation method thereof |
| CN102737953B (en) * | 2011-04-08 | 2016-03-02 | 高永生 | A kind of HF lamp without electrodes |
| CN105565790B (en) * | 2014-10-09 | 2020-06-26 | 桐乡市耀润电子有限公司 | YR950 wide-temperature high-direct-current superposition low-power-consumption manganese-zinc ferrite material and preparation method thereof |
| CN104575925A (en) * | 2015-02-11 | 2015-04-29 | 海安县巨力磁材有限责任公司 | Corrosion-resistance radial heterogenous magnetic ring |
| CN104891976A (en) * | 2015-04-24 | 2015-09-09 | 马鞍山科信咨询有限公司 | Low-loss nickel-zinc ferrite material and preparation method |
| CN106903319A (en) * | 2017-02-20 | 2017-06-30 | 歌尔股份有限公司 | A kind of Multi-layer spherical material and preparation method thereof |
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