CN116003118A - Preparation method of low-temperature-coefficient nickel-zinc ferrite material - Google Patents
Preparation method of low-temperature-coefficient nickel-zinc ferrite material Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 74
- 229910001053 Nickel-zinc ferrite Inorganic materials 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims description 16
- 239000002994 raw material Substances 0.000 claims abstract description 73
- 239000000203 mixture Substances 0.000 claims description 25
- 238000000034 method Methods 0.000 claims description 18
- 239000000843 powder Substances 0.000 claims description 18
- 238000005245 sintering Methods 0.000 claims description 18
- 238000000227 grinding Methods 0.000 claims description 14
- 238000009472 formulation Methods 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 4
- 238000004891 communication Methods 0.000 abstract description 7
- 239000013078 crystal Substances 0.000 abstract description 6
- 230000005540 biological transmission Effects 0.000 abstract description 5
- 238000013461 design Methods 0.000 abstract description 4
- 238000012545 processing Methods 0.000 abstract description 2
- 230000008054 signal transmission Effects 0.000 abstract description 2
- 229910000859 α-Fe Inorganic materials 0.000 description 34
- 230000035699 permeability Effects 0.000 description 15
- 238000012360 testing method Methods 0.000 description 13
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 12
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 10
- 239000012535 impurity Substances 0.000 description 8
- 230000008569 process Effects 0.000 description 8
- 230000009286 beneficial effect Effects 0.000 description 7
- QELJHCBNGDEXLD-UHFFFAOYSA-N nickel zinc Chemical compound [Ni].[Zn] QELJHCBNGDEXLD-UHFFFAOYSA-N 0.000 description 5
- 239000011787 zinc oxide Substances 0.000 description 5
- 101100513612 Microdochium nivale MnCO gene Proteins 0.000 description 4
- 239000000654 additive Substances 0.000 description 4
- 238000000498 ball milling Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 3
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 230000002401 inhibitory effect Effects 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910000480 nickel oxide Inorganic materials 0.000 description 2
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 238000003746 solid phase reaction Methods 0.000 description 2
- 229910018605 Ni—Zn Inorganic materials 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 229910052729 chemical element Inorganic materials 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- -1 iron peroxide Chemical class 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- WJZHMLNIAZSFDO-UHFFFAOYSA-N manganese zinc Chemical compound [Mn].[Zn] WJZHMLNIAZSFDO-UHFFFAOYSA-N 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 238000009700 powder processing Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
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Abstract
The invention relates to a low temperature coefficient nickel zinc ferrite material, which comprises main formula raw materials and doping raw materials, wherein the main formula raw materials are prepared by the following components in percentage by weight: fe (Fe) 2 O 3 58 to 60.5mol percent, 18.5 to 22.5mol percent of NiO and 18.5 to 20.0mol percent of ZnO; the doping raw materials are calculated according to the total mass percentage of the main formula raw materials: mnCO 3 1.5wt％～2.0wt％；Co 2 O 3 0.25wt％～0.45wt％、BaCO 3 0.15wt％～0.5wt％、LiCO 3 0.1 to 0.15 weight percent. The material provided by the invention can be widely applied to circuit module designs in the communication fields of crystal oscillators, signal transmission and processing, high-frequency transmission and transmission sensing devices and the like.
Description
Technical Field
The invention relates to a preparation method of a low-temperature coefficient nickel-zinc ferrite material, belonging to the technical field of ferrite materials.
Background
Ferrite material is a new nonmetallic magnetic material developed in the 40 s of the 20 th century, is generally classified into manganese zinc and nickel zinc materials, and is widely applied to the module design of power supply and communication circuits, and is used as a transformer, an inductance device and the like.
The product prepared from the nickel-zinc ferrite material is mainly applied to circuit module designs of high-frequency (2-30 MHz) transmission inductance devices, broadband interference suppressors, balance converters and the like in the military and civil communication fields at present or in the future, and the use frequency is from 1MH to 30MHz. The temperature range of the current civil product application is 20-60 ℃, the environment temperature of the current civil product application is generally-55-125 ℃ in the field of military communication, the examination requirements on the high-low temperature characteristics of the component products are strict, and the material with larger high-low temperature inductance performance change can not meet the use requirements. Most of the existing domestic and foreign materials are aimed at products with the temperature of 20-60 ℃, and the working temperature of-55-125 ℃ is poor in stability, so that the technical problem to be solved is that materials with low temperature coefficients at-55-125 ℃ can be provided.
Disclosure of Invention
First, the technical problem to be solved
In order to solve the problems in the prior art, the invention provides a preparation method of a low-temperature coefficient nickel zinc ferrite material, and the obtained material can meet the use requirement of-55 ℃ to 125 ℃, is a ferrite material with stable inductance performance at high temperature and low temperature, and meets the use requirement of a high frequency band.
(II) technical scheme
In order to achieve the above purpose, the main technical scheme adopted by the invention comprises the following steps:
a low temperature coefficient nickel zinc ferrite material comprising main formulation raw materials and doping raw materials, wherein the main formulation raw materials are dosed according to the percentage of the total substances thereof, and the main formulation raw materials comprise: fe (Fe) 2 O 3 58mol% -60.5 mol%, niO18.5mol% -22.5 mol%, znO 18.5mol% -20.0 mol%; the doping raw material is MnCO calculated according to the percentage of the total mass of the raw materials of the main formula 3 1.5wt％～2.0wt％；Co 2 O 3 0.25wt％～0.45wt％、BaCO 3 0.15wt％～0.5wt％、LiCO 3 0.1wt％～0.15wt％。
The preparation method of the nickel-zinc ferrite material with low temperature coefficient comprises the following steps:
s1, preparing main formula raw materials, wherein the main formula raw materials are prepared according to the weight percentage of the total substances, and the main formula raw materials comprise the following components: fe (Fe) 2 O 3 58mol％～60.5mol％，NiO 18.5mol％～22.5mol％，ZnO18.5mol％～20.0mol％；
S2, preparing doping raw materials, wherein the doping raw materials comprise the following raw materials in percentage by mass of the total mass of the raw materials in the main formula: mn CO 3 1.5wt％～2.0wt％；Co 2 O 3 0.25wt％～0.45wt％、BaCO 3 0.15wt％～0.5wt％、LiCO 3 0.1wt％～0.15wt％；
S3, grinding and mixing the main formula raw materials and the doping raw materials, placing the mixture in a furnace, heating the mixture, preserving heat for a period of time, and cooling the mixture to room temperature to obtain a presintered blank;
s4, grinding the presintered blank to obtain presintered powder;
s5, after the presintered powder is made into a blank with a required shape, the blank is placed in a furnace for sintering, and then the blank is cooled to room temperature, so that the nickel-zinc ferrite material with high temperature stability is obtained.
The magnetic permeability of the nickel-zinc ferrite material with high temperature stability obtained by the invention is 100+/-25 percent (namely, the magnetic permeability is in the range of 75-125), and the magnetic permeability in the range is called as a product with the magnetic permeability of 100.
In the above preparation method, preferably, in the step S3, the grinding time is 2 to 4 hours, and the heat preservation time is 2 to 4 hours after the temperature is raised to 1040 to 1060 ℃ at a rate of 1.5 to 2.5 ℃/S at room temperature.
In the above-described production method, preferably, in step S4, the grinding condition is such that the particle diameter is between 0.3 and 5.0 μm and occupies 80% to 90%.
In the preparation method, preferably, in the step S5, the sintering condition is that the temperature is raised to 1230-1250 ℃ from room temperature, the heating rate is less than or equal to 2.5 ℃/min, and the temperature is kept for 3-4 hours.
(1) The nickel-zinc ferrite material with the low temperature coefficient and the magnetic conductivity of 100 provided by the invention has the advantages of high temperature stability, reduced temperature peak fluctuation and improved frequency characteristic by adding the nickel-zinc ferrite material on the basis of a main formula, and has the advantages of low temperature peak fluctuation, high magnetic conductivity, low temperature coefficient and low temperature coefficient,Doping materials with little influence on parameters such as Q, curie temperature and the like so as to ensure realization of various performance indexes; it was found that the addition of a specific amount of Co 2 O 3 The induced anisotropy can be generated, which is beneficial to improving the cut-off frequency and reducing the loss; on the other hand, co addition 2 O 3 After that, due to Co 3+ Will be at mu i The second peak on the T curve is advantageous for improving the temperature characteristics, preferably Co 2 O 3 The dosage of (2) is 0.25-0.45 wt%; adding a specific amount of MnCO 3 Can obviously reduce sintering temperature, increase crystal wall thickness, improve impedance value, improve dielectric constant and high-frequency characteristics of ferrite material, and is preferably MnCO 3 The dosage of (2) is 1.5-2.0 wt%; adding a specific amount of BaCO 3 Is beneficial to reducing sintering temperature, inhibiting grain growth, obviously improving cut-off frequency, and is preferably BaCO 3 The dosage of (2) is 0.15-0.5 wt%; liCO may also be added 3 The LiCO is preferable for adjusting the temperature profile by the impurities such as 3 0.1 to 0.15 weight percent.
(2) The presintering temperature of the nickel-zinc ferrite is closely related to the structure of spinel grains, and the discontinuous growth of the grains is easily formed due to the overhigh temperature, so that the grains are oversized or uneven, and the magnetic performance is seriously influenced; too low a temperature lowers the sintering density and increases the loss; the invention not only preserves the activity of raw materials but also increases the shrinkage of the raw materials through preliminary solid phase reaction by a specific pre-sintering and sintering process, thereby improving the green density of the materials, reducing the sintering temperature of the products and further reducing the temperature coefficient; the grain size of the presintered powder is refined, so that the grain size of the presintered powder is fine, the powder processing, the forming and the sintering are easy, the activity of the grain is kept, and the solid phase reaction is facilitated to obtain the ferrite material with better performance; the ferrite material provided by the invention is a nickel-zinc low-temperature coefficient material with high frequency, high magnetic conductivity and wide temperature application, and the ferrite material with excellent performance is obtained by controlling the presintering-ball milling-sintering process.
(III) beneficial effects
The beneficial effects of the invention are as follows:
the invention providesThe nickel-zinc ferrite material with low temperature coefficient has stable temperature characteristic and electric performance in working, meets the wide-temperature stable use requirement of-55 ℃ to 125 ℃, and has specific temperature coefficient smaller than 2 multiplied by 10 -6 Has wide application prospect in the communication field.
The low temperature coefficient nickel zinc ferrite material provided by the invention is prepared by adding Co 2 O 3 Induced anisotropy is generated, which is beneficial to increasing the cut-off frequency, reducing loss and improving temperature characteristics, improving temperature stability and adding MnO 2 Obviously reduce sintering temperature, increase crystal wall thickness, improve impedance value, improve dielectric constant, improve high frequency characteristics of ferrite material, and add BaCO 3 The material is favorable for reducing sintering temperature, inhibiting grain growth and obviously improving cut-off frequency, and can be widely applied to circuit module designs in the communication fields of crystal oscillators, signal transmission and processing, high-frequency transmission and transmission sensing devices and the like.
Drawings
FIG. 1 is a graph showing inductance of a sample loop prepared in an example of the present invention as a function of temperature.
Detailed Description
The ferrite material with stable inductance performance and magnetic permeability of about 100 at the high temperature and the low temperature, which meets the use requirement of a high frequency band, is prepared to solve the problems in the prior art. The method provided by the invention obtains a formula of raw materials and additives with optimal performance through the method of adjusting the content ratio of the raw materials and adding specific chemical elements, and prepares a finished product through specific technological parameters, thereby improving the stability of the electrical performance of the material and the performance quality of the finished ferrite material.
Specifically, the invention provides a preparation method of a low temperature coefficient nickel zinc ferrite material, which is considered as follows:
1. the manufacturing process of the ferrite material comprises the following steps: the ferrite material is mainly composed of ferric oxide, nickel oxide and zinc oxide, and the three materials are uniformly mixed, presintered, ball-milled and dried according to a certain formula proportion to prepare a ferrite base material, and the addition and adjustment of impurity elements are carried out on the base material until the ferrite base material reaches the requirements of certain performance, and the ferrite base material is prepared into a product with a certain specification and shape, and the performance of the material is tested. And finally, carrying out formula fixing and process repeated verification. The fabrication of ferrite materials thus involves two important aspects, one being the formulation ratio and the other being the fabrication process.
The raw materials comprise main formula raw materials and doping raw materials, wherein the main formula raw materials are determined by a large number of experimental researches to comprise the following components in percentage of the total substances: fe (Fe) 2 O 3 58 to 60.5mol percent, 18.5 to 22.5mol percent of NiO, 18.5 to 20.0mol percent of ZnO and the balance of unavoidable impurities; determining a main formula: the main component of ferrite is ferric oxide, wherein the main formula content refers to the molar content, and the ferric oxide content is determined as the iron peroxide formula, namely Fe 2 O 3 The molar content of (2) exceeds 50%.
2. Adding and adjusting doping raw materials:
the purpose is as follows: the wide temperature performance of the material is improved by joint doping: doping means that additives with certain types and contents are added into ferrite, generally oxides of metal or nonmetal elements are added into ferrite to improve the microstructure of the ferrite, so that the aim of improving magnetic performance is fulfilled, and after the content proportion of Fe-Ni-Zn is determined, the types and contents of impurities are selected to be added into ferrite to improve the crystal structure, and materials with high temperature stability are preferred. The method is beneficial to reducing temperature peak fluctuation and improving frequency characteristics, and the method is used for selecting the impurity adding material with little influence on parameters such as magnetic permeability, Q, curie temperature and the like so as to ensure realization of various performance indexes.
The function of the additive used in the invention is as follows: a. co addition 2 O 3 The function of (3): the addition of a small amount of cobalt in ferrite preparation can generate induced anisotropy, which is beneficial to improving the cut-off frequency and reducing the loss. On the other hand due to Co 3+ The presence of (2) will exhibit a second peak on the mu i-T curve, which is advantageous for improving the temperature characteristics. b. Adding MnO 2 The function of (3): the sintering temperature is reduced, the thickness of the crystal wall is increased, and the impedance value is improved. c. Additive BaCO 3 : the reduction of sintering temperature suppresses grain growth, which reduces permeability, but can raise cut-off frequency. Preferably, the doping raw materials are prepared according to a main formulaThe total mass percentage of the raw materials comprises: mnCO 3 1.5wt％～2.0wt％；Co 2 O 3 0.25wt％～0.45wt％、BaCO 3 0.15wt％～0.5wt％、LiCO 3 0.1wt％～0.15wt％。
4. Selection and control of a process
The most critical ferrite obtaining process is a sintering process, proper temperature rising curve and temperature rising rate are mastered as key factors for obtaining a ferrite core with stable and excellent performance, and the ferrite core is preferably heated to 1040-1060 ℃ from room temperature at the speed of 1.5-2.5 ℃/s, then is insulated for 2-4h, and is cooled to room temperature, so that a presintered blank is obtained. Secondly, refining the powder particles to obtain ferrite blanks with proper ball milling particle size, which is also an important factor with excellent performance, preferably grinding the presintered blanks until the particle size is 80% -90% of 0.3-5.0 mu m, and obtaining presintered powder; finally, after the presintered powder is made into a blank with a required shape, the blank is placed in a furnace, the temperature is raised to 1230-1250 ℃ from room temperature, the heating rate is less than or equal to 2.5 ℃/min, the heat is preserved for 3-4 hours, and then the blank is cooled to room temperature, so that the nickel-zinc ferrite material with high temperature stability is obtained.
The invention provides a preparation method of a nickel-zinc ferrite material with a low temperature coefficient and a magnetic conductivity of 100, which comprises the following steps:
s1, raw materials comprise main formula raw materials and doping raw materials, wherein the main formula raw materials are prepared by the following materials in percentage by weight of the total substances: fe (Fe) 2 O 3 58mol％～60.5mol％，NiO 18.5mol％～22.5mol％，ZnO 18.5molt％～20.0mol％；
S2, the doping raw materials comprise the following raw materials in percentage by mass of the total mass of the raw materials in the main formula: mnCO 3 1.5wt％～2.0wt％；Co 2 O 3 0.25wt％～0.45wt％、BaCO 3 0.15wt％～0.5wt％、LiCO 3 0.1wt％～0.15wt％；
S3, grinding and mixing the main formula raw materials and the doping raw materials for 2-4 hours, placing the mixture in a furnace, heating the mixture to 1040-1060 ℃ from room temperature at a speed of 1.5-2.5 ℃/S, preserving heat for 2-4 hours, and cooling the mixture to room temperature to obtain a presintered blank;
s4, grinding the presintered blank until the particle size is between 0.3 and 5.0 mu m and accounts for 80 to 90 percent, and obtaining presintered powder;
s5, after the presintered powder is made into a blank with a required shape, placing the blank in a furnace, heating to 1230-1250 ℃ from room temperature, keeping the temperature for 3-4 hours at a heating rate of less than or equal to 2.5 ℃/min, and cooling to the room temperature to obtain the nickel-zinc ferrite material with high temperature stability.
The invention will be better explained by the following detailed description of the embodiments with reference to the drawings.
Example 1
In the embodiment, the dosage of the main formula raw materials of the low-temperature coefficient nickel-zinc ferrite material is determined through experiments, and the specific main formula raw materials select Fe 2 O 3 NiO, znO and raw materials of Fe are weighed according to mole percent 2 O 3 High purity iron (purity 99.05%) was selected in japan, nickel oxide (purity 99.43%) was used for NiO, zinc oxide (purity 99.74%) was used for ZnO, which was produced in tandem. The different raw material dosages are specifically shown in table 1, the raw materials are mixed and then subjected to planetary ball milling for 2.5 hours, then dried, presintered for 2 hours at 1060 ℃, the presintered materials are placed in a rolling ball milling tank for secondary grinding for 24 hours, the grain size of the raw materials is 80% -90% of that of the raw materials between 0.3 and 5.0 mu m, and then the raw materials are subjected to heat preservation for 3.5 hours at 1185 ℃ in a sintering kiln (box furnace).
The results of performance testing of the materials obtained by the above preparation are shown in table 1.
TABLE 1 Performance test results when the amounts of the main recipe raw materials are different
As can be seen from the results of the table, the raw materials numbered 5 and 6 have better performance, so that the final determination of the percentage of each component in the raw materials of the main formula according to the total substances of the raw materials of the main formula in the invention is as follows: fe (Fe) 2 O 3 59mol% -60.5 mol%, niO 19.5mol% -21.5 mol%, znO19mol% -21.2 mol% (unavoidable impurities if any) and tested at room temperature to meet the existing nickelZinc permeability 100 material properties.
Examples 2 to 4
The amount of doping raw materials is determined in this example, and the doping raw materials are added based on the total weight of the main formulation raw materials, which are always in accordance with Fe 2 O 3 59.8mol%, niO20.5mol%, znO 19.7mol%, and the doping raw materials comprise MnCO 3 、Co 2 O 3 、BaCO 3 、LiCO 3 The method comprises the steps of carrying out a first treatment on the surface of the Ingredients were prepared at the levels indicated in table 2. Grinding and mixing the main formula raw materials and the doping raw materials for 3 hours, placing the mixture in a furnace, heating the mixture to 1060 ℃ from room temperature at a speed of 2 ℃/s, preserving heat for 2 hours, and cooling the mixture to the room temperature to obtain a presintered blank; grinding the presintered blank to 80-85 percent of the particle size of 0.3-5.0 mu m to obtain powder after ball milling; and (3) after the pre-sintered powder is made into a blank with a required shape, placing the blank in a furnace, heating to 1230 ℃ from room temperature, keeping the temperature for 3.5 hours at a heating rate of less than or equal to 2.5 ℃/min, and cooling to the room temperature to obtain the nickel-zinc ferrite material with high temperature stability.
TABLE 2 impurity levels
The 18X 8X 5 ferrite material sample ring prepared by the powder prepared by the formula is sintered according to heat preservation for 3.5h at 1230 ℃, 20 turns of enamelled wire with 0.31mm are wound to test inductance, magnetic conductivity and quality factor, the test is carried out according to the requirement of the soft magnetic ferrite material measuring method of the military standard SJ20966-2006 of the electronic industry, the basic electric performance accords with the current nickel zinc magnetic conductivity 100 material characteristic, and the test has a temperature coefficient of relatively wide temperature (-55 ℃ to 125 ℃), and the results are shown in the following tables 3 and 4.
Temperature coefficient alpha mu industry standard calculation formula:
αμ＝△L/[L25℃×△T]……………………………………………(1)
wherein:
Δl: the maximum and minimum values of inductance within a specified temperature range are poor (the inductance value at higher temperature is subtracted);
l25 ℃ C:: testing inductance at 25+/-2 ℃;
Δt: the specified temperature difference range (-55 ℃ to 125 ℃).
TABLE 3 test results and temperature coefficients
Table 4 results of inductance values at different temperature test points
From the above repeated experiments, it was concluded that: examples 2 to 4 are significantly smaller in temperature coefficient αμ and lower in negative temperature range (-55 ℃ C. To 0 ℃ C.) than comparative examples 1 to 6, and the temperature coefficient is less than 100X 10 -6 a/DEG C; the temperature coefficient of the positive temperature section (0 ℃ to 125 ℃) is less than 200 multiplied by 10 -6 The temperature is lower than 150 multiplied by 10 in the wide temperature range (-55 ℃ to 125 ℃) -6 Temperature coefficient shows a significant increase in temperature coefficient compared to that of conventional materials of NXO-100.
According to the embodiment, through a large number of doping tests, repeated tests and performance tests, various performance indexes of the material are realized, and the optimal doping impurity types and content formulas including MnCO31.5wt% -2.0wt%; co (Co) 2 O 3 0.25wt％～0.45wt％、BaCO 3 0.15wt％～0.5wt％、LiCO 3 0.1 to 0.15 weight percent of the total mass of the ferrite raw material.
Preparing a plurality of ferrite material samples by using the ferrite formulations provided in the examples 3 and 2, respectively, wherein the two ferrite material samples are randomly selected by the two formulations, and are respectively marked as a series 1 and a series 2; the inductance-temperature profiles for both formulations, series 1 and series 2, were each measured and the results for both formulations are shown in figure 1.
The results show that example 3 was achieved by reducing Co 3+ Content, make the temperature curve levelIn the embodiment 2, the formulation is further optimized, so that the curve of the inductance change along with the temperature is more gentle, and the temperature characteristic is more excellent.
Example 5
The powder prepared in examples 2 and 3 and the powder prepared in comparative examples 1 and 2 are respectively prepared into 18X 8X 5 ferrite material sample rings, the temperature is kept at 1230 ℃ for 3.5 hours, the powder is wound into 20 turns by using a 0.31mm enamelled wire to test inductance, magnetic permeability, quality factor and temperature coefficient, the powder is tested according to the requirement of the soft magnetic ferrite material measurement method of the military standard SJ20966-2006 in the electronic industry, the basic electric performance accords with the current nickel zinc magnetic permeability 100 material characteristic, the specific temperature coefficient of the wide temperature (-55 ℃ to 125 ℃) is tested and compared, the current domestic manufacturer product manual only marks the temperature coefficient of the positive temperature, and the measured data of the invention are compared with the performance of the existing manufacturer, and the results are shown in the following table 5, so that the invention is greatly improved compared with the current manufacturer.
Permeability is a measure of the magnetization obtained by a material in response to an applied magnetic field. Indicated by mu i in the electronics industry. Permeability means inductance per unit length and is typically calculated in an application by testing the core inductance.
The method for testing the inductance comprises the following steps: adopts the wire diameter and the turns: 0.35mm x 20 turns, inductance L was measured with an LCR test meter (100 kHz,0.1 v), and permeability was calculated as follows:
mu i= (le×l×1000)/(0.4×pi×n2×ae) formula (2)
Le, effective magnetic path length, mm;
ae-effective cross-sectional area, mm 2 ；
L-inductance value, μH;
n-turns.
Specific temperature coefficient is the temperature coefficient divided by the magnetic core permeability: the smaller the specific temperature coefficient, the better the temperature performance of the core.
The relative loss factor (tan delta/mu i) is the ratio of loss factor to permeability, and the lower the value is, the smaller the loss of the material is, the higher the electromagnetic performance is, calculated as follows:
tan δ/μi=1/(q×μi) formula (3)
tan delta, a core loss, is reciprocal to the core quality factor Q (tan delta=1/Q),
mu i-permeability.
TABLE 5 comparison of the properties of the materials of the invention with those of the factories at home and abroad
The result shows that the nickel-zinc ferrite material with the low temperature coefficient and the magnetic conductivity of about 100 is obtained by the preparation method, has stable temperature characteristics in the working process, meets the wide-temperature stable use requirement of-55 ℃ to 125 ℃, and has wide application prospect in the communication field at present and in the future.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any person skilled in the art may make modifications or alterations to the above disclosed technical content to equivalent embodiments. However, any simple modification, equivalent variation and variation of the above embodiments according to the technical substance of the present invention still fall within the protection scope of the technical solution of the present invention.
Claims (7)
1. The low temperature coefficient nickel zinc ferrite material is characterized by comprising main formula raw materials and doping raw materials, wherein the main formula raw materials are prepared by the following components in percentage of the total substances: fe (Fe) 2 O 3 58 to 60.5mol percent, 18.5 to 22.5mol percent of NiO and 18.5 to 20.0mol percent of ZnO; the doping raw materials are calculated according to the total mass percentage of the main formula raw materials: mn CO 3 1.5wt％～2.0wt％；Co 2 O 3 0.25wt％～0.45wt％、BaCO 3 0.15wt％～0.5wt％、LiCO 3 0.1wt％～0.15wt％。
2. The preparation method of the nickel-zinc ferrite material with the low temperature coefficient is characterized by comprising the following steps:
s1, preparing main formula raw materials, wherein the main formula raw materials comprise: fe (Fe) 2 O 3 ，NiO 18.5，ZnO 18.5；
S2, preparing doping raw materials, wherein the preparation method comprises the following steps: mnCO 3 ；Co 2 O 3 、BaCO 3 0.15、LiCO 3 0.1；
S3, grinding and mixing the main formula raw materials and the doping raw materials, placing the mixture in a furnace, heating the mixture, preserving heat for a period of time, and cooling the mixture to room temperature to obtain a presintered blank;
s4, grinding the presintered blank to obtain presintered powder;
s5, after the presintered powder is made into a blank with a required shape, the blank is placed in a furnace for sintering, and then the blank is cooled to room temperature, so that the nickel-zinc ferrite material with high temperature stability is obtained.
3. The preparation method according to claim 2, wherein in step S1, the main formulation raw materials include, in percentage by total mass of the main formulation raw materials: fe (Fe) 2 O 3 58mol％～60.5mol％，NiO 18.5mol％～22.5mol％，ZnO 18.5mol％～20.0mol％。
4. The preparation method according to claim 2, wherein in step S2, the doping raw materials comprise, in percentage by total mass of the raw materials of the main formulation: mnCO 3 1.5wt％～2.0wt％；Co 2 O 3 0.25wt％～0.45wt％、BaCO 3 0.15wt％～0.5wt％、LiCO 3 0.1wt％～0.15wt％。
5. The method according to claim 2, wherein in the step S3, the grinding time is 2 to 4 hours, and the holding time is 2 to 4 hours after the room temperature is raised to 1040 to 1060 ℃ at a rate of 1.5 to 2.5 ℃/S.
6. The method according to claim 2, wherein in step S4, the grinding is performed under such a condition that the particle diameter is 80% -90% of the particle diameter of 0.3-5.0 μm.
7. The method according to claim 2, wherein in step S5, the sintering is performed under the condition that the temperature is raised from room temperature to 1230 ℃ to 1250 ℃, the temperature raising rate is less than or equal to 2.5 ℃/min, and the temperature is kept for 3 to 4 hours.
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| CN103626484A (en) * | 2013-12-04 | 2014-03-12 | 南京深宁磁电有限公司 | Wide-temperature-range nickel-zinc soft-magnetic ferrite and preparation method thereof |
| CN104402428A (en) * | 2014-11-21 | 2015-03-11 | 钢铁研究总院 | Nickel, zinc and ferrite material with high frequency, high permeability and high Q value and preparation method thereof |
| JP2022039923A (en) * | 2020-08-28 | 2022-03-10 | 日立金属株式会社 | Nickel zinc-based ferrite |
| CN114262221A (en) * | 2021-12-28 | 2022-04-01 | 北京七星飞行电子有限公司 | High-temperature stable nickel-zinc ferrite material and preparation method and application thereof |
| JP2022145508A (en) * | 2021-03-19 | 2022-10-04 | 日立金属株式会社 | NiZn-BASED FERRITE |
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| CN103626484A (en) * | 2013-12-04 | 2014-03-12 | 南京深宁磁电有限公司 | Wide-temperature-range nickel-zinc soft-magnetic ferrite and preparation method thereof |
| CN104402428A (en) * | 2014-11-21 | 2015-03-11 | 钢铁研究总院 | Nickel, zinc and ferrite material with high frequency, high permeability and high Q value and preparation method thereof |
| JP2022039923A (en) * | 2020-08-28 | 2022-03-10 | 日立金属株式会社 | Nickel zinc-based ferrite |
| JP2022145508A (en) * | 2021-03-19 | 2022-10-04 | 日立金属株式会社 | NiZn-BASED FERRITE |
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