CN101723657A - Method for preparing NiCuZn microwave ferrite material - Google Patents
Method for preparing NiCuZn microwave ferrite material Download PDFInfo
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- CN101723657A CN101723657A CN200910263434A CN200910263434A CN101723657A CN 101723657 A CN101723657 A CN 101723657A CN 200910263434 A CN200910263434 A CN 200910263434A CN 200910263434 A CN200910263434 A CN 200910263434A CN 101723657 A CN101723657 A CN 101723657A
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Abstract
The invention discloses a method for preparing a NiCuZn microwave ferrite material, which belongs to the technical field of a functional material and relates to a magnetic material. The method comprises: firstly, weighing and mixing analytically pure raw materials including Fe2O3, NiO, ZnO and CuO in a molar ratio of Ni to Cu to Zn to Fe of (1-x):y:(x-y):2; secondary performing ball milling, drying as well as presintering at 900 DEG C for 2 to 4 hours; and finally, grinding the presintered product, adding 1 to 5 percent of Bi2O3 serving as a low-temperature sintering aid, performing secondary ball milling, drying as well as sintering at 900 DEG C for 4 to 6 hours, and grinding the sintered product to obtain a target product. In the method, a solid phase method process is adopted to obtain the NiCuZn microwave ferrite material which has a spinel structure and is adaptable to an LTCC process by optimizing material formula and using the Bi2O3 as a sintering aid. The prepared NiCuZn microwave ferrite material has low ferromagnetic resonance line width and microwave dielectric loss and high saturation magnetization and Curie temperature, meets requirements of the LTCC process in machining performance, can be used to prepare sheet small-sized microwave ferrite elements and microwave passive integrated functional substrates and can realize the miniaturization, planarizartion and integration of the microwave ferrite elements.
Description
Technical field
The invention belongs to technical field of function materials, relate to magneticsubstance, relate in particular to microwave NiCuZn Ferrite Material and preparation method thereof.
Background technology
Microwave ferrite material is to make the base mateiral that comprises microwave devices such as circulator, shield retaining.The principle of work of microwave device mainly is to have utilized the tensor characteristic and the ferro resonance effect of material magnetic permeability, so microwave ferrite material and device are called gyromagnetic material and device again.This class device is widely used in various communication systems, radar system at present, and operating frequency has also been crossed over L, S, C, X, K wave band and millimeter wave frequency band.Microwave gyromagnetic ferrite miniaturization of devices, low cost, be easy to batch making and high conformity is technical problem and the developing direction that such device needs to be resolved hurrily.The ideal solution that realizes above-mentioned developing direction is LTCC (LTCC and the ferrite) technology of using based on low-temperature sintering (being lower than 900 ℃) microwave ferrite material, solve the problem of Microwave Iron Oxide Elements chip miniaturization, but also be the integrated proposition solution of microwave circuit modularization.When adopting LTCC prepared microwave device, will realize that at first low sintering ceramics powder or ferrite powder make accurate, the even and fine and close green band of thickness; On the green band, utilize technologies such as punching, filling perforation, accurate conductor paste silk screen printing to produce the circuitry needed figure then; Force together at last, at 900 ℃ of following sintering, make three-dimension device and high-density circuit structure behind process cutting, the binder removal.Therefore LTCC technology is at the miniaturization that realizes Microwave Iron Oxide Elements, preparation technology's mass and realize that aspects such as the modularization of microwave components is integrated have advantageous advantage.And the core that addresses this problem is developed exactly and is a kind ofly had low cost, high-performance and be suitable for low sintering microwave ferrite material (sintering temperature is lower than 900 ℃)-can burn altogether with silver slurry below 900 ℃, can guarantee that again material has excellent electromagnetic performance (comprising characteristics such as lower ferromagnetic resonance line width and microwave dielectric loss, moderate saturation magnetization, high Curie temperature).The realization of low-temperature sintered microwave gyromagnetic ferrite material can not only utilize LTCC technology to guarantee that Microwave Iron Oxide Elements realize the chip miniaturizationization, and the low microwave dielectric loss characteristics that can also utilize material is realized passive integrated as baseplate material and other device and circuit.
For this reason, the microwave ferrite baseplate material that how to prepare a kind of low-loss, sintering temperature and low becomes the technical bottleneck of present restriction Microwave Iron Oxide Elements chip miniaturization and passive integrated development.The gordian technique of realizing this goal just is that research and development are a kind of and has lower ferromagnetic resonance line width Δ H, a lower microwave dielectric loss tg δ ε, saturation magnetization Ms is moderate and adjustable, high Curie temperature, and can be at 900 ℃ of following agglomerating microwave ferrite materials.
Summary of the invention
The invention provides a kind of preparation method of NiCuZn microwave ferrite material, prepared NiCuZn microwave ferrite material is a spinel structure, have good electromagnetic performance and (comprise lower ferromagnetic resonance line width and microwave dielectric loss, higher saturation magnetization and Curie temperature), on processing characteristics, can satisfy the LTCC processing requirement, can be used for preparing the passive integrated functionality substrate of chip miniaturization Microwave Iron Oxide Elements and microwave.
Technical solution of the present invention is as follows:
A kind of preparation method of NiCuZn microwave ferrite material as shown in Figure 1, may further comprise the steps:
Step 1: adopt analytically pure Fe
2O
3, NiO, ZnO and CuO be raw material, with Ni: Cu: Zn: Fe=(1-x): y: (x-y): 2 mol ratio is carried out weighing and batch mixing, obtains mixing raw material A; X=0.3～0.6 wherein, y=0.02～0.08.
Step 2: mixing raw material A is carried out ball milling, obtain ball milling slurry B.
Concrete ball-milling technology is: 1) mass ratio of abrading-ball, mixing raw material A and water, i.e. ball: material: water is 2.5: 1: 1.1; 2) the ball milling time is 4～8 hours.
Step 3: ball milling slurry B is dried, obtains preburning powdered material C after 900 ℃ of pre-burnings 2～4 hours, grinding.
Step 4: in preburning powdered material C, mix the low temperature sintering agent Bi that is equivalent to preburning powdered material C total quality 1～5%
2O
3, obtain rerolling D.
Step 5: rerolling D is carried out secondary ball milling, obtain secondary ball milling slurry E.
Concrete secondary ball milling technology is: 1) mass ratio of abrading-ball, rerolling D and water, i.e. ball: material: water is 2.5: 1: 1.1; 2) the ball milling time is 8～12 hours.
Step 6: secondary ball milling slurry E is dried, obtains target product after 900 ℃ of following sintering 4～6 hours, grinding.
Essence of the present invention is to adopt the conventional solid-state method technical process, (adopts Ni by optimizing material prescription
1-xCu
yZn
X-yFe
2O
4Be prescription) and select Bi for use
2O
3Be sintering agent, obtain having spinel structure and adapt to the NiCuZn microwave ferrite material of LTCC technology.Prepared NiCuZn microwave ferrite material has good electromagnetic performance and (comprises lower ferromagnetic resonance line width and microwave dielectric loss, higher saturation magnetization and Curie temperature), can adjust simultaneously the saturation magnetization Ms of material by the appropriate change prescription easily, to satisfy user's demand at different microwave frequency bands.On processing characteristics, can satisfy the LTCC processing requirement, can be used for preparing the passive integrated functionality substrate of chip miniaturization Microwave Iron Oxide Elements and microwave, realize miniaturization, the complanation, integrated of Microwave Iron Oxide Elements.
Description of drawings
Fig. 1 is the preparation method's of a NiCuZn microwave ferrite material provided by the invention schema.
Embodiment
Embodiment 1:
A kind of preparation method of NiCuZn microwave ferrite material may further comprise the steps:
Step 1: adopt analytically pure Fe
2O
3, NiO, ZnO and CuO be raw material, with Ni: Cu: Zn: Fe=0.7: 0.05: 0.25: 2 mol ratio is carried out weighing and batch mixing, obtains mixing raw material A.
Step 2: mixing raw material A is carried out ball milling, obtain ball milling slurry B.
Concrete ball-milling technology is: 1) mass ratio of abrading-ball, mixing raw material A and water, i.e. ball: material: water is 2.5: 1: 1.1; 2) the ball milling time is 6 hours.
Step 3: ball milling slurry B is dried, obtains preburning powdered material C after 900 ℃ of pre-burnings 3 hours, grinding.
Step 4: in preburning powdered material C, mix the low temperature sintering agent Bi that is equivalent to preburning powdered material C total quality 3%
2O
3, obtain rerolling D.
Step 5: rerolling D is carried out ball milling, obtain secondary ball milling slurry E.
Concrete secondary ball milling technology is: 1) mass ratio of abrading-ball, rerolling D and water, i.e. ball: material: water is 2.5: 1: 1.1; 2) the ball milling time is 8 hours.
Step 6: secondary ball milling slurry E is dried, obtains target product after 900 ℃ of following sintering 4 hours, grinding.
NiCuZn microwave ferrite material to above-mentioned embodiment preparation carries out the correlated performance test according to electron trade military standard GJB 4410-2002 of the People's Republic of China (PRC) and State Standard of the People's Republic of China GB/T 9633-1988, and the microwave dielectric loss that records material is 4.49 * 10
-4(test frequency 10GHz), ferromagnetic resonance line width Δ H are 15.15KA/m (test frequency 10GHz), 900 ℃ of sintering temperatures, and Curie temperature is 351.2 ℃, saturation magnetization Ms is 314.27KA/m.
Embodiment 2:
A kind of preparation method of NiCuZn microwave ferrite material may further comprise the steps:
Step 1: adopt analytically pure Fe
2O
3, NiO, ZnO and CuO be raw material, with Ni: Cu: Zn: Fe=0.55: 0.02: 0.43: 2 mol ratio is carried out weighing and batch mixing, obtains mixing raw material A.
Step 2: mixing raw material A is carried out ball milling, obtain ball milling slurry B.
Concrete ball-milling technology is: 1) mass ratio of abrading-ball, mixing raw material A and water, i.e. ball: material: water is 2.5: 1: 1.1; 2) the ball milling time is 4 hours.
Step 3: ball milling slurry B is dried, obtains preburning powdered material C after 900 ℃ of pre-burnings 2 hours, grinding.
Step 4: in preburning powdered material C, mix the low temperature sintering agent Bi that is equivalent to preburning powdered material C total quality 1%
2O
3, obtain rerolling D.
Step 5: rerolling D is carried out ball milling, obtain secondary ball milling slurry E.
Concrete secondary ball milling technology is: 1) mass ratio of abrading-ball, rerolling D and water, i.e. ball: material: water is 2.5: 1: 1.1; 2) the ball milling time is 10 hours.
Step 6: secondary ball milling slurry E is dried, obtains target product after 900 ℃ of following sintering 6 hours, grinding.
NiCuZn microwave ferrite material to above-mentioned embodiment preparation carries out the correlated performance test according to electron trade military standard GJB 4410-2002 of the People's Republic of China (PRC) and State Standard of the People's Republic of China GB/T 9633-1988, and the microwave dielectric loss that records material is 4.01 * 10
-4(test frequency 10GHz), ferromagnetic resonance line width Δ H are 13.48KA/m (test frequency 10GHz), 900 ℃ of sintering temperatures, and Curie temperature is 347.6 ℃, saturation magnetization Ms is 352.35KA/m.
Embodiment 2:
A kind of preparation method of NiCuZn microwave ferrite material may further comprise the steps:
Step 1: adopt analytically pure Fe
2O
3, NiO, ZnO and CuO be raw material, with Ni: Cu: Zn: Fe=0.4: 0.08: 0.52: 2 mol ratio is carried out weighing and batch mixing, obtains mixing raw material A.
Step 2: mixing raw material A is carried out ball milling, obtain ball milling slurry B.
Concrete ball-milling technology is: 1) mass ratio of abrading-ball, mixing raw material A and water, i.e. ball: material: water is 2.5: 1: 1.1; 2) the ball milling time is 8 hours.
Step 3: ball milling slurry B is dried, obtains preburning powdered material C after 900 ℃ of pre-burnings 3 hours, grinding.
Step 4: in preburning powdered material C, mix the low temperature sintering agent Bi that is equivalent to preburning powdered material C total quality 5%
2O
3, obtain rerolling D.
Step 5: rerolling D is carried out ball milling, obtain secondary ball milling slurry E.
Concrete secondary ball milling technology is: 1) mass ratio of abrading-ball, rerolling D and water, i.e. ball: material: water is 2.5: 1: 1.1; 2) the ball milling time is 12 hours.
Step 6: secondary ball milling slurry E is dried, obtains target product after 900 ℃ of following sintering 5 hours, grinding.
NiCuZn microwave ferrite material to above-mentioned embodiment preparation carries out the correlated performance test according to electron trade military standard GJB 4410-2002 of the People's Republic of China (PRC) and State Standard of the People's Republic of China GB/T 9633-1988, and the microwave dielectric loss that records material is 4.22 * 10
-4(test frequency 10GHz), ferromagnetic resonance line width Δ H are 14.37KA/m (test frequency 10GHz), 900 ℃ of sintering temperatures, and Curie temperature is 342.9 ℃, saturation magnetization Ms is 328.65KA/m.
Claims (3)
1. the preparation method of a NiCuZn microwave ferrite material may further comprise the steps:
Step 1: adopt analytically pure Fe
2O
3, NiO, ZnO and CuO be raw material, with Ni: Cu: Zn: Fe=(1-x): y: (x-y): 2 mol ratio is carried out weighing and batch mixing, obtains mixing raw material A; X=0.3～0.6 wherein, y=0.02～0.08;
Step 2: mixing raw material A is carried out ball milling, obtain ball milling slurry B;
Step 3: ball milling slurry B is dried, obtains preburning powdered material C after 900 ℃ of pre-burnings 2～4 hours, grinding;
Step 4: in preburning powdered material C, mix the low temperature sintering agent Bi that is equivalent to preburning powdered material C total quality 1～5%
2O
3, obtain rerolling D;
Step 5: rerolling D is carried out secondary ball milling, obtain secondary ball milling slurry E;
Step 6: secondary ball milling slurry E is dried, obtains target product after 900 ℃ of following sintering 4～6 hours, grinding.
2. the preparation method of NiCuZn microwave ferrite material according to claim 1 is characterized in that, concrete ball-milling technology is in the step 2: 1) mass ratio of abrading-ball, mixing raw material A and water, i.e. ball: material: water is 2.5: 1: 1.1; 2) the ball milling time is 4～8 hours.
3. the preparation method of NiCuZn microwave ferrite material according to claim 1 is characterized in that, secondary ball milling technology concrete in the step 5 is: 1) mass ratio of abrading-ball, rerolling D and water, i.e. ball: material: water is 2.5: 1: 1.1; 2) the ball milling time is 8～12 hours.
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| CN102241507A (en) * | 2011-05-19 | 2011-11-16 | 陕西金山电器有限公司 | Ni-Zn ferrite material with high magnetic permeability and high impedance and preparation method thereof |
| CN102390985A (en) * | 2011-08-06 | 2012-03-28 | 江苏华兴电子有限公司 | Broadband and high-magnetic-permeability ferrite teflon tape and production method thereof |
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| CN102976726A (en) * | 2012-08-07 | 2013-03-20 | 横店集团东磁股份有限公司 | Method for preparing ultrathin type ferrite sheet by using microwave sintering |
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| CN103113094A (en) * | 2011-08-06 | 2013-05-22 | 江苏华兴电子有限公司 | Broadband high-permeability ferrite raw material belt and method for manufacturing same into chip-inductor element |
| CN103113094B (en) * | 2011-08-06 | 2014-04-16 | 江苏华兴电子有限公司 | Broadband high-permeability ferrite raw material belt and method for manufacturing same into chip-inductor element |
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| CN102683791B (en) * | 2012-04-28 | 2015-08-12 | 深圳光启创新技术有限公司 | A kind of Meta-material harmonic oscillator based on LTCC and preparation method thereof |
| CN102807361A (en) * | 2012-07-03 | 2012-12-05 | 天通控股股份有限公司 | Nickel-zinc ferrite material for wireless signal sensing, sheet core and preparation method thereof |
| CN102807361B (en) * | 2012-07-03 | 2014-10-22 | 天通控股股份有限公司 | Nickel-zinc ferrite material for wireless signal sensing, sheet core and preparation method thereof |
| CN102976726A (en) * | 2012-08-07 | 2013-03-20 | 横店集团东磁股份有限公司 | Method for preparing ultrathin type ferrite sheet by using microwave sintering |
| CN103011793A (en) * | 2012-12-27 | 2013-04-03 | 中南大学 | Method for preparing nickel-zinc ferrite by using microwave technology |
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| CN113603472B (en) * | 2021-08-17 | 2023-02-28 | 杭州电子科技大学 | Preparation method of NiCuZn ferrite based on LTCC technology |
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Application publication date: 20100609 |