CN105234387A - Method for improving electromagnetic wave absorption performance of micron-grade cobalt particles - Google Patents
Method for improving electromagnetic wave absorption performance of micron-grade cobalt particles Download PDFInfo
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- CN105234387A CN105234387A CN201510557621.4A CN201510557621A CN105234387A CN 105234387 A CN105234387 A CN 105234387A CN 201510557621 A CN201510557621 A CN 201510557621A CN 105234387 A CN105234387 A CN 105234387A
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Abstract
A method for improving the electromagnetic wave absorption performance of micron-grade cobalt particles comprises the steps that (1) the micron-grade cobalt particles are subjected to acid pickling in an acid solution for 0.5-30 minutes, then repeatedly washed three times by deionized water and absolute ethyl alcohol and dried in a vacuum drying chamber for standby application; (2) the washed micron-grade cobalt particles in the step (1) are subjected to wet ball-milling for 5-80 hours in a ball grinding mill according to the ball-to-powder ratio of 5:1-10:1, the ball grinding rotary speed is 100-1200 RPM, and the medium is methylbenzene; the cobalt particles which are subjected to ball-milling are repeatedly washed three times by deionized water and absolute ethyl alcohol and are dried in the vacuum drying chamber for standby application; and (3) the micron-grade cobalt particles which are subjected to ball-milling in the step (2) are placed in an oxygen-free environment and are subjected to thermal treatment for 2-300 minutes under a magnetic field state, the heating speed is 0.5-20 DEG C per minute, the temperature is 300-1400 DEG C, the cooling speed is 0.5-20 DEG C per minute, and the magnetic field intensity is 0.5-14 T. The magnetic field state is kept in the whole thermal treatment process. The cobalt particles are collected after being cooled to be at the room temperature, and the micron-grade cobalt particles with the excellent electromagnetic wave absorption performance are obtained.
Description
Technical field
The present invention relates to a kind of method improving micron order cobalt granule electromagnetic wave absorption performance.
Background technology
Micron order cobalt material is a kind of typical ferrimagnet, because it has high specific saturation magnetization (162emu/g), higher magnetic loss can be produced with electromagnetic wave phase mutual effect in 2-18GHz frequency range, thus obtain excellent electromagnetic wave absorption performance, therefore it has potential application prospect in stealth technology, electromagnetic shielding and field of electromagnetic compatibility.Compared with traditional Fe base electromagnetic-wave absorbent, cobalt material has significant non-oxidizability and high-curie temperature (Co:1131 DEG C, Fe:770 DEG C), can be on active service in the environment that temperature is higher, therefore the electromagnetic wave absorption performance study of cobalt material is subject to the extensive concern of domestic and international researcher.As the people such as Wang have studied the electromagnetic wave absorption performance of flower-shaped cobalt granule, find that it is when coating layer thickness is 2mm, maximum reflection loss is-13.6dB, the people such as Liu have studied the electromagnetic wave absorption performance of flower-shaped cobalt granule, and with the electromagnetic wave absorption Performance comparision of spherical cobalt granule, find that the maximum reflection loss of flower-shaped cobalt granule when coating layer thickness is 2mm is for-25.00dB, and the maximum reflection loss of spherical cobalt granule is-11dB under same thickness, the people such as Ma find that flower-shaped cobalt granule is when the coating layer thickness of 5mm, maximum reflection loss is-23.5dB ([1] WangC., X.J.Han, P.Xu, X.L.Zhang, Y.C.Du, S.R.Hu, J.Y.Wang, X.H.Wang, Theelectromagneticpropertyofchemicallyreducedgrapheneoxi deanditsapplicationasmicrowaveabsorbingmaterial [J] .AppliedPhysicsLetters, 2011, 98 (7): 3. [2] LiuT., P.H.Zhou, D.F.Liang, L.J.Deng, Electromagneticabsorptionpropertiesofflowerlikecobaltcom positesatmicrowavefrequencies [J] .Chin.Phys.B, 2012, 21 (5): 4. [3] MaZ., Q.Liu, J.Yuan, Z.Wang, C.Cao, J.Wang, Analysesonmultipleresonancebehaviorsandmicrowavereflecti onlossinmagneticComicroflowers [J] .Phys.StatusSolidiB, 2012, 249 (3): 575.).So far, the research of researcher to micron order cobalt granule electromagnetic wave absorption performance mainly concentrates on the pattern and the crystal structure that are regulated cobalt granule by change synthetic method and technological parameter, improve its electromagnetic wave absorption performance with this, and achieve certain positive achievement.But these methods also exist, and cost is high, productive rate is low, poor repeatability, is difficult to the problem of actual popularization, therefore how adopting simple and easy to do method to improve cobalt granule electromagnetic wave absorption performance further becomes a challenging research topic.
In addition, the research of the material modified performance of magnetic-field heat treatment technology also becomes one of hot issue of vast researcher in recent years.People's reports such as Ma effectively can improve the feature performance (LuoW.J. of BiFeO3 material by high-intensity magnetic field heat treatment, D.L.Wang, F.W.Wang, T.Liu, J.W.Cai, L.Y.Zhang, Y.L.Liu, Room-temperaturesimultaneouslyenhancedmagnetizationandel ectricpolarizationinBiFeO3ceramicsynthesizedbymagnetican nealing [J] .AppliedPhysicsLetters, 2009, 94 (20): 3.), Zhang Shuling etc. are respectively at 0.05T, Co base amorphous microwires standby to melt pull legal system under the magnetic field of 0.16T and 0.4T carries out annealing heat treatment, result shows that transverse magnetic field heat treatment can improve the hoop anisotropy of microfilament, and then significantly improve GMI (Zhang Shuling, Sun Jianfei, Xing great Wei, magnetic-field annealing is on the impact [J] of Co base melt pull silk giant magnetoresistance effect. Acta Physica Sinica, 2010, 3): 2068.).This illustrates that high-intensity magnetic field heat treatment has a good application prospect in material modification.Improve electromagnetic wave absorption aspect of performance by high-intensity magnetic field heat treatment modified cobalt particle and not yet do not see relevant report.
Summary of the invention
The object of the invention is the shortcoming overcoming prior art, a kind of method improving micron order cobalt granule electromagnetic wave absorption performance is provided.
The present invention adopts magnetic field heat treatment process, and the defect state of the micron order cobalt granule inside regulating ball-milling treatment to cross by contactless mode, stress state and crystal structure, significantly improve the electromagnetic wave absorption performance of cobalt granule.
The concrete steps of the inventive method are:
1., by the pickling 0.5 ~ 30 minute in the acid solution in 0.1 ~ 10wt% concentration of micron order cobalt granule, remove the oxide layer on surface, then repeatedly clean three times, drying for standby in vacuum drying chamber with deionized water and absolute ethyl alcohol;
2. the micron order cobalt granule for subsequent use cleaned through step 1 is adopted wet ball grinding process 5 ~ 80 hours according to the ratio of grinding media to material of 5:1 ~ 10:1 in ball mill, rotational speed of ball-mill is 100 ~ 1200 revs/min, and medium is toluene.Cobalt granule deionized water after ball-milling treatment and absolute ethyl alcohol are cleaned three times repeatedly, is placed in vacuum drying chamber drying for standby;
3. the micron order cobalt granule after step 2 ball milling is placed in oxygen-free environment, heat treatment 2 ~ 300/min under magnetic field state, heating rate is 0.5 ~ 20 DEG C, and temperature is 300 ~ 1400 DEG C, and rate of temperature fall is 0.5 ~ 20 DEG C/min, and magnetic field intensity is 0.5 ~ 14T.In whole heat treatment process, all keep magnetic field state, comprise temperature-rise period, insulating process and temperature-fall period.Collect cobalt granule after being cooled to room temperature, the micron order cobalt granule with excellent electromagnetic wave absorption performance can be obtained.
In described step 3, the oxygen-free environment of heat treatment process is vacuum is 10
-6-10
-1the vacuum environment of Pa, or adopt argon shield.
In described step 1, the particle size range of described cobalt granule is 0.5 ~ 30 micron.
The principle of the invention is: because cobalt has face-centered cubic and Patterns for Close-Packed Hexagonal Crystal structure, in time there is stacking fault defects in face-centered cubic crystal structure, defect area can be considered Patterns for Close-Packed Hexagonal Crystal structure, and in time there is stacking fault defects in Patterns for Close-Packed Hexagonal Crystal structure, defect area can be considered face-centred cubic structure.The complexity of the generation of this stacking fault defects depends on the size of stacking fault energy.For cobalt material, stacking fault energy is very low, which results in it, under high-energy strong magnetic field action, atom directional migration occurs, make that original at room temperature the close-packed hexagonal structure of stable state or the cobalt granule of close-packed hexagonal and face-centered cubic mixed structure change into only stable in condition of high temperature face-centred cubic structure, and under high-energy strong magnetic field action, this face-centred cubic structure is more complete.Face-centred cubic structure, for Patterns for Close-Packed Hexagonal Crystal structure, has high symmetry, and therefore, under electromagnetic wave absorption effect, the magnetic response of its inside is restricted less, can produce strong magnetic loss, significantly consume electromagnetic wave.
Accompanying drawing explanation
Fig. 1 a is embodiment 1 original cobalt granule sample SampleA pattern in the secure execution mode (sem;
Fig. 1 b is that embodiment 1 does not add magnetic field, but through heat treated cobalt granule sample SampleB pattern in the secure execution mode (sem;
Fig. 1 c is that embodiment 1 applies magnetic field and through heat treated cobalt granule sample SampleC pattern in the secure execution mode (sem;
Fig. 1 d is the XRD collection of illustrative plates of three cobalt granule samples SampleA, SampleB and SampleC of embodiment 1;
Fig. 2 is the comparison of the electromagnetic wave absorption performance of three kinds of cobalt granule samples SampleA, SampleB and SampleC of embodiment 1.
Detailed description of the invention
Embodiment 1
1., by the pickling 5 minutes in the acid solution of 5wt% concentration of micron order cobalt granule, remove the oxide layer on surface, then repeatedly clean three times, drying for standby in vacuum drying chamber with deionized water and absolute ethyl alcohol;
2. the micron order cobalt granule cleaned through step 1 is adopted wet ball grinding process 30 hours according to the ratio of grinding media to material of 10:1 in ball mill, rotational speed of ball-mill is 824 revs/min, and medium is toluene.Cobalt granule deionized water after ball-milling treatment and absolute ethyl alcohol are cleaned three times repeatedly, is placed in vacuum drying chamber drying for standby;
3. micron order cobalt granule step 2 prepared is placed in argon shield environment, heat treatment 30 minutes under high-intensity magnetic field state, and heating rate is 10 DEG C/min, and temperature is 720 DEG C, and rate of temperature fall is 10 DEG C/min, and magnetic field intensity is 10T.In whole heat treatment process, all keep high-intensity magnetic field state, comprise temperature-rise period, insulating process and temperature-fall period.Collect cobalt powder after being cooled to room temperature, the micron order cobalt granule with excellent electromagnetic wave absorption performance can be obtained.
Figure 1 shows that the SEM picture of embodiment 1, Figure 2 shows that the electromagnetic wave absorption performance of embodiment 1.
Following table is be three kinds of micron order cobalt granule electromagnetic wave absorption Performance comparision in example 1
Fig. 1 a, Fig. 1 b and Fig. 1 c is respectively SampleA, the SEM picture of SampleB, SampleC tri-kinds of cobalt powders.Fig. 1 d is the XRD collection of illustrative plates of three kinds of cobalt powders, by Fig. 1 a, Fig. 1 b and Fig. 1 c is known, original cobalt powder SampleA is close-packed hexagonal (HCP) and face-centered cubic (FCC) crystal structure, after the heat treatment not applying magnetic field, cobalt powder SampleB becomes face-centered cubic crystal structure, and after applying magnetic-field heat treatment, cobalt powder SampleC is also face-centered cubic crystal structure, and for the XRD collection of illustrative plates of SampleB, diffraction peak intensity increases to some extent, and this shows that corresponding crystal face increases, and under proving magnetic field, heat treatment can make cobalt powder occur oriented growth.Fig. 2 is the electromagnetic wave absorption performance of three kinds of cobalt powders.Electromagnetic performance is drawn according to transmission line principle by vector network analyzer.In associative list, data are known, and relative to original cobalt powder SampleA with do not apply for magnetic-field heat treatment cobalt powder SamplB, after magnetic-field heat treatment, the electromagnetic wave absorption performance increase of cobalt granule SampleC is about 60%, has increased substantially electromagnetic wave absorption loss.
Embodiment 2
1., by the pickling 0.5 minute in the acid solution of 0.1wt% concentration of micron order cobalt granule, remove the oxide layer on surface, then repeatedly clean three times, drying for standby in vacuum drying chamber with deionized water and absolute ethyl alcohol;
2. the micron order cobalt granule cleaned through step 1 is adopted wet ball grinding process 5 hours according to the ratio of grinding media to material of 5:1 in ball mill, rotational speed of ball-mill is 100 revs/min, and medium is toluene.Cobalt granule deionized water after ball-milling treatment and absolute ethyl alcohol are cleaned three times repeatedly, is placed in vacuum drying chamber drying for standby;
3. micron order cobalt granule step 2 prepared is placed in argon shield environment, heat treatment 5 minutes under high-intensity magnetic field state, and heating rate is 0.5 DEG C/min, and temperature is 300 DEG C, and rate of temperature fall is 0.5 DEG C/min, and magnetic field intensity is 0.5T.In whole process, all keep high-intensity magnetic field state, comprise temperature-rise period, insulating process and temperature-fall period.Collect cobalt powder after being cooled to room temperature, the micron order cobalt granule with excellent electromagnetic wave absorption performance can be obtained.
Embodiment 3
1., by the pickling 30 minutes in the acid solution of 0.1wt% concentration of micron order cobalt granule, remove the oxide layer on surface, then repeatedly clean three times, drying for standby in vacuum drying chamber with deionized water and absolute ethyl alcohol;
2. the micron order cobalt granule cleaned through step 1 is adopted wet ball grinding process 5 hours according to the ratio of grinding media to material of 5:1 in ball mill, rotational speed of ball-mill is 100 revs/min, and medium is toluene.Cobalt granule deionized water after ball-milling treatment and absolute ethyl alcohol are cleaned three times repeatedly, is placed in vacuum drying chamber drying for standby;
3. micron order cobalt granule step 2 prepared is placed in argon shield environment, heat treatment 5 minutes under high-intensity magnetic field state, and heating rate is 0.5 DEG C/min, and temperature is 300 DEG C, and rate of temperature fall is 0.5 DEG C/min, and magnetic field intensity is 0.5T.In whole process, all keep high-intensity magnetic field state, comprise temperature-rise period, insulating process and temperature-fall period.Collect cobalt powder after being cooled to room temperature, the micron order cobalt granule with excellent electromagnetic wave absorption performance can be obtained.
Embodiment 4
1., by the pickling 0.5 minute in the acid solution of 0.1wt% concentration of micron order cobalt granule, remove the oxide layer on surface, then repeatedly clean three times, drying for standby in vacuum drying chamber with deionized water and absolute ethyl alcohol;
2. the micron order cobalt granule cleaned through step 1 is adopted wet ball grinding process 5 hours according to the ratio of grinding media to material of 20:1 in ball mill, rotational speed of ball-mill is 100 revs/min, and medium is toluene.Cobalt granule deionized water after ball-milling treatment and absolute ethyl alcohol are cleaned three times repeatedly, is placed in vacuum drying chamber drying for standby;
3. micron order cobalt granule step 2 prepared is placed in argon shield environment, heat treatment 5 minutes under high-intensity magnetic field state, and heating rate is 0.5 DEG C/min, and temperature is 300 DEG C, and rate of temperature fall is 0.5 DEG C/min, and magnetic field intensity is 0.5T.In whole process, all keep high-intensity magnetic field state, comprise temperature-rise period, insulating process and temperature-fall period.Collect cobalt powder after being cooled to room temperature, the micron order cobalt granule with excellent electromagnetic wave absorption performance can be obtained.
Embodiment 5
1., by the pickling 0.5 minute in the acid solution of 0.1wt% concentration of micron order cobalt granule, remove the oxide layer on surface, then repeatedly clean three times, drying for standby in vacuum drying chamber with deionized water and absolute ethyl alcohol;
2. the micron order cobalt granule cleaned through step 1 is adopted wet ball grinding process 80 hours according to the ratio of grinding media to material of 5:1 in ball mill, rotational speed of ball-mill is 100 revs/min, and medium is toluene.Cobalt granule deionized water after ball-milling treatment and absolute ethyl alcohol are cleaned three times repeatedly, is placed in vacuum drying chamber drying for standby;
3. micron order cobalt granule step 2 prepared is placed in argon shield environment, heat treatment 5 minutes under high-intensity magnetic field state, and heating rate is 0.5 DEG C/min, and temperature is 300 DEG C, and rate of temperature fall is 0.5 DEG C/min, and magnetic field intensity is 0.5T.In whole process, all keep high-intensity magnetic field state, comprise temperature-rise period, insulating process and temperature-fall period.Collect cobalt powder after being cooled to room temperature, the micron order cobalt granule with excellent electromagnetic wave absorption performance can be obtained.
Embodiment 6
1., by the pickling 0.5 minute in the acid solution of 0.1wt% concentration of micron order cobalt granule, remove the oxide layer on surface, then repeatedly clean three times, drying for standby in vacuum drying chamber with deionized water and absolute ethyl alcohol;
2. the micron order cobalt granule cleaned through step 1 is adopted wet ball grinding process 5 hours according to the ratio of grinding media to material of 5:1 in ball mill, rotational speed of ball-mill is 1200 revs/min, and medium is toluene.Cobalt granule deionized water after ball-milling treatment and absolute ethyl alcohol are cleaned three times repeatedly, is placed in vacuum drying chamber drying for standby;
3. micron order cobalt granule step 2 prepared is placed in argon shield environment, heat treatment 5 minutes under high-intensity magnetic field state, and heating rate is 0.5 DEG C/min, and temperature is 300 DEG C, and rate of temperature fall is 0.5 DEG C/min, and magnetic field intensity is 0.5T.In whole process, all keep high-intensity magnetic field state, comprise temperature-rise period, insulating process and temperature-fall period.Collect cobalt powder after being cooled to room temperature, the micron order cobalt granule with excellent electromagnetic wave absorption performance can be obtained.
Embodiment 7
1., by the pickling 0.5 minute in the acid solution of 0.1wt% concentration of micron order cobalt granule, remove the oxide layer on surface, then repeatedly clean three times, drying for standby in vacuum drying chamber with deionized water and absolute ethyl alcohol;
2. the micron order cobalt granule cleaned through step 1 is adopted wet ball grinding process 5 hours according to the ratio of grinding media to material of 5:1 in ball mill, rotational speed of ball-mill is 100 revs/min, and medium is toluene.Cobalt granule deionized water after ball-milling treatment and absolute ethyl alcohol are cleaned three times repeatedly, is placed in vacuum drying chamber drying for standby;
3. micron order cobalt granule step 2 prepared is placed in argon shield environment, heat treatment 300 minutes under high-intensity magnetic field state, and heating rate is 0.5 DEG C/min, and temperature is 300 DEG C, and rate of temperature fall is 0.5 DEG C/min, and magnetic field intensity is 0.5T.In whole process, all keep high-intensity magnetic field state, comprise temperature-rise period, insulating process and temperature-fall period.Collect cobalt powder after being cooled to room temperature, the micron order cobalt granule with excellent electromagnetic wave absorption performance can be obtained.
Embodiment 8
1., by the pickling 0.5 minute in the acid solution of 0.1wt% concentration of micron order cobalt granule, remove the oxide layer on surface, then repeatedly clean three times, drying for standby in vacuum drying chamber with deionized water and absolute ethyl alcohol;
2. the micron order cobalt granule cleaned through step 1 is adopted wet ball grinding process 5 hours according to the ratio of grinding media to material of 5:1 in ball mill, rotational speed of ball-mill is 100 revs/min, and medium is toluene.Cobalt granule deionized water after ball-milling treatment and absolute ethyl alcohol are cleaned three times repeatedly, is placed in vacuum drying chamber drying for standby;
3. micron order cobalt granule step 2 prepared is placed in argon shield environment, heat treatment 5 minutes under high-intensity magnetic field state, and heating rate is 20 DEG C/min, and temperature is 300 DEG C, and rate of temperature fall is 0.5 DEG C/min, and magnetic field intensity is 0.5T.In whole process, all keep high-intensity magnetic field state, comprise temperature-rise period, insulating process and temperature-fall period.Collect cobalt powder after being cooled to room temperature, the micron order cobalt granule with excellent electromagnetic wave absorption performance can be obtained.
Embodiment 9
1., by the pickling 0.5 minute in the acid solution of 0.1wt% concentration of micron order cobalt granule, remove the oxide layer on surface, then repeatedly clean three times, drying for standby in vacuum drying chamber with deionized water and absolute ethyl alcohol;
2. the micron order cobalt granule cleaned through step 1 is adopted wet ball grinding process 5 hours according to the ratio of grinding media to material of 5:1 in ball mill, rotational speed of ball-mill is 100 revs/min, and medium is toluene.Cobalt granule deionized water after ball-milling treatment and absolute ethyl alcohol are cleaned three times repeatedly, is placed in vacuum drying chamber drying for standby;
3. micron order cobalt granule step 2 prepared is placed in argon shield environment, heat treatment 5 minutes under high-intensity magnetic field state, and heating rate is 0.5 DEG C/min, and temperature is 1400 DEG C, and rate of temperature fall is 0.5 DEG C/min, and magnetic field intensity is 0.5T.In whole process, all keep high-intensity magnetic field state, comprise temperature-rise period, insulating process and temperature-fall period.Collect cobalt powder after being cooled to room temperature, the micron order cobalt granule with excellent electromagnetic wave absorption performance can be obtained.
Embodiment 10
1., by the pickling 0.5 minute in the acid solution of 0.1wt% concentration of micron order cobalt granule, remove the oxide layer on surface, then repeatedly clean three times, drying for standby in vacuum drying chamber with deionized water and absolute ethyl alcohol;
2. the micron order cobalt granule cleaned through step 1 is adopted wet ball grinding process 5 hours according to the ratio of grinding media to material of 5:1 in ball mill, rotational speed of ball-mill is 100 revs/min, and medium is toluene.Cobalt granule deionized water after ball-milling treatment and absolute ethyl alcohol are cleaned three times repeatedly, is placed in vacuum drying chamber drying for standby;
3. micron order cobalt granule step 2 prepared is placed in argon shield environment, heat treatment 5 minutes under high-intensity magnetic field state, and heating rate is 0.5 DEG C/min, and temperature is 300 DEG C, and rate of temperature fall is 20 DEG C/min, and magnetic field intensity is 0.5T.In whole process, all keep high-intensity magnetic field state, comprise temperature-rise period, insulating process and temperature-fall period.Collect cobalt powder after being cooled to room temperature, the micron order cobalt granule with excellent electromagnetic wave absorption performance can be obtained.
Embodiment 11
1., by the pickling 0.5 minute in the acid solution of 0.1wt% concentration of micron order cobalt granule, remove the oxide layer on surface, then repeatedly clean three times, drying for standby in vacuum drying chamber with deionized water and absolute ethyl alcohol;
2. the micron order cobalt granule cleaned through step 1 is adopted wet ball grinding process 5 hours according to the ratio of grinding media to material of 5:1 in ball mill, rotational speed of ball-mill is 100 revs/min, and medium is toluene.Cobalt granule deionized water after ball-milling treatment and absolute ethyl alcohol are cleaned three times repeatedly, is placed in vacuum drying chamber drying for standby;
3. micron order cobalt granule step 2 prepared is placed in argon shield environment, heat treatment 5 minutes under high-intensity magnetic field state, and heating rate is 0.5 DEG C/min, and temperature is 300 DEG C, and rate of temperature fall is 0.5 DEG C/min, and magnetic field intensity is 14T.In whole process, all keep high-intensity magnetic field state, comprise temperature-rise period, insulating process and temperature-fall period.Collect cobalt powder after being cooled to room temperature, the micron order cobalt granule with excellent electromagnetic wave absorption performance can be obtained.
Embodiment 12
1., by the pickling 0.5 minute in the acid solution of 10wt% concentration of micron order cobalt granule, remove the oxide layer on surface, then repeatedly clean three times, drying for standby in vacuum drying chamber with deionized water and absolute ethyl alcohol;
2. the micron order cobalt granule cleaned through step 1 is adopted wet ball grinding process 5 hours according to the ratio of grinding media to material of 5:1 in ball mill, rotational speed of ball-mill is 100 revs/min, and medium is toluene.Cobalt granule deionized water after ball-milling treatment and absolute ethyl alcohol are cleaned three times repeatedly, is placed in vacuum drying chamber drying for standby;
3. micron order cobalt granule step 2 prepared is placed in argon shield environment, heat treatment 5 minutes under high-intensity magnetic field state, and heating rate is 0.5 DEG C/min, and temperature is 300 DEG C, and rate of temperature fall is 0.5 DEG C/min, and magnetic field intensity is 14T.In whole process, all keep high-intensity magnetic field state, comprise temperature-rise period, insulating process and temperature-fall period.Collect cobalt powder after being cooled to room temperature, the micron order cobalt granule with excellent electromagnetic wave absorption performance can be obtained.
Embodiment 13
1., by the pickling 30 minutes in the acid solution of 10wt% concentration of micron order cobalt granule, remove the oxide layer on surface, then repeatedly clean three times, drying for standby in vacuum drying chamber with deionized water and absolute ethyl alcohol;
2. the micron order cobalt granule cleaned through step 1 is adopted wet ball grinding process 5 hours according to the ratio of grinding media to material of 5:1 in ball mill, rotational speed of ball-mill is 100 revs/min, and medium is toluene.Cobalt granule deionized water after ball-milling treatment and absolute ethyl alcohol are cleaned three times repeatedly, is placed in vacuum drying chamber drying for standby;
3. micron order cobalt granule step 2 prepared is placed in argon shield environment, heat treatment 5 minutes under high-intensity magnetic field state, and heating rate is 0.5 DEG C/min, and temperature is 300 DEG C, and rate of temperature fall is 0.5 DEG C/min, and magnetic field intensity is 14T.In whole process, all keep high-intensity magnetic field state, comprise temperature-rise period, insulating process and temperature-fall period.Collect cobalt powder after being cooled to room temperature, the micron order cobalt granule with excellent electromagnetic wave absorption performance can be obtained.
Embodiment 14
1., by the pickling 30 minutes in the acid solution of 10wt% concentration of micron order cobalt granule, remove the oxide layer on surface, then repeatedly clean three times, drying for standby in vacuum drying chamber with deionized water and absolute ethyl alcohol;
2. the micron order cobalt granule cleaned through step 1 is adopted wet ball grinding process 5 hours according to the ratio of grinding media to material of 20:1 in ball mill, rotational speed of ball-mill is 100 revs/min, and medium is toluene.Cobalt granule deionized water after ball-milling treatment and absolute ethyl alcohol are cleaned three times repeatedly, is placed in vacuum drying chamber drying for standby;
3. micron order cobalt granule step 2 prepared is placed in argon shield environment, heat treatment 5 minutes under high-intensity magnetic field state, and heating rate is 0.5 DEG C/min, and temperature is 300 DEG C, and rate of temperature fall is 0.5 DEG C/min, and magnetic field intensity is 14T.In whole process, all keep high-intensity magnetic field state, comprise temperature-rise period, insulating process and temperature-fall period.Collect cobalt powder after being cooled to room temperature, the micron order cobalt granule with excellent electromagnetic wave absorption performance can be obtained.
Embodiment 15
1., by the pickling 30 minutes in the acid solution of 10wt% concentration of micron order cobalt granule, remove the oxide layer on surface, then repeatedly clean three times, drying for standby in vacuum drying chamber with deionized water and absolute ethyl alcohol;
2. the micron order cobalt granule cleaned through step 1 is adopted wet ball grinding process 80 hours according to the ratio of grinding media to material of 20:1 in ball mill, rotational speed of ball-mill is 100 revs/min, and medium is toluene.Cobalt granule deionized water after ball-milling treatment and absolute ethyl alcohol are cleaned three times repeatedly, is placed in vacuum drying chamber drying for standby;
3. it is 10 that micron order cobalt granule step 2 prepared is placed in vacuum
-6in Pa environment, heat treatment 5 minutes under high-intensity magnetic field state, heating rate is 0.5 DEG C/min, and temperature is 300 DEG C, and rate of temperature fall is 0.5 DEG C/min, and magnetic field intensity is 14T.In whole process, all keep high-intensity magnetic field state, comprise temperature-rise period, insulating process and temperature-fall period.Collect cobalt powder after being cooled to room temperature, the micron order cobalt granule with excellent electromagnetic wave absorption performance can be obtained.
Embodiment 16
1., by the pickling 30 minutes in the acid solution of 10wt% concentration of micron order cobalt granule, remove the oxide layer on surface, then repeatedly clean three times, drying for standby in vacuum drying chamber with deionized water and absolute ethyl alcohol;
2. the micron order cobalt granule in cleaning through step 1 is adopted wet ball grinding process 80 hours according to the ratio of grinding media to material of 20:1 in ball mill, rotational speed of ball-mill is 1400 revs/min, and medium is toluene.Cobalt granule deionized water after ball-milling treatment and absolute ethyl alcohol are cleaned three times repeatedly, is placed in vacuum drying chamber drying for standby;
3. it is 10 that micron order cobalt granule step 2 prepared is placed in vacuum
-6in Pa environment, heat treatment 5 minutes under high-intensity magnetic field state, heating rate is 0.5 DEG C/min, and temperature is 300 DEG C, and rate of temperature fall is 0.5 DEG C/min, and magnetic field intensity is 14T.In whole process, all keep high-intensity magnetic field state, comprise temperature-rise period, insulating process and temperature-fall period.Collect cobalt powder after being cooled to room temperature, the micron order cobalt granule with excellent electromagnetic wave absorption performance can be obtained.
Embodiment 17
1., by the pickling 30 minutes in the acid solution of 10wt% concentration of micron order cobalt granule, remove the oxide layer on surface, then repeatedly clean three times, drying for standby in vacuum drying chamber with deionized water and absolute ethyl alcohol;
2. the micron order cobalt granule in cleaning through step 1 is adopted wet ball grinding process 80 hours according to the ratio of grinding media to material of 20:1 in ball mill, rotational speed of ball-mill is 1400 revs/min, and medium is toluene.Cobalt granule deionized water after ball-milling treatment and absolute ethyl alcohol are cleaned three times repeatedly, is placed in vacuum drying chamber drying for standby;
3. it is 10 that micron order cobalt granule step 2 prepared is placed in vacuum
-6in Pa environment, heat treatment 300 minutes under high-intensity magnetic field state, heating rate is 0.5 DEG C/min, and temperature is 300 DEG C, and rate of temperature fall is 0.5 DEG C/min, and magnetic field intensity is 14T.In whole process, all keep high-intensity magnetic field state, comprise temperature-rise period, insulating process and temperature-fall period.Collect cobalt powder after being cooled to room temperature, the micron order cobalt granule with excellent electromagnetic wave absorption performance can be obtained.
Embodiment 18
1., by the pickling 30 minutes in the acid solution of 10wt% concentration of micron order cobalt granule, remove the oxide layer on surface, then repeatedly clean three times, drying for standby in vacuum drying chamber with deionized water and absolute ethyl alcohol;
2. the micron order cobalt granule cleaned through step 1 is adopted wet ball grinding process 80 hours according to the ratio of grinding media to material of 20:1 in ball mill, rotational speed of ball-mill is 1400 revs/min, and medium is toluene.Cobalt granule deionized water after ball-milling treatment and absolute ethyl alcohol are cleaned three times repeatedly, is placed in vacuum drying chamber drying for standby;
3. it is 10 that micron order cobalt granule step 2 prepared is placed in vacuum
-6in Pa environment, heat treatment 300 minutes under high-intensity magnetic field state, heating rate is 20 DEG C/min, and temperature is 300 DEG C, and rate of temperature fall is 0.5 DEG C/min, and magnetic field intensity is 14T.In whole process, all keep high-intensity magnetic field state, comprise temperature-rise period, insulating process and temperature-fall period.Collect cobalt powder after being cooled to room temperature, the micron order cobalt granule with excellent electromagnetic wave absorption performance can be obtained.
Embodiment 19
1., by the pickling 30 minutes in the acid solution of 10wt% concentration of micron order cobalt granule, remove the oxide layer on surface, then repeatedly clean three times, drying for standby in vacuum drying chamber with deionized water and absolute ethyl alcohol;
2. the micron order cobalt granule cleaned through step 1 is adopted wet ball grinding process 80 hours according to the ratio of grinding media to material of 20:1 in ball mill, rotational speed of ball-mill is 1400 revs/min, and medium is toluene.Cobalt granule deionized water after ball-milling treatment and absolute ethyl alcohol are cleaned three times repeatedly, is placed in vacuum drying chamber drying for standby;
3. it is 10 that micron order cobalt granule step 2 prepared is placed in vacuum
-6in Pa environment, heat treatment 300 minutes under high-intensity magnetic field state, heating rate is 20 DEG C/min, and temperature is 1400 DEG C, and rate of temperature fall is 0.5 DEG C/min, and magnetic field intensity is 14T.In whole process, all keep high-intensity magnetic field state, comprise temperature-rise period, insulating process and temperature-fall period.Collect cobalt powder after being cooled to room temperature, the micron order cobalt granule with excellent electromagnetic wave absorption performance can be obtained.
Embodiment 20
1., by the pickling 30 minutes in the acid solution of 10wt% concentration of micron order cobalt granule, remove the oxide layer on surface, then repeatedly clean three times, drying for standby in vacuum drying chamber with deionized water and absolute ethyl alcohol;
2. the micron order cobalt granule cleaned through step 1 is adopted wet ball grinding process 80 hours according to the ratio of grinding media to material of 20:1 in ball mill, rotational speed of ball-mill is 1400 revs/min, and medium is toluene.Cobalt granule deionized water after ball-milling treatment and absolute ethyl alcohol are cleaned three times repeatedly, is placed in vacuum drying chamber drying for standby;
3. it is 10 that micron order cobalt granule step 2 prepared is placed in vacuum
-6in Pa environment, heat treatment 300 minutes under high-intensity magnetic field state, heating rate is 20 DEG C/min, and temperature is 1400 DEG C, and rate of temperature fall is 20 DEG C/min, and magnetic field intensity is 14T.In whole process, all keep high-intensity magnetic field state, comprise temperature-rise period, insulating process and temperature-fall period.Collect cobalt powder after being cooled to room temperature, the micron order cobalt granule with excellent electromagnetic wave absorption performance can be obtained.
Embodiment 21
1., by the pickling 30 minutes in the acid solution of 10wt% concentration of micron order cobalt granule, remove the oxide layer on surface, then repeatedly clean three times, drying for standby in vacuum drying chamber with deionized water and absolute ethyl alcohol;
2. the micron order cobalt granule cleaned through step 1 is adopted wet ball grinding process 80 hours according to the ratio of grinding media to material of 20:1 in ball mill, rotational speed of ball-mill is 1400 revs/min, and medium is toluene.Cobalt granule deionized water after ball-milling treatment and absolute ethyl alcohol are cleaned three times repeatedly, is placed in vacuum drying chamber drying for standby;
3. it is 10 that micron order cobalt granule step 2 prepared is placed in vacuum
-6in Pa environment, heat treatment 300 minutes under high-intensity magnetic field state, heating rate is 20 DEG C/min, and temperature is 1400 DEG C, and rate of temperature fall is 20 DEG C/min, and magnetic field intensity is 0.5T.In whole process, all keep high-intensity magnetic field state, comprise temperature-rise period, insulating process and temperature-fall period.Collect cobalt powder after being cooled to room temperature, the micron order cobalt granule with excellent electromagnetic wave absorption performance can be obtained.
Embodiment 22
1., by the pickling 30 minutes in the acid solution of 5wt% concentration of micron order cobalt granule, remove the oxide layer on surface, then repeatedly clean three times, drying for standby in vacuum drying chamber with deionized water and absolute ethyl alcohol;
2. the micron order cobalt granule cleaned through step 1 is adopted wet ball grinding process 80 hours according to the ratio of grinding media to material of 20:1 in ball mill, rotational speed of ball-mill is 1400 revs/min, and medium is toluene.Cobalt granule deionized water after ball-milling treatment and absolute ethyl alcohol are cleaned three times repeatedly, is placed in vacuum drying chamber drying for standby;
3. it is 10 that micron order cobalt granule step 2 prepared is placed in vacuum
-6in Pa environment, heat treatment 300 minutes under high-intensity magnetic field state, heating rate is 20 DEG C/min, and temperature is 1400 DEG C, and rate of temperature fall is 20 DEG C/min, and magnetic field intensity is 0.5T.In whole process, all keep high-intensity magnetic field state, comprise temperature-rise period, insulating process and temperature-fall period.Collect cobalt powder after being cooled to room temperature, the micron order cobalt granule with excellent electromagnetic wave absorption performance can be obtained.
Embodiment 23
1., by the pickling 15 minutes in the acid solution of 5wt% concentration of micron order cobalt granule, remove the oxide layer on surface, then repeatedly clean three times, drying for standby in vacuum drying chamber with deionized water and absolute ethyl alcohol;
2. the micron order cobalt granule cleaned through step 1 is adopted wet ball grinding process 80 hours according to the ratio of grinding media to material of 20:1 in ball mill, rotational speed of ball-mill is 1400 revs/min, and medium is toluene.Cobalt granule deionized water after ball-milling treatment and absolute ethyl alcohol are cleaned three times repeatedly, is placed in vacuum drying chamber drying for standby;
3. it is 10 that micron order cobalt granule step 2 prepared is placed in vacuum
-6in Pa environment, heat treatment 300 minutes under high-intensity magnetic field state, heating rate is 20 DEG C/min, and temperature is 1400 DEG C, and rate of temperature fall is 20 DEG C/min, and magnetic field intensity is 0.5T.In whole process, all keep high-intensity magnetic field state, comprise temperature-rise period, insulating process and temperature-fall period.Collect cobalt powder after being cooled to room temperature, the micron order cobalt granule with excellent electromagnetic wave absorption performance can be obtained.
Embodiment 24
1., by the pickling 15 minutes in the acid solution of 5wt% concentration of micron order cobalt granule, remove the oxide layer on surface, then repeatedly clean three times, drying for standby in vacuum drying chamber with deionized water and absolute ethyl alcohol;
2. the micron order cobalt granule cleaned through step 1 is adopted wet ball grinding process 80 hours according to the ratio of grinding media to material of 10:1 in ball mill, rotational speed of ball-mill is 1400 revs/min, and medium is toluene.Cobalt granule deionized water after ball-milling treatment and absolute ethyl alcohol are cleaned three times repeatedly, is placed in vacuum drying chamber drying for standby;
3. it is 10 that micron order cobalt granule step 2 prepared is placed in vacuum
-1in Pa environment, heat treatment 300 minutes under high-intensity magnetic field state, heating rate is 20 DEG C/min, and temperature is 1400 DEG C, and rate of temperature fall is 20 DEG C/min, and magnetic field intensity is 0.5T.In whole process, all keep high-intensity magnetic field state, comprise temperature-rise period, insulating process and temperature-fall period.Collect cobalt powder after being cooled to room temperature, the micron order cobalt granule with excellent electromagnetic wave absorption performance can be obtained.
Embodiment 25
1., by the pickling 15 minutes in the acid solution of 5wt% concentration of micron order cobalt granule, remove the oxide layer on surface, then repeatedly clean three times, drying for standby in vacuum drying chamber with deionized water and absolute ethyl alcohol;
2. the micron order cobalt granule cleaned through step 1 is adopted wet ball grinding process 40 hours according to the ratio of grinding media to material of 10:1 in ball mill, rotational speed of ball-mill is 560 revs/min, and medium is toluene.Cobalt granule deionized water after ball-milling treatment and absolute ethyl alcohol are cleaned three times repeatedly, is placed in vacuum drying chamber drying for standby;
3. it is 10 that micron order cobalt granule step 2 prepared is placed in vacuum
-1in Pa environment, heat treatment 300 minutes under high-intensity magnetic field state, heating rate is 20 DEG C/min, and temperature is 1400 DEG C, and rate of temperature fall is 20 DEG C/min, and magnetic field intensity is 0.5T.In whole process, all keep high-intensity magnetic field state, comprise temperature-rise period, insulating process and temperature-fall period.Collect cobalt powder after being cooled to room temperature, the micron order cobalt granule with excellent electromagnetic wave absorption performance can be obtained.
Embodiment 26
1., by the pickling 15 minutes in the acid solution of 5wt% concentration of micron order cobalt granule, remove the oxide layer on surface, then repeatedly clean three times, drying for standby in vacuum drying chamber with deionized water and absolute ethyl alcohol;
2. the micron order cobalt granule cleaned through step 1 is adopted wet ball grinding process 40 hours according to the ratio of grinding media to material of 10:1 in ball mill, rotational speed of ball-mill is 560 revs/min, and medium is toluene.Cobalt granule deionized water after ball-milling treatment and absolute ethyl alcohol are cleaned three times repeatedly, is placed in vacuum drying chamber drying for standby;
3. it is 10 that micron order cobalt granule step 2 prepared is placed in vacuum
-1in Pa environment, heat treatment 150 minutes under high-intensity magnetic field state, heating rate is 20 DEG C/min, and temperature is 1400 DEG C, and rate of temperature fall is 20 DEG C/min, and magnetic field intensity is 0.5T.In whole process, all keep high-intensity magnetic field state, comprise temperature-rise period, insulating process and temperature-fall period.Collect cobalt powder after being cooled to room temperature, the micron order cobalt granule with excellent electromagnetic wave absorption performance can be obtained.
Embodiment 27
1., by the pickling 15 minutes in the acid solution of 5wt% concentration of micron order cobalt granule, remove the oxide layer on surface, then repeatedly clean three times, drying for standby in vacuum drying chamber with deionized water and absolute ethyl alcohol;
2. the micron order cobalt granule cleaned through step 1 is adopted wet ball grinding process 40 hours according to the ratio of grinding media to material of 10:1 in ball mill, rotational speed of ball-mill is 560 revs/min, and medium is toluene.Cobalt granule deionized water after ball-milling treatment and absolute ethyl alcohol are cleaned three times repeatedly, is placed in vacuum drying chamber drying for standby;
3. it is 10 that micron order cobalt granule step 2 prepared is placed in vacuum
-1in Pa environment, heat treatment 150 minutes under high-intensity magnetic field state, heating rate is 10 DEG C/min, and temperature is 1400 DEG C, and rate of temperature fall is 20 DEG C/min, and magnetic field intensity is 0.5T.In whole process, all keep high-intensity magnetic field state, comprise temperature-rise period, insulating process and temperature-fall period.Collect cobalt powder after being cooled to room temperature, the micron order cobalt granule with excellent electromagnetic wave absorption performance can be obtained.
Embodiment 28
1., by the pickling 15 minutes in the acid solution of 5wt% concentration of micron order cobalt granule, remove the oxide layer on surface, then repeatedly clean three times, drying for standby in vacuum drying chamber with deionized water and absolute ethyl alcohol;
2. the micron order cobalt granule cleaned through step 1 is adopted wet ball grinding process 40 hours according to the ratio of grinding media to material of 10:1 in ball mill, rotational speed of ball-mill is 560 revs/min, and medium is toluene.Cobalt granule deionized water after ball-milling treatment and absolute ethyl alcohol are cleaned three times repeatedly, is placed in vacuum drying chamber drying for standby;
3. it is 10 that micron order cobalt granule step 2 prepared is placed in vacuum
-1in Pa environment, heat treatment 150 minutes under high-intensity magnetic field state, heating rate is 10 DEG C/min, and temperature is 750 DEG C, and rate of temperature fall is 20 DEG C/min, and magnetic field intensity is 0.5T.In whole process, all keep high-intensity magnetic field state, comprise temperature-rise period, insulating process and temperature-fall period.Collect cobalt powder after being cooled to room temperature, the micron order cobalt granule with excellent electromagnetic wave absorption performance can be obtained.
Embodiment 29
1., by the pickling 15 minutes in the acid solution of 5wt% concentration of micron order cobalt granule, remove the oxide layer on surface, then repeatedly clean three times, drying for standby in vacuum drying chamber with deionized water and absolute ethyl alcohol;
2. the micron order cobalt granule cleaned through step 1 is adopted wet ball grinding process 40 hours according to the ratio of grinding media to material of 10:1 in ball mill, rotational speed of ball-mill is 560 revs/min, and medium is toluene.Cobalt granule deionized water after ball-milling treatment and absolute ethyl alcohol are cleaned three times repeatedly, is placed in vacuum drying chamber drying for standby;
3. it is 10 that micron order cobalt granule step 2 prepared is placed in vacuum
-3in Pa environment, heat treatment 150 minutes under high-intensity magnetic field state, heating rate is 10 DEG C/min, and temperature is 750 DEG C, and rate of temperature fall is 10 DEG C/min, and magnetic field intensity is 0.5T.In whole process, all keep high-intensity magnetic field state, comprise temperature-rise period, insulating process and temperature-fall period.Collect cobalt powder after being cooled to room temperature, the micron order cobalt granule with excellent electromagnetic wave absorption performance can be obtained.
Embodiment 30
1., by the pickling 15 minutes in the acid solution of 5wt% concentration of micron order cobalt granule, remove the oxide layer on surface, then repeatedly clean three times, drying for standby in vacuum drying chamber with deionized water and absolute ethyl alcohol;
2. the micron order cobalt granule cleaned through step 1 is adopted wet ball grinding process 40 hours according to the ratio of grinding media to material of 10:1 in ball mill, rotational speed of ball-mill is 560 revs/min, and medium is toluene.Cobalt granule deionized water after ball-milling treatment and absolute ethyl alcohol are cleaned three times repeatedly, is placed in vacuum drying chamber drying for standby;
3. it is 10 that micron order cobalt granule step 2 prepared is placed in vacuum
-3in Pa environment, heat treatment 150 minutes under high-intensity magnetic field state, heating rate is 10 DEG C/min, and temperature is 750 DEG C, and rate of temperature fall is 10 DEG C/min, and magnetic field intensity is 6T.In whole process, all keep high-intensity magnetic field state, comprise temperature-rise period, insulating process and temperature-fall period.Collect cobalt powder after being cooled to room temperature, the micron order cobalt granule with excellent electromagnetic wave absorption performance can be obtained.
Claims (4)
1. improve a method for micron order cobalt granule electromagnetic wave absorption performance, it is characterized in that, described method comprises the following steps:
(1) micron order cobalt granule is placed in the acid solution pickling 0.5 ~ 30 minute of 0.1 ~ 10wt% concentration, removes the oxide layer on surface, then repeatedly clean three times, drying for standby in vacuum drying chamber with deionized water and absolute ethyl alcohol;
(2) the micron order cobalt granule for subsequent use after step (1) cleaning is adopted wet ball grinding process 5 ~ 80 hours according to the ratio of grinding media to material of 5:1 ~ 10:1 in ball mill, rotational speed of ball-mill is 100 ~ 1200 revs/min, and medium is toluene; Cobalt granule deionized water after ball-milling treatment and absolute ethyl alcohol are cleaned three times repeatedly, is placed in vacuum drying chamber drying for standby;
(3) the micron order cobalt granule after step (2) ball milling is placed in oxygen-free environment, heat treatment 2 ~ 300/min under magnetic field state, heating rate is 0.5 ~ 20 DEG C, and temperature is 300 ~ 1400 DEG C, rate of temperature fall is 0.5 ~ 20 DEG C/min, and magnetic field intensity is 0.5 ~ 14T; All magnetic field state is kept in whole heat treatment process; Collect cobalt granule after being cooled to room temperature, the micron order cobalt granule with excellent electromagnetic wave absorption performance can be obtained.
2. the method improving micron order cobalt granule electromagnetic wave absorption performance as claimed in claim 1, is characterized in that: in described step (3), whole heat treatment process comprises insulating process and temperature-fall period.
3. the method improving micron order cobalt granule electromagnetic wave absorption performance as claimed in claim 1, it is characterized in that: in described step (3), the oxygen-free environment of heat treatment process is vacuum is 10
-6-10
-1the vacuum environment of Pa or employing argon shield.
4. the method improving micron order cobalt granule electromagnetic wave absorption performance as claimed in claim 1, is characterized in that: the particle size range of the cobalt granule in described step (1) is 0.5 ~ 30 micron.
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