CN106957985A - A kind of DyHoFe electromagnetic wave absorbing materials and preparation method thereof - Google Patents
A kind of DyHoFe electromagnetic wave absorbing materials and preparation method thereof Download PDFInfo
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- CN106957985A CN106957985A CN201710290632.XA CN201710290632A CN106957985A CN 106957985 A CN106957985 A CN 106957985A CN 201710290632 A CN201710290632 A CN 201710290632A CN 106957985 A CN106957985 A CN 106957985A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/041—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by mechanical alloying, e.g. blending, milling
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Abstract
The invention discloses a kind of DyHoFe electromagnetic wave absorbing materials and preparation method thereof, the stoichiometric proportion of its molecular formula is：Dy：0~1.5、Ho：9.0~10.5、Fe：89.5.It is prepared from by the technique comprising following key steps：Using Dy, Ho, Fe of purity >=99.90% as raw material, the melting under argon gas protection, ingot casting is heat-treated in 800~1000 DEG C under vacuo, afterwards with ice water quenching, is then sieved after Mechanical Crushing, then ball powder-grinding.A kind of DyHoFe electromagnetic wave absorbing materials of the present invention, in 2~18GHz microwave bands, there are preferable Microwave Absorption Properties especially in 2 8GHz, absorption band is wider, oxidation resistance, corrosion resistance and temperature stability preferably, and have the features such as preparation technology is simple.In electromagnetic wave absorbing material, DyHoFe alloys electromagnetic wave absorbing material of the invention is applied to prepare with absorption band is wide, absorbing property is good, heat endurance is good and the microwave absorption product with certain oxidation resistance and decay resistance.
Description
Technical field
The invention belongs to magnetic microwave absorbing material field, specifically a kind of DyHoFe electromagnetic wave absorbing materials and its preparation side
Method.
Background technology
In recent years, with the development of science and technology, substantial amounts of electronic equipment enters daily life, and electromagnetic radiation pollution is increasingly
Seriously.The electromagnetic environment of deterioration can not only disturb electronic instrument, the normal work of equipment, and can influence the health of the mankind.Army
In thing, the international competition of weaponry is growing more intense, due to developing rapidly for modern Detection Techniques and precision guided weapon, to force
The existence of device causes great threat, therefore studies the stealthy imperative of weapon.And absorbing material is exactly military stealthy, micro-
The defence and militaries such as ripple darkroom, microwave communication, electromagnetic information leakage protection, electromagnetic interference shielding, electromagnetic radiation protection and civilian skill
One of critical material in art field, particularly electromagnetic shielding, the development of stealth technology in recent years, make the research of absorbing material increasingly
Paid attention to by people.
Therefore the application market of absorbing material is very big.At present, conventional absorbing material mainly have ferrite,
Conductive fiber, CNT, SiC material and magnetic material etc..Wherein because ferrite is that the class for studying comparative maturity is inhaled
Wave material, but there is also saturation magnetization is low, the suction wide narrower, density of wave frequency is larger, preparation process pollutes environment etc. simultaneously
Feature, limits its extensive use in specific environment.Because soft magnetic metal micro mist possesses high Curie's temperature in magnetic material
Degree, good temperature stability, high saturation magnetization can obtain higher magnetic loss in 2~18GHz band limits,
And relatively low eddy-current loss, and it is relatively small applied to microwave absorbing coating matching thickness, have as absorbing material and well should
Use prospect.And it is mainly Fe, Co, Ni and its alloy powder etc. using most magnetically soft alloy micro mists at present.Due to Fe resource
Compare abundant, compare Co and Ni less expensive, and also the absorbing property of Fe based alloy electromagnetic wave absorbing materials is preferable, institute
There is certain application prospect with Fe based alloy electromagnetic wave absorbing materials.
Rare earth element is and very strong due to its unique 4f electronic structures, big atomic magnetic moment, high magnetocrystalline anisotropy
The feature such as Quantum geometrical phase magnetic moment, particularly when rare earth element and other elements formation complex, with more abundant
Magnetics, electricity and optical signature.Therefore, some thuliums that adulterated in Fe sills can effectively improve the suction of its microwave
Performance is received, and with preferable frequency range effect.
Existing absorbing material is less desirable in 2~18GHz Microwave Absorption Properties, especially in S-band (2-4GHz) and C
Wave band (4-8GHz), has that the thick too big, absorption band of microwave absorbing coating is narrow and absorbing property.
Absorption band is wide, light weight, thickness of thin, physical and mechanical property are good, it is easy to use the features such as be electromagnetic wave absorbing material
Developing direction.With deepization of research work, the study hotspot that quality-high and inexpensive electromagnetic wave absorbing material is researcher is developed.
The content of the invention
It is an object of the invention to overcome the deficiencies in the prior art, and one kind is provided in 2~18GHz microwave bands, especially
It has preferable Microwave Absorption Properties in 4-8GHz wave bands, and absorption band is wide, wave absorbing efficiency is high, heat endurance is good and with one
Determine DyHoFe electromagnetic wave absorbing materials of oxidation resistance and decay resistance and preparation method thereof.
A kind of DyHoFe electromagnetic wave absorbing materials, the stoichiometric proportion of its molecular formula is that atomic percent is：Dy：0~1.5,
Ho：9~10.5, Fe：89.5, above-mentioned each component percentage composition sum is 100.
A kind of DyHoFe electromagnetic wave absorbing materials preparation method, it is characterized in that, include following key steps：
1) dispensing：Dy, Ho, Fe metal using purity >=99.90% is raw material, by Dy0~1.5Ho9~10.5Fe89.5Atom hundred
Divide the stoichiometric equation dispensing of ratio, above-mentioned each component percentage composition sum is 100；
2) melting：By step 1) in dispensing melting in non-consumable arc furnace under argon gas or vacuum protection；
3) homogenization heat treatment：In the quartz ampoule that melted ingot casting is sealed in vacuum or argon gas, 800 DEG C~1000
Homogenization Treatments are carried out at a temperature of DEG C；
4) coarse crushing：Obtained alloy pig is broken into meal, and carries out sieving processing；
5) ball milling：Meal after sieving is subjected to ball milling；
By above-mentioned steps, DyHoFe electromagnetic wave absorbing materials are made.
Step 1) in, with Dy0~1.5Ho9~10.5Fe89.5On the basis of the stoichiometric proportion of atomic percent, add 2%~3%
Dy and 2%~3%Ho.
Step 2) in, in order to ensure the uniformity of alloy, melting need to be overturn 3~4 times.
Step 3) in, the Homogenization Treatments process includes insulation 3~15 days, and frozen water/Quenching in liquid nitrogen is carried out afterwards.
Step 4) in, meal is sieved using the metallic screen of 100 mesh pore sizes, makes described coarse powder particles degree small
In 0.2mm.
Step 5) in, the meal after sieving is put into zirconia ball grinding jar and carried out under conditions of ethanol makees protective agent
Ball-milling treatment, Ball-milling Time is 15~24h, and drum's speed of rotation is 300~350 revs/min, described zirconia ball and meal
Mass ratio is 15~20:1.
The electromagnetic parameter of product is detected as follows and calculates reflectivity R：
By DyHoFe alloy powders：Paraffin=4:The ratio mixing of 1 (mass ratio), is made external diameter and internal diameter respectively 7mm
And 3mm, thickness is 2.5~3.5mm or so coaxial sample, and examination is measured respectively using HP8722ES microwave vector network analyzers
Complex permeability and complex dielectric permittivity of the sample in 2-18GHz frequency ranges.Go out the reflectivity of single-layer absorber using following formula calculating simulation
R：
ε in formular、μrIt is respectively the relative dielectric constant, relative permeability and thickness of absorbing material with d, f is electromagnetic wave
Frequency, C be electromagnetic wave in the spread speed (i.e. the light velocity) of free space, j is imaginary unit.
It is demonstrated experimentally that the DyHoFe alloy electromagnetic wave absorbing materials of the present invention, when DyHoFe alloy powders with paraffin by 4:1 ratio
Example (mass ratio) is mixed into compound, in 2~18GHz microwave bands, and microwave absorbing coating thickness is combined between 1.2~4.0mm
Thing is respectively less than -10dB to the reflectivity minimum peak of microwave, and absorptivity is more than 90%；And with preferable wideband effect.When multiple
When compound thickness is 1.5mm, -44.02dB is can reach in 10.72GHz reflections at frequencies rate peak value minimums, and with preferably micro-
Ripple assimilation effect and wideband effect.In addition, having in S-band (2~4GHz) and C-band (4~8GHz) interior compound preferable
Microwave absorption effect, Dy1.0Ho9.5Fe89.5Powder, can to the absorption peak of microwave in S-band compound when thickness is 4.0mm
Reach -27.18dB, Ho10.5Fe89.5Powder is reachable to the absorption peak of microwave in C-band compound when thickness is 2.0mm
To -26.02dB, and with preferable wideband effect.
The DyHoFe electromagnetic wave absorbing materials of the present invention, in 2~18GHz microwave bands, have preferable especially in 2-8GH
Microwave Absorption Properties, absorption band is wider, oxidation resistance, corrosion resistance and temperature stability preferably, and preparation technology
Fairly simple the features such as.In electromagnetic wave absorbing material, DyHoFe alloy electromagnetic wave absorbing materials of the invention have suitable for preparation
Absorption band is wide, absorbing property is good, heat endurance is good and the microwave absorption production with certain oxidation resistance and decay resistance
Product.
Brief description of the drawings
Fig. 1 is the preparation method process chart of the present invention；
Fig. 2 is Ho10.5Fe89.5Alloy electromagnetic wave absorbing material test result figure；
Fig. 3 is Dy0.5Ho10.0Fe89.5Alloy electromagnetic wave absorbing material test result figure；
Fig. 4 is Dy1.0Ho9.5Fe89.5Alloy electromagnetic wave absorbing material test result figure；
Fig. 5 is Dy1.5Ho9.0Fe89.5Alloy electromagnetic wave absorbing material test result figure；
Embodiment
Embodiment 1
Prepare Ho10.5Fe89.5The specific implementation step of atomic percent electromagnetic wave absorbing material is：
1) dispensing：By Ho, Fe metal of purity >=99.90%, by Ho10.5Fe89.5The stoichiometric proportion of molecular formula is matched somebody with somebody
Expect, add 2%~3% Dy and Ho during dispensing.
2) melting：By step 1) in dispensing argon gas protection under the melting in non-consumable arc furnace, in order to ensure
The composition of alloy is uniform, and melting 4 times is overturn repeatedly.
3) homogenization heat treatment：Melted ingot casting is sealed in vitreosil pipe, 3 days are incubated at a temperature of 800 DEG C
Ice water quenching afterwards；
4) coarse crushing：Obtained alloy pig is broken into the meal that granularity is respectively less than 0.2mm, and it is big using 100 mesh holes
Small metallic screen is sieved；
5) ball milling：Meal after sieving is put into zirconia ball grinding jar and carries out ball-milling treatment.The zirconia ball with
The mass ratio of meal is 15:1, the ball-milling technology is in the case that ethanol makees protective agent, and Ball-milling Time is 15h, and ball mill turns
Speed is 300 revs/min.
Product test：By alloy powder:Paraffin=4:The ratio mixing of 1 (mass ratio), is made external diameter and internal diameter is respectively
7mm and 3mm, 2.5~3.5mm of thickness or so coaxial sample, are measured respectively using HP8722ES microwave vector network analyzers
The complex permeability and complex dielectric permittivity of sample 2~18GHz frequency ranges.Then single-layer absorber is gone out in thickness using following formula calculating simulation
Degree is respectively 1.2mm, 1.6mm, 2.0mm, 2.4mm, 2.8mm, 3.0mm reflectivity R.
ε in formula Chinese styler、μrIt is respectively the relative dielectric constant, relative permeability and thickness of absorbing material with d, f is electromagnetism
The frequency of ripple, C be electromagnetic wave in the spread speed (i.e. the light velocity) of free space, j is imaginary unit.
The performance test results:
Fig. 2 is Ho10.5Fe89.5/ paraffin compound [powder:Paraffin=4:1 (mass ratio)] in 2~18GHz microwave bands
Thickness is respectively 1.2mm, 1.6mm, 2.0mm, 2.4mm, 2.8mm, reflectivity during 3.0mm.It can be obtained from figure：In all thickness
In degree, minimum reflectance peak value is respectively less than -10dB (absorptivity is more than 90%), and<- 10dB frequency range is wider, with preferable
Wideband effect.It is about -35.11dB in 9.76GHz reflections at frequencies rate peak values when composite thickness is 1.6mm.In addition, working as
When composite thickness is 2.0mm, -26.02dB, and tool are can reach to the absorption peak of microwave in C-band (4~8GHz) compound
There is preferable wideband effect.
Embodiment 2
Prepare Dy0.5Ho10.0Fe89.5The specific implementation step of atomic percent electromagnetic wave absorbing material is：
1) dispensing：By Dy, Ho, Fe metal of purity >=99.90%, by Dy0.5Ho10.0Fe89.5The chemistry meter of molecular formula
Measure than dispensing, add 2%~3% Dy and Ho during dispensing.
2) melting：By step 1) in dispensing argon gas protection under the melting in non-consumable arc furnace, in order to ensure
The composition of alloy is uniform, and melting 3~4 times is overturn repeatedly.
3) homogenization heat treatment：Melted ingot casting is sealed in vitreosil pipe, 7 days are incubated at a temperature of 850 DEG C
Ice water quenching afterwards；
4) coarse crushing：Obtained alloy pig is broken into the meal that granularity is respectively less than 0.2mm, and it is big using 100 mesh holes
Small metallic screen is sieved；
5) ball milling：Meal after sieving is put into zirconia ball grinding jar and carries out ball-milling treatment.The zirconia ball with
The mass ratio of meal is 20:1, the ball-milling technology is in the case that ethanol makees protective agent, and Ball-milling Time is 20h, and ball mill turns
Speed is 320 revs/min.
Product test：By alloy powder:Paraffin=4:The ratio mixing of 1 (mass ratio), is made external diameter and internal diameter is respectively
7mm and 3mm, 2.5~3.5mm of thickness or so coaxial sample, are measured respectively using HP8722ES microwave vector network analyzers
The complex permeability and complex dielectric permittivity of sample 2~18GHz frequency ranges.Measurement and calculating are with example 1, then using computer simulator
Simulate the reflectivity that single-layer absorber thickness is respectively 1.2mm, 1.5mm, 2.0mm, 2.4mm, 2.8mm, 3.0mm.
The performance test results:
Fig. 3 is Dy0.5Ho10.0Fe89.5/ paraffin compound [powder:Paraffin=4:1 (mass ratio)] in 2~18GHz microwave ripples
Reflectivity when thickness is respectively 1.2mm, 1.5mm, 2.0mm, 2.4mm, 2.8mm, 3.0mm in section.It can be obtained from figure：All
Thickness in, minimum reflectance peak value is respectively less than -10dB (absorptivity be more than 90%), there is preferable wideband effect.Work as compound
It is about -44.02dB in 10.72GHz reflections at frequencies rate peak values, with preferable microwave wave-absorbing effect when thickness is 1.5mm.
In addition, when composite thickness is 2.0~3.0mm, compound has excellent microwave absorption effect in C-band (4~8GHz),
It is about -24.67dB in 7.52GHz reflections at frequencies rate peak values when the thickness of compound is 2.0mm, and<- 10dB frequency range
Reach 1.68GHz.
Embodiment 3
Prepare Dy1.0Ho9.5Fe89.5The specific implementation step of atomic percent electromagnetic wave absorbing material is：
1) dispensing：By Dy, Ho, Fe metal of purity >=99.90%, by Dy1.0Ho9.5Fe89.5The chemistry meter of molecular formula
Measure than dispensing, add 2%~3% Dy and Ho during dispensing.
2) melting：By step 1) in dispensing argon gas protection under the melting in non-consumable arc furnace, in order to ensure
The composition of alloy is uniform, and melting 3~4 times is overturn repeatedly.
3) homogenization heat treatment：Melted ingot casting is sealed in vitreosil pipe, 10 days are incubated at a temperature of 900 DEG C
Ice water quenching afterwards；
4) coarse crushing：Obtained alloy pig is broken into the meal that granularity is respectively less than 0.2mm, and it is big using 100 mesh holes
Small metallic screen is sieved；
5) ball milling：Meal after sieving is put into zirconia ball grinding jar and carries out ball-milling treatment.The zirconia ball with
The mass ratio of meal is 15:1, the ball-milling technology is in the case that ethanol makees protective agent, and Ball-milling Time is 24h, and ball mill turns
Speed is 350 revs/min.
Product test：By alloy powder:Paraffin=4:The ratio mixing of 1 (mass ratio), is made external diameter and internal diameter is respectively
7mm and 3mm, 2.5~3.5mm of thickness or so coaxial sample, are measured respectively using HP8722ES microwave vector network analyzers
The complex permeability and complex dielectric permittivity of sample 2~18GHz frequency ranges.Measurement and calculating are with example 1, then using computer simulator
Simulate the reflectivity that single-layer absorber thickness is respectively 2.0mm, 2.4mm, 2.8mm, 3.2mm, 3.6mm, 4.0mm.
The performance test results:
Fig. 4 is Dy1.0Ho9.5Fe89.5/ paraffin compound [powder:Paraffin=4:1 (mass ratio)] in 2~18GHz microwave ripples
Reflectivity when thickness is respectively 2.0mm, 2.4mm, 2.8mm, 3.2mm, 3.6mm, 4.0mm in section.It can be obtained from figure：All
Thickness in, minimum reflectance peak value is respectively less than -10dB (absorptivity be more than 90%), there is preferable wideband effect.In addition, in S
Wave band (2~4GHz) compound has preferable microwave absorption effect, when composite thickness is 4.0mm, in 2.88GHz frequencies
It is about -27.18dB to locate reflectance peak, and<- 10dB frequency range reaches 0.72GHz, has preferable wave absorbtion in low-frequency range
Energy.
Embodiment 4
Prepare Dy1.5Ho9.0Fe89.5The specific implementation step of atomic percent electromagnetic wave absorbing material is：
1) dispensing：By Dy, Ho, Fe metal of purity >=99.90%, by Dy1.5Ho9.0Fe89.5The chemistry meter of molecular formula
Measure than dispensing, add 2%~3% Dy and Ho during dispensing.
2) melting：By step 1) in dispensing argon gas protection under the melting in non-consumable arc furnace, in order to ensure
The composition of alloy is uniform, and melting 3~4 times is overturn repeatedly.
3) homogenization heat treatment：Melted ingot casting is sealed in vitreosil pipe, 3 days are incubated at a temperature of 1000 DEG C
Ice water quenching afterwards；
4) coarse crushing：Obtained alloy pig is broken into the meal that granularity is respectively less than 0.2mm, and it is big using 100 mesh holes
Small metallic screen is sieved；
5) ball milling：Meal after sieving is put into zirconia ball grinding jar and carries out ball-milling treatment.The zirconia ball with
The mass ratio of meal is 20:1, the ball-milling technology is in the case that ethanol makees protective agent, and Ball-milling Time is 20h, and ball mill turns
Speed is 300 revs/min.
Product test：By alloy powder:Paraffin=4:The ratio mixing of 1 (mass ratio), is made external diameter and internal diameter is respectively
7mm and 3mm, 2.5~3.5mm of thickness or so coaxial sample, are measured respectively using HP8722ES microwave vector network analyzers
The complex permeability of sample 2~18GHz frequency ranges, complex dielectric permittivity.Measurement and calculating are with example 1, then using computer simulator
Simulate reflectivity when single-layer absorber thickness is respectively 2.0mm, 2.2mm, 2.4mm, 2.6mm, 2.8mm, 3.0mm.
The performance test results:
Fig. 5 is Dy1.5Ho9.0Fe89.5/ paraffin compound [powder:Paraffin=4:1 (mass ratio)] in 2~18GHz microwave ripples
Reflectivity when thickness is respectively 2.0mm, 2.2mm, 2.4mm, 2.6mm, 2.8mm, 3.0mm in section.It can be obtained from figure：All
Thickness in, minimum reflectance peak value is respectively less than -10dB (absorptivity be more than 90%), there is preferable wideband effect.In addition, institute
Have in thickness, all there is preferable microwave absorption effect in C-band (4~8GHz), when composite thickness is 2.0mm,
7.84GHz reflections at frequencies rate peak values are about -22.74dB.
Claims (7)
1. a kind of DyHoFe electromagnetic wave absorbing materials, it is characterised in that the stoichiometric proportion of its molecular formula is that atomic percent is：
Dy：0~1.5、Ho：9.0~10.5、Fe：89.5, above-mentioned each component percentage composition sum is 100.
2. a kind of preparation method of DyHoFe magnetic microwave absorbing material, it is characterised in that specifically include following steps：
1）Dispensing：Dy, Ho, Fe metal using purity >=99.90% is raw material, by Dy0~1.5Ho9~10.5Fe89.5Atomic percent
Stoichiometric equation dispensing, above-mentioned each component percentage composition sum is 100；
2）Melting：By step 1）In dispensing melting in non-consumable arc furnace under argon gas or vacuum protection；
3）Homogenization heat treatment：In the quartz ampoule that melted ingot casting is sealed in vacuum or argon gas, in 800 DEG C ~ 1000 DEG C temperature
Degree is lower to carry out Homogenization Treatments；
4）Coarse crushing：Obtained alloy pig is broken into meal, and carries out sieving processing；
5）Ball milling：Meal after sieving is subjected to ball milling；
By above-mentioned steps, DyHoFe electromagnetic wave absorbing materials are made.
3. preparation method according to claim 2, it is characterised in that step 1）In, with Dy0~1.5Ho9~10.5Fe89.5Atom
On the basis of the stoichiometric proportion of percentage, add 2% ~ 3% Dy and 2% ~ 3%Ho.
4. preparation method according to claim 2, it is characterised in that described step 2）In melting, in the non-of standard
Carry out, in order to ensure the homogeneity of ingredients of alloy, need to overturn 3 ~ 4 times in consumable vacuum arc furnace ignition.
5. preparation method according to claim 2, it is characterised in that described step 3）In Homogenization Treatments process bag
Include insulation 3 ~ 15 days, frozen water/Quenching in liquid nitrogen is carried out afterwards.
6. preparation method according to claim 2, it is characterised in that described step 4）In meal, granularity is less than
0.2mm, and sieved using the metallic screen of 100 mesh pore sizes.
7. preparation method according to claim 2, it is characterised in that step 5）In, the meal after sieving is put into oxygen
Change and carry out ball-milling treatment in zirconium ball grinder under conditions of ethanol makees protective agent, Ball-milling Time is 15 ~ 24h, and drum's speed of rotation is
300 ~ 350 revs/min, described zirconia ball and the mass ratio of meal are 15 ~ 20:1.
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