CN106801160A - Blacker-than-black nanoporous Fe and preparation method thereof - Google Patents
Blacker-than-black nanoporous Fe and preparation method thereof Download PDFInfo
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- CN106801160A CN106801160A CN201710003628.0A CN201710003628A CN106801160A CN 106801160 A CN106801160 A CN 106801160A CN 201710003628 A CN201710003628 A CN 201710003628A CN 106801160 A CN106801160 A CN 106801160A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C3/00—Removing material from alloys to produce alloys of different constitution separation of the constituents of alloys
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C33/00—Making ferrous alloys
Abstract
The invention discloses a kind of preparation method of blacker-than-black nanoporous Fe, belong to technical field of nanometer material preparation, including：1) synthesis Mn contents are in 68 90at%, and Cu contents carry out fast quenching and obtain single-phase alloy less than the FeMnCu prealloy liquations in the range of 0.3at% in 1,240 1700 degrees Celsius of liquation；2) by under 4 25 degrees celsius, FeMnCu prealloys are placed in be stood in the hydrochloric acid solution that volumetric concentration is 1% 5% carries out de- alloy treatment for 30 60 minutes；3) the complete product of de- alloy is taken out, difference is successively 0.1% in volumetric concentration, is rinsed in 0.01% hydrochloric acid solution, and the time is no more than 10 seconds, then is rinsed in ultra-pure water, and the time is no more than 30s；Product after rinsing is taken out, blacker-than-black nanoporous Fe materials are obtained by being dried under the conditions of inert gas shielding.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, and in particular to blacker-than-black nanoporous Fe and preparation method thereof.
Background technology
Blacker-than-black material, is that one kind is less than 1%, material of the absorptivity higher than 99% to a range of incident ray reflectivity
Material.On many optical devices, sensor and solar energy converter, because the interface reflection unnecessary to incident light can be to property
Many adverse effects can be produced, therefore such devices are very urgent to the demand of blacker-than-black material.Simultaneously because blacker-than-black material is in itself
Excellent Stealth Fighter, also has very big purposes in military aspect.
In consideration of it, blacker-than-black material obtains extensive research and applies in recent years.It is by Surrey that current performance is most prominent
The Vantablack that Nanosys Inc. develops, the CNT composition that it is mainly arranged vertically, but cost of manufacture is very
It is high.Other common used materials also include amorphous carbon and the black silicon class nonmetallic materials of polycrystalline, and nickel phosphorus intermediate alloy material, simple metal surpasses
There is not been reported for black-materials.Its form includes the irregular surface of nano-tube array, dimpling array and roughening, with three-dimensional even
The blacker-than-black device of logical nano-porous structure has not been reported.Preparation method is mainly including chemical vapor deposition, biological template method etc..
There is high cost in these methods, it is impossible to the shortcomings of being mass produced mostly.And the present invention prepares blacker-than-black using de- alloyage
Material, preparation method is simple and easy to apply.The product of acquisition is the nano-porous structure Fe with three-dimensional communication structure, and finished product price is low
It is honest and clean, the wide advantage of light abstraction width.
The content of the invention
Technical problem：It is an object of the invention to provide a kind of preparation method of blacker-than-black nanoporous Fe, the preparation method
Simply, there is the pore passage structure of three-dimensional communication using its blacker-than-black nanoporous Fe for preparing；Another object of the present invention is to carry
For blacker-than-black nanoporous Fe prepared by the method, the material has the advantages that light abstraction width is wide.
Technical scheme：For achieving the above object, the present invention is adopted the following technical scheme that：
The preparation method of blacker-than-black nanoporous Fe, comprises the following steps：
1) homogeneous metal liquation is obtained by sensing heating after the mixing of the Fe by purity more than 99%, Mn and Cu simple metal
After carry out fast quenching, obtain the FeMnCu prealloys of single phase structure；Wherein, raw material simple metal atomic percent is Mn contents
68-90at%, Cu content 0-0.3at%；Induction heating temperature is not higher than 1700 degrees Celsius, and the heat time is no longer than 20 minutes,
Heating times are not less than 2 times；1240-1700 degrees Celsius of molten metal fast quenching temperature after uniform, obtains phase structure
FeMnCu prealloys；
2) by under 4-25 degrees celsius, FeMnCu alloys are placed in quiet in the hydrochloric acid solution that volumetric concentration is 1%-5%
Putting carries out de- alloy treatment for 30-60 minutes；
3) the complete product of de- alloy is taken out, difference is successively 0.1% in volumetric concentration, is entered in 0.01% hydrochloric acid solution
Row rinsing, the time is no more than 10 seconds,
4) sample after pickling is rinsed in ultra-pure water, and the time is no more than 30s；
5) product after rinsing is taken out, is dried under the conditions of inert gas shielding, inert gas oxygen content is less than
A ten thousandth, drying temperature is no more than 30 degrees Celsius, you can obtain blacker-than-black nanoporous Fe materials.
Beneficial effect：Compared with prior art, the preparation method for preparing blacker-than-black material of the invention is simple to operate, using its system
Standby blacker-than-black material is the Fe with nano-porous structure.Research shows that taking off alloyage in use is preparing blacker-than-black material in wavelength
There is good absorbing property in the range of 350-1000nm.
Specific embodiment
Below by way of specific embodiment, the present invention is described further.
The preparation method of blacker-than-black nanoporous Fe, comprises the following steps：
1) homogeneous metal liquation is obtained by sensing heating after the mixing of the Fe by purity more than 99%, Mn and Cu simple metal
After carry out fast quenching, obtain the FeMnCu prealloys of single phase structure；Wherein, raw material simple metal atomic percent is Mn contents
68-90at%, Fe content 31.7-9.7at%, Cu content are less than 0.3at%；Induction heating temperature is not higher than 1700 degrees Celsius,
Heat time is no longer than 20 minutes, and heating times are not less than 2 times；Molten metal fast quenching temperature 1240-1700 after uniform is Celsius
Degree, obtains the FeMnCu prealloys of phase structure；
2) by under 4-25 degrees celsius, FeMnCu prealloys are placed in the hydrochloric acid solution that volumetric concentration is 1%-5%
Standing carries out de- alloy treatment for 30-60 minutes；
3) the complete product of de- alloy is taken out, difference is successively 0.1% in volumetric concentration, is entered in 0.01% hydrochloric acid solution
Row rinsing, the time is no more than 10 seconds,
4) sample after pickling is rinsed in ultra-pure water, and the time is no more than 30s；
5) product after rinsing is taken out, is dried under the conditions of inert gas shielding, inert gas oxygen content is less than
A ten thousandth, drying temperature is no more than 30 degrees Celsius, you can obtain blacker-than-black nanoporous Fe materials.Material is in wavelength 350-
There is good absorbing property in the range of 1000nm.
Embodiment 1
Fe and Mn simple metal by purity more than 99% is according to 32at%：By sensing after the ratio mixing of 67.9at%
Heating 10 minutes every time, obtains homogeneous metal liquation after 1240 degrees Celsius of fast quenchings in 1700 degrees Celsius of meltings 2 times, obtains single
The FeMnCu prealloys of one phase structure.FeMnCu prealloys are placed in the hydrochloric acid solution that volumetric concentration is 1% and stand 60 minutes
Carry out de- alloy treatment；The complete product of de- alloy takes out, and it is successively 0.1% in volumetric concentration to distinguish afterwards, and 0.01% hydrochloric acid is molten
Rinsed 10 seconds in liquid, then 30s is rinsed in ultra-pure water；Product after rinsing is taken out, in 30 degrees Celsius, inert gas shielding bar
It is dried under part, blacker-than-black nanoporous Fe materials can be obtained.Between 10-30nm, oxygen content is 16-19at% to nano-pore,
Material reflectivity in the range of wavelength 350-1000nm is 0.5-0.8%.
Embodiment 2
Fe by purity more than 99%, Mn and Cu simple metal are according to 31.7at%：68at%：The ratio of 0.3at% is mixed
Homogeneous metal liquation 10 minutes every time, is obtained after 1500 degrees Celsius in 1500 degrees Celsius of meltings 2 times by sensing heating after conjunction
Fast quenching, obtains the FeMnCu prealloys of single phase structure.FeMnCu prealloys are placed in the hydrochloric acid solution that volumetric concentration is 1%
Standing carries out de- alloy treatment for 60 minutes；The complete product of de- alloy takes out, and it is successively 0.1% in volumetric concentration to distinguish afterwards,
Rinsed 10 seconds in 0.01% hydrochloric acid solution, then 30s is rinsed in ultra-pure water；By after rinsing product take out, 30 degrees Celsius,
It is dried under the conditions of inert gas shielding, blacker-than-black nanoporous Fe materials can be obtained.Nano-pore is oxygen-containing between 30-50nm
It is 12-17at% to measure, and material reflectivity in the range of wavelength 350-1000nm is 0.7-0.9%.
Embodiment 3
Fe by purity more than 99%, Mn and Cu simple metal are according to 9.7at%：90at%：The ratio mixing of 0.3at%
Homogeneous metal liquation 10 minutes every time, is obtained fast after 1240 degrees Celsius in 1240 degrees Celsius of meltings 2 times by sensing heating afterwards
Quench, obtain the FeMnCu prealloys of single phase structure.FeMnCu prealloys are placed in quiet in the hydrochloric acid solution that volumetric concentration is 1%
Putting carries out de- alloy treatment for 60 minutes；The complete product of de- alloy takes out, and it is successively 0.1%, 0.01% in volumetric concentration to distinguish afterwards
Hydrochloric acid solution in rinse 5 seconds, then 10s is rinsed in ultra-pure water；Product after rinsing is taken out, in 30 degrees Celsius, indifferent gas
It is dried under body protective condition, blacker-than-black nanoporous Fe materials can be obtained.Between 70-100nm, oxygen content is nano-pore
12-17at%, material reflectivity in the range of wavelength 350-1000nm is 0.9-0.1%.
Embodiment 4
Fe and Mn simple metal by purity more than 99% is according to 32at%：Added by sensing after the ratio mixing of 68at%
Heat 5 minutes every time, obtains homogeneous metal liquation after 1500 degrees Celsius of fast quenchings in 1500 degrees Celsius of meltings 2 times, obtains single-phase
The FeMnCu prealloys of structure.FeMnCu prealloys are placed in be stood in the hydrochloric acid solution that volumetric concentration is 5% is carried out for 30 minutes
De- alloy treatment；The complete product of de- alloy takes out, and it is successively 0.1% in volumetric concentration to distinguish afterwards, in 0.01% hydrochloric acid solution
Rinsing 5 seconds, then 10s is rinsed in ultra-pure water；Product after rinsing is taken out, under the conditions of 30 degrees Celsius, inert gas shielding
It is dried, blacker-than-black nanoporous Fe materials can be obtained.Between 10-20nm, oxygen content is 8-10at% to nano-pore, and material exists
Reflectivity is 0.5-0.7% in the range of wavelength 350-1000nm.
Embodiment 5
Fe by purity more than 99%, Mn and Cu simple metal are according to 31.7at%：68at%：The ratio of 0.3at% is mixed
Homogeneous metal liquation 5 minutes every time, is obtained after 1700 degrees Celsius in 1500 degrees Celsius of meltings 2 times by sensing heating after conjunction
Fast quenching, obtains the FeMnCu prealloys of single phase structure.FeMnCu prealloys are placed in the hydrochloric acid solution that volumetric concentration is 5%
Standing carries out de- alloy treatment for 30 minutes；The complete product of de- alloy takes out, and it is successively 0.1% in volumetric concentration to distinguish afterwards,
Rinsed 5 seconds in 0.01% hydrochloric acid solution, then 10s is rinsed in ultra-pure water；By after rinsing product take out, 30 degrees Celsius,
It is dried under the conditions of inert gas shielding, blacker-than-black nanoporous Fe materials can be obtained.Nano-pore is oxygen-containing between 20-30nm
It is 5-8at% to measure, and material reflectivity in the range of wavelength 350-1000nm is 0.6-0.8%.
Claims (7)
1. a kind of preparation method of blacker-than-black nanoporous Fe, it is characterised in that comprise the following steps：
1) by Fe, fast quenching is carried out after sensing heating obtains homogeneous metal liquation after the mixing of Mn and Cu simple metal, is obtained single
The FeMnCu prealloys of phase structure；
2) step 1 is obtained into FeMnCu prealloys and is placed in standing in hydrochloric acid solution, carry out de- alloy treatment；
3) step 2 obtained product is carried out into pickling in watery hydrochloric acid liquation；
4) step 3 obtained product is rinsed in ultra-pure water；
5) step 4 obtained product is dried treatment under an inert atmosphere, you can obtain blacker-than-black nanoporous iron.
2. the preparation method of the blacker-than-black nanoporous Fe according to right 1, it is characterised in that：Step 1) in, the simple metal
Purity more than 99%, atomic percent be Mn contents 67-90at%, Cu content be less than 0.3at%, Fe contents 31.7-
9.7at%；Induction heating temperature is less than 1700 degrees Celsius, and the heat time is less than 20 minutes, and heating times are more than 2 times；To uniform
Molten metal afterwards carries out fast quenching in 1240-1700 degree Celsius ranges, obtains the FeMnCu prealloys of phase structure.
3. the preparation method of the blacker-than-black nanoporous Fe according to right 1, it is characterised in that：Step 2) in, alloy is taken off certainly
Carried out by under etching condition, temperature is 4-30 degrees Celsius, hydrochloric acid liquation volumetric concentration is 1%-5%, take off the alloy time for 30-60
Minute.
4. the preparation method of the blacker-than-black nanoporous Fe according to right 1, it is characterised in that：Step 3) in, watery hydrochloric acid pickling
Be by step 2) obtained product successively volumetric concentration be 0.1%, rinsed in 0.01% hydrochloric acid solution, each time
Time is no more than 10 seconds.
5. the preparation method of the blacker-than-black nanoporous Fe according to right 1, it is characterised in that：Step 4) in float in ultra-pure water
Wash, the time is no more than 30s.
6. the preparation method of the blacker-than-black nanoporous Fe according to right 1, it is characterised in that：Step 5) in, inert gas contains
Oxygen amount is less than a ten thousandth, and drying temperature is no more than 30 degrees Celsius.
7. the nanoporous Fe that in a kind of use claim 1~6 prepared by the preparation method of any one blacker-than-black nanoporous Fe,
It is characterized in that：Nano-pore aperture between 10-100 nanometers, oxygen content in below 20at%, in wavelength 350-1000nm scopes
Internal reflection rate is below 1%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110724848A (en) * | 2019-11-28 | 2020-01-24 | 重庆大学 | Method for extracting Al-Ce tubular intermetallic compound from magnesium alloy and product |
| CN113263744A (en) * | 2021-04-14 | 2021-08-17 | 哈尔滨工业大学 | Preparation method of 3D printing ultra-black material with high infrared band absorption |
Citations (3)
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| JPS61124580A (en) * | 1984-11-22 | 1986-06-12 | Nippon Steel Corp | Production of solar heat absorption plate |
| CN102534687A (en) * | 2011-12-30 | 2012-07-04 | 东南大学 | PdNiCu ternary nanoporous metal and preparation and application thereof |
| CN105081305A (en) * | 2014-05-04 | 2015-11-25 | 中国人民解放军63971部队 | Porous nanometer zero-valent iron and porous nanometer zero-valent iron composite material |
-
2017
- 2017-01-05 CN CN201710003628.0A patent/CN106801160B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61124580A (en) * | 1984-11-22 | 1986-06-12 | Nippon Steel Corp | Production of solar heat absorption plate |
| CN102534687A (en) * | 2011-12-30 | 2012-07-04 | 东南大学 | PdNiCu ternary nanoporous metal and preparation and application thereof |
| CN105081305A (en) * | 2014-05-04 | 2015-11-25 | 中国人民解放军63971部队 | Porous nanometer zero-valent iron and porous nanometer zero-valent iron composite material |
Non-Patent Citations (1)
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| MICHAEL HEIDEN ET AL: "Surface modifications through dealloying of Fe–Mn and Fe–Mn–Zn alloys developed to create tailorable, nanoporous, bioresorbable surfaces", 《ACTA MATERIALIA》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110724848A (en) * | 2019-11-28 | 2020-01-24 | 重庆大学 | Method for extracting Al-Ce tubular intermetallic compound from magnesium alloy and product |
| CN110724848B (en) * | 2019-11-28 | 2021-04-02 | 重庆大学 | Method for extracting Al-Ce tubular intermetallic compound from magnesium alloy and product |
| CN113263744A (en) * | 2021-04-14 | 2021-08-17 | 哈尔滨工业大学 | Preparation method of 3D printing ultra-black material with high infrared band absorption |
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| CN106801160B (en) | 2018-09-21 |
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Inventor after: Zhang Xuhai Inventor after: Jiang Jianqing Inventor after: Zhu Kui Inventor after: Li Juan Inventor after: Ji Baorong Inventor after: Xiao Jingcai Inventor after: Zeng Yuqiao Inventor after: Shao Qiyue Inventor after: Yang Xingmei Inventor after: Chen Long Inventor before: Zeng Yuqiao |
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