CN106801160B - Blacker-than-black nanoporous Fe and preparation method thereof - Google Patents
Blacker-than-black nanoporous Fe and preparation method thereof Download PDFInfo
- Publication number
- CN106801160B CN106801160B CN201710003628.0A CN201710003628A CN106801160B CN 106801160 B CN106801160 B CN 106801160B CN 201710003628 A CN201710003628 A CN 201710003628A CN 106801160 B CN106801160 B CN 106801160B
- Authority
- CN
- China
- Prior art keywords
- blacker
- black
- nanoporous
- preparation
- hydrochloric acid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C3/00—Removing material from alloys to produce alloys of different constitution separation of the constituents of alloys
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Powder Metallurgy (AREA)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
Abstract
The invention discloses a kind of preparation methods of blacker-than-black nanoporous Fe, belong to technical field of nanometer material preparation, including：1) for synthesis Mn contents in 68 90at%, Cu contents are less than the FeMnCu prealloy melts within the scope of 0.3at%, and carry out fast quenching in 1,240 1700 degrees Celsius of melt and obtain single-phase alloy；2) by under 4 25 degrees celsius, FeMnCu prealloys is placed in and stands 30 60 minutes in the hydrochloric acid solution that volumetric concentration is 1% 5% and carries out taking off alloy treatment；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, is dried under the conditions of inert gas shielding and can be obtained blacker-than-black nanoporous Fe materials.
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 being less than 1% to a certain range of incident ray reflectivity, and absorptivity is higher than 99% material
Material.On many optical devices, sensor and solar energy converter, since interface can be to property to the unnecessary reflection of incident light
Many adverse effects can be generated, therefore demand of the such devices to blacker-than-black material is very urgent.Simultaneously because blacker-than-black material itself
Excellent Stealth Fighter also has very big purposes in military aspect.
In consideration of it, blacker-than-black material obtains extensive research and application in recent years.It is by Surrey that performance is most outstanding at present
The Vantablack that Nanosys Inc. develops, the carbon nanotube composition that it is mainly arranged vertically, but cost of manufacture is very
It is high.Other common used materials further include amorphous carbon and the black silicon class nonmetallic materials of polycrystalline, nickel phosphorus intermediate alloy material, and simple metal is super
There is not been reported for black-materials.Its form includes nano-tube array, dimpling array and roughened irregular surface, has three-dimensional connect
The blacker-than-black device of logical nano-porous structure has not been reported.Preparation method includes mainly chemical vapor deposition, biological template method etc..
There is the shortcomings of of high cost, can not to be mass produced mostly in these methods.And the present invention prepares blacker-than-black using alloyage is taken off
Material, preparation method is simple.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.
Invention content
Technical problem：The purpose of the present invention is to provide a kind of preparation method of blacker-than-black nanoporous Fe, the preparation methods
Simply, there is the pore passage structure of three-dimensional communication using the blacker-than-black nanoporous Fe of its preparation；Another object of the present invention is to carry
For blacker-than-black nanoporous Fe prepared by this method, which has the advantages that light abstraction width is wide.
Technical solution：For achieving the above object, the present invention adopts the following technical scheme that：
The preparation method of blacker-than-black nanoporous Fe, includes the following steps：
1) homogeneous metal melt is obtained by sensing heating after the mixing of the Fe by purity 99% or more, 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 heating 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 uniformly, 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%
It sets and carries out within 30-60 minutes de- alloy treatment；
3) the complete product of de- alloy is taken out, in volumetric concentration is successively respectively 0.1%, in 0.01% hydrochloric acid solution into
Row rinsing, time are no more than 10 seconds,
4) sample after pickling rinses 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 are no more than 30 degrees Celsius, you can obtain blacker-than-black nanoporous Fe materials.
Advantageous effect：Compared with prior art, the present invention prepare blacker-than-black material preparation method it is easy to operate, using its system
Standby blacker-than-black material is the Fe with nano-porous structure.Studies have shown that preparing blacker-than-black material in wavelength using de- alloyage
There is good absorbing property within the scope of 350-1000nm.
Specific implementation mode
Below by way of specific implementation mode, the present invention is described further.
The preparation method of blacker-than-black nanoporous Fe, includes the following steps：
1) homogeneous metal melt is obtained by sensing heating after the mixing of the Fe by purity 99% or more, 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,
Heating time is no longer than 20 minutes, and heating times are not less than 2 times；Molten metal fast quenching temperature 1240-1700 after uniformly 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%
It stands 30-60 minutes and carries out de- alloy treatment；
3) the complete product of de- alloy is taken out, in volumetric concentration is successively respectively 0.1%, in 0.01% hydrochloric acid solution into
Row rinsing, time are no more than 10 seconds,
4) sample after pickling rinses 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 are 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 within the scope of 1000nm.
Embodiment 1
By purity 99% or more Fe and Mn simple metal according to 32at%：Pass through induction after the ratio mixing of 67.9at%
Heating is in 1700 degrees Celsius of meltings 2 times, 10 minutes every time, obtains after homogeneous metal melt in 1240 degrees Celsius of fast quenchings, 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 rear difference is successively 0.1% in volumetric concentration, and 0.01% hydrochloric acid is molten
It is rinsed 10 seconds in liquid, then rinses 30s in ultra-pure water；Product after rinsing is taken out, in 30 degrees Celsius, inert gas shielding item
It is dried under part, can get blacker-than-black nanoporous Fe materials.Nano-pore is between 10-30nm, oxygen content 16-19at%,
Material is 0.5-0.8% in wavelength 350-1000nm range internal reflection rates.
Embodiment 2
By purity 99% or more Fe, Mn and Cu simple metal according to 31.7at%：68at%：The ratio of 0.3at% is mixed
By sensing heating in 1500 degrees Celsius of meltings 2 times after conjunction, 10 minutes every time, obtain after homogeneous metal melt in 1500 degrees Celsius
Fast quenching obtains the FeMnCu prealloys of single phase structure.FeMnCu prealloys are placed in the hydrochloric acid solution that volumetric concentration is 1%
It stands 60 minutes and carries out de- alloy treatment；The complete product of de- alloy takes out, and rear difference is successively 0.1% in volumetric concentration,
It is rinsed 10 seconds in 0.01% hydrochloric acid solution, then rinses 30s in ultra-pure water；By after rinsing product take out, 30 degrees Celsius,
It is dried under the conditions of inert gas shielding, can get blacker-than-black nanoporous Fe materials.Nano-pore is oxygen-containing between 30-50nm
Amount is 12-17at%, and material is 0.7-0.9% in wavelength 350-1000nm range internal reflection rates.
Embodiment 3
By purity 99% or more Fe, Mn and Cu simple metal according to 9.7at%：90at%：The ratio of 0.3at% mixes
Afterwards by sensing heating in 1240 degrees Celsius of meltings 2 times, 10 minutes every time, obtain fast in 1240 degrees Celsius after homogeneous metal melt
It quenches, obtains the FeMnCu prealloys of single phase structure.FeMnCu prealloys are placed in quiet in the hydrochloric acid solution that volumetric concentration is 1%
It sets and carries out within 60 minutes de- alloy treatment；The complete product of de- alloy takes out, and rear difference is successively 0.1%, 0.01% in volumetric concentration
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, can get blacker-than-black nanoporous Fe materials.Between 70-100nm, oxygen content is nano-pore
12-17at%, material are 0.9-0.1% in wavelength 350-1000nm range internal reflection rates.
Embodiment 4
By purity 99% or more Fe and Mn simple metal according to 32at%：Added by induction after the ratio mixing of 68at%
Heat is in 1500 degrees Celsius of meltings 2 times, 5 minutes every time, obtains after homogeneous metal melt in 1500 degrees Celsius of fast quenchings, obtains single-phase
The FeMnCu prealloys of structure.FeMnCu prealloys are placed in the hydrochloric acid solution that volumetric concentration is 5% and stand progress in 30 minutes
De- alloy treatment；The complete product of de- alloy takes out, and rear difference is successively 0.1% in volumetric concentration, 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, can get blacker-than-black nanoporous Fe materials.Between 10-20nm, oxygen content 8-10at%, material exists nano-pore
Wavelength 350-1000nm range internal reflection rates are 0.5-0.7%.
Embodiment 5
By purity 99% or more Fe, Mn and Cu simple metal according to 31.7at%：68at%：The ratio of 0.3at% is mixed
By sensing heating in 1500 degrees Celsius of meltings 2 times after conjunction, 5 minutes every time, obtain after homogeneous metal melt in 1700 degrees Celsius
Fast quenching obtains the FeMnCu prealloys of single phase structure.FeMnCu prealloys are placed in the hydrochloric acid solution that volumetric concentration is 5%
It stands 30 minutes and carries out de- alloy treatment；The complete product of de- alloy takes out, and rear difference is successively 0.1% in volumetric concentration,
It is rinsed 5 seconds in 0.01% hydrochloric acid solution, then rinses 10s in ultra-pure water；By after rinsing product take out, 30 degrees Celsius,
It is dried under the conditions of inert gas shielding, can get blacker-than-black nanoporous Fe materials.Nano-pore is oxygen-containing between 20-30nm
Amount is 5-8at%, and material is 0.6-0.8% in wavelength 350-1000nm range internal reflection rates.
Claims (6)
1. a kind of preparation method of blacker-than-black nanoporous Fe, which is characterized in that include the following steps：
1) by Fe, fast quenching is carried out after obtaining homogeneous metal melt by sensing heating after the mixing of Mn and Cu simple metal, is obtained single
The FeMnCu prealloys of phase structure；
2) the obtained FeMnCu prealloys of step 1) are placed in hydrochloric acid solution and are stood, carry out de- alloy treatment；
3) step 2) obtained product is subjected to pickling in dilute hydrochloric acid solution；
4) step 3) obtained product is rinsed in ultra-pure water；
5) processing is dried in step 4) obtained product under an inert atmosphere, you can obtain blacker-than-black nanoporous iron；
Wherein,
In step 1), for the purity of the simple metal 99% or more, atomic percent is that Mn contents 67-90at%, Cu content is small
In 0.3at%, Fe contents 31.7-9.7at%；Induction heating temperature is less than 1700 degrees Celsius, and heating time is less than 20 minutes, adds
Hot number is more than 2 times；Fast quenching is carried out in 1240-1700 degree Celsius ranges to the molten metal after uniformly, obtains phase structure
FeMnCu prealloys.
2. the preparation method of blacker-than-black nanoporous Fe according to claim 1, it is characterised in that：In step 2), alloy is taken off
It is carried out under free etching condition, temperature is 4-30 degrees Celsius, and hydrochloric acid solution volumetric concentration is 1%-5%, and the de- alloy time is
30-60 minutes.
3. the preparation method of blacker-than-black nanoporous Fe according to claim 1, it is characterised in that：In step 3), dilute hydrochloric acid
It in volumetric concentration is successively 0.1% that pickling, which is by step 2) obtained product, is rinsed in 0.01% hydrochloric acid solution, each time
Time is no more than 10 seconds.
4. the preparation method of blacker-than-black nanoporous Fe according to claim 1, it is characterised in that：In step 4) in ultra-pure water
Rinsing, time are no more than 30s.
5. the preparation method of blacker-than-black nanoporous Fe according to claim 1, it is characterised in that：In step 5), indifferent gas
Body oxygen content is less than a ten thousandth, and drying temperature is no more than 30 degrees Celsius.
6. nanoporous Fe prepared by a kind of preparation method using any one blacker-than-black nanoporous Fe in Claims 1 to 5,
It is characterized in that：Nano-pore aperture is between 10-100 nanometers, and oxygen content is in 20at% hereinafter, in wavelength 350-1000nm ranges
Internal reflection rate is below 1%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710003628.0A CN106801160B (en) | 2017-01-05 | 2017-01-05 | Blacker-than-black nanoporous Fe and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710003628.0A CN106801160B (en) | 2017-01-05 | 2017-01-05 | Blacker-than-black nanoporous Fe and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106801160A CN106801160A (en) | 2017-06-06 |
| CN106801160B true CN106801160B (en) | 2018-09-21 |
Family
ID=58984295
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710003628.0A Active CN106801160B (en) | 2017-01-05 | 2017-01-05 | Blacker-than-black nanoporous Fe and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106801160B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN113263744B (en) * | 2021-04-14 | 2022-06-14 | 哈尔滨工业大学 | Preparation method of 3D printing ultra-black material with high infrared band absorption |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Family Cites Families (1)
| 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 |
-
2017
- 2017-01-05 CN CN201710003628.0A patent/CN106801160B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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)
| Title |
|---|
| Surface modifications through dealloying of Fe–Mn and Fe–Mn–Zn alloys developed to create tailorable, nanoporous, bioresorbable surfaces;Michael Heiden et al;《Acta Materialia》;20151106;第103卷;第115-127页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106801160A (en) | 2017-06-06 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Zhang et al. | Black silicon with order-disordered structures for enhanced light trapping and photothermic conversion | |
| CN102660740B (en) | Graphene and metal nanoparticle composite film preparation method | |
| CN106801160B (en) | Blacker-than-black nanoporous Fe and preparation method thereof | |
| Lu et al. | Plasmonic enhancement of Au nanoparticle—embedded single-crystalline ZnO nanowire dye-sensitized solar cells | |
| CN102942178A (en) | Compound base of precious metal nanometer array and single layer graphene and preparation method thereof | |
| Ishikawa et al. | Hydrogen permeation in rapidly quenched amorphous and crystallized Nb20Ti40Ni40 alloy ribbons | |
| Oseni et al. | Bimetallic nanocomposites and the performance of inverted organic solar cell | |
| Tian et al. | A new strategy towards spectral selectivity: Selective leaching alloy to achieve selective plasmonic solar absorption and infrared suppression | |
| Tang et al. | Cu-assisted chemical etching of bulk c-Si: A rapid and novel method to obtain 45 μm ultrathin flexible c-Si solar cells with asymmetric front and back light trapping structures | |
| Meng et al. | Hybrid conjugated polymer/magnetic nanoparticle composite nanofibers through cooperative non-covalent interactions | |
| Feng et al. | PEDOT: PSS and Ni-based thermoelectric generator for solar thermal energy conversion | |
| CN107012438A (en) | A kind of preparation method of the reinforced porous silver-colored magnesium alloy film of heat endurance | |
| Xia et al. | Enhanced film conductance of silver nanowire-based flexible transparent & conductive networks by bending | |
| Mdluli et al. | Time dependant evolution of silver nanodendrites | |
| CN106894112A (en) | A kind of nanometer of graphene fiber of modified by silver and preparation method thereof | |
| Yang et al. | Preparation of Er2O3 coating on a low activation martensitic steel substrate via the route of sol–gel | |
| Chen et al. | General and scalable fabrication of plasmonic solar selective absorbers by electrodeposition | |
| He et al. | Enhancing thermal robustness of a high-entropy nitride based solar selective absorber by the incorporation of Al element | |
| Liu et al. | Biomass‐Inspired Solar Evaporator for Simultaneous Steam and Power Generation Enhanced by Thermal‐Electric Effect | |
| CN102751105B (en) | Preparation method of dye-sensitized solar cell photoanode | |
| Mohamadbeigi et al. | Improving the multi-step fabrication approach of copper nanofiber networks based transparent electrode for achieving superb conductivity and transparency | |
| CN102873938A (en) | Fe-Si-B amorphous alloy-copper laminated composite material and preparation method thereof | |
| CN108611511A (en) | A kind of three-dimensional intercommunication CNTs/Cu composite material and preparation methods | |
| Li et al. | Thermal conductivity of a single Bi0. 5Sb1. 5Te3 single-crystalline nanowire | |
| Mishima et al. | Recent results on beryllium and beryllides in Japan |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB03 | Change of inventor or designer information |
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 |
|
| CB03 | Change of inventor or designer information | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |