CN106834763A - A kind of blacker-than-black nanometer column Co and preparation method thereof - Google Patents
A kind of blacker-than-black nanometer column Co and preparation method thereof Download PDFInfo
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- CN106834763A CN106834763A CN201710003629.5A CN201710003629A CN106834763A CN 106834763 A CN106834763 A CN 106834763A CN 201710003629 A CN201710003629 A CN 201710003629A CN 106834763 A CN106834763 A CN 106834763A
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- blacker
- preparation
- nanometer column
- black
- hydrochloric acid
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/16—Acidic compositions
- C23F1/30—Acidic compositions for etching other metallic material
Abstract
The invention discloses a kind of blacker-than-black nanometer column cobalt and preparation method thereof, belong to technical field of nanometer material preparation, including：1) synthesis Co contents are in 10 20at%, CoMn prealloy liquations, and liquation carries out fast quenching acquisition single-phase alloy more than 1300 degrees Celsius；2) by under 4 30 degrees celsius, CoMn prealloys are placed in be stood in the hydrochloric acid solution that volumetric concentration is 5% 15% carries out de- alloy treatment for 50 180 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 nanometer column cobalt is 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 nanometer column Co and preparation method thereof.
Background technology
Black object is relatively low to the reflectivity of light with respect to other color objects, and the absorbability to light is stronger, therefore wide
It is general to be applied to solar energy conversion, astronomical telescope, sensor and military installations and device.It is anti-to a range of incident ray
Rate is penetrated less than 1%, black material of the absorptivity higher than 99% turns into blacker-than-black material.Due to its extremely low reflectivity, pole is caused
Big concern.Classical blacker-than-black material is ferrophosphor(us), and its preparation method is, in material surface iron-phosphorus alloy, then to carry out thick
Rough treatment forms netted irregular projection with surface.The reflectivity of this kind of material in the range of 350-700nm up to 1% with
Under, inhale ripple scope smaller.CNTs of the newest blacker-than-black Vantablack for developing then by being arranged vertically is constituted, its reflectivity
Up to less than 0.5, but its preparation cost is very high.Other blacker-than-black material devices method also including biological template method, vapour deposition etc.
The array-like materials such as the amorphous carbon of preparation, brilliant black silicon.There is high cost in material prepared by the above method, it is impossible to advised greatly mostly
The shortcomings of mould is produced and suction ripple is limited in scope.And the present invention prepares blacker-than-black material using de- alloyage, preparation method is simple and easy to apply.
The product of acquisition is the Co with nano-pillar, and finished product has cheap, the wide advantage of light abstraction width.
The content of the invention
Technical problem：It is an object of the invention to provide blacker-than-black nanometer column Co and preparation method thereof, preparation method letter
It is single, there is the morphological feature of array column using its blacker-than-black nanometer column Co for preparing；Another object of the present invention is to provide
Blacker-than-black nanometer column Co 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 black nanometer column Co, comprises the following steps：
1) after Co the and Mn simple metal mixing by purity more than 99% after sensing heating obtains homogeneous metal liquation
Fast quenching is carried out, the CoMn prealloys of single phase structure are obtained；Wherein, raw material simple metal atomic percent is Co contents 10-
20at%, Mn content 80-90at%；Induction heating temperature is not higher than 1800 degrees Celsius, and the heat time is no longer than 20 minutes, heating
Number of times is not less than 2 times；Molten metal fast quenching temperature range after uniform is 1300-1800 degrees Celsius, obtains phase structure
CoMn prealloys；
2) by under 4-30 degrees celsius, CoMn prealloys are placed in quiet in the hydrochloric acid solution that volumetric concentration is 5%-15%
Putting carries out de- alloy treatment for 50-180 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 nanometer column Co 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 with nanometer column Co.Research shows that taking off alloyage in use is preparing blacker-than-black material in wavelength 350-
There is good absorbing property in the range of 1000nm.
Specific embodiment
Below by way of specific embodiment, the present invention is described further.
The preparation method of blacker-than-black nanometer column Co, comprises the following steps：
1) after Co the and Mn simple metal mixing by purity more than 99% after sensing heating obtains homogeneous metal liquation
Fast quenching is carried out, the CoMn prealloys of single phase structure are obtained；Wherein, raw material simple metal atomic percent is Co contents 10-
20at%, Mn content 80-90at%；Induction heating temperature is not higher than 1800 degrees Celsius, and the heat time is no longer than 20 minutes, heating
Number of times is not less than 2 times；Molten metal fast quenching temperature range after uniform is 1300-1800 degrees Celsius, obtains phase structure
CoMn prealloys；
2) by under 4-30 degrees celsius, CoMn prealloys are placed in quiet in the hydrochloric acid solution that volumetric concentration is 5%-15%
Putting carries out de- alloy treatment for 50-180 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 nanometer column Co materials.Material is in wavelength 350-
There is good absorbing property in the range of 1000nm.
Embodiment 1
Co and Mn simple metal by purity more than 99% is according to 10at%：Added by sensing after the ratio mixing of 90at%
Heat 10 minutes every time, obtains homogeneous metal liquation after 1300 degrees Celsius of fast quenchings in 1800 degrees Celsius of meltings 2 times, obtains single
The CoMn prealloys of phase structure.CoMn prealloys are placed in be stood in the hydrochloric acid solution that volumetric concentration is 5% and are taken off within 50 minutes
Alloy treatment；The complete product of de- alloy takes out, and it is successively 0.1% in volumetric concentration to distinguish afterwards, is floated in 0.01% hydrochloric acid solution
Wash 10 seconds, then 30s is rinsed in ultra-pure water；Product after rinsing is taken out, is entered under the conditions of 30 degrees Celsius, inert gas shielding
Row drying, can obtain blacker-than-black nanometer column Co materials.Between 100-300nm, oxygen content is 7-10at% to nano-pore, and material exists
Reflectivity is 0.5-0.7% in the range of wavelength 350-1000nm.
Embodiment 2
Co and Mn simple metal by purity more than 99% is according to 10at%：Added by sensing after the ratio mixing of 90at%
Heat 10 minutes every time, obtains homogeneous metal liquation after 1300 degrees Celsius of fast quenchings in 1300 degrees Celsius of meltings 3 times, obtains single
The CoMn prealloys of phase structure.CoMn prealloys are placed in be stood in the hydrochloric acid solution that volumetric concentration is 5% and are taken off within 180 minutes
Alloy treatment；The complete product of de- alloy takes out, and it is successively 0.1% in volumetric concentration to distinguish afterwards, is floated in 0.01% hydrochloric acid solution
Wash 10 seconds, then 30s is rinsed in ultra-pure water；Product after rinsing is taken out, is entered under the conditions of 30 degrees Celsius, inert gas shielding
Row drying, can obtain blacker-than-black nanometer column Co materials.Between 500-1000nm, oxygen content is 12-15at%, material to nano-pore
Reflectivity is 0.7-1.0% in the range of wavelength 350-1000nm.
Embodiment 3
Co and Mn simple metal by purity more than 99% is according to 20at%：Added by sensing after the ratio mixing of 80at%
Heat 10 minutes every time, obtains homogeneous metal liquation after 1300 degrees Celsius of fast quenchings in 1300 degrees Celsius of meltings 3 times, obtains single
The CoMn prealloys of phase structure.CoMn prealloys are placed in be stood in the hydrochloric acid solution that volumetric concentration is 15% and are taken off within 50 minutes
Alloy treatment；The complete product of de- alloy takes out, and it is successively 0.1% in volumetric concentration to distinguish afterwards, is floated in 0.01% hydrochloric acid solution
Wash 10 seconds, then 30s is rinsed in ultra-pure water；Product after rinsing is taken out, is entered under the conditions of 30 degrees Celsius, inert gas shielding
Row drying, can obtain blacker-than-black nanometer column Co materials.Between 500-100nm, oxygen content is 5-10at% to nano-pore, and material exists
Reflectivity is 0.8-1.0% in the range of wavelength 350-1000nm.
Claims (7)
1. the preparation method of a kind of blacker-than-black nanometer column Co, it is characterised in that comprise the following steps：
1) fast quenching is carried out after sensing heating obtains homogeneous metal liquation after Co and Mn simple metal is mixed, single-phase knot is obtained
The CoMn prealloys of structure；
2) step 1 is obtained into CoMn prealloys and is placed in standing in concentrated hydrochloric acid solution, carry out corrosion 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) blacker-than-black nanometer column Co is obtained by step 4 obtained product being dried into treatment under an inert atmosphere.
2. the preparation method of blacker-than-black nanometer column Co according to right 1, it is characterised in that：Step 1) in, raw material proof gold
More than 99%, atomic percent is Co contents 10-20at%, Mn content 80-90at% to category purity.Induction heating temperature is less than
1800 degrees Celsius, the heat time is less than 20 minutes, and heating times are more than 2 times；Molten metal after uniform is taken the photograph in 1300-1800
Fast quenching is carried out in the range of family name's degree, the CoMn prealloys of phase structure are obtained.
3. the preparation method of blacker-than-black nanometer column Co 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 5%-15%, take off the alloy time for 50-
180 minutes.
4. the preparation method of blacker-than-black nanometer column Co 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 the time
No more than 10 seconds.
5. the preparation method of blacker-than-black nanometer column Co according to right 1, it is characterised in that：Step 4) in ultra-pure water float
Wash, the time is less than 30s.
6. the preparation method of blacker-than-black nanometer column Co 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 nanometer column Co that in a kind of use claim 1~6 prepared by the preparation method of any one blacker-than-black nanometer column Co,
It is characterized in that：Nano-pillar between 100-1000 nanometers, oxygen content in below 15at%, in the range of wavelength 300-1100nm
Reflectivity is below 1%.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4361630A (en) * | 1979-04-20 | 1982-11-30 | The United States Of America As Represented By The Secretary Of The Commerce | Ultra-black coating due to surface morphology |
| EP0317838A2 (en) * | 1987-11-10 | 1989-05-31 | Anritsu Corporation | Ultra-Black film and method of manufacturing the same |
| CN102811829A (en) * | 2010-03-17 | 2012-12-05 | 新日铁化学株式会社 | Nickel-cobalt nanoparticle and manufacturing method therefor |
| CN104607651A (en) * | 2015-01-09 | 2015-05-13 | 北京科技大学 | Chemical method for preparing spherical porous hollow nanometer cobalt powder |
-
2017
- 2017-01-05 CN CN201710003629.5A patent/CN106834763B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4361630A (en) * | 1979-04-20 | 1982-11-30 | The United States Of America As Represented By The Secretary Of The Commerce | Ultra-black coating due to surface morphology |
| EP0317838A2 (en) * | 1987-11-10 | 1989-05-31 | Anritsu Corporation | Ultra-Black film and method of manufacturing the same |
| CN102811829A (en) * | 2010-03-17 | 2012-12-05 | 新日铁化学株式会社 | Nickel-cobalt nanoparticle and manufacturing method therefor |
| CN104607651A (en) * | 2015-01-09 | 2015-05-13 | 北京科技大学 | Chemical method for preparing spherical porous hollow nanometer cobalt powder |
Non-Patent Citations (2)
| Title |
|---|
| TONG LIU ET AL: "Microporous Co@CoO nanoparticles with superior microwave absorption properties", 《NANOSCALE》 * |
| 丁轶: "纳米多孔金属：一种新型能源纳米材料", 《山东大学学报(理学版）》 * |
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Inventor after: Zeng Yuqiao Inventor after: Jiang Jianqing Inventor after: Lu Qianwen Inventor after: Yang Zhi Inventor after: Ding Xuehui Inventor after: Zheng Yunxi Inventor after: Mo Dan Inventor after: Shao Qiyue Inventor after: Zhang Xuhai Inventor after: Chen Long Inventor before: Zeng Yuqiao |
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