CN106801160B - 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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- 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
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- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000011261 inert gas Substances 0.000 claims abstract description 11
- 229910021642 ultra pure water Inorganic materials 0.000 claims abstract description 10
- 239000012498 ultrapure water Substances 0.000 claims abstract description 10
- 238000010791 quenching Methods 0.000 claims abstract description 8
- 230000000171 quenching effect Effects 0.000 claims abstract description 8
- 229910052802 copper Inorganic materials 0.000 claims abstract description 7
- 239000002184 metal Substances 0.000 claims description 25
- 229910052751 metal Inorganic materials 0.000 claims description 25
- 238000010438 heat treatment Methods 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 11
- 230000006698 induction Effects 0.000 claims description 11
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 9
- 229910052742 iron Inorganic materials 0.000 claims description 9
- 229910052760 oxygen Inorganic materials 0.000 claims description 9
- 239000001301 oxygen Substances 0.000 claims description 9
- 229910052748 manganese Inorganic materials 0.000 claims description 8
- 150000002739 metals Chemical class 0.000 claims description 8
- 239000011148 porous material Substances 0.000 claims description 8
- 238000002310 reflectometry Methods 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims 10
- 238000005260 corrosion Methods 0.000 claims 1
- 230000007797 corrosion Effects 0.000 claims 1
- 238000005554 pickling Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 27
- 239000000956 alloy Substances 0.000 abstract description 4
- 229910045601 alloy Inorganic materials 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 239000000155 melt Substances 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- 238000003723 Smelting Methods 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 230000031700 light absorption Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000001154 acute effect Effects 0.000 description 1
- 229910003481 amorphous carbon Inorganic materials 0.000 description 1
- 229910021418 black silicon Inorganic materials 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- OFNHPGDEEMZPFG-UHFFFAOYSA-N phosphanylidynenickel Chemical compound [P].[Ni] OFNHPGDEEMZPFG-UHFFFAOYSA-N 0.000 description 1
Classifications
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- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
- Powder Metallurgy (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 the technical field of nano material preparation, and particularly relates to ultra-black nano porous Fe and a preparation method thereof.
Background
The ultra-black material has a reflectivity lower than 1% and an absorptivity higher than 99% for incident light within a certain range. The need for ultra-black materials in such devices is very acute in many optical applications, sensors, and solar converters, as unwanted reflections of incident light from the interface can have many detrimental effects on performance. Meanwhile, due to the excellent stealth performance of the ultra-black material, the ultra-black material has great application in military.
In view of this, ultra black materials have been widely studied and applied in recent years. At present, the most outstanding performance is Vantablak developed by the Saili nano system company, which mainly consists of vertically arranged carbon nanotubes, but the manufacturing cost is very high. Other common materials also comprise amorphous carbon and polycrystalline black silicon non-metallic materials, nickel-phosphorus intermediate alloy materials and pure metal ultra-black materials which are not reported yet. The form of the ultra-black device comprises a nanotube array, a micro-convex array and a roughened irregular surface, and the ultra-black device with a three-dimensional communicated nano porous structure is not reported. The preparation method mainly comprises chemical vapor deposition, a biological template method and the like. Most of the methods have the defects of high cost, incapability of large-scale production and the like. The invention adopts the dealloying method to prepare the ultra-black material, and the preparation method is simple and easy to implement. The obtained product is the nano porous structure Fe with a three-dimensional communicated structure, and the finished product has the advantages of low price and wide light absorption range.
Disclosure of Invention
The technical problem is as follows: the invention aims to provide a preparation method of ultra-black nano porous Fe, which is simple and has a three-dimensional communicated pore channel structure; the invention also aims to provide the ultra-black nano-porous Fe prepared by the method, and the material has the advantage of wide light absorption range.
The technical scheme is as follows: in order to achieve the purpose, the invention adopts the following technical scheme:
the preparation method of the ultra-black nano-porous Fe comprises the following steps:
1) mixing pure metals of Fe, Mn and Cu with the purity of more than 99%, performing induction heating to obtain uniform molten metal, and performing rapid quenching to obtain a FeMnCu prealloy with a single-phase structure; wherein, the pure metal atom percentage of the raw material is 68-90 at% of Mn content and 0-0.3 at% of Cu content; the induction heating temperature is not higher than 1700 ℃, the heating time is not longer than 20 minutes, and the heating frequency is not lower than 2 times; the temperature of the uniform molten metal is 1240 ℃ and 1700 ℃, and the FeMnCu prealloy with a single-phase structure is obtained;
2) placing the FeMnCu alloy in a hydrochloric acid solution with the volume concentration of 1% -5% at 4-25 ℃ and standing for 30-60 minutes to perform dealloying treatment;
3) taking out the product after the dealloying, respectively rinsing in 0.1 percent by volume concentration and 0.01 percent by volume concentration hydrochloric acid solution for no more than 10 seconds,
4) rinsing the sample after acid washing in ultrapure water for no more than 30 s;
5) and taking out the rinsed product, and drying under the protection of inert gas, wherein the oxygen content of the inert gas is lower than one ten thousandth, and the drying temperature is not higher than 30 ℃, so that the ultra-black nano porous Fe material can be obtained.
Has the advantages that: compared with the prior art, the preparation method for preparing the ultra-black material is simple to operate, and the ultra-black material prepared by the method is Fe with a nano porous structure. Research shows that the ultra-black material prepared by the dealloying method has good wave-absorbing performance in the range of the wavelength of 350-1000 nm.
Detailed Description
The present invention will be further described below with reference to specific embodiments.
The preparation method of the ultra-black nano-porous Fe comprises the following steps:
1) mixing pure metals of Fe, Mn and Cu with the purity of more than 99%, performing induction heating to obtain uniform molten metal, and performing rapid quenching to obtain a FeMnCu prealloy with a single-phase structure; wherein, the pure metal atom percentage of the raw material is 68-90 at% of Mn content, 31.7-9.7 at% of Fe content and less than 0.3 at% of Cu content; the induction heating temperature is not higher than 1700 ℃, the heating time is not longer than 20 minutes, and the heating frequency is not lower than 2 times; the temperature of the uniform molten metal is 1240 ℃ and 1700 ℃, and the FeMnCu prealloy with a single-phase structure is obtained;
2) placing the FeMnCu prealloy in a hydrochloric acid solution with the volume concentration of 1% -5% at 4-25 ℃ and standing for 30-60 minutes to perform dealloying treatment;
3) taking out the product after the dealloying, respectively rinsing in 0.1 percent by volume concentration and 0.01 percent by volume concentration hydrochloric acid solution for no more than 10 seconds,
4) rinsing the sample after acid washing in ultrapure water for no more than 30 s;
5) and taking out the rinsed product, and drying under the protection of inert gas, wherein the oxygen content of the inert gas is lower than one ten thousandth, and the drying temperature is not higher than 30 ℃, so that the ultra-black nano porous Fe material can be obtained. The material has good wave absorbing performance in the wavelength range of 350-1000 nm.
Example 1
Fe and Mn pure metals with the purity of more than 99 percent are mixed according to the ratio of 32at percent: mixing the components in a ratio of 67.9 at%, smelting for 2 times at 1700 ℃ by induction heating, each time for 10 minutes, obtaining uniform molten metal, and then rapidly quenching at 1240 ℃ to obtain the FeMnCu prealloy with a single-phase structure. Placing the FeMnCu prealloy in a hydrochloric acid solution with the volume concentration of 1% and standing for 60 minutes for dealloying; taking out the product after the dealloying, sequentially rinsing in 0.1% hydrochloric acid solution with volume concentration for 10 seconds and 0.01% hydrochloric acid solution respectively, and rinsing in ultrapure water for 30 seconds; and taking out the rinsed product, and drying at 30 ℃ under the protection of inert gas to obtain the ultra-black nano porous Fe material. The nano-pores are between 10 and 30nm, the oxygen content is between 16 and 19at percent, and the reflectivity of the material is between 0.5 and 0.8 percent within the wavelength range of 350 and 1000 nm.
Example 2
Fe, Mn and Cu pure metals with the purity of more than 99% are mixed according to the ratio of 31.7 at%: 68 at%: after being mixed in a proportion of 0.3 at%, the mixture is smelted for 2 times at 1500 ℃ by induction heating, each time lasts for 10 minutes, and after uniform molten metal is obtained, the molten metal is rapidly quenched at 1500 ℃ to obtain the FeMnCu prealloy with a single-phase structure. Placing the FeMnCu prealloy in a hydrochloric acid solution with the volume concentration of 1% and standing for 60 minutes for dealloying; taking out the product after the dealloying, sequentially rinsing in 0.1% hydrochloric acid solution with volume concentration for 10 seconds and 0.01% hydrochloric acid solution respectively, and rinsing in ultrapure water for 30 seconds; and taking out the rinsed product, and drying at 30 ℃ under the protection of inert gas to obtain the ultra-black nano porous Fe material. The nano-pores are between 30 and 50nm, the oxygen content is between 12 and 17at percent, and the reflectivity of the material is between 0.7 and 0.9 percent within the wavelength range of 350 and 1000 nm.
Example 3
Fe, Mn and Cu pure metals with the purity of more than 99% are mixed according to the mass ratio of 9.7 at%: 90 at%: after being mixed in a proportion of 0.3 at%, the mixture is smelted for 2 times at 1240 ℃ by induction heating, each time lasts for 10 minutes, and after uniform molten metal is obtained, the molten metal is rapidly quenched at 1240 ℃ to obtain the FeMnCu prealloy with a single-phase structure. Placing the FeMnCu prealloy in a hydrochloric acid solution with the volume concentration of 1% and standing for 60 minutes for dealloying; taking out the product after the dealloying, sequentially rinsing in 0.1% hydrochloric acid solution with volume concentration for 5 seconds and then rinsing in ultrapure water for 10 seconds; and taking out the rinsed product, and drying at 30 ℃ under the protection of inert gas to obtain the ultra-black nano porous Fe material. The nano-pores are between 70 and 100nm, the oxygen content is between 12 and 17at percent, and the reflectivity of the material is between 0.9 and 0.1 percent within the wavelength range of 350 and 1000 nm.
Example 4
Fe and Mn pure metals with the purity of more than 99 percent are mixed according to the ratio of 32at percent: mixing 68 at%, smelting at 1500 deg.C for 2 times (5 min each) by induction heating to obtain homogeneous molten metal, and rapidly quenching at 1500 deg.C to obtain single-phase FeMnCu prealloy. Placing the FeMnCu prealloy in a hydrochloric acid solution with the volume concentration of 5% and standing for 30 minutes for dealloying; taking out the product after the dealloying, sequentially rinsing in 0.1% hydrochloric acid solution with volume concentration for 5 seconds and then rinsing in ultrapure water for 10 seconds; and taking out the rinsed product, and drying at 30 ℃ under the protection of inert gas to obtain the ultra-black nano porous Fe material. The nano-pores are between 10 and 20nm, the oxygen content is between 8 and 10at percent, and the reflectivity of the material is between 0.5 and 0.7 percent within the wavelength range of 350 and 1000 nm.
Example 5
Fe, Mn and Cu pure metals with the purity of more than 99% are mixed according to the ratio of 31.7 at%: 68 at%: 0.3 at% and smelting for 2 times at 1500 ℃ by induction heating for 5 minutes each time after mixing, obtaining uniform molten metal, and then rapidly quenching at 1700 ℃ to obtain the FeMnCu prealloy with a single-phase structure. Placing the FeMnCu prealloy in a hydrochloric acid solution with the volume concentration of 5% and standing for 30 minutes for dealloying; taking out the product after the dealloying, sequentially rinsing in 0.1% hydrochloric acid solution with volume concentration for 5 seconds and then rinsing in ultrapure water for 10 seconds; and taking out the rinsed product, and drying at 30 ℃ under the protection of inert gas to obtain the ultra-black nano porous Fe material. The nano-pores are between 20 and 30nm, the oxygen content is between 5 and 8at percent, and the reflectivity of the material is between 0.6 and 0.8 percent within the wavelength range of 350 and 1000 nm.
Claims (6)
1. A preparation method of ultra-black nano-porous Fe is characterized by comprising the following steps:
1) mixing pure metals of Fe, Mn and Cu, carrying out induction heating to obtain uniform molten metal, and then carrying out rapid quenching to obtain a FeMnCu prealloy with a single-phase structure;
2) placing the FeMnCu prealloy obtained in the step 1) in a hydrochloric acid solution for standing, and performing dealloying treatment;
3) pickling the product obtained in the step 2) in a dilute hydrochloric acid solution;
4) rinsing the product obtained in the step 3) in ultrapure water;
5) drying the product obtained in the step 4) in an inert atmosphere to obtain the ultra-black nano porous iron;
wherein,
in the step 1), the purity of the pure metal is more than 99 percent, and the atomic percentage is that the Mn content is 67 to 90at percent, the Cu content is less than 0.3at percent, and the Fe content is 31.7 to 9.7at percent; the induction heating temperature is lower than 1700 ℃, the heating time is lower than 20 minutes, and the heating times are more than 2 times; and performing rapid quenching on the uniform molten metal within the range of 1240-1700 ℃ to obtain the FeMnCu prealloy with a single-phase structure.
2. The method of preparing ultra-black nanoporous Fe according to claim 1, wherein: in the step 2), the dealloying is carried out under the free corrosion condition, the temperature is 4-30 ℃, the volume concentration of the hydrochloric acid solution is 1% -5%, and the dealloying time is 30-60 minutes.
3. The method of preparing ultra-black nanoporous Fe according to claim 1, wherein: in the step 3), the dilute hydrochloric acid washing is to rinse the products obtained in the step 2) in a hydrochloric acid solution with the volume concentration of 0.1 percent and the volume concentration of 0.01 percent in sequence, and the time of each time is not more than 10 seconds.
4. The method of preparing ultra-black nanoporous Fe according to claim 1, wherein: rinsing in ultrapure water in the step 4) for no more than 30 s.
5. The method of preparing ultra-black nanoporous Fe according to claim 1, wherein: in the step 5), the oxygen content of the inert gas is lower than one ten thousandth, and the drying temperature is not higher than 30 ℃.
6. A nano-porous Fe prepared by the method of any one of claims 1 to 5, wherein the method comprises the following steps: the pore diameter of the nano-pore is between 10 and 100 nanometers, the oxygen content is below 20at percent, and the reflectivity is below 1 percent in the wavelength range of 350-1000 nm.
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| 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 |
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| 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 * |
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