CN110029377A - A kind of long-wave band blacker-than-black is composite porous and preparation method thereof - Google Patents

A kind of long-wave band blacker-than-black is composite porous and preparation method thereof Download PDF

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CN110029377A
CN110029377A CN201910403992.5A CN201910403992A CN110029377A CN 110029377 A CN110029377 A CN 110029377A CN 201910403992 A CN201910403992 A CN 201910403992A CN 110029377 A CN110029377 A CN 110029377A
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blacker
black
long
wave band
composite porous
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CN110029377B (en
Inventor
曾宇乔
丁雪卉
季宝荣
张旭海
朱奎
吕宙
郑新健
邵起越
董岩
蒋建清
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Southeast University
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Southeast University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • 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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C19/00—Alloys based on nickel or cobalt
    • C22C19/03—Alloys based on nickel or cobalt based on nickel
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/56—Electroplating: Baths therefor from solutions of alloys
    • C25D3/562—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of iron or nickel or cobalt
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/48—After-treatment of electroplated surfaces
    • C25D5/50—After-treatment of electroplated surfaces by heat-treatment
    • C25D5/505—After-treatment of electroplated surfaces by heat-treatment of electroplated tin coatings, e.g. by melting

Abstract

Composite porous and preparation method thereof the invention discloses a kind of long-wave band blacker-than-black, which has um porous structure, and hole wall is made of NiCuFe dendrite, and on dendrite surface, uniform fold has NiO layer；Preparation method includes the following steps: 1) working electrode being placed in NiSO4、CuSO4、FeSO4、(NH4)2SO4、Na3C6H5O7And H3BO3Electrochemical deposition is carried out in mixed solution, obtains NiCuFe coating；2) it is heat-treated after coating being rinsed, dried, forms NiO layer on the surface of the material, it is composite porous to obtain the long-wave band blacker-than-black.The long-wave band blacker-than-black it is composite porous it is cheap, light abstraction width is wide, have the advantages that also not fission under the conditions of strong illumination, and preparation method is simple.

Description

A kind of long-wave band blacker-than-black is composite porous and preparation method thereof
Technical field
It is composite porous and preparation method thereof the present invention relates to a kind of long-wave band blacker-than-black, belong to micro-nano material preparation neck Domain.
Background technique
Blacker-than-black material converts the ultra-low reflectance of incident ray in many optical devices, sensor and solar energy because of it Extensive utilization is obtained on device.Blacker-than-black performance material outstanding mainly includes the plasma enhancings such as olefinic carbon material, Au and Ag at present The conventional semiconductor materials such as metal material, the silicon of superior, nickel phosphorus intermediate alloy material and organic material etc..Its morphosis Including nano-tube array, dimpling array and roughened irregular surface and three-dimensional connected porous structure structure etc..Preparation method It mainly include chemical vapor deposition, biological template method etc..There is with high costs, ageingization easy to crack, only mostly in above-mentioned blacker-than-black material The problem of limited wavelength band shows blacker-than-black.
Summary of the invention
Technical problem: the object of the present invention is to provide a kind of long-wave band blacker-than-black is composite porous, the material price is cheap, Light abstraction width is wide, has the advantages that also not fission under the conditions of strong illumination.
It is a further object of the present invention to provide a kind of preparation method that long-wave band blacker-than-black is composite porous, this method is simple It is easy.
Technical solution: the present invention provides a kind of long-wave band blacker-than-black is composite porous, which has um porous knot Structure, hole wall are made of NiCuFe dendrite, and on dendrite surface, uniform fold has NiO layer.
Wherein:
The size of micron openings is 5~25 μm in the um porous structure.
During the hole wall is made of NiCuFe dendrite, dendrite length is 1~2um, secondary dendrite size 100~ 1000nm。
The NiO layer with a thickness of 5~50nm.
The long-wave band blacker-than-black it is composite porous the μ m internal reflection rate of 250nm~2.5 be 0.7%~7.0%.
The present invention also provides a kind of preparation method that long-wave band blacker-than-black is composite porous, this method includes following step It is rapid:
1) working electrode is placed in NiSO4、CuSO4、FeSO4、(NH4)2SO4、Na3C6H5O7And H3BO3In mixed solution into Row electrochemical deposition obtains NiCuFe coating；
2) it is heat-treated after coating being rinsed, dried, forms NiO layer on the surface of the material, it is super to obtain the long-wave band Black composite porous, which shows very low reflectivity to infrared region from ultraviolet.
Wherein:
NiSO described in step 1)4、CuSO4、FeSO4、(NH4)2SO4、Na3C6H5O7And H3BO3In mixed solution, NiSO4 Concentration be 0.15~0.25M, CuSO4Concentration is 0.01~0.03M, FeSO4Concentration is 0.01~0.02M, (NH4)2SO4Concentration For 0.3~0.5M, Na3C6H5O7Concentration is 0.2~0.4M, H3BO3Concentration is 0.3~0.5M.
The technological parameter of electrochemical deposition process described in step 1) are as follows: the current density of constant current deposition is 0.5~1.5A/ cm2, sedimentation time is 50~180s.
Cu atomic percent 5~25% in NiCuFe coating described in step 1), Fe atomic percent 0.5~1% are remaining It is Ni.
In being heat-treated after coating is rinsed, dried described in step 2), rinsing agents useful for same is ultrapure water, and drying is Finger dries in atmospheric atmosphere；Heat treatment temperature is 380~420 DEG C, and heat treatment atmosphere is atmospheric atmosphere, heat treatment time 30 ~80min.
The utility model has the advantages that compared with prior art, the invention has the following advantages:
1, preparation method provided by the invention does not use vacuum facility, simple and easy, and the prices of raw materials are cheap；
2, the long-wave band blacker-than-black that the present invention is prepared is composite porous while having micro-nano compound structure, light absorption model Enclose wide (the μ m internal reflection rate of 250nm~2.5 is 0.7%~7.0%)；
3, the composite porous surface of long-wave band blacker-than-black that the present invention is prepared is metal oxide, strong illumination condition Lower material is not fissioned, long service life.
Detailed description of the invention
Fig. 1 be the composite porous low power of long-wave band blacker-than-black of the present invention and high power scanning electron microscope shape appearance figure, wherein Illustration is low power scanning electron microscope shape appearance figure.
Specific embodiment
It is composite porous and preparation method thereof the present invention provides a kind of long-wave band blacker-than-black, below by embodiment into one Step is illustrated technology of the invention.
Embodiment 1
A kind of long-wave band blacker-than-black is composite porous, which has um porous structure, and hole wall is by NiCuFe dendrite structure At on dendrite surface, uniform fold has NiO layer.
Wherein:
The size of micron openings is 5~15 μm in the um porous structure.
During the hole wall is made of NiCuFe dendrite, dendrite length is 1~2 μm, secondary dendrite size 500~ 1000nm。
The NiO layer with a thickness of 40nm.
The long-wave band blacker-than-black it is composite porous the μ m internal reflection rate of 250nm~2.5 be 0.8%~1.2%.
The composite porous preparation method of the long-wave band blacker-than-black, method includes the following steps:
1) working electrode is placed in 0.15M NiSO4+0.03CuSO4+0.01FeSO4+0.5M(NH4)2SO4+0.2M Na3C6H5O7+0.3M H3BO3In mixed solution, with 0.5A/cm2It carries out electrochemical deposition 180 seconds, obtains under current density condition NiCuFe coating, Cu atomic percent 25% in the NiCuFe coating, Fe atomic percent 0.5%；
2) coating is rinsed, then after being dried in atmospheric atmosphere in ultrapure water, is placed in air hot under the conditions of 380 DEG C 80min is handled, forms NiO layer on the surface of the material, the long-wave band blacker-than-black obtained after cooling is composite porous.
Embodiment 2
A kind of long-wave band blacker-than-black is composite porous, which has um porous structure, and hole wall is by NiCuFe dendrite structure At on dendrite surface, uniform fold has NiO layer.
Wherein:
The size of micron openings is 5~15 μm in the um porous structure.
During the hole wall is made of NiCuFe dendrite, dendrite length is 1~2 μm, secondary dendrite size 100~ 800nm。
The NiO layer with a thickness of 50nm.
The long-wave band blacker-than-black it is composite porous the μ m internal reflection rate of 250nm~2.5 be 0.8%~7%.
The composite porous preparation method of the long-wave band blacker-than-black, method includes the following steps:
1) working electrode is placed in 0.25M NiSO4+0.01CuSO4+0.02FeSO4+0.5M(NH4)2SO4+0.4M Na3C6H5O7+0.5M H3BO3In mixed solution, with 1.5A/cm2It carries out electrochemical deposition 50 seconds, obtains under current density condition NiCuFe coating, Cu atomic percent 5% in the NiCuFe coating, Fe atomic percent 1%；
2) coating is rinsed, then after being dried in atmospheric atmosphere in ultrapure water, is placed in air hot under the conditions of 420 DEG C 80min is handled, forms NiO layer on the surface of the material, the long-wave band blacker-than-black obtained after cooling is composite porous.
Embodiment 3
A kind of long-wave band blacker-than-black is composite porous, which has um porous structure, and hole wall is by NiCuFe dendrite structure At on dendrite surface, uniform fold has NiO layer.
Wherein:
The size of micron openings is 5~20 μm in the um porous structure.
During the hole wall is made of NiCuFe dendrite, dendrite length is 1~2 μm, secondary dendrite size 300~ 900nm。
The NiO layer with a thickness of 5nm.
The long-wave band blacker-than-black it is composite porous the μ m internal reflection rate of 250nm~2.5 be 0.7%~1%.
The composite porous preparation method of the long-wave band blacker-than-black, method includes the following steps:
1) working electrode is placed in 0.2M NiSO4+0.02CuSO4+0.05FeSO4+0.5M(NH4)2SO4+0.3M Na3C6H5O7+0.4M H3BO3In mixed solution, with 0.8A/cm2It carries out electrochemical deposition 100 seconds, obtains under current density condition NiCuFe coating, Cu atomic percent 20% in the NiCuFe coating, Fe atomic percent 0.5%；
2) coating is rinsed, then after being dried in atmospheric atmosphere in ultrapure water, is placed in air hot under the conditions of 380 DEG C 30min is handled, forms NiO layer on the surface of the material, the long-wave band blacker-than-black obtained after cooling is composite porous.
Embodiment 4
A kind of long-wave band blacker-than-black is composite porous, which has um porous structure, and hole wall is by NiCuFe dendrite structure At on dendrite surface, uniform fold has NiO layer.
Wherein:
The size of micron openings is 5~20 μm in the um porous structure.
During the hole wall is made of NiCuFe dendrite, dendrite length is 1~2 μm, secondary dendrite size 300~ 900nm。
The NiO layer with a thickness of 5nm.
The long-wave band blacker-than-black it is composite porous the μ m internal reflection rate of 250nm~2.5 be 2%~5%.
The composite porous preparation method of the long-wave band blacker-than-black, method includes the following steps:
1) working electrode is placed in 0.2M NiSO4+0.02CuSO4+0.05FeSO4+0.3M(NH4)2SO4+0.3M Na3C6H5O7+0.4M H3BO3In mixed solution, with 0.8A/cm2It carries out electrochemical deposition 100 seconds, obtains under current density condition NiCuFe coating, Cu atomic percent 25% in the NiCuFe coating, Fe atomic percent 0.5%；
2) coating is rinsed, then after being dried in atmospheric atmosphere in ultrapure water, is placed in air hot under the conditions of 380 DEG C 30min is handled, forms NiO layer on the surface of the material, the long-wave band blacker-than-black obtained after cooling is composite porous.

Claims (10)

1. a kind of long-wave band blacker-than-black is composite porous, it is characterised in that: the material have um porous structure, hole wall by NiCuFe dendrite is constituted, and on dendrite surface, uniform fold has NiO layer.
2. a kind of long-wave band blacker-than-black as described in claim 1 is composite porous, it is characterised in that: the um porous knot The size of micron openings is 5~25 μm in structure.
3. a kind of long-wave band blacker-than-black as described in claim 1 is composite porous, it is characterised in that: the hole wall by During NiCuFe dendrite is constituted, a dendrite length is 1~2 μm, and secondary dendrite size is in 100~1000nm.
4. a kind of long-wave band blacker-than-black as described in claim 1 is composite porous, it is characterised in that: the thickness of the NiO layer Degree is 5~50nm.
5. a kind of long-wave band blacker-than-black as described in claim 1 is composite porous, it is characterised in that: the long-wave band blacker-than-black It is composite porous the μ m internal reflection rate of 250nm~2.5 be 0.7%~7.0%.
6. a kind of preparation method that long-wave band blacker-than-black as described in claim 1 is composite porous, it is characterised in that: this method The following steps are included:
1) working electrode is placed in NiSO4、CuSO4、FeSO4、(NH4)2SO4、Na3C6H5O7And H3BO3Electricity is carried out in mixed solution Chemical deposition obtains NiCuFe coating；
2) it is heat-treated after coating being rinsed, dried, forms NiO layer on the surface of the material, it is more to obtain the long-wave band blacker-than-black Hole composite material.
7. a kind of preparation method that long-wave band blacker-than-black is composite porous as claimed in claim 6, it is characterised in that: step 1) The NiSO4、CuSO4、FeSO4、(NH4)2SO4、Na3C6H5O7And H3BO3In mixed solution, NiSO4Concentration be 0.15~ 0.25M, CuSO4Concentration is 0.01~0.03M, FeSO4Concentration is 0.01~0.02M, (NH4)2SO4Concentration is 0.3~0.5M, Na3C6H5O7Concentration is 0.2~0.4M, H3BO3Concentration is 0.3~0.5M.
8. a kind of preparation method that long-wave band blacker-than-black is composite porous as claimed in claim 6, it is characterised in that: step 1) The technological parameter of the electrochemical deposition process are as follows: the current density of constant current deposition is 0.5~1.5A/cm2, sedimentation time is 50~180s.
9. a kind of preparation method that long-wave band blacker-than-black is composite porous as claimed in claim 6, it is characterised in that: step 1) Cu atomic percent 5~25%, Fe atomic percent 0.5~1% in the NiCuFe coating, remaining is Ni.
10. a kind of preparation method that long-wave band blacker-than-black is composite porous as claimed in claim 6, it is characterised in that: step 2) described in by coating rinsing, dry after be heat-treated, rinsing agents useful for same is ultrapure water, dries and refers in atmospheric atmosphere In dry；Heat treatment temperature is 380~420 DEG C, and heat treatment atmosphere is atmospheric atmosphere, and heat treatment time is 30~80min.
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