CN110029377B - A kind of long-wavelength ultra-black porous composite material and preparation method thereof - Google Patents

A kind of long-wavelength ultra-black porous composite material and preparation method thereof Download PDF

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CN110029377B
CN110029377B CN201910403992.5A CN201910403992A CN110029377B CN 110029377 B CN110029377 B CN 110029377B CN 201910403992 A CN201910403992 A CN 201910403992A CN 110029377 B CN110029377 B CN 110029377B
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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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Abstract

本发明公开了一种长波段超黑多孔复合材料及其制备方法，该材料具有微米多孔结构，孔壁由NiCuFe枝晶构成，在枝晶表面均匀覆盖有NiO层；其制备方法包括以下步骤：1)将工作电极置于NiSO4、CuSO4、FeSO4、(NH4)2SO4、Na3C6H5O7和H3BO3混合溶液中进行电化学沉积，获得NiCuFe镀层；2)将镀层漂洗、晾干后进行热处理，在材料表面形成NiO层，得到所述的长波段超黑多孔复合材料。该长波段超黑多孔复合材料价格低廉、光吸收范围广，具有强光照射条件下也不裂变的优点，且制备方法简单易行。

Figure 201910403992

The invention discloses a long-wavelength ultra-black porous composite material and a preparation method thereof. The material has a micron porous structure, the pore walls are composed of NiCuFe dendrites, and the surface of the dendrites is uniformly covered with a NiO layer; the preparation method includes the following steps: 1) The working electrode is placed in a mixed solution of NiSO 4 , CuSO 4 , FeSO 4 , (NH4) 2 SO 4 , Na 3 C 6 H 5 O 7 and H 3 BO 3 for electrochemical deposition to obtain a NiCuFe coating; 2) After rinsing and drying the plating layer, heat treatment is performed to form a NiO layer on the surface of the material to obtain the long-wavelength ultra-black porous composite material. The long-wavelength ultra-black porous composite material has the advantages of low price, wide light absorption range, no fission under strong light irradiation, and simple and easy preparation method.

Figure 201910403992

Description

Long-wave-band ultra-black porous composite material and preparation method thereof
Technical Field
The invention relates to a long-wave band ultra-black porous composite material and a preparation method thereof, belonging to the field of micro-nano material preparation.
Background
Ultra-black materials have found widespread use in many optical applications, sensors, and solar energy converters due to their ultra-low reflectivity to incident light. At present, materials with prominent super-black performance mainly comprise olefinic carbon materials, metal materials with superior plasma enhancement effect such as Au and Ag, traditional semiconductor materials such as silicon, nickel-phosphorus intermediate alloy materials, organic materials and the like. The morphological structure of the porous structure comprises a nanotube array, a micro-convex array, a roughened irregular surface, a three-dimensional communicated porous structure and the like. The preparation method mainly comprises chemical vapor deposition, a biological template method and the like. The ultra-black materials have the problems of high cost, easy fission and aging and ultra-black only in a limited wave band.
Disclosure of Invention
The technical problem is as follows: the invention aims to provide a long-wave band ultra-black porous composite material which is low in price, wide in light absorption range and has the advantage of being not cracked under the condition of strong light irradiation.
The invention also aims to provide a preparation method of the long-wave band ultra-black porous composite material, which is simple and feasible.
The technical scheme is as follows: the invention provides a long-wave band ultra-black porous composite material which has a micron porous structure, wherein a hole wall is formed by NiCuFe dendrites, and a NiO layer is uniformly covered on the surfaces of the dendrites.
Wherein:
the size of the micropores in the microporous structure is 5-25 microns.
The pore wall is composed of NiCuFe dendrites, the length of the primary dendrite is 1-2 um, and the size of the secondary dendrite is 100-1000 nm.
The thickness of the NiO layer is 5-50 nm.
The reflectivity of the long-wave band ultra-black porous composite material is 0.7-7.0% within the range of 250 nm-2.5 mu m.
The invention also provides a preparation method of the long-wave band ultra-black porous composite material, which comprises the following steps:
1) placing the working electrode in NiSO4、CuSO4、FeSO4、(NH4)2SO4、Na3C6H5O7And H3BO3Carrying out electrochemical deposition in the mixed solution to obtain a NiCuFe coating;
2) and rinsing and airing the coating, and then carrying out heat treatment to form a NiO layer on the surface of the material to obtain the long-wave-band ultra-black porous composite material, wherein the material shows very low reflectivity from ultraviolet to infrared regions.
Wherein:
NiSO described in step 1)4、CuSO4、FeSO4、(NH4)2SO4、Na3C6H5O7And H3BO3In the mixed solution, NiSO4The concentration of (A) is 0.15-0.25M, CuSO4The concentration is 0.01-0.03M, FeSO4The concentration is 0.01-0.02M, (NH)4)2SO4The concentration is 0.3-0.5M, Na3C6H5O7The concentration is 0.2-0.4M, H3BO3The concentration is 0.3-0.5M.
The process parameters of the electrochemical deposition process in the step 1) are as follows: the current density of constant current deposition is 0.5-1.5A/cm2The deposition time is 50-180 s.
In the NiCuFe coating in the step 1), the atomic percent of Cu is 5-25%, the atomic percent of Fe is 0.5-1%, and the balance is Ni.
Rinsing and air-drying the plating layer in the step 2), and then carrying out heat treatment, wherein the rinsing reagent is ultrapure water, and the air-drying refers to air-drying in the atmospheric atmosphere; the heat treatment temperature is 380-420 ℃, the heat treatment atmosphere is atmospheric atmosphere, and the heat treatment time is 30-80 min.
Has the advantages that: compared with the prior art, the invention has the following beneficial effects:
1. the preparation method provided by the invention does not adopt vacuum facilities, is simple and feasible, and has low raw material price;
2. the prepared long-wave band ultra-black porous composite material has a micro-nano composite structure, and the light absorption range is wide (the reflectivity is 0.7-7.0% within the range of 250 nm-2.5 mu m);
3. the surface of the long-wave band ultra-black porous composite material prepared by the invention is metal oxide, the material is not fissile under the condition of strong light irradiation, and the service life is long.
Drawings
FIG. 1 is a low-power and high-power scanning electron microscope topography of the long-wave band ultra-black porous composite material, wherein an inset is the low-power scanning electron microscope topography.
Detailed Description
The invention provides a long-wave band ultra-black porous composite material and a preparation method thereof, and the technology of the invention is further explained by the following embodiments.
Example 1
A long-wave band ultra-black porous composite material has a micron porous structure, wherein the pore wall is composed of NiCuFe dendrites, and NiO layers are uniformly covered on the surfaces of the dendrites.
Wherein:
the size of the micropores in the microporous structure is 5-15 microns.
The hole wall is composed of NiCuFe dendrites, the length of the primary dendrite is 1-2 mu m, and the size of the secondary dendrite is 500-1000 nm.
The thickness of the NiO layer is 40 nm.
The reflectivity of the long-wave band ultra-black porous composite material is 0.8-1.2% within the range of 250 nm-2.5 mu m.
The preparation method of the long-wave band ultra-black porous composite material comprises the following steps:
1) the working electrode was placed in 0.15M NiSO4+0.03CuSO4+0.01FeSO4+0.5M(NH4)2SO4+0.2M Na3C6H5O7+0.3M H3BO3In the mixed solution, at a rate of 0.5A/cm2Carrying out electrochemical deposition for 180 seconds under the current density condition to obtain a NiCuFe coating, wherein the atomic percent of Cu in the NiCuFe coating is 25%, and the atomic percent of Fe in the NiCuFe coating is 0.5%;
2) rinsing the plating layer in ultrapure water, drying in the air, placing in the air, performing heat treatment at 380 ℃ for 80min to form a NiO layer on the surface of the material, and cooling to obtain the long-wave-band ultra-black porous composite material.
Example 2
A long-wave band ultra-black porous composite material has a micron porous structure, wherein the pore wall is composed of NiCuFe dendrites, and NiO layers are uniformly covered on the surfaces of the dendrites.
Wherein:
the size of the micropores in the microporous structure is 5-15 microns.
The hole wall is composed of NiCuFe dendrites, the length of the primary dendrite is 1-2 mu m, and the size of the secondary dendrite is 100-800 nm.
The thickness of the NiO layer is 50 nm.
The reflectivity of the long-wave band ultra-black porous composite material is 0.8-7% within the range of 250 nm-2.5 mu m.
The preparation method of the long-wave band ultra-black porous composite material comprises the following steps:
1) the working electrode was placed in 0.25M NiSO4+0.01CuSO4+0.02FeSO4+0.5M(NH4)2SO4+0.4M Na3C6H5O7+0.5M H3BO3In the mixed solution, at a rate of 1.5A/cm2Carrying out electrochemical deposition for 50 seconds under the current density condition to obtain a NiCuFe coating, wherein the atomic percent of Cu in the NiCuFe coating is 5%, and the atomic percent of Fe in the NiCuFe coating is 1%;
2) rinsing the coating in ultrapure water, drying in the air, placing in the air, performing heat treatment at 420 ℃ for 80min to form a NiO layer on the surface of the material, and cooling to obtain the long-wave-band ultra-black porous composite material.
Example 3
A long-wave band ultra-black porous composite material has a micron porous structure, wherein the pore wall is composed of NiCuFe dendrites, and NiO layers are uniformly covered on the surfaces of the dendrites.
Wherein:
the size of the micropores in the microporous structure is 5-20 microns.
The hole wall is composed of NiCuFe dendrites, the length of the primary dendrite is 1-2 mu m, and the size of the secondary dendrite is 300-900 nm.
The thickness of the NiO layer is 5 nm.
The reflectivity of the long-wave band ultra-black porous composite material is 0.7-1% within the range of 250 nm-2.5 mu m.
The preparation method of the long-wave band ultra-black porous composite material comprises the following steps:
1) the working electrode was placed in 0.2M NiSO4+0.02CuSO4+0.05FeSO4+0.5M(NH4)2SO4+0.3M Na3C6H5O7+0.4M H3BO3In the mixed solution, at a rate of 0.8A/cm2Carrying out electrochemical deposition for 100 seconds under the current density condition to obtain a NiCuFe coating, wherein the atomic percent of Cu in the NiCuFe coating is 20%, and the atomic percent of Fe in the NiCuFe coating is 0.5%;
2) rinsing the plating layer in ultrapure water, drying in the air, placing in the air, carrying out heat treatment at 380 ℃ for 30min, forming a NiO layer on the surface of the material, and cooling to obtain the long-wave-band ultra-black porous composite material.
Example 4
A long-wave band ultra-black porous composite material has a micron porous structure, wherein the pore wall is composed of NiCuFe dendrites, and NiO layers are uniformly covered on the surfaces of the dendrites.
Wherein:
the size of the micropores in the microporous structure is 5-20 microns.
The hole wall is composed of NiCuFe dendrites, the length of the primary dendrite is 1-2 mu m, and the size of the secondary dendrite is 300-900 nm.
The thickness of the NiO layer is 5 nm.
The reflectivity of the long-wave band ultra-black porous composite material is 2-5% within the range of 250 nm-2.5 mu m.
The preparation method of the long-wave band ultra-black porous composite material comprises the following steps:
1) the working electrode was placed in 0.2M NiSO4+0.02CuSO4+0.05FeSO4+0.3M(NH4)2SO4+0.3M Na3C6H5O7+0.4M H3BO3In the mixed solution, at a rate of 0.8A/cm2Carrying out electrochemical deposition for 100 seconds under the current density condition to obtain a NiCuFe coating, wherein the atomic percent of Cu in the NiCuFe coating is 25%, and the atomic percent of Fe in the NiCuFe coating is 0.5%;
2) rinsing the plating layer in ultrapure water, drying in the air, placing in the air, carrying out heat treatment at 380 ℃ for 30min, forming a NiO layer on the surface of the material, and cooling to obtain the long-wave-band ultra-black porous composite material.

Claims (5)

1.一种长波段超黑多孔复合材料，其特征在于：该材料具有微米多孔结构，孔壁由NiCuFe枝晶构成，在枝晶表面均匀覆盖有NiO层；1. a long-wavelength ultra-black porous composite material, is characterized in that: this material has micron porous structure, and pore wall is made up of NiCuFe dendrite, and is evenly covered with NiO layer on dendrite surface; 所述的微米多孔结构中微米孔的尺寸为5～25μm；The size of the micro-pores in the micro-porous structure is 5-25 μm; 所述的孔壁由NiCuFe枝晶构成中，一次枝晶长度为1～2μm，二次枝晶尺寸在100～1000nm；The pore wall is composed of NiCuFe dendrites, the length of the primary dendrite is 1-2 μm, and the size of the secondary dendrite is 100-1000 nm; 所述的NiO层的厚度为5～50 nm；The thickness of the NiO layer is 5-50 nm; 所述的长波段超黑多孔复合材料在250nm～2.5μm范围内反射率为0.7%～7.0%。The long-wavelength ultra-black porous composite material has a reflectivity of 0.7% to 7.0% in the range of 250 nm to 2.5 μm. 2.一种如权利要求1所述的长波段超黑多孔复合材料的制备方法，其特征在于：该方法包括以下步骤：2. a preparation method of long-wavelength ultra-black porous composite material as claimed in claim 1, is characterized in that: this method comprises the following steps: 1）将工作电极置于NiSO4、CuSO4、FeSO4、(NH4)2SO4、Na3C6H5O7和H3BO3混合溶液中进行电化学沉积，获得NiCuFe镀层；1) The working electrode is placed in a mixed solution of NiSO 4 , CuSO 4 , FeSO 4 , (NH4) 2 SO 4 , Na 3 C 6 H 5 O 7 and H 3 BO 3 for electrochemical deposition to obtain a NiCuFe coating; 2）将镀层漂洗、晾干后进行热处理，在材料表面形成NiO层，得到所述的长波段超黑多孔复合材料；2) heat treatment after rinsing and drying the coating to form a NiO layer on the surface of the material to obtain the long-wavelength ultra-black porous composite material; 其中，步骤1）所述的NiCuFe镀层中Cu原子百分比5～25%、Fe原子百分比0.5～1%，剩余的为Ni。Wherein, in the NiCuFe coating described in step 1), the atomic percentage of Cu is 5-25%, the atomic percentage of Fe is 0.5-1%, and the rest is Ni. 3.如权利要求2所述的一种长波段超黑多孔复合材料的制备方法，其特征在于：步骤1）所述的NiSO4、CuSO4、FeSO4、(NH4)2SO4、Na3C6H5O7和H3BO3混合溶液中，NiSO4的浓度为0.15～0.25 M，CuSO4浓度为0.01～0.03 M，FeSO4浓度为 0.01～0.02 M，(NH4)2SO4浓度为0.3～0.5M, Na3C6H5O7浓度为0.2～0.4 M, H3BO3 浓度为0.3～0.5 M。3 . The method for preparing a long-wavelength ultra-black porous composite material according to claim 2 , wherein the NiSO 4 , CuSO 4 , FeSO 4 , (NH 4 ) 2 SO 4 , Na 3 described in step 1). In the mixed solution of C 6 H 5 O 7 and H 3 BO 3 , the concentration of NiSO 4 is 0.15-0.25 M, the concentration of CuSO 4 is 0.01-0.03 M, the concentration of FeSO 4 is 0.01-0.02 M, (NH 4 ) 2 SO 4 The concentration is 0.3-0.5M, the concentration of Na 3 C 6 H 5 O 7 is 0.2-0.4 M, and the concentration of H 3 BO 3 is 0.3-0.5 M. 4.如权利要求2所述的一种长波段超黑多孔复合材料的制备方法，其特征在于：步骤1）所述的电化学沉积过程的工艺参数为：恒流沉积的电流密度为0.5～1.5 A/cm2，沉积时间为50～180 s。4 . The preparation method of a long-wavelength ultra-black porous composite material according to claim 2 , wherein the process parameters of the electrochemical deposition process in step 1) are: the current density of the constant current deposition is 0.5～5 . 1.5 A/cm 2 , the deposition time is 50-180 s. 5.如权利要求2所述的一种长波段超黑多孔复合材料的制备方法，其特征在于：步骤2）所述的将镀层漂洗、晾干后进行热处理中，漂洗所用试剂为超纯水，晾干是指在大气氛围中晾干；热处理温度为380～420℃，热处理氛围为大气氛围，热处理时间为30～80min。5. The preparation method of a long-wavelength ultra-black porous composite material according to claim 2, characterized in that: in the step 2) of rinsing and air-drying the coating and performing heat treatment, the rinsing reagent is ultrapure water , Drying refers to drying in the atmosphere; the heat treatment temperature is 380 ~ 420 ℃, the heat treatment atmosphere is the atmospheric atmosphere, and the heat treatment time is 30 ~ 80min.
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