CN117192660A - Composite film with ultralow reflectivity and preparation method and application thereof - Google Patents
Composite film with ultralow reflectivity and preparation method and application thereof Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 87
- 238000002310 reflectometry Methods 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title abstract description 23
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 99
- 229910052802 copper Inorganic materials 0.000 claims abstract description 86
- 239000010949 copper Substances 0.000 claims abstract description 86
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 69
- 229910001369 Brass Inorganic materials 0.000 claims description 67
- 239000010951 brass Substances 0.000 claims description 67
- OMZSGWSJDCOLKM-UHFFFAOYSA-N copper(II) sulfide Chemical group [S-2].[Cu+2] OMZSGWSJDCOLKM-UHFFFAOYSA-N 0.000 claims description 54
- 238000000034 method Methods 0.000 claims description 47
- ORUIBWPALBXDOA-UHFFFAOYSA-L magnesium fluoride Chemical group [F-].[F-].[Mg+2] ORUIBWPALBXDOA-UHFFFAOYSA-L 0.000 claims description 46
- 229910001635 magnesium fluoride Inorganic materials 0.000 claims description 46
- 238000010926 purge Methods 0.000 claims description 40
- 239000000758 substrate Substances 0.000 claims description 36
- 238000006243 chemical reaction Methods 0.000 claims description 32
- 239000007787 solid Substances 0.000 claims description 32
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 26
- 229910052749 magnesium Inorganic materials 0.000 claims description 26
- 239000011777 magnesium Substances 0.000 claims description 26
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 24
- 238000010521 absorption reaction Methods 0.000 claims description 22
- 238000001035 drying Methods 0.000 claims description 20
- 238000002791 soaking Methods 0.000 claims description 19
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 18
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 18
- 238000000151 deposition Methods 0.000 claims description 17
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims description 16
- 229910000037 hydrogen sulfide Inorganic materials 0.000 claims description 16
- 238000004140 cleaning Methods 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 15
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 14
- 238000000231 atomic layer deposition Methods 0.000 claims description 14
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims description 14
- 239000011259 mixed solution Substances 0.000 claims description 14
- 229910052757 nitrogen Inorganic materials 0.000 claims description 12
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 9
- 229910052717 sulfur Inorganic materials 0.000 claims description 9
- 239000011593 sulfur Substances 0.000 claims description 9
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 8
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims description 8
- 229910052731 fluorine Inorganic materials 0.000 claims description 8
- 239000011737 fluorine Substances 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- BIVNKSDKIFWKFA-UHFFFAOYSA-N N-propan-2-yl-N-silylpropan-2-amine Chemical compound CC(C)N([SiH3])C(C)C BIVNKSDKIFWKFA-UHFFFAOYSA-N 0.000 claims description 7
- 238000000861 blow drying Methods 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 5
- 239000001301 oxygen Substances 0.000 claims description 5
- 229910052760 oxygen Inorganic materials 0.000 claims description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 5
- 239000010703 silicon Substances 0.000 claims description 5
- 230000001351 cycling effect Effects 0.000 claims description 4
- 239000012528 membrane Substances 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- VWJYWUZXVWYSPL-UHFFFAOYSA-N 2-[amino(propan-2-yl)silyl]propane Chemical compound CC(C)[SiH](N)C(C)C VWJYWUZXVWYSPL-UHFFFAOYSA-N 0.000 claims 1
- 239000006096 absorbing agent Substances 0.000 claims 1
- 239000010410 layer Substances 0.000 description 125
- 239000000243 solution Substances 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 10
- 230000001788 irregular Effects 0.000 description 10
- 239000002070 nanowire Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
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- 239000000463 material Substances 0.000 description 4
- 238000007747 plating Methods 0.000 description 4
- 238000000985 reflectance spectrum Methods 0.000 description 4
- BWFPGXWASODCHM-UHFFFAOYSA-N copper monosulfide Chemical compound [Cu]=S BWFPGXWASODCHM-UHFFFAOYSA-N 0.000 description 3
- QWDJLDTYWNBUKE-UHFFFAOYSA-L magnesium bicarbonate Chemical compound [Mg+2].OC([O-])=O.OC([O-])=O QWDJLDTYWNBUKE-UHFFFAOYSA-L 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 239000003973 paint Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 2
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- JRKICGRDRMAZLK-UHFFFAOYSA-L persulfate group Chemical group S(=O)(=O)([O-])OOS(=O)(=O)[O-] JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 241001391944 Commicarpus scandens Species 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000011358 absorbing material Substances 0.000 description 1
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- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
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- 239000002086 nanomaterial Substances 0.000 description 1
- 229940082569 selenite Drugs 0.000 description 1
- MCAHWIHFGHIESP-UHFFFAOYSA-L selenite(2-) Chemical compound [O-][Se]([O-])=O MCAHWIHFGHIESP-UHFFFAOYSA-L 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
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- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention relates to a composite film with ultralow reflectivity, a preparation method and application thereof. The composite film is specially used for precise copper product parts, has high binding force and has the reflectivity of less than 0.3 percent in the wavelength range of 400-800 nm.
Description
Technical Field
The invention relates to the technical field of metal blackening treatment, in particular to a composite film with ultralow reflectivity, and a preparation method and application thereof.
Background
Copper has a large amount of storage on the earth, and has excellent electric and heat conductivity, so that the copper has wider application. In some critical parts of instruments, it is often necessary to blacken the copper surface to increase its ability to absorb light and heat. The oxidation blackening of the surface of a copper workpiece is a method commonly used in the treatment of chemical conversion films of copper. There are many kinds of blackening oxidants concerning copper, and persulfates and selenites are oxidants that are frequently used in the prior art. However, persulfate has poor stability, and a film layer is loose after blackening and is easy to fall off; selenite is toxic and causes environmental pollution. In the application of oxidation blackening, after the brass optical workpiece is blackened, high requirements such as blackness, matte, low reflectivity and the like are often met; meanwhile, the blackening difficulty is increased due to the existence of zinc in the brass.
It is also practical to spray light absorbing materials on copper surfaces, such as black paint. The black paint is composed of organic matters, and starts to decompose and fade at the temperature of more than 400 ℃. In the case of severe vacuum degassing, about 10% of its own weight is evolved, and some of the evolved gases are strongly corrosive, are liable to corrode other parts, and the black paint layer is liable to crack and fall off during repeated cold and hot cycles. Therefore, a new blackening process is developed, the binding force is improved, the blackening effect is improved, and the meaning is great.
Disclosure of Invention
In view of the above, the main object of the present invention is to provide a composite film with ultra-low reflectivity, and a preparation method and application thereof, wherein the composite film is specially used for precise copper workpieces, has high binding force, and has a reflectivity of less than 0.3% in a wavelength range of 400-800 nm; after the treatment by the method, the surface of the copper workpiece is uniform and fine, and the blackened film has high firmness.
The aim and the technical problems of the invention are realized by adopting the following technical proposal. The invention provides a composite film with ultralow reflectivity, which comprises an absorption layer and a light matching layer which are sequentially and alternately arranged on a copper substrate.
Preferably, the composite film with ultralow reflectivity is the composite film with ultralow reflectivity, wherein the absorption layer is a copper sulfide layer; the light matching layer is a magnesium fluoride layer or a silicon oxide layer.
Preferably, the aforementioned composite film having ultra-low reflectivity, wherein the number of the alternating arrangement is at least three.
Preferably, the aforementioned composite film having ultra-low reflectivity, wherein the number of times of the alternating arrangement is three; the film system structure of the composite film is as follows: the first copper sulfide layer I, the first magnesium fluoride layer I, the second copper sulfide layer I, the second magnesium fluoride layer I, the third copper sulfide layer I and the third magnesium fluoride layer, and the thicknesses of the layers are 150-250nm,10-30nm,20-40nm,30-50nm,10-30nm and 50-150nm in sequence.
Preferably, the aforementioned composite film having ultra-low reflectivity, wherein a plurality of copper nanowires are formed in the composite film, and the size thereof is 0.5-10 μm.
The aim and the technical problems of the invention are realized by adopting the following technical proposal. The invention provides a preparation method of a composite film with ultralow reflectivity, which comprises the following steps: and depositing an absorption layer and a light matching layer on the copper substrate alternately in turn.
Preferably, the method for preparing the composite film with ultralow reflectivity comprises the following steps:
1) Soaking copper substrate in NaOH and (NH) 4 ) 2 SO 4 Cleaning and drying the mixture in the mixed solution;
2) Depositing copper sulfide on the surface of a copper substrate to obtain an absorption layer; then depositing magnesium fluoride or silicon oxide on the surface of the absorption layer to obtain a light matching layer; and cycling for multiple times to obtain the composite membrane.
Preferably, the method for preparing the composite film with ultralow reflectivity comprises the following steps:
1) Immersing the cleaned and dried copper substrateSoaking in NaOH and (NH) 4 ) 2 SO 4 After soaking for 60s-180s, taking out the copper substrate, cleaning and drying;
2) Depositing copper sulfide on the surface of a copper substrate: bis (2, 6-tetramethyl-3, 5-pimelic acid) copper is used as a solid copper source, the heating temperature of the solid copper source is 130 ℃, hydrogen sulfide is used as a sulfur source, and a copper sulfide layer is obtained through reaction, wherein the reaction temperature is 120-400 ℃; and then depositing magnesium fluoride or silicon oxide on the surface of the copper sulfide layer: bis (2, 6-tetramethyl-3, 5-heptanedioic acid) magnesium is used as a solid magnesium source, hydrogen fluoride is used as a fluorine source, the heating temperature of the solid magnesium source is 100 ℃, the reaction temperature is 120-400 ℃, and the magnesium fluoride layer is obtained through the reaction; diisopropylaminosilane is used as a silicon source, ozone is used as an oxygen source, the reaction temperature is 300-400 ℃, and a silicon oxide layer is obtained through the reaction; and cycling for multiple times to obtain the composite membrane.
Preferably, in the aforementioned method for producing a composite film having ultra-low reflectance, in step 1), the NaOH and (NH 4 ) 2 SO 4 In the mixed solution of (2), the concentration of NaOH is 0.75mol/L, (NH) 4 ) 2 SO 4 The concentration of (C) was 0.03mol/L.
Preferably, in the method for preparing a composite film with ultra-low reflectivity, in the step 1), the cleaning includes sequentially ultrasonic cleaning with absolute ethanol and deionized water for 10-20min; and the drying or blow-drying is carried out by adopting high-purity nitrogen for 30-60s.
Preferably, in the aforementioned method for preparing a composite film having ultra-low reflectivity, in step 2), the number of cycles is at least three.
Preferably, in the aforementioned method for producing a composite film having ultra-low reflectance, wherein in step 2), the growth process per cycle comprises 0.5 to 2s of bis (2, 6-tetramethyl-3, 5-pimelic acid) copper pulse, 10 to 120sN 2 (g) Purging, 0.2-1s hydrogen sulfide pulse and 10-120s N 2 (g) Purging; the growth process of each cycle comprises 0.5-2s of magnesium pulse of bis (2, 6, -tetramethyl-3, 5-heptanedioic acid), 10-120s N 2 (g) Purging, 0.2-1s hydrogen fluoride pulse and 10-120s N 2 (g) And (5) purging. The growth process of each cycle comprises 0.2-1s of diisoPropylamino) silane pulse, 10-120s N 2 (g) Purging, 0.5-2s ozone pulse and 10-120s N 2 (g) And (5) purging.
Preferably, in the method for preparing a composite film with ultra-low reflectivity, in step 2), the method of alternate deposition is an atomic layer deposition method.
The aim and the technical problems of the invention are realized by adopting the following technical proposal. The invention provides a copper component, which sequentially comprises a substrate, and an absorption layer and a light matching layer which are alternately arranged from inside to outside.
Preferably, the foregoing copper component, wherein the absorbing layer is a copper sulfide layer; the light matching layer is a magnesium fluoride layer.
Preferably, in the foregoing copper component, wherein the substrate is a brass component.
Preferably, the foregoing copper component, wherein the number of alternating is at least three.
By means of the technical scheme, the composite film with the ultralow reflectivity, the preparation method and the application thereof have at least the following advantages:
1. the method is simple and quick, is particularly suitable for samples with complex 3D structures such as copper lens barrels and brass sheets, forms a light trapping surface through a large number of micro-structures such as micro-pits of the micro-nano structure, and the length of the nanowire is 0.5-10 mu m, so that light rays are incident and then reflected and absorbed for multiple times, and only a small amount of light rays are emitted, so that the reflectivity of the samples is reduced from 10% to below 0.3%;
2. the invention adopts copper sulfide as an absorption layer, and the expansion coefficients of the copper substrate and the copper sulfide are similar, so that the binding force between the film and the substrate is improved;
3. the preparation method combines an atomic layer deposition technology with a simple chemical solution method, has the advantages of strong repeatability, high yield, high preparation efficiency, suitability for large-scale preparation and the like compared with the traditional preparation method, and is particularly suitable for being applied to the optical field.
The foregoing description is only an overview of the present invention, and is intended to provide a more thorough understanding of the present invention, and is to be accorded the full scope of the present invention.
Drawings
FIG. 1 is a surface view of an untreated brass sheet of comparative example 1 of the present invention;
FIG. 2 is a surface view of a brass sheet treated with a solution in examples 1-4 of the present invention;
FIG. 3 is a surface view of a composite film with ultra-low reflectivity according to example 1 of the present invention;
FIG. 4 is a schematic structural diagram of a composite film with ultra-low reflectivity according to example 1 of the present invention;
FIG. 5 is a graph showing the comparison of reflectance spectra of the samples of comparative example 1 before and after coating with the solutions of example 1;
FIG. 6 is a graph showing the comparison of reflectance spectra of samples coated with the solutions of examples 2-4 of the present invention.
Detailed Description
In order to further describe the technical means and effects adopted by the present invention to achieve the preset purpose, the following description is provided with a composite film with ultra-low reflectivity, a preparation method thereof, a specific implementation mode, a structure, characteristics and effects thereof according to the present invention by combining with the preferred embodiment. In the following description, different "an embodiment" or "an embodiment" do not necessarily refer to the same embodiment. Furthermore, the particular features, structures, or characteristics of one or more embodiments may be combined in any suitable manner.
The following materials or reagents, unless otherwise specified, are all commercially available.
According to some embodiments of the present invention there is provided a composite film having ultra-low reflectivity comprising absorbing layers and light matching layers alternately disposed in sequence on a copper substrate. The film system structure refers to a structure of an antireflection film, and is formed by alternately stacking at least two film layers with high and low refractive indexes: wherein the high refractive index film layer is made of a material with absorption in the wave band of 400-800nm, namely, the extinction coefficient k is more than 0, and the material is used as an absorption layer; the low refractive index film layer is made of a material which is not absorbed by light in the wave band of 400-800nm and is used as a light matching layer. The absorption layer is selected as a copper sulfide layer in consideration of the difference in expansion coefficients of the copper substrate and the absorption film; the light matching layer is selected to be a magnesium fluoride layer or a silicon oxide layer for matching the copper sulfide optical constant (refractive index).
In the above technical solution, the number of times of the alternating arrangement is at least three. If less than three times, the reflectivity of the composite film does not reach the target value, and considering too many times, the process is complicated, alternatively, the number of times of the alternate arrangement may be three times.
In practice, films of different thickness and samples have different reflectivities. The reflectivity of the sample can be adjusted by adjusting the thickness. For this reason, the number of times of the alternate arrangement is three times; the film system structure of the composite film can be set as follows: the first copper sulfide layer (150-250 nm) | the first magnesium fluoride layer (10-30 nm) | the second copper sulfide layer (20-40 nm) | the second magnesium fluoride layer (30-50 nm) | the third copper sulfide layer (10-30 nm) | the third magnesium fluoride layer 6 (50-150 nm). The composite film has a plurality of irregular copper nanowires formed therein, the size of which is 0.5-10 μm. The reflectance of the composite film is 0.18% -0.29% between 400-800 nm. If the size of the copper nanowire is smaller than 0.5 μm, the reflectivity is high due to the too small size; if the size of the copper nanowire is larger than 10 mu m, the nanowire is easy to break due to the fact that the size is too large, so that the mechanical property is poor; therefore, the size of the copper nanowire should be controlled between 0.5 and 10 μm.
Further preferably, as shown in fig. 4, the composite film has a film structure as follows: first copper sulfide layer 1 (200 nm) | first magnesium fluoride layer 2 (20 nm) | second copper sulfide layer 3 (30 nm) | second magnesium fluoride layer 4 (40 nm) | third copper sulfide layer 5 (15 nm) | third magnesium fluoride layer 6 (100 nm). The morphology of the composite film is shown in fig. 3, and as can be seen from fig. 3, a plurality of irregular copper nanowires with a size of 6 μm are formed in the composite film. Through the test, the reflectance of the composite film at a wavelength of 400-800nm is preferably the lowest, and is 0.18%.
Furthermore, the copper substrate is selected to be a brass component, such as brass sheet, having dimensions of 30mmx30mmx2mm; other copper components, such as copper barrels, etc., are also possible.
The above composite film having ultra-low reflectivity refers to a composite film having a reflectivity of less than 0.3%, for example, between 0.18% and 0.29%, at a wavelength of 400-800 nm.
There is also provided in accordance with some embodiments of the present invention a method of preparing a composite film having ultra-low reflectivity, comprising the steps of: and depositing an absorption layer and a light matching layer on the copper substrate alternately in turn.
In some embodiments, optionally, wherein the method comprises the steps of:
1) Soaking the cleaned and dried copper substrate in NaOH and (NH) 4 ) 2 SO 4 After soaking for 60s-180s, taking out the copper substrate, cleaning and drying; in particular, the NaOH and (NH 4 ) 2 SO 4 In the mixed solution of (2), the concentration of NaOH is 0.75mol/L, (NH) 4 ) 2 SO 4 The concentration of (C) was 0.03mol/L. Soaking copper substrate in NaOH and (NH) 4 ) 2 SO 4 In order to reduce the reflectivity of the copper substrate. The cleaning comprises the steps of sequentially carrying out ultrasonic cleaning for 10-20min by using absolute ethyl alcohol and deionized water; the drying or blow-drying is carried out by adopting high-purity nitrogen (the purity is 99.99%) to blow-dry for 30-60s. NaOH and (NH) 4 ) 2 SO 4 The concentration of (2) is fixed, and the reflectivity of the copper substrate is indirectly influenced only by changing the structure of the surface of the copper substrate through adjusting the soaking time.
2) Depositing copper sulfide on the surface of a copper substrate: setting the reaction temperature to be 120-400 ℃, taking bis (2, 6-tetramethyl-3, 5-pimelic acid) copper as a solid copper source, heating the solid copper source to be 130 ℃, taking hydrogen sulfide as a sulfur source, and reacting the solid copper source with the sulfur source to obtain a copper sulfide layer; and then depositing magnesium fluoride or silicon oxide on the surface of the copper sulfide layer: setting the reaction temperature to be 120-400 ℃, taking bis (2, 6-tetramethyl-3, 5-heptanedioic acid) magnesium as a solid magnesium source, taking hydrogen fluoride as a fluorine source, and reacting the solid magnesium source and the fluorine source to obtain the magnesium fluoride layer, wherein the heating temperature of the solid magnesium source is 100 ℃. Setting the reaction temperature to 300-400 ℃, taking (diisopropylamino) silane as a silicon source, taking ozone as an oxygen source, and reacting the silicon source with the oxygen source to obtain the silicon oxide layer. The number of cyclical depositions is set to at least three. The copper sulfide layer and the magnesium fluoride layer with target thickness can be obtained by controlling the precipitation speed and the precipitation cycle number.
In step 2) of the above preparation method, the growth process of each cycle comprises 0.5-2s of copper pulses of bis (2, 6-tetramethyl-3, 5-heptanedioic acid), 10-120sN 2 (g) Purging, 0.2-1s hydrogen sulfide pulse and 10-120s N 2 (g) Purging; the growth process of each cycle comprises 0.5-2s of magnesium pulse of bis (2, 6, -tetramethyl-3, 5-heptanedioic acid), 10-120s N 2 (g) Purging, 0.2-1s hydrogen fluoride pulse and 10-120s N 2 (g) And (5) purging. The growth process of each cycle comprises 0.2-1s diisopropylamino silane pulse, 10-120sN 2 (g) Purging, 0.5-2s ozone pulse and 10-120s N 2 (g) And (5) purging. Thus, by changing the pulse time, the purpose of changing the thickness of the single-layer film can be achieved.
In step 2) of the above preparation method, in step 2), the alternate deposition method is selected as an atomic layer deposition method.
There is also provided, in accordance with some embodiments of the present invention, a copper component that is a substrate in sequence from the inside to the outside, and an absorption layer and a light matching layer that are alternately arranged; the absorption layer is a copper sulfide layer; the light matching layer is a magnesium fluoride layer or a silicon oxide layer; the number of alternating settings is at least three.
In practice, the substrate is chosen to be a brass component, such as brass sheet, having dimensions of 30mmx30mmx2mm; other copper components, such as copper barrels, etc., are also possible.
The invention is further illustrated below with reference to specific examples.
Example 1
As shown in fig. 4, the film system structure of this embodiment is: the morphology of the first copper sulfide layer 1 (200 nm) | the first magnesium fluoride layer 2 (20 nm) | the second copper sulfide layer 3 (30 nm) | the second magnesium fluoride layer 4 (40 nm) | the third copper sulfide layer 5 (15 nm) | the third magnesium fluoride layer 6 (100 nm) is shown in fig. 3. As can be seen from fig. 3, a plurality of random copper nanowires having a size of 6 μm are formed in the composite film.
The embodiment provides a preparation method of a composite film with ultralow reflectivity, which comprises the following steps:
(1) Compounding NaOH and (NH) 4 ) 2 SO 4 The concentration of NaOH in the mixed solution is 0.75mol/L, (NH) 4 ) 2 SO 4 The concentration of (2) is 0.03mol/L;
(2) Taking the cleaned and dried brass sheet (30 mmx30mmx2mm, the surface of the sample is smooth, the appearance of the sample is shown in figure 1) as a substrate, soaking the brass sheet in the mixed solution for 100s, taking out the brass sheet after soaking, cleaning, and drying by adopting high-purity nitrogen, wherein the appearance of the brass sheet obtained by drying is shown in figure 2. As can be seen from fig. 2, a plurality of irregular copper nanowires having a size of 6 μm are formed in the composite film; the cleaning comprises the steps of sequentially carrying out ultrasonic cleaning for 15min by using absolute ethyl alcohol and deionized water, and drying or blow-drying by adopting high-purity nitrogen with the purity of 99.99 percent for 45 s.
(3) Putting the dried brass sheet into a reaction cavity of an atomic layer deposition film system, preparing a copper sulfide layer by adopting an atomic layer deposition method, wherein the set reaction temperature is 300 ℃, bis (2, 6-tetramethyl-3, 5-pimelic acid) copper is selected as a solid copper source, hydrogen sulfide is selected as a sulfur source, and the heating temperature of the solid copper source is set to be 130 ℃; then, a magnesium fluoride layer was prepared, wherein the reaction temperature was set at 300 ℃, bis (2, 6, -tetramethyl-3, 5-heptanedionato) magnesium was selected as a solid magnesium source, hydrogen fluoride was used as a fluorine source, and the heating temperature of the solid magnesium source was set at 100 ℃. And (3) alternately preparing 6 layers of films to obtain the composite film with ultralow reflectivity, namely obtaining the brass sheet product with the composite film.
In step 3) of the above preparation method, the growth process of each cycle comprises 1s of copper pulse of bis (2, 6-tetramethyl-3, 5-pimelic acid), 70sN 2 (g) Purging, 0.6s hydrogen sulfide pulse and 70s N2 (g) purging; the growth process per cycle included 1.2s pulses of magnesium bis (2, 6, -tetramethyl-3, 5-heptanedionate), 70s N 2 (g) Purge, 0.6s pulse of hydrogen fluoride and 70s N 2 (g) And (5) purging. The growth process for each cycle included a 0.6s diisopropylaminosilane pulse, 70s N2 (g) purge, 1.2s ozonePulse sum 70s N 2 (g) And (5) purging.
The brass sheet product obtained above was tested by a spectrophotometer, and the reflectance of the brass sheet product was tested to be 0.18% at a wavelength of 400-800nm, see fig. 5.
Example 2
The film system structure of this embodiment is: a first copper sulfide layer (200 nm) | a first silicon oxide layer (20 nm) | a second copper sulfide layer (30 nm) | a second silicon oxide layer (40 nm) | a third copper sulfide layer (15 nm) | a third silicon oxide layer (100 nm); the morphology of the composite film of this example was similar to that of the composite film of example 1. The composite film has a plurality of irregular copper nanowires formed therein, which have a size of 6 μm.
The embodiment provides a preparation method of a composite film with ultralow reflectivity, which comprises the following steps:
(1) Compounding NaOH and (NH) 4 ) 2 SO 4 The concentration of NaOH in the mixed solution is 0.75mol/L, (NH) 4 ) 2 SO 4 The concentration of (2) is 0.03mol/L;
(2) Taking the cleaned and dried brass sheet (30 mmx30mmx2mm, the surface of the sample is smooth, the appearance of the sample is shown in figure 1) as a substrate, soaking the brass sheet in the mixed solution for 100s, taking out the brass sheet after soaking, cleaning, and drying by adopting high-purity nitrogen, wherein the appearance of the brass sheet obtained by drying is shown in figure 2. As can be seen from fig. 2, a plurality of irregular copper nanowires having a size of 6 μm are formed in the composite film; the cleaning comprises the steps of sequentially carrying out ultrasonic cleaning for 15min by using absolute ethyl alcohol and deionized water, and drying or blow-drying by adopting high-purity nitrogen with the purity of 99.99 percent for 45 s.
(3) Putting the dried brass sheet into a reaction cavity of an atomic layer deposition film system, preparing a copper sulfide layer by adopting an atomic layer deposition method, wherein the set reaction temperature is 300 ℃, bis (2, 6-tetramethyl-3, 5-pimelic acid) copper is selected as a solid copper source, hydrogen sulfide is selected as a sulfur source, and the heating temperature of the solid copper source is set to be 130 ℃; and then preparing a silicon oxide layer, wherein the reaction temperature is set to 300 ℃, diisopropylaminosilane is used as a silicon source, ozone is used as an oxygen source, and the silicon oxide is obtained through reaction. And (3) alternately preparing 6 layers of films to obtain the composite film with ultralow reflectivity, namely obtaining the brass sheet product with the composite film.
In step 3) of the above preparation method, the growth process of each cycle comprises 1s of copper pulse of bis (2, 6-tetramethyl-3, 5-pimelic acid), 70sN 2 (g) Purging, 0.6s hydrogen sulfide pulse and 70s N2 (g) purging; the growth process for each cycle included a 0.6s diisopropylaminosilane pulse, 70s N2 (g) purge, 1.2s ozone pulse and 70s N 2 (g) And (5) purging.
The brass sheet product obtained above was tested by a spectrophotometer, and the reflectance of the brass sheet product was tested to be 0.29% at a wavelength of 400-800nm, see fig. 6.
Example 3
The film system structure of this embodiment is: first copper sulfide layer 1 (250 nm) | first magnesium fluoride layer 2 (20 nm) | second copper sulfide layer 3 (40 nm) | second magnesium fluoride layer 4 (40 nm) | third copper sulfide layer 5 (30 nm) | third magnesium fluoride layer 6 (100 nm). The morphology of the composite film of this example was similar to that of the composite film of example 1. The composite film has a plurality of irregular copper nanowires formed therein, which have a size of 6 μm.
The embodiment provides a preparation method of a composite film with ultralow reflectivity, which comprises the following steps:
(1) Compounding NaOH and (NH) 4 ) 2 SO 4 The concentration of NaOH in the mixed solution is 0.75mol/L, (NH) 4 ) 2 SO 4 The concentration of (2) is 0.03mol/L;
(2) Taking the cleaned and dried brass sheet (30 mmx30mmx2mm, the surface of the sample is smooth, the appearance of the sample is shown in figure 1) as a substrate, soaking the brass sheet in the mixed solution for 100s, taking out the brass sheet after soaking, cleaning, and drying by adopting high-purity nitrogen, wherein the appearance of the brass sheet obtained by drying is shown in figure 2. As can be seen from fig. 2, a plurality of irregular copper nanowires having a size of 6 μm are formed in the composite film; the cleaning comprises the steps of sequentially carrying out ultrasonic cleaning for 15min by using absolute ethyl alcohol and deionized water, and drying or blow-drying by adopting high-purity nitrogen with the purity of 99.99 percent for 45 s.
(3) Putting the dried brass sheet into a reaction cavity of an atomic layer deposition film system, preparing a copper sulfide layer by adopting an atomic layer deposition method, wherein the set reaction temperature is 300 ℃, bis (2, 6-tetramethyl-3, 5-pimelic acid) copper is selected as a solid copper source, hydrogen sulfide is selected as a sulfur source, and the heating temperature of the solid copper source is set to be 130 ℃; then, a magnesium fluoride layer was prepared, wherein the reaction temperature was set at 300 ℃, bis (2, 6, -tetramethyl-3, 5-heptanedionato) magnesium was selected as a solid magnesium source, hydrogen fluoride was used as a fluorine source, and the heating temperature of the solid magnesium source was set at 100 ℃. And (3) alternately preparing 6 layers of films to obtain the composite film with ultralow reflectivity, namely obtaining the brass sheet product with the composite film.
In step 3) of the above preparation method, the growth process of each cycle comprises a 2s bis (2, 6-tetramethyl-3, 5-heptanedioic acid) copper pulse of 120sN 2 (g) Purging, 1s hydrogen sulfide pulse and 70s N2 (g) purging; the growth process per cycle included 1.2s pulses of magnesium bis (2, 6, -tetramethyl-3, 5-heptanedionate), 70s N 2 (g) Purge, 0.6s pulse of hydrogen fluoride and 70s N 2 (g) And (5) purging.
The brass sheet product obtained above was tested by a spectrophotometer, and the reflectance of the brass sheet product in the wavelength range of 400-800nm was tested to be 0.23%, see fig. 6.
Example 4
The film system structure of this embodiment is: first copper sulfide layer 1 (200 nm) | first magnesium fluoride layer 2 (30 nm) | second copper sulfide layer 3 (30 nm) | second magnesium fluoride layer 4 (50 nm) | third copper sulfide layer 5 (15 nm) | third magnesium fluoride layer 6 (150 nm). The morphology of the composite film of this example was similar to that of the composite film of example 1. The composite film has a plurality of irregular copper nanowires formed therein, which have a size of 6 μm.
The embodiment provides a preparation method of a composite film with ultralow reflectivity, which comprises the following steps:
(1) Compounding NaOH and (NH) 4 ) 2 SO 4 The concentration of NaOH in the mixed solution is 0.75mol/L, (NH) 4 ) 2 SO 4 The concentration of (2) is 0.03mol/L;
(2) And taking the washed and dried brass sheet (30 mmx30mmx2mm, the surface of a sample is smooth, the appearance of the sample is shown in figure 1) as a substrate, soaking the brass sheet in the mixed solution for 100s, taking out the brass sheet after soaking, washing, and drying by adopting high-purity nitrogen with the purity of 99.99%, wherein the appearance of the brass sheet obtained by drying is shown in figure 2. As can be seen from fig. 2, a plurality of irregular copper nanowires having a size of 6 μm are formed in the composite film; the cleaning comprises the steps of sequentially carrying out ultrasonic cleaning for 15min by using absolute ethyl alcohol and deionized water, and drying or blow-drying by adopting high-purity nitrogen with the purity of 99.99 percent for 45 s.
(3) Putting the dried brass sheet into a reaction cavity of an atomic layer deposition film system, preparing a copper sulfide layer by adopting an atomic layer deposition method, wherein the set reaction temperature is 300 ℃, bis (2, 6-tetramethyl-3, 5-pimelic acid) copper is selected as a solid copper source, hydrogen sulfide is selected as a sulfur source, and the heating temperature of the solid copper source is set to be 130 ℃; then, a magnesium fluoride layer was prepared, wherein the reaction temperature was set at 300 ℃, bis (2, 6, -tetramethyl-3, 5-heptanedionato) magnesium was selected as a solid magnesium source, hydrogen fluoride was used as a fluorine source, and the heating temperature of the solid magnesium source was set at 100 ℃. And (3) alternately preparing 6 layers of films to obtain the composite film with ultralow reflectivity, namely obtaining the brass sheet product with the composite film.
In step 3) of the above preparation method, the growth process of each cycle comprises 1s of copper pulse of bis (2, 6-tetramethyl-3, 5-pimelic acid), 70sN 2 (g) Purging, 0.6s hydrogen sulfide pulse and 70s N2 (g) purging; the growth process of each cycle included 2s of magnesium pulses of bis (2, 6, -tetramethyl-3, 5-heptanedionate), 120s N 2 (g) Purge, 1s pulse of hydrogen fluoride and 120s N 2 (g) And (5) purging.
The brass sheet product obtained above was tested by a spectrophotometer, and the reflectance of the brass sheet product was tested to be 0.21% at a wavelength of 400-800nm, see fig. 6.
Comparative example 1
The film system structure of this comparative example is: first copper sulfide layer (200 nm) | first magnesium fluoride layer (20 nm) | second copper sulfide layer (30 nm) | second magnesium fluoride layer (40 nm)) Third copper sulfide layer (15 nm) third magnesium fluoride layer (100 nm). The brass sheet is not soaked with NaOH and (NH) 4 ) 2 SO 4 The morphology of the mixed solution is shown in figure 1.
The comparative example provides a method for preparing a composite film, comprising the following steps:
(1) Putting a brass sheet (30 mmx30mmx2 mm) dried by 45s with high-purity nitrogen with the purity of 99.99% into a reaction cavity of an atomic layer deposition film system, and preparing a copper sulfide layer by adopting an atomic layer deposition method, wherein the reaction temperature is set to 300 ℃, bis (2, 6-tetramethyl-3, 5-pimelic acid) copper is selected as a solid copper source, hydrogen sulfide is selected as a sulfur source, and the heating temperature of the solid copper source is set to 130 ℃; then, a magnesium fluoride layer was prepared, wherein the reaction temperature was set at 300 ℃, bis (2, 6, -tetramethyl-3, 5-heptanedionato) magnesium was selected as a solid magnesium source, hydrogen fluoride was used as a fluorine source, and the heating temperature of the solid magnesium source was set at 100 ℃. And (3) alternately preparing 6 layers of films to obtain the composite film with ultralow reflectivity, namely obtaining the brass sheet product with the composite film.
In step 3) of the above preparation method, the growth process of each cycle comprises 1s of copper pulse of bis (2, 6-tetramethyl-3, 5-pimelic acid), 70sN 2 (g) Purging, 0.6s hydrogen sulfide pulse and 70s N2 (g) purging; the growth process per cycle included 1.2s pulses of magnesium bis (2, 6, -tetramethyl-3, 5-heptanedionate), 70s N 2 (g) Purge, 0.6s pulse of hydrogen fluoride and 70s N 2 (g) And (5) purging.
The brass sheet product obtained above was tested by a spectrophotometer, and the reflectance of the brass sheet product was 1.8% at a wavelength of 400-800nm, see fig. 5.
The reflectance data for examples 1-4 and comparative example 1 are summarized in Table 1 below.
TABLE 1
As can be seen from Table 1, brass sheet samples having composite films according to examples 1 to 4 of the present inventionThe reflectance at a wavelength of 400-800nm was 0.18% -0.29%, whereas the brass sheet of comparative example 1 was not immersed in NaOH and (NH) 4 ) 2 SO 4 The reflectance of the brass sheet sample with composite film obtained in comparative example 1 at a wavelength of 400-800nm was 1.8%, which is explained by: the thicknesses were different and the reflectivities of the samples were different. By adjusting the sample thickness of the different layers, the reflectance of the brass sheet article can be adjusted.
A part of the incident light enters the third copper sulphide layer 5 via the third magnesium fluoride layer 6 and a part is absorbed during the passage through the third copper sulphide layer 3. The unabsorbed portion continues to be incident downward and after passing through the second magnesium fluoride layer 4 enters the second copper sulfide 3 where it continues to be absorbed. Light that has not yet been absorbed continues to enter downwards through the first magnesium fluoride layer 2 and enters the first copper sulphide layer 1 where it is absorbed. In general, light entering the composite film is continually absorbed between the layers by the absorbing layer, with the remainder being absorbed for the most part, except for a minority which is reflected off the composite film.
FIG. 5 is a graph showing the reflectance spectrum of brass sheets before and after treatment with the treatment solution and before and after coating. FIG. 6 is a graph showing the comparison of reflectance spectra of samples coated with the solutions of examples 2-4 of the present invention. As can be seen from fig. 5, the reflectance before the brass sheet plating of the non-immersed solution was 15%, the reflectance before the brass sheet plating of the immersed solution was 5%, the reflectance after the brass sheet plating of the non-immersed solution (comparative example 1) was 1.8%, and the reflectance after the brass sheet plating of the immersed solution (example 1) was 0.18%. As can be seen from FIG. 5, the reflectance after the brass sheets were coated with the immersion solutions of examples 2, 3 and 4 were 0.29%, 0.23% and 0.21% in this order, which are lower than that of comparative example 1. The surface of the brass sheet which is not soaked in the solution is smooth. For an object with a smooth and flat surface, such as a brass sheet without soaking solution, light can be reflected and absorbed once when entering the surface of the brass sheet, and the absorption effect of the brass sheet is still relatively limited even after the brass sheet surface is plated with a light absorption film. The surface of the brass sheet is treated by the soaking solution, and a micro-uneven structure (copper nanowire) is formed on the surface of the brass sheet, so that a plurality of irregular copper nanowires with the size of 6 μm are formed in the finally obtained composite film. When the light irradiates the surface of the micro uneven structure, multiple reflection and absorption can occur, so that the light escaping from the surface of the brass sheet is further reduced, the absorption effect is improved, and the reflectivity of the brass sheet is reduced.
In the foregoing embodiments, the descriptions of the embodiments are emphasized, and for parts of one embodiment that are not described in detail, reference may be made to related descriptions of other embodiments.
The numerical ranges recited herein include all numbers within the range and include any two of the range values within the range. The different values of the same index appearing in all embodiments of the invention can be combined arbitrarily to form a range value.
The technical features of the claims and/or the description of the present invention may be combined in a manner not limited to the combination of the claims by the relation of reference. The technical scheme obtained by combining the technical features in the claims and/or the specification is also the protection scope of the invention.
The above description is only of the preferred embodiments of the present invention, and is not intended to limit the present invention in any way, but any simple modification, equivalent variation and modification made to the above embodiments according to the technical substance of the present invention still fall within the scope of the technical solution of the present invention.
Claims (10)
1. A composite film with ultra-low reflectivity is characterized by comprising an absorption layer and a light matching layer which are sequentially and alternately arranged on a copper substrate.
2. The composite film with ultra-low reflectivity as defined in claim 1, wherein said absorbing layer is a copper sulfide layer; the light matching layer is a magnesium fluoride layer or a silicon oxide layer; the number of alternating settings is at least three.
3. The composite film having ultra-low reflectivity as defined in claim 1, wherein said alternating number of times is three; the film system structure of the composite film is as follows: the first copper sulfide layer I, the first magnesium fluoride layer I, the second copper sulfide layer I, the second magnesium fluoride layer I, the third copper sulfide layer I and the third magnesium fluoride layer, and the thicknesses of the layers are 150-250nm,10-30nm,20-40nm,30-50nm,10-30nm and 50-150nm in sequence; the composite film has a plurality of copper nanowires formed therein, which have a size of 0.5-10 μm.
4. A method for preparing a composite film with ultra-low reflectivity, comprising the steps of: and depositing an absorption layer and a light matching layer on the copper substrate alternately in turn.
5. The method for preparing a composite film having ultra-low reflectivity as claimed in claim 4, comprising the steps of:
1) Soaking copper substrate in NaOH and (NH) 4 ) 2 SO 4 Cleaning and drying the mixture in the mixed solution;
2) Depositing copper sulfide on the surface of a copper substrate to obtain an absorption layer; then depositing magnesium fluoride or silicon oxide on the surface of the absorption layer to obtain a light matching layer; and cycling for multiple times to obtain the composite membrane.
6. The method for preparing a composite film having ultra-low reflectivity as claimed in claim 5, comprising the steps of:
1) Soaking the cleaned and dried copper substrate in NaOH and (NH) 4 ) 2 SO 4 After soaking for 60s-180s, taking out the copper substrate, cleaning and drying;
2) Depositing copper sulfide on the surface of a copper substrate: bis (2, 6-tetramethyl-3, 5-pimelic acid) copper is used as a solid copper source, the heating temperature of the solid copper source is 130 ℃, hydrogen sulfide is used as a sulfur source, the reaction temperature is 120-400 ℃, and a copper sulfide layer is obtained through reaction; and then depositing magnesium fluoride or silicon oxide on the surface of the copper sulfide layer: bis (2, 6-tetramethyl-3, 5-heptanedioic acid) magnesium is used as a solid magnesium source, hydrogen fluoride is used as a fluorine source, the heating temperature of the solid magnesium source is 100 ℃, the reaction temperature is 120-400 ℃, and the magnesium fluoride layer is obtained through the reaction; or diisopropyl aminosilane is used as a silicon source, ozone is used as an oxygen source, the reaction temperature is 300-400 ℃, and the silicon oxide layer is obtained by reaction; and cycling for multiple times to obtain the composite membrane.
7. The method for producing a composite film having ultra-low reflectivity as claimed in claim 5 or 6, wherein in step 1), said NaOH and (NH 4 ) 2 SO 4 In the mixed solution of (2), the concentration of NaOH is 0.75mol/L, (NH) 4 ) 2 SO 4 The concentration of (2) is 0.03mol/L; the cleaning comprises the steps of sequentially carrying out ultrasonic cleaning for 10-20min by using absolute ethyl alcohol and deionized water; and the drying or blow-drying is carried out by adopting high-purity nitrogen for 30-60s.
8. The method of producing a composite film having ultra-low reflectivity as claimed in claim 5 or 6, wherein in step 2), the number of cycles is at least three; the growth process of each cycle comprises 0.5-2s of copper pulse of di (2, 6-tetramethyl-3, 5-pimelic acid) and 10-120sN 2 (g) Purging, 0.2-1s hydrogen sulfide pulse and 10-120s N 2 (g) Purging; the growth process of each cycle comprises 0.5-2s of magnesium pulse of bis (2, 6, -tetramethyl-3, 5-heptanedioic acid), 10-120s N 2 (g) Purging, 0.2-1s hydrogen fluoride pulse and 10-120s N 2 (g) And (5) purging. The growth process of each cycle comprises 0.2-1s diisopropylamino silane pulse, 10-120s N 2 (g) Purging, 0.5-2s ozone pulse and 10-120s N 2 (g) Purging; the alternating deposition method is an atomic layer deposition method.
9. A copper component, characterized in that the copper component is a substrate, and an absorption layer and a light matching layer are alternately arranged from inside to outside.
10. The copper component of claim 9, wherein the absorber layer is a copper sulfide layer; the light matching layer is a magnesium fluoride layer or a silicon oxide layer; the substrate is a brass component; the number of alternating settings is at least three.
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