CN114210992B - Gold micro-nano pine needle composite structure and preparation method thereof - Google Patents
Gold micro-nano pine needle composite structure and preparation method thereof Download PDFInfo
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- CN114210992B CN114210992B CN202111548688.3A CN202111548688A CN114210992B CN 114210992 B CN114210992 B CN 114210992B CN 202111548688 A CN202111548688 A CN 202111548688A CN 114210992 B CN114210992 B CN 114210992B
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- 229910052737 gold Inorganic materials 0.000 title claims abstract description 53
- 239000010931 gold Substances 0.000 title claims abstract description 53
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 239000002131 composite material Substances 0.000 title claims abstract description 43
- 235000008331 Pinus X rigitaeda Nutrition 0.000 title claims abstract description 37
- 235000011613 Pinus brutia Nutrition 0.000 title claims abstract description 37
- 241000018646 Pinus brutia Species 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000002086 nanomaterial Substances 0.000 claims abstract description 36
- 239000000243 solution Substances 0.000 claims abstract description 28
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000011259 mixed solution Substances 0.000 claims abstract description 10
- 239000002253 acid Substances 0.000 claims abstract description 9
- 239000004323 potassium nitrate Substances 0.000 claims abstract description 8
- 239000000126 substance Substances 0.000 claims abstract description 8
- 235000010333 potassium nitrate Nutrition 0.000 claims abstract description 7
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 5
- 239000010703 silicon Substances 0.000 claims abstract description 5
- 239000000758 substrate Substances 0.000 claims abstract description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000007605 air drying Methods 0.000 claims abstract description 4
- 230000001678 irradiating effect Effects 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 230000008859 change Effects 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 17
- 238000012545 processing Methods 0.000 claims description 16
- SHMVRUMGFMGYGG-UHFFFAOYSA-N [Mo].S=O Chemical compound [Mo].S=O SHMVRUMGFMGYGG-UHFFFAOYSA-N 0.000 claims description 13
- IJZPACDOFYWLKH-UHFFFAOYSA-N sulfinyltungsten Chemical compound O=S=[W] IJZPACDOFYWLKH-UHFFFAOYSA-N 0.000 claims description 9
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims description 7
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims description 6
- ITRNXVSDJBHYNJ-UHFFFAOYSA-N tungsten disulfide Chemical compound S=[W]=S ITRNXVSDJBHYNJ-UHFFFAOYSA-N 0.000 claims description 4
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 3
- 230000002776 aggregation Effects 0.000 claims description 2
- 238000004220 aggregation Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 239000002105 nanoparticle Substances 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- -1 transition metal sulfide Chemical class 0.000 abstract description 15
- 229910052723 transition metal Inorganic materials 0.000 abstract description 14
- 230000000694 effects Effects 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 5
- 230000006872 improvement Effects 0.000 abstract description 2
- 238000005286 illumination Methods 0.000 description 11
- 239000004065 semiconductor Substances 0.000 description 10
- 238000003384 imaging method Methods 0.000 description 9
- 238000013519 translation Methods 0.000 description 8
- 230000002238 attenuated effect Effects 0.000 description 5
- 238000004416 surface enhanced Raman spectroscopy Methods 0.000 description 5
- 238000004299 exfoliation Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 239000003638 chemical reducing agent Substances 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- TXKMVPPZCYKFAC-UHFFFAOYSA-N disulfur monoxide Inorganic materials O=S=S TXKMVPPZCYKFAC-UHFFFAOYSA-N 0.000 description 2
- 230000002687 intercalation Effects 0.000 description 2
- 238000009830 intercalation Methods 0.000 description 2
- 238000001208 nuclear magnetic resonance pulse sequence Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 238000012984 biological imaging Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- VYXSBFYARXAAKO-WTKGSRSZSA-N chembl402140 Chemical compound Cl.C1=2C=C(C)C(NCC)=CC=2OC2=C\C(=N/CC)C(C)=CC2=C1C1=CC=CC=C1C(=O)OCC VYXSBFYARXAAKO-WTKGSRSZSA-N 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000012377 drug delivery Methods 0.000 description 1
- 230000005672 electromagnetic field Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000007626 photothermal therapy Methods 0.000 description 1
- 238000011197 physicochemical method Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- XTQHKBHJIVJGKJ-UHFFFAOYSA-N sulfur monoxide Chemical compound S=O XTQHKBHJIVJGKJ-UHFFFAOYSA-N 0.000 description 1
- 229910052815 sulfur oxide Inorganic materials 0.000 description 1
- 238000002198 surface plasmon resonance spectroscopy Methods 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
-
- 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
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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
- B82Y40/00—Manufacture or treatment of nanostructures
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- Crystallography & Structural Chemistry (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Manufacturing & Machinery (AREA)
- Composite Materials (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Laser Beam Processing (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention discloses a preparation method of a gold micro-nano pine needle composite structure, which comprises the following steps: step one, immersing a two-dimensional transition metal sulfide block in a potassium nitrate solution; focusing ultra-fast laser pulse on the surface of a bulk phase two-dimensional transition metal sulfide block, and scanning to obtain a transition metal oxysulfide nano-structure solution; step three, ultrasonically mixing the transition metal oxysulfide nano-structure solution with chloroauric acid solution and irradiating with white light; and fourthly, dripping the mixed solution after color change on the surface of the silicon substrate, and air-drying to obtain the gold micro-nano pine needle composite structure. The invention also discloses a gold micro-nano pine needle composite structure and a preparation system. The preparation method has the advantages of simple and green flow, no need of special environment, good crystallinity of the nano structure, great improvement of chemical activity of the material and strong adaptability.
Description
Technical Field
The invention relates to a micro-nano material and a preparation method thereof, in particular to a gold micro-nano pine needle composite structure and a preparation method thereof, and belongs to the technical field of micro-nano manufacturing.
Background
Local surface plasmon resonance of gold micro-nanostructures is of great interest due to its unique properties, including enhancement of sensor signals, photothermal effects, light emission properties, etc., and has important applications and prospects in numerous fields, such as chemical-biomolecular sensing detection (e.g., surface Enhanced Raman Scattering (SERS)), electro/photochemical catalysis, biological imaging, photothermal therapy, drug delivery, etc. Two-dimensional semiconductors have wide applications in sensing, catalysis, energy conversion, electronics, optoelectronics, and the like, due to their unique atomic structures. Therefore, the gold micro-nano structure and the two-dimensional semiconductor material are organically combined to form a gold and semiconductor composite structure system, and unexpected phenomena are expected to be generated or the application performance of the gold and semiconductor composite structure system is expected to be improved.
In the prior art, the gold and the semiconductor are independent and cannot be fused into each other, and in the prior art, the gold micro-nano structure and the semiconductor nano structure are prepared independently in the process of preparing the gold and semiconductor composite structure, two independent synthesis/preparation processes are needed, and then the gold micro-nano structure and the semiconductor nano structure are compounded. Among them, a general method for preparing gold micro-nano structures is a chemical reducing agent reduction method, but the method requires special chemical environments (acidic, alkaline, high temperature, etc.), complex chemical synthesis processes, various inorganic and organic chemical reagents (reducing agents, stabilizers, etc.), so that it is not easy to control, easy to introduce impurity elements, and environmental protection is not facilitated by using various chemical reagents. Common methods for preparing the transition metal sulfide nanostructures are hydrothermal methods and exfoliation methods (including chemical intercalation exfoliation, electrochemical intercalation exfoliation, microwave-assisted exfoliation, etc.), which require various chemical reagents, complicated steps, special environments such as specific temperatures and pressures, etc., and the prepared nanostructures have poor crystallinity.
Ultrafast laser processing is a novel technology in the field of micro-nano manufacturing. The laser processing method has the advantages of high speed, flexibility, non-contact, no pollution, no need of harsh conditions, short pulse duration, high pulse peak power, accurate focusing, positioning and processing of micro-nano structures, great improvement of chemical activity of materials and the like. However, at present, no ultra-fast laser preparation method aiming at the gold micro-nano pine needle composite structure exists.
Disclosure of Invention
The invention aims to solve the problems of independent components, complex preparation steps, special environment requirement, poor crystallinity of a nano structure and the like in the existing physicochemical method for preparing the gold micro-nano composite structure, and provides a preparation method for the gold micro-nano pine needle composite structure.
The invention is realized in the following way:
a preparation method of a gold micro-nano pine needle composite structure comprises the following steps:
step one, immersing a two-dimensional transition metal sulfide block in a potassium nitrate solution;
focusing ultra-fast laser pulse on the surface of a bulk phase two-dimensional transition metal sulfide block, and scanning to obtain a transition metal oxysulfide nano-structure solution;
step three, ultrasonically mixing the transition metal oxysulfide nano-structure solution with chloroauric acid solution and irradiating with white light;
and fourthly, dripping the mixed solution after color change on the surface of the silicon substrate, and air-drying to obtain the gold micro-nano pine needle composite structure.
The further scheme is as follows:
in the first step, the two-dimensional transition metal sulfide is molybdenum disulfide or tungsten disulfide, and the block form comprises a natural block and a powder pressed block;
the concentration of the potassium nitrate solution is 1-8 mM/L, and the volume is 2-8 mL.
The further scheme is as follows:
in the second step, the ultrafast laser is picosecond laser or femtosecond laser, and the transition metal oxysulfide is molybdenum oxysulfide or tungsten oxysulfide.
The further scheme is as follows:
in the second step, focusing is realized by a focusing objective lens, and the focusing objective lens is a plano-convex lens or a cylindrical lens.
The further scheme is as follows:
in the second step, the scanning processing parameters are that the laser energy is 200-500 mu J, the scanning speed is 100-600 mu m/s, the scanning interval is 10-20 mu m, and the scanning time is 1-3 hours.
The further scheme is as follows:
in the second step, the obtained molybdenum oxysulfide or tungsten oxysulfide nano-structure has the chemical composition of MoO x S y Or WO x S y Wherein x+y=2.5 or 3; the nano structure is nano dots and nano particles.
The further scheme is as follows:
in the third step, the concentration of chloroauric acid solution is 1-6 mM/L, the volume ratio of chloroauric acid solution to molybdenum oxysulfide or tungsten oxysulfide nano-structure solution is 1:1, the ultrasonic dispersion time is 3-10 minutes, and the white light irradiation time is 24 hours.
The further scheme is as follows:
in the fourth step, the mixed solution turns to dark green.
The invention further aims to provide a gold micro-nano pine needle composite structure, which is prepared by the preparation method of the gold micro-nano pine needle composite structure, wherein the whole structure of the gold micro-nano pine needle composite structure is a micron structure and is formed by aggregation of nano needles; the main component is gold, and the composite component is molybdenum oxysulfide or tungsten oxysulfide.
The invention discloses a gold micro-nano pine needle composite structure, which comprises a picosecond or femtosecond laser, an attenuation sheet set, a continuous gradual attenuation sheet, a mechanical switch and a first dichroic mirror, wherein the picosecond or femtosecond laser, the attenuation sheet set, the mechanical switch and the first dichroic mirror are sequentially arranged, a focusing objective lens is arranged below the dichroic mirror, a sample to be processed is arranged below the focusing objective lens, the sample to be processed is placed on a precise electronic control translation stage, a white light illumination source is arranged above the sample to be processed, a second dichroic mirror is arranged below the white light illumination source, a focusing lens and a CCD dynamic imaging unit are sequentially arranged on one side of the dichroic mirror, and the computer is respectively connected with the picosecond or femtosecond laser, the CCD dynamic imaging unit and the mechanical switch in a control manner. The method comprises the steps that the energy of a femtosecond laser pulse sequence emitted by a femtosecond laser is attenuated once through an attenuation sheet set, then is attenuated continuously and gradually through a continuous gradual attenuation sheet, the energy is attenuated continuously and gradually to an energy value meeting preset use requirements, then is reflected by a first dichroic mirror through a mechanical switch, is focused on a sample to be processed on a precision electric control translation table through a focusing objective lens, illumination light emitted by a white light illumination light source 0 positioned at the top irradiates the sample to be processed through a second dichroic mirror and a focusing lens to be reflected, the reflected illumination light returns through the focusing objective lens and the first dichroic mirror, is reflected by the dichroic mirror, reaches a CCD dynamic imaging unit through the focusing lens, is connected with the femtosecond laser through a computer, is controlled to be opened and closed, is controlled to move in the XYZ direction, meets the speed, the position and the route of the preset use requirements, and is connected with a CCD dynamic imaging unit to monitor the surface of the processed sample. The processing parameters, processing position and scanning route of the femtosecond laser pulse are controlled, namely the speed, position and movement route of the precise electronic control translation stage and the energy value of the femtosecond laser pulse are controlled.
Compared with the prior art, the invention has at least the following outstanding technical effects:
1. according to the preparation method of the gold micro-nano pine needle composite structure, the prepared transition metal sulfur oxide nano structure is used as a reducing agent to react with gold ions, so that the gold micro-nano pine needle composite structure is directly prepared, and in a gold and transition metal sulfur oxide semiconductor composite structure system, gold and transition metal sulfur oxides are mutually fused.
2. According to the preparation method of the gold micro-nano pine needle composite structure, the process of compounding after the original gold micro-nano structure and the semiconductor nano structure are prepared independently is simplified and green, no special environment is needed, and the nano structure has good crystallinity.
3. According to the preparation method of the gold micro-nano pine needle composite structure, step two, as the ultrafast laser has the characteristics of short pulse duration and high pulse peak power, the micro-nano structure is processed, and meanwhile, the chemical activity of a material is greatly improved.
4. According to the preparation method of the gold micro-nano pine needle composite structure, in the second step, the ultrafast laser can be suitable for preparing the micro-nano structure by liquid phase processing of almost all two-dimensional materials, and has strong adaptability.
5. The prepared gold micro-nano pine needle composite structure has excellent electromagnetic field enhancement characteristic, and can be applied to the fields of chemical biosensing of surface enhanced Raman scattering, photocatalytic hydrogen production energy and the like.
Drawings
FIG. 1 is a schematic diagram of a process of the method of the present invention;
FIG. 2 is a schematic view of an ultrafast laser pulse processing optical path;
FIG. 3 is a schematic representation of the molybdenum oxysulfide nano-structure obtained in example 1;
fig. 4 is a gold micro-nano pine needle composite structure obtained in example 1.
In the figure 1, the device comprises an A1-molybdenum disulfide block, an A2-potassium nitrate solution, an A3-femtosecond laser pulse, an A4-molybdenum oxysulfide nano-structure solution, an A5-chloroauric acid solution, an A6-ultrasonic vibrator, an A7-white light lamp, an A8-mixed solution, an A9-silicon substrate and an A10-gold micro-nano pine needle composite structure.
The device comprises a 1-picosecond or femtosecond laser, a 2-attenuation sheet set, a 3-continuously gradual-change attenuation sheet, a 4-mechanical switch, a 5-first dichroic mirror, a 6-focusing objective lens, a 7-sample to be processed, an 8-precision electronic control translation stage, a 9-second dichroic mirror, a 10-white light illumination light source, an 11-focusing lens, a 12-CCD dynamic imaging unit and a 13-computer in the figure 2.
Detailed Description
The invention is further described below with reference to the drawings and examples.
It should be noted that, the process of the method implemented by the invention is schematically shown in fig. 1, and the optical path of the ultrafast laser pulse processing is schematically shown in fig. 2.
Example 1
The embodiment discloses a preparation method of a gold micro-nano pine needle composite structure, which comprises the following specific steps:
(1) The natural molybdenum disulfide block A1 was immersed in a 4mL volume of potassium nitrate solution A2 at a concentration of 8 mM/L. There is no requirement for the size of the block as long as it is completely immersed in the potassium nitrate solution.
(2) The femtosecond laser generates femtosecond laser, and the pulse form is single pulse.
(3) Focusing the femtosecond laser pulse A3 in the step (2) on the surface of the molybdenum disulfide block in the step (1), and carrying out scanning processing. The focusing objective lens used was a plano-convex lens with a focal length of 100mm. The processing parameters are laser energy 300 mu J, scanning speed 250 mu m/s, scanning interval 15 mu m and scanning time 2 hours. And obtaining molybdenum oxysulfide nano-structure solution A4.
(4) After the processing (3), the obtained molybdenum oxysulfide nano-structure is shown in figure 3, is nano-dots with the average diameter of about 5nm, and is chemically formedDivided into MoO x S y (where x+y=2.5).
(5) Mixing the molybdenum oxysulfide nano-structure solution A4 in the step (4) with 3mM/L chloroauric acid solution A5 according to the volume ratio of 1:1, performing ultrasonic dispersion for 4 minutes by using an ultrasonic vibrator A6, and irradiating with white light by using a white light lamp A7 for 24 hours to obtain a mixed solution A8.
The white light has the main function of assisting in promoting the chemical reaction speed, and has no requirement on the intensity of the white light.
(6) And (3) after the mixed solution in the step (5) turns into dark green, dripping the mixed solution on the surface of the silicon substrate A9 by using a suction pipe, and naturally air-drying the mixed solution to obtain the gold micro-nano pine needle composite structure A10 shown in figure 4.
Example 2
The gold micro-nano pine needle composite structure obtained in the embodiment 1 can be applied to surface enhanced Raman scattering. The surface enhanced Raman scattering method can be used for detecting the types and the concentrations of organic matters and biological molecules, and the key basis for judging the detection performance is the Raman enhancement factor. The prepared gold micro-nano pine needle composite structure is applied to detecting rhodamine 6G, and the enhancement factor can reach 10 11 The detection limit of low concentration can be as low as 10 -13 M/L。
Example 3
The embodiment provides an ultrafast laser pulse processing light path for preparing a gold micro-nano pine needle composite structure, which comprises a picosecond or femtosecond laser 1, an attenuation sheet group 2, a continuous gradual attenuation sheet 3, a mechanical switch 4 and a first dichroic mirror 5 which are sequentially arranged, wherein a focusing objective 6 is arranged below the first dichroic mirror 5, a sample 7 to be processed is arranged below the focusing objective, the sample to be processed is placed on a precise electronic control translation table 8, a white light illumination light source is arranged above the sample to be processed, a second dichroic mirror 9 is arranged below the white light illumination light source, a focusing lens and a CCD dynamic imaging unit are sequentially arranged on one side of the dichroic mirror, and the ultrafast laser pulse processing light path further comprises a computer which is respectively connected with the picosecond or femtosecond laser, the CCD dynamic imaging unit and the mechanical switch in a control manner. The energy of the femtosecond laser pulse sequence emitted by the femtosecond laser 1 is attenuated once through the attenuation sheet group 2, then is attenuated continuously and gradually to an energy value meeting the preset use requirement through the continuous gradual attenuation sheet 3, then is reflected by the first dichroic mirror 5 through the mechanical switch 4, is focused on a sample 7 to be processed on the precision electronic control translation table 8 through the focusing objective lens 6, the illumination light emitted by the uppermost white light illumination light source 10 irradiates the sample 7 to be processed through the second dichroic mirror 9, the first dichroic mirror 5 and the focusing lens 6, is reflected, the reflected illumination light returns through the focusing objective lens 6 and the first dichroic mirror 5, is reflected through the second dichroic mirror 9, reaches the CCD dynamic imaging unit 12 through the focusing lens 11, the computer 13 is connected with the femtosecond laser 1, controls the opening and closing of the mechanical switch 4, controls the precision electronic control translation table 8 to move in the XYZ direction, and the movement meets the speed, the position and the route of the preset use requirement, and is connected with the dynamic imaging unit 12 to monitor the surface of the processed sample 7. The processing parameters, processing position and scanning route of the femtosecond laser pulse are controlled, namely the speed, position and movement route of the precise electronic control translation stage and the energy value of the femtosecond laser pulse are controlled.
Although the invention has been described herein with reference to the above-described illustrative embodiments thereof, the above-described embodiments are merely preferred embodiments of the present invention, and the embodiments of the present invention are not limited by the above-described embodiments, it should be understood that numerous other modifications and embodiments can be devised by those skilled in the art that will fall within the scope and spirit of the principles of this disclosure.
Claims (7)
1. The preparation method of the gold micro-nano pine needle composite structure is characterized by comprising the following steps of:
step one, immersing a molybdenum disulfide or tungsten disulfide block in a potassium nitrate solution with the concentration of 1-8 mM/L;
step two, focusing ultrafast laser pulses on the surface of a bulk molybdenum disulfide or tungsten disulfide block, and scanning to obtain molybdenum oxysulfide or tungsten oxysulfide nano-structure solution; the obtained molybdenum oxysulfide or tungsten oxysulfide nano-structure has the chemical composition of MoO x S y Or WO x S y Wherein x+y=2.5 or 3; the nanostructure is a nanoparticle;
step three, ultrasonically mixing molybdenum oxysulfide or tungsten oxysulfide nano-structure solution with chloroauric acid solution and irradiating with white light; wherein the concentration of chloroauric acid solution is 1-6 mM/L, the volume ratio of the chloroauric acid solution to the molybdenum oxysulfide or tungsten oxysulfide nano-structure solution is 1:1, the ultrasonic dispersion time is 3-10 minutes, and the white light irradiation time is 24 hours;
and fourthly, dripping the mixed solution after color change on the surface of the silicon substrate, and air-drying to obtain the gold micro-nano pine needle composite structure.
2. The method for preparing the gold micro-nano pine needle composite structure according to claim 1, which is characterized in that:
in the first step, the molybdenum disulfide or tungsten disulfide block forms comprise natural blocks and powder pressed blocks;
the volume of the potassium nitrate solution is 2-8 mL.
3. The method for preparing the gold micro-nano pine needle composite structure according to claim 1, which is characterized in that:
in the second step, the ultrafast laser is picosecond laser or femtosecond laser.
4. The method for preparing the gold micro-nano pine needle composite structure according to claim 1, which is characterized in that:
in the second step, focusing is realized by a focusing objective lens, and the focusing objective lens is a plano-convex lens or a cylindrical lens.
5. The method for preparing the gold micro-nano pine needle composite structure according to claim 1, which is characterized in that:
in the second step, the scanning processing parameters are that the laser energy is 200-500 mu J, the scanning speed is 100-600 mu m/s, the scanning interval is 10-20 mu m, and the scanning time is 1-3 hours.
6. The method for preparing the gold micro-nano pine needle composite structure according to claim 1, which is characterized in that:
in the fourth step, the mixed solution turns to dark green.
7. The gold micro-nano pine needle composite structure prepared by the preparation method of the gold micro-nano pine needle composite structure according to any one of claims 1 to 6 is characterized in that: the whole structure of the gold micro-nano pine needle composite structure is a micron structure and is formed by aggregation of nano needles; the main component is gold, and the composite component is molybdenum oxysulfide or tungsten oxysulfide.
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| Publication number | Priority date | Publication date | Assignee | Title |
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