CN110844876B - Process method for preparing large-area metal nanoparticle array with assistance of graphene - Google Patents
Process method for preparing large-area metal nanoparticle array with assistance of graphene Download PDFInfo
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Abstract
A process method for preparing a large-area metal nanoparticle array with the assistance of graphene belongs to the field of micro-nano processing. On the basis of the traditional process, firstly, a surface periodic treatment process is adopted, and the nano-columns 106 are prepared on the surface of the substrate 101, so that the implanted regions of the metal atoms 102 are separated, the graphene 105 is transferred and annealed, and the metal atoms 102 are agglomerated into the metal nano-particles 103 in the annealing process. The graphene 105 acts as a perfect barrier to prevent evaporation of the metal atoms 102. Therefore, the annealing temperature can be much higher than that in the conventional process. In addition, the periodic surface treatment enables the metal nanoparticles to be regularly arranged, so that a metal nanoparticle array with adjustable structural arrangement can be obtained. Meanwhile, the prepared graphene is protected by the metal nanoparticles, so that the contact between the graphene and air is prevented, and the long-term stable property of the metal nanoparticles is effectively ensured.
Description
Technical Field
The invention relates to a preparation process of a metal nanoparticle array, and belongs to the field of micro-nano processing.
Background
The metal nanostructure has a surface plasmon effect, and the main reason is that a large amount of free electrons exist inside and on the surface of the metal to form free electron gas mass, namely plasma (plasma). The surface plasma optics of the metal nanostructure has wide application prospects in the fields of photocatalysis, optical sensing, biological labeling, medical imaging, solar cells, surface-enhanced Raman spectroscopy and the like, and the functions are closely related to surface plasma resonance generated when the metal nanostructure interacts with light.
The metal nano-particles are one of metal nano-structures, and some corresponding optical functions can be realized by designing the diameter, the interval and the period of the metal nano-particles. At present, there are many methods for preparing metal nanoparticles, such as: nano-imprinting, electron beam exposure, sputtering annealing, chemical synthesis, metal ion implantation and annealing. Among them, metal ion implantation and annealing are one of the commonly used methods for preparing metal nanoparticles. The process flow is as follows: step 1, as shown in fig. 1, preparing a substrate 101 required for metal ion implantation, wherein the substrate can be an insulating substrate or a semiconductor substrate; step 2, as shown in fig. 2, performing metal ion implantation, and implanting metal atoms 102 into the substrate 101; step 3, as shown in fig. 3, obtaining the implanted substrate 101, in which the metal atoms 102 are located; step 4, as shown in fig. 4, annealing is performed, and in the annealing process, metal atoms 102 are agglomerated and polymerized into metal nanoparticles 103; step 5, as shown in fig. 5, finally obtaining the metal nanoparticles 103 inside and on the surface layer of the substrate 101. The method can realize the preparation of the large-area metal nano-particles, and simultaneously, the crystal lattice quality of the obtained metal nano-particles is better due to the introduction of an annealing process in the preparation process. However, the following problems still exist in the current method:
1) the annealing temperature cannot be too high, otherwise, metal atoms are evaporated after being separated from the surface of the substrate, and the metal atoms are lost. The low annealing temperature results in a small diameter of the obtained metal nanoparticles, and it is difficult to obtain large-sized metal nanoparticles.
2) The arrangement of the obtained metal nanoparticles is disordered and random, so that the controllable preparation of the metal nanoparticles is difficult to realize.
3) For some easily oxidized metals, such as copper, silver and the like, the prepared metal nanoparticles lack effective protection and are easily oxidized, so that the metal nanoparticles are ineffective.
At present, no effective solution for the above problems is available.
Disclosure of Invention
The invention aims to provide a process method for preparing a large-area metal nanoparticle array with the assistance of graphene. On the basis of a method for preparing metal nano particles by ion implantation and annealing, firstly, a method called surface periodic treatment is adopted to carry out dry etching treatment on the surface of a substrate after metal atoms are implanted, and periodically and closely arranged nano columns are prepared on the surface of the substrate, so that an implanted region of the metal atoms is separated. Then, a layer of graphene (graphene is a single-atomic-layer two-dimensional thin film material formed by hybridizing carbon atoms in sp 2) is transferred on the surface of the substrate, and the graphene is introduced to serve as a metal atom barrier layer to prevent evaporation of metal atoms in the annealing process. Finally, the periodic regular metal nanoparticle array can be obtained on the surface of the substrate through annealing. The diameter and the arrangement period of the obtained metal nano-particles are adjustable. The method solves all the problems existing in the preparation of metal nano particles by metal ion implantation and annealing at present, and realizes the controllable large-area periodic preparation of the metal nano particles.
The specific process steps are as follows:
s1, preparing a substrate 101 required for metal ion implantation; as shown in fig. 1.
S2, injecting metal atoms 102 into the shallow surface layer inside the surface of the substrate 101 by adopting a metal ion injection mode, wherein the injection depth of the metal atoms 102 is controlled to be less than 100nm from the surface to the shallow surface layer of the substrate; as shown in fig. 2;
the steps S3-S5 are collectively referred to as surface periodic processing of the substrate.
S3, transferring the silica nanospheres 104 to the surface of the substrate 101 in the step S2 by a silica nanosphere transferring method; as shown in fig. 6, after the silicon dioxide nanospheres 104 are transferred to the surface of the substrate 101 by the solution transfer method, they will be in close periodic arrangement on the surface of the substrate 101 due to the transfer mechanism, as shown in fig. 12;
s4, using the silicon dioxide nanospheres 104 as a mask, performing vertical dry etching on the surface of the substrate, wherein the etching depth is greater than the injection depth of the metal atoms 102, and finally obtaining the nanopillars 106 which are closely and regularly arranged on the surface of the substrate; the purpose of the etching is to separate the implanted regions of metal atoms 102, the top surface of each nano-pillar 106 is a silicon dioxide nanosphere 104, the diameter of each nano-pillar 106 is approximately equal to the diameter of the silicon dioxide nanosphere 104, and each nano-pillar 106 contains metal atoms 102; as shown in fig. 7;
s5, removing the silicon dioxide nanospheres 104 on the top surface of the nanopillars 106 from the surface of the substrate 101 by deionized water ultrasound, as shown in fig. 8;
s6, transferring a layer of graphene 105 on the surface of the substrate 101 through a wet transfer method; as shown in fig. 9.
S7, separating out the metal atoms 102 from the nano-pillars 106 on the surface of the substrate 101 to the top surfaces of the nano-pillars 106 by annealing and agglomerating, wherein the metal atoms 102 inside each nano-pillar 106 are thermally agglomerated and form a metal nanoparticle 103 on the top surfaces of the nano-pillars 106 during the annealing process, as shown in fig. 10, the arrangement of the obtained metal nanoparticles 103 is consistent with the nano-pillars 106 and also consistent with the arrangement of the silicon dioxide nanospheres 104;
s8, finally, obtaining the metal nano-particles 103 which are periodically arranged on the surface of the substrate 101; as shown in fig. 11.
The substrate used in the present invention may be a silicon substrate having a silicon dioxide layer on the surface layer, a quartz substrate, or another insulating substrate.
In the present invention, the metal formed by the metal ion implantation may be a noble metal such as gold, platinum, silver, or copper, or may be another metal such as aluminum or iron.
The annealing temperature is equal to or higher than the melting point temperature of the corresponding metal of the metal atoms.
Compared with the traditional method for preparing metal nano particles by injecting and annealing metal ions, the method has the following main differences: difference (1) after metal atoms are injected into the surface layer of the substrate, a surface periodic treatment process is introduced. The transfer method of the silica nanospheres is a commonly used wet transfer method, and is characterized in that after the silica nanospheres are transferred to the surface of the substrate, the silica nanospheres are arranged in a regular equilateral triangle, as shown in fig. 12. And then, dry etching the substrate to obtain nano columns on the surface of the substrate so as to separate the injection regions of the metal atoms and form a small region. Each nano column and the silicon dioxide nanosphere are in consistent regular arrangement of equilateral triangles. The surface periodic treatment process is to prepare for the subsequent annealing to obtain periodically arranged metal nanoparticles. After annealing, the precipitated metal nanoparticles can keep the arrangement mode consistent with that of the nano-columns. As shown in fig. 17, taking metal silver as an example, the white origin in the figure is silver nanoparticles, the left side of the figure is silver nanoparticles obtained by surface periodic treatment, and the right side of the figure is silver nanoparticles obtained without surface periodic treatment. It can be seen that the silver metal nanoparticles are in regular ordered arrangement on the left side, while none are on the right side. Difference (2) a layer of graphene 105 is transferred on the etched substrate surface as a barrier layer. This is done to prevent evaporation of the metal atoms. The research shows that for the complete crystal lattice graphene, metal atoms cannot penetrate through the complete crystal lattice graphene, and meanwhile, the complete crystal lattice graphene has super-strong mechanical properties. The two characteristics make graphene very suitable as a barrier layer for metal atom evaporation. After the graphene is transferred to the surface of the substrate, in the annealing process, once metal atoms are separated out to the surface of the substrate, the metal atoms cannot be evaporated due to the blocking of the graphene, but can be bound by the graphene and remain on the surface of the substrate, so that the loss of the metal atoms caused by evaporation is reduced. Therefore, the annealing temperature can be greatly increased without fear of evaporation of metal atoms. Experiments prove that in the absence of graphene, metal atoms precipitated on the surface during annealing can be completely evaporated, and metal nanoparticles cannot be obtained on the surface of the substrate.
In the invention, the mask for carrying out surface periodic treatment on the substrate can be used as a mask by transferring the silicon dioxide nanospheres, and can also be used for manufacturing a periodic mask by nano-imprinting or transferring nanospheres made of other materials.
The invention has the advantages that:
1. the graphene is used as a barrier layer for metal atom evaporation, so that the loss of metal atoms can be effectively prevented, the annealing temperature can be greatly increased, and metal nano-particles with larger sizes can be obtained.
2. After the metal nanoparticles are formed on the surface of the substrate, the metal nanoparticles are wrapped by graphene, and the graphene protects the metal nanoparticles and prevents the metal nanoparticles from contacting air. Therefore, the method is suitable for preparing the nano particles of the easily oxidized metal, such as silver, copper and the like, and can realize long-term storage of the nano particles.
3. The periodic regular arrangement of the metal nanoparticles can be realized by periodically processing the surface of the substrate, so that the whole preparation method is more controllable.
4. Since it is found experimentally that the surface of each etched nano-pillar is fixed to form one metal nano-particle, the diameter of the metal nano-particle is affected by the number of metal atoms in each nano-pillar. Therefore, the adjustment of the size of the final metal nanoparticles can be achieved by changing the dose of ion implantation or the diameter of the nanopillar.
5. The periodic etching mask is prepared by other methods such as nanoimprint lithography and the like, so that the nano-columns in different arrangement modes can be obtained by etching, and further the metal nano-particles in different arrangement modes can be obtained.
Drawings
FIG. 1: schematic illustration of a substrate for metal ion implantation;
FIG. 2: a schematic diagram of a metal ion implantation process;
FIG. 3: after the metal ions are implanted, the distribution of metal atoms in the substrate is shown schematically;
FIG. 4: a schematic diagram of a process of forming metal nanoparticles by agglomeration of metal atoms during annealing;
FIG. 5: the distribution and the structure schematic diagram of the metal nano particles obtained in the annealing process in the substrate;
FIG. 6: after the metal ions are injected, the structure schematic diagram of the sample after the silicon dioxide nanospheres are transferred on the surface of the substrate;
FIG. 7 is a schematic view of: a process schematic diagram of performing dry etching;
FIG. 8: removing the silicon dioxide nanospheres by deionized water ultrasound to obtain a sample structure schematic diagram;
FIG. 9: a sample structure schematic diagram after transferring a layer of graphene on the surface of a sample;
FIG. 10: annealing, wherein metal atoms are agglomerated on the surface of the substrate to form a schematic process diagram of metal nanoparticles;
FIG. 11: finally obtaining a structural schematic diagram of the metal nanoparticle samples which are regularly arranged on the surface of the substrate;
FIG. 12: a Scanning Electron Microscope (SEM) top view of the structural sample shown in fig. 6, i.e., a top view of the SEM of the sample surface after transfer of the silica nanospheres. The circle enclosed by the black dotted line in the figure is the silica nanosphere, which has a diameter of about 600 nm.
FIG. 13: SEM top view at 70 degrees tilt angle of the structural sample shown in fig. 8, SEM top view at 70 degrees tilt angle of the sample after etching out the nanopillars and removing the silica nanospheres.
FIG. 14: the SEM top view of the prepared silver nanoparticles shows that white dots indicated by black arrows in the figure are the silver nanoparticles.
FIG. 15: and (3) taking the SEM top view of the sample with the graphene removed, wherein a circle encircled by a black dotted line in the figure is the top view of the nano column, and white dots in the figure are silver nano particles.
FIG. 16: schematic structural diagram of silver nanoparticles on the surface of the circular nano-pillar.
FIG. 17: and (3) an optical microscope picture of the silver nanoparticle real object, wherein the white original point in the picture is the silver nanoparticle. The left graph is the silver nanoparticles obtained by surface periodic treatment, and the right graph is the silver nanoparticles obtained without surface periodic treatment.
Detailed Description
The practice of the present invention is illustrated by the following examples, but the present invention is not limited to the following examples.
Example 1: large area preparation of silver nanoparticles
Taking the preparation of silver nanoparticles as an example, the method of the invention is adopted to prepare:
s1 cleaning silicon wafer with 300nm silicon dioxide layer, implanting silver atoms into shallow surface of substrate by ion implantation with dosage of 5 × 1015/cm2The implantation energy was 30keV, and the implantation depth of silver atoms was about 22 nm.
S2 transferring silica nanospheres, which have a diameter of about 600nm, onto the surface of the substrate impregnated with silver atoms. The transfer method of the silica nanospheres is a common wet transfer method, namely, the silica nanospheres are uniformly dispersed in a solution, and then the solution mixed with the silica nanospheres is dripped on the surface of deionized water. Due to the surface tension effect of water (other solute can be added to increase the surface tension), the silica nanospheres will float on the surface of the deionized water and form a regular arrangement of equilateral triangles. And finally, the substrate is used for directly moving upwards from the water in parallel to the water surface to fish out the silicon dioxide nanospheres from the deionized water, the silicon dioxide nanospheres are attached to the surface of the substrate, and the regular arrangement of the original equilateral triangle is kept. Fig. 12 is an SEM top view of silica nanospheres on the substrate surface.
S3 dry-etching the substrate with the silicon dioxide nanospheres as a mask using a Reactive Ion Etching (RIE) system. The etching conditions are as follows: power 300W, trifluoromethane: 100sccm, etch time: for 50 s. Under the etching condition, the etching depth is about 40nm (the silver atom injection depth is more than 22 nm), and the silver atom injection regions can be separated. And after etching, removing the silicon dioxide nanospheres from the surface of the substrate by adopting a deionized water ultrasonic method. Fig. 13 is an SEM image of the substrate surface at an inclination angle of 70 degrees after etching, and it can be seen that the substrate surface forms individual circular nano-pillars.
S4, transferring a layer of single-layer graphene on the surface of the substrate by adopting a wet transfer method.
S5 annealing the substrate. Annealing conditions: 1050 degrees Celsius, 15 minutes, argon/hydrogen (960sccm/40sccm) atmosphere. The annealing temperature is far higher than the melting point of the nano silver. During the annealing process, silver atoms can be separated out from the substrate, and due to the blocking of the graphene, the silver atoms cannot be evaporated from the surface of the substrate, but can be bound between the graphene and the substrate interface. Finally, the silver atoms agglomerate to form silver nanoparticles. The diameter of the silver nanoparticles is around 144 nm. Fig. 14 is a top view of SEM of silver nanoparticles obtained after annealing, which can be seen to be uniform in size and in regular arrangement of equilateral triangles in accordance with silica nanospheres.
S6 is to etch away the graphene with oxygen plasma, the relative position relationship between the silver nanoparticles and the circular nanopillars can be visually observed, and as can be seen from fig. 15, the silver nanoparticles are located in the center of the circular nanopillars, and one silver nanoparticle is formed on the surface of each nanopillar. Fig. 16 is a schematic structural diagram of silver nanoparticles on the surface of a circular nano-pillar.
Claims (6)
1. A process method for preparing a large-area metal nanoparticle array with the assistance of graphene is characterized by comprising the following steps:
s1, preparing a substrate (101) required by metal ion implantation;
s2, injecting metal atoms (102) into the shallow surface layer inside the surface of the substrate (101) by adopting a metal ion injection mode;
the steps S3-S5 are collectively referred to as surface periodic processing of the substrate;
s3, transferring the silicon dioxide nanospheres (104) to the surface of the substrate (101) in the step S2 by adopting a silicon dioxide nanosphere transferring method; by adopting a solution transfer method, after the silicon dioxide nanospheres (104) are transferred to the surface of the substrate (101), the silicon dioxide nanospheres can be in close periodic arrangement on the surface of the substrate (101) due to the transfer mechanism;
s4, taking the silicon dioxide nanospheres (104) as a mask, carrying out vertical dry etching on the surface of the substrate, wherein the etching depth is greater than the injection depth of the metal atoms (102), and finally obtaining the nanopillars (106) which are closely and regularly arranged on the surface of the substrate; the purpose of the etching is to separate the implanted regions of metal atoms (102), and the top surface of each nano-pillar (106) is a silicon dioxide nano-sphere (104);
s5, removing the silicon dioxide nanospheres (104) on the top surfaces of the nano columns (106) from the surface of the substrate (101) by a deionized water ultrasonic method;
s6, transferring a layer of graphene (105) on the surface of the substrate (101) by a wet transfer method;
s7, metal atoms (102) are precipitated from the nano columns (106) on the surface of the substrate (101) to the top surfaces of the nano columns (106) and are agglomerated, the metal atoms (102) inside each nano column (106) are agglomerated by heating in the annealing process and form a metal nano particle (103) on the top surfaces of the nano columns (106), and the arrangement mode of the obtained metal nano particles (103) is consistent with that of the nano columns (106) and is also consistent with that of the silicon dioxide nanospheres (104);
and S8, finally, obtaining the metal nano particles (103) which are periodically arranged on the surface of the substrate (101).
2. A method according to claim 1, characterized in that the implantation depth of the metal atoms (102) is controlled to be < 100nm from the surface at a shallow surface of the substrate.
3. The method of claim 1, wherein each of the nanopillars (106) has a diameter approximately equal to a diameter of the silica nanospheres (104), each of the nanopillars (106) comprising metal atoms (102).
4. The method according to claim 1, wherein a silicon substrate having a silicon dioxide layer on the surface layer of the substrate or a quartz substrate is used.
5. The method of claim 1, wherein the metal is selected from one or more of noble metals, aluminum, and iron.
6. The method of claim 1, wherein the annealing is at a temperature equal to or greater than the melting point temperature of the corresponding metal of the metal atom.
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| CN102180438A (en) * | 2011-03-28 | 2011-09-14 | 中国科学院光电技术研究所 | Manufacturing method of tunable triangular metal nano particle array structure |
| CN102259832A (en) * | 2010-05-27 | 2011-11-30 | 清华大学 | Preparation method of three-dimensional nano structure array |
| CN102320557A (en) * | 2011-09-08 | 2012-01-18 | 中国科学院研究生院 | Method for preparing metal nanometer particles with hexagonal network in lattice distribution on substrate |
| CN102747320A (en) * | 2012-07-31 | 2012-10-24 | 武汉大学 | Preparation method of noble metal nano-particle array |
| KR101478604B1 (en) * | 2014-11-11 | 2015-01-02 | 연세대학교 산학협력단 | Method of patterning nano particle by tapping on patterned template using impact member and manufacturing method of nano electrode thereby |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102259832A (en) * | 2010-05-27 | 2011-11-30 | 清华大学 | Preparation method of three-dimensional nano structure array |
| CN102180438A (en) * | 2011-03-28 | 2011-09-14 | 中国科学院光电技术研究所 | Manufacturing method of tunable triangular metal nano particle array structure |
| CN102320557A (en) * | 2011-09-08 | 2012-01-18 | 中国科学院研究生院 | Method for preparing metal nanometer particles with hexagonal network in lattice distribution on substrate |
| CN102747320A (en) * | 2012-07-31 | 2012-10-24 | 武汉大学 | Preparation method of noble metal nano-particle array |
| KR101478604B1 (en) * | 2014-11-11 | 2015-01-02 | 연세대학교 산학협력단 | Method of patterning nano particle by tapping on patterned template using impact member and manufacturing method of nano electrode thereby |
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