CN102747320A - Preparation method of noble metal nano-particle array - Google Patents
Preparation method of noble metal nano-particle array Download PDFInfo
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Abstract
The invention provides a method for preparing a nano-particle array with adjustable size, shape and material type. The method comprises the following steps: preparing a two-dimensional single layer of hexagonal dense structural template with single grain size on a substrate through utilizing self-assembly between polystyrene colloid balls, depositing a noble metal film on the template, and ultrasonically removing a colloid ball mask board with an organic solvent so as to obtain a triangular noble metal nano-particle array on the substrate. The ultrasonic treated polystyrene colloid balls are immersed into chloroform solution to dissolve colloid balls so as to obtain a bowl-shaped shell layer noble metal nano-array. According to the method, the polystyrene colloid balls are not tightly arranged through ion etching/annealing technical manners, so that an annular noble metal nano-particle array is formed on the substrate. The ordered nano-particle array has wide application prospect on chemical and biological sensors, ultra-high density data memory mediums, photo-electric devices and chemical catalysts.
Description
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Technical field
The present invention relates to the preparation method of noble metal nano particles array, relate in particular to the preparation method that can prepare the adjustable noble metal nano array of size, shape and material category.
Background technology
Noble metal nano particles is attended by the intense absorption peak in visible-range, this is owing to the vibrational frequency of conduction electrons a large amount of in the particle is equal with the incident light wave frequency, produces the surface plasma body resonant vibration effect, thereby produces the intense absorption peak.The surface plasma resonance optical spectrum peak position is very responsive to the variation of the shape of nano particle, size, distribution, external agency environment.Along with the development of modern nanotechnology, the preparation of the noble metal nano particles of different-shape and their respective optical The Characteristic Study have caused people's extensive interest.In the noble metal nano structure of different-shape, the sequential 2 D nano-grain array receives people's attention day by day.
So-called sequential 2 D nano-grain array is meant nano particle structure according to the certain rules ordered arrangement on two-dimensional directional, and people can assign to control its characteristic on a large scale through particle size, spacing and even one-tenth.Nano-grain array has the potential application prospect in fields such as bio-sensing, medical science, photoelectricity, catalysis, detections.Based on this, develop and derived the technology of a large amount of preparation nanometers or the following yardstick structure of micron, like photoetch method, electron beam lithography method, X ray etching method etc.But these lithographic technique complex equipments, cost are expensive, efficient is low, also have difficulties for the nano-grain array system of making big scale.
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation method who prepares size, shape and the adjustable nano-grain array of material category, and this method equipment is simple, the convenient dexterity of laboratory facilities, efficient are efficient.
Preparing method of the present invention is the method that adopts polystyrene colloid ball self-assembly and film deposition techniques to combine, and whole thinking is following:
(1) this method is utilized the self-assembly between the polystyrene colloid ball, on substrate, prepares the hexagonal solid matter template of two-dimension single layer polystyrene colloid ball;
(2) adopt vertical evaporation or inclination sputtering technology depositing noble metal film on polystyrene colloid ball self-assembly two-dimension single layer template;
(3) ultrasonic dissolution is removed the polystyrene colloid ball template, with the precious metal sodium rice array of particles that has obtained the different-shape structure.
According to the difference of prepared nano-grain array pattern, the inventive method can be subdivided into several concrete technical schemes.
Scheme one,
(1) utilizes self-assembly between the polystyrene colloid ball, on substrate, prepare the hexagonal solid matter structure of individual layer two dimension polystyrene colloid ball;
(2) adopt the electron beam evaporation plating technology on polystyrene colloid ball single tier templates, to deposit the noble metal film of 50～200nm thickness;
(3) ultrasonic dissolution is removed polystyrene colloid spherolite, on substrate, obtains the noble metal nano particles array that triangular element is formed.
Described substrate can be Al
2O
3, GaN or silica glass.
When the polystyrene colloid ball of unified particle diameter is closely arranged when being hexagonal solid matter structure, because in this moment polystyrene colloid ball mask plate, the arrangement between the colloidal spheres is tightr, the gap is less.Vertical evaporation through the electron beam evaporation plating technology makes noble metal nano particles impinge perpendicularly on substrate through the gap between the polystyrene colloid ball.Though in the middle of the vapor deposition process, in rotation, the diffraction property of electron beam evaporation plating is relatively poor with certain circular frequency for substrate, so just the gap location between the polystyrene colloid ball forms similar triangular shape noble metal nano particles.After polystyrene colloid ball mask plate is by ultrasonic dissolution, will on substrate, form the noble metal nano particles array of being formed by similar trilateral particulate units.Route 1 in the corresponding experiment of this process synoptic diagram 1.
Scheme two,
(1) utilizes self-assembly between the polystyrene colloid ball, on substrate, prepare the hexagonal solid matter structure of individual layer two dimension polystyrene colloid ball;
(2) adopt the electron beam evaporation plating technology on polystyrene colloid ball single tier templates, to deposit the noble metal film of 100～300nm thickness;
(3) substrate is immersed in the chloroformic solution, the vertical nano particle shell of polystyrene colloid ball is peeled off from the colloidal spheres template, form bowl-shape shell nano-array.
Described substrate can be Al
2O
3, GaN or silica glass.
In above-mentioned experimentation, longer when the noble metal film depositing time, the polystyrene colloid surface will cover one deck noble metal film.At this moment, immerse substrate in the chloroformic solution, solubilized also peels off the vertical shell of polystyrene colloid ball from substrate, dissolve polystyrene colloid ball " core " after, be bowl-shape shell structure nano-array with the precious metal shell that obtains.Bowl-shape shell nano-array is still keeping the periodicity ordered structure of polystyrene colloid ball lamina membranacea; This is owing to contact with each other between polystyrene colloid ball and the ball; In the process of depositing noble metal; Noble metal granule can be built up at the contact area between the polystyrene colloid ball, thereby bowl-shape shell unit can be connected with each other and forms ordered structure.Bowl-shape shell structure is solid, even stand in TEM specimen preparation process also can guarantee under the ultransonic situation of long period that structural integrity is orderly.As mask plate, we can adjust the thickness and the inside diameter of semisphere nanometer shell through the different big or small polystyrene colloid balls with selection of the depositing time of control noble metal film.These bowl-shape shells have the character of many uniquenesses, as: big specific surface area, ordered structure, weak symmetry etc., they have a good application prospect at aspects such as plasma device, biosensor, little reaction vessel, catalyzer.(route 2 in the corresponding experiment of this process synoptic diagram 1)
Scheme three,
(1) utilizes self-assembly between the polystyrene colloid ball, on substrate, prepare the hexagonal solid matter structure of individual layer two dimension polystyrene colloid ball;
(2) adopt magnetron sputtering technique, tilting in polystyrene colloid ball single tier templates deposits the noble metal film of 50～200nm thickness;
(3) ultrasonic dissolution is removed polystyrene colloid spherolite, on substrate, obtains the noble metal nano particles array that grid cell is formed.
Described substrate can be Al
2O
3, GaN or silica glass.
When the tight arrangement of polystyrene colloid ball of unified particle diameter was hexagonal solid matter structure, because the arrangement between the colloidal spheres is tightr among the polystyrene colloid ball mask plate, so the gap between the polystyrene colloid ball was less.Select magnetron sputtering as the noble metal film deposition technique; Because magnetic control sputtering system is in the depositing noble metal thin-film process; Noble metal granule is that oblique incidence is to the polystyrene colloid ball template; And the diffraction property of magnetron sputtering is stronger, and therefore along with the increase of sputtering time, the noble metal granule major sedimentary is in the shade edge and the gap of colloidal spheres.When polystyrene colloid ball mask plate by trichloromethane (CHCl
3) etc. after the organic solution ultrasonic dissolution, will form the noble metal nano array of forming by latticed unit on the substrate.(route 3 in the corresponding experiment of this process synoptic diagram 1)
Scheme four,
(1) utilizes self-assembly between the polystyrene colloid ball, on substrate, prepare the hexagonal solid matter structure of individual layer two dimension polystyrene colloid ball;
(2) through ion beam etching and thermal annealing technology the polystyrene colloid spherolite is directly diminished;
(3) adopt magnetron sputtering technique at the tilt noble metal film of sputtering sedimentation 50～200nm thickness of polystyrene colloid ball single tier templates;
(4) ultrasonic dissolution is removed polystyrene colloid spherolite, on substrate, obtains the noble metal nano particles array that annular unit is formed.
Described substrate can be Al
2O
3, GaN or silica glass.
Behind polystyrene colloid spherolite process ion beam etching, the colloidal spheres particle alignment between the polystyrene colloid ball individual layer mask plate is no longer tight, the big gap that promptly exists between the polystyrene colloid ball.Select magnetron sputtering as the noble metal film deposition technique; Because magnetic control sputtering system is in the depositing noble metal thin-film process; Noble metal granule is that polystyrene colloid ball mask plate is arrived in oblique incidence; Along with the rotation of substrate in the sputter procedure, the noble metal granule major sedimentary is in polystyrene colloid ball one week of bottom.After polystyrene colloid ball mask plate is by ultrasonic dissolution, will on substrate, form the noble metal nano array of forming by annular unit.The oldered array structure of this nano-rings has great application prospect at aspects such as surface-enhanced Raman substrate, transmitter, chips.(route 4 in the corresponding experiment of this process synoptic diagram 1)
This preparation method among the present invention can be extended to other material, because magnetron sputtering and electron beam evaporation plating technology can deposit the various differing materials of controllable thickness.In addition, select the polystyrene colloid ball of different sizes can prepare the unitary nano-grain array of different size structures.Resulting this array structure can be used as the surface-enhanced Raman substrate and uses, because the surface plasma of incident light and resulting noble metal granule can strengthen EM field when taking place to resonate greatly.
Description of drawings
Fig. 1 is the synoptic diagram for preparing the nano-array of different structure with the inventive method.
Fig. 2 is the drift method synoptic diagram of the preparation polystyrene colloid ball that proposes of the present invention.
Fig. 3 is the scanning electron microscope diagram sheet of the trilateral nano-array of the inventive method preparation.
Fig. 4 is the scanning electron microscope diagram sheet of the bowl-shape shell nano-array of the inventive method preparation.
Fig. 5 is the scanning electron microscope diagram sheet of the latticed nano-array of the inventive method preparation.
Fig. 6 is the scanning electron microscope diagram sheet of the ring-type nano-array of the inventive method preparation.
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Embodiment
Combine accompanying drawing that the present invention is described further through embodiment below.
1) experiment reagent and instrument: slide glass, polystyrene microsphere, quartz plate, 95% ethanol, 2%, 10% sodium lauryl sulphate (dodecylsodiumsulfate, SDS), distilled water, petridish, liquid-transfering gun, polystyrene colloid ball.
2) substrate cleans: substrate is put into acetone, 95%ETOH each ultrasonic 10 min respectively, water flushing more earlier; Substrate after the flushing is put into the 10%SDS solution that had before prepared soak 24 h; Substrate after the immersion is again through water flushing, removes to remain in that to put into distilled water behind the SDS on the substrate subsequent use.Quartz plate after the cleaning uses as substrate, and slide glass uses as the drainage sheet in dripping polystyrene colloid ball solution process.
This method mainly is based on the self-assembly of polystyrene colloid spherocolloid particle at two phases (solution-air) interface; Through the drainage sheet polystyrene colloid ball solution of being prepared is incorporated into liquid level slowly; Reduced by polystyrene colloid ball drop gravity and caused the liquid level turbid phenomenon; Effectively avoided the polystyrene colloid ball to arrange, and self-organization form unordered unitary film in the multilayer of liquid level.After leaving standstill several minutes; The 2%SDS that makes is added drop-wise to the liquid level white space changes water surface tension; Purpose is the individual layer polystyrene colloid spherocolloid ball film that forms high-density, big area, ordered arrangement at WS, leave standstill treat liquid level stabilizing after, clamp the clean back substrate with tweezers one jiao; It is immersed in blank liquid level place; From orderly polystyrene colloid ball zone it is slowly lifted out the water surface from liquid level, put into empty watch-glass to it again, under metastable air-flow and temperature, it is dried.Above working method is simple, can prepare the structure of big area by hexagonal solid matter structural arrangement on any substrate.
Next adopt magnetron sputtering and electron beam evaporation plating technology deposition method, use two kinds of technology on polystyrene colloid ball (diameter 460nm) single layer mask plate, to deposit the noble metal film of different thickness as noble metal film; Subsequently, ultrasonic dissolution is removed polystyrene colloid spherolite, on substrate, has obtained the noble metal granule array of different-shape structure.
1. metal refining:, adopt the method (vacuum pressure 1 * 10 of electron beam evaporation plating in order to obtain the trilateral silver nano-grain array
-4Pa) depositing noble metal silver film (about 100 nm of thickness) on polystyrene colloid ball individual layer mask plate.2. remove the polystyrene colloid ball template: through at trichloromethane (CHCl
3) etc. organic solvent for ultrasonic remove the polystyrene colloid ball template.3. the large-scale two-dimensional and periodic trilateral of gained nanoparticle array structure can characterize with sem, AFM etc.Gained result's trilateral silver nano-grain array the scanning electron microscope diagram sheet as shown in Figure 3.
Through changing depositing time, can obtain the particle size unification and highly different silver-colored array of particles, on this template basis, what the particulate size was concentrated relatively is distributed between the 110-140 nm.The nano particle that this method is prepared, its shape size is unified, and distribution rule is even, parameters such as the size that size that can be through changing polystyrene colloid ball ball and deposit thickness are regulated nano particle, spacing, thus be convenient to its optical property of quantitative examination.
1. metal refining:, adopt the method (vacuum pressure 1 * 10 of electron beam evaporation plating in order to obtain the silver-colored nano-array of bowl-shape shell structure
-4Pa) depositing noble metal silver film (about 100 nm of thickness) on polystyrene colloid ball individual layer mask plate.2. remove the polystyrene colloid ball template: immerse trichloromethane (CHCl to substrate
3) ultrasonic in the solution, to promote the vertical shell of polystyrene colloid ball " peeling off " from the substrate, at last with the Yin Nami shell that obtains ultrasonic cleaning 2-3 time in 95% ethanol.To obtain bowl-shape shell structure nano-array.3. the silver-colored nano-array of the bowl-shape shell structure of the large-scale two-dimensional and periodic of gained can characterize with sem, AFM and projection electron microscope etc.The transmission electron micrograph of the silver-colored nano-array of gained result's bowl-shape shell structure is as shown in Figure 4.
Embodiment 4
1. metal refining:, adopt the method (vacuum pressure 2.5 * 10 of magnetron sputtering in order to obtain latticed silver nano-grain array
-4Pa, power=120w) be depositing noble metal silver film (about 200 nm of thickness) on polystyrene colloid ball individual layer mask plate.2. remove the polystyrene colloid ball template: immerse trichloromethane (CHCl to substrate
3) the ultrasonic polystyrene colloid ball template of removing in the solution.3. the large-scale latticed silver nano-grain array structure of gained can characterize with sem, AFM etc.The scanning electron microscope diagram sheet of gained result's latticed silver nano-grain array is as shown in Figure 5.
Embodiment 5
1. ion beam etching: through ion beam etching (power=80w, time=20s), the polystyrene colloid spherolite is directly diminished, it is big that the spacing between ball and the ball becomes.2. metal refining:, adopt the method (vacuum pressure 2.5 * 10 of magnetron sputtering in order to obtain the ring-type silver nano-grain array
-4Pa, power=120w) be depositing noble metal silver film (about 200 nm of thickness) on polystyrene colloid ball individual layer mask plate.3. remove the polystyrene colloid ball template: immerse trichloromethane (CHCl to substrate
3) the ultrasonic polystyrene colloid ball template of removing in the solution.4. the large-scale ring-type silver nano-grain array of gained structure can characterize with sem, AFM etc.The scanning electron microscope diagram sheet of gained result's ring-type silver nano-grain array is as shown in Figure 6.
The position of nano-rings just is positioned at polystyrene colloid ball bottom, about 200 nm of its diameter, and nano-rings has kept the periodicity ordered arrangement structure of polystyrene colloid ball.Through selecting the big or small polystyrene colloid ball of different-grain diameter, can regulate and control the cycle of nano-rings array structure as template.In addition, select different elementary composition targets, also can prepare the nano-rings array structure of different components.
Claims (10)
1. preparation method that can prepare size, shape and the adjustable nano-grain array of material category is characterized in that: the method that adopts polystyrene colloid ball self-assembly means and film deposition techniques to combine prepares, and concrete steps are following:
(1) this method is utilized the self-assembly between the polystyrene colloid ball, at Al
2O
3, prepare the hexagonal solid matter template of two-dimension single layer polystyrene colloid ball on GaN or the silica glass substrate;
(2) adopt vertical evaporation or inclination sputtering technology depositing noble metal film on polystyrene colloid ball self-assembly two-dimension single layer template;
(3) ultrasonic dissolution is removed the polystyrene colloid ball template, obtains the precious metal sodium rice array of particles of different-shape structure.
2. the preparation method who prepares size, shape and the adjustable nano-grain array of material category according to claim 1; It is characterized in that: adopt vertical evaporation technique depositing noble metal on template, obtain the trilateral nano-grain array on the template back substrate through removing in organic solvent for ultrasonic.
3. the preparation method who prepares size, shape and the adjustable nano-grain array of material category according to claim 1; It is characterized in that: after adopting vertical evaporation technique depositing noble metal; Immerse in the chloroformic solution substrate ultrasonic; The vertical nano particle shell of polystyrene colloid ball is peeled off from the colloidal spheres template, form bowl-shape shell nano-array.
4. the preparation method who prepares size, shape and the adjustable nano-grain array of material category according to claim 1; It is characterized in that: adopt inclination sputtering technology depositing noble metal on template, place organic solvent for ultrasonic to remove substrate and obtain latticed nano-grain array on the template back substrate.
5. the preparation method who prepares size, shape and the adjustable nano-grain array of material category according to claim 1; It is characterized in that: the polystyrene colloid ball is diminished; Arrange no longer tight between ball and the ball; Adopt inclination sputtering technology depositing noble metal on template, place organic solvent for ultrasonic to remove substrate and obtain the ring-type nano-grain array on the template back substrate.
6. the preparation method who prepares size, shape and the adjustable nano-grain array of material category according to claim 1 is characterized in that: select the polystyrene colloid ball of different sizes to prepare the unitary nano-grain array of different size structures.
7. the preparation method who prepares size, shape and the adjustable nano-grain array of material category according to claim 1 is characterized in that: the nano-grain array that obtains heterogeneity through the different precious metal material of sputtering sedimentation.
8. the preparation method who prepares size, shape and the adjustable nano-grain array of material category according to claim 3 is characterized in that: thickness and the inside diameter of adjusting semisphere nanometer shell through the size of regulating thin film deposition time and change colloidal spheres.
9. the preparation method who prepares size, shape and the adjustable nano-grain array of material category according to claim 5 is characterized in that: make that through technology such as reactive ion beam etching (RIBE) and thermal annealings arrangement is not tight between the polystyrene colloid ball.
10. the preparation method who prepares size, shape and the adjustable nano-grain array of material category according to claim 9 is characterized in that: through energy and the time and the thermal annealing temperature parameter realization regulation and control big or small to the colloidal spheres inter-particle voids of reactive ion beam etching (RIBE).
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| 刘斌斌等: "基于纳米球刻蚀的银纳米颗粒阵列和有序纳米壳层的制备", 《武汉大学学报（理学版）》 * |
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