CN104445058B - Orderly assembling method for micro-nano composite system of PS small ball and gold nano-particles - Google Patents
Orderly assembling method for micro-nano composite system of PS small ball and gold nano-particles Download PDFInfo
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Abstract
The invention discloses an orderly assembling method for a micro-nano composite system of a PS small ball and gold nano-particles and belongs to the field of nano materials. The orderly assembling method includes the steps that firstly, the PS small ball with the diameter of 1.4 microns is prepared through an emulsion polymerization method; secondly, a needed array silicon pillar is etched in a silicon wafer in the depth direction through a photoetching technology; thirdly, the array silicon pillar and a P type silicon wafer substrate are cleaned through oxygen plasma; fourthly, the gold nano-particles cover the PS small ball to form the micro-nano composite system through evaporating assembling and the physical gold plating technology. According to the orderly assembling method, solvent evaporation and the template method are combined, accurate positioning and programming assembling on the micro-nano particles are achieved by regulating capillary force, and a large-area one-dimensional micro-nano line assembling array is obtained. Rhodamine 6G molecules serve as the detection molecules, a Raman test is conducted on the obtained nano array, and it is found that the array has the obvious enhancing function on detection signals.
Description
Technical field
The invention belongs to field of nanometer material technology, it is related to the assemble method of nano-particle, particularly a kind of ps bead and Jenner
The ordered fabrication method of the micro-nano hybrid system of rice grain.
Background technology
Nano material is a kind of material with brand new that the mid-80 grows up, and is that size is in cluster
One class special particles of the transitional region having a common boundary with macro object.A kind of size limitation defining nano particle as material
To 1-100nm scope.When particle size enters nanometer scale, nanoparticle can be made to possess the effect of following four aspects:
Small-size effect, skin effect, quantum size effect, macro quanta tunnel effect.These four effects are the basic of nano-particle
Characteristic, they make nano material can present peculiar physics of all kinds, chemical property.For example: metal is conductor, but nanometer
Metal particle is in low temperature because quantum size effect can assume electrical insulating property；Ferromagnetic material enter nanoscale (5nm) due to
Single domain is become by multidomain and shows extremely strong paramagnetic effect；Chemically inert metal platinum but becomes after making nanoparticle (platinum black)
For the fabulous catalyst of activity.Nano material presented these with the diverse Strange properties of body phase material so as to
Pottery, microelectronics, bioengineering, photoelectricity, chemical industry, medical science etc. are multi-field to show tempting application prospect.
Many critical natures of one peacekeeping multidimensional ordered fabrication structure of nano-particle have caused people widely to weigh in recent years
Depending on, and show potential answering in all many-sides such as optical material, high density data holder, microreactor, biology sensors
With.In general, assemble nanometer particle ordered structure has two kinds of strategies, various photoetching techniques of " from top to bottom " and " from lower
On " self-assembling technique.Document 1 (adv.mater., 2014；26 [15]: 2353) report, author's p-type silicon chip is substrate, with
Polymer poly methyl methacrylate (pmma) is raw material, carries out spin coating under 2000rpm rotating speed, is prepared into the thin of 160nm thickness
Film, then selects upper laxative remedy strategy, with electron beam lithography and in-situ etch technology, nanometer star topology is carried out in order
Arrangement.Document 2 (acsnano, 2013,7 [5]: 4,326 4333) is reported, author spin coating pmma in p-type silicon chip, and anneals
(120 DEG C) process 1h, then build local space with spherical lens, fill dna solution, subsequently in not equality of temperature in local space
Carry out self assembly under degree, eventually form wheel bar radial array.
Polystyrene microsphere has that specific surface area is big, and adsorptivity is strong, the characteristic such as agglutination is big and surface respond is strong,
Have a wide range of applications, the uniform polymer microballoon of micron particles degree, as functional high molecule material, in analysisization
There is extensive purposes in, biochemistry, immune medical science, standard metering and some high-technology fields, thus to this kind of
The research of material increasingly causes attention.Polystyrene micron ball is carried out assembling and obtained ps by solvent volatilization and template
Ball array, is aided with physics plating alloying technology, constitutes orderly micro-nano composite array, constructs the sers detection substrate of a new generation.
Content of the invention
Key technical problem to be solved by this invention is to provide a kind of short-cut method constructing micro-nano array in order.
Particular content is that solvent volatilization and template combine, using the hair evaporating surface tension when liquid is shunk back and template edge
Thin masterpiece is driving force, drives micro-nano granules to form the micro-nano battle array of regular ordered structure in short time, different surfaces substrate
Row.
A kind of ordered fabrication method of the micro-nano hybrid system of ps bead and gold nano grain, specifically comprises the following steps that
1), the synthesis of hydrophilic styrene (ps) ball
Styrene cross pillar purify (using alkali alumina filling pillar as adsorbent, subsequent styrene adds wash-out post,
Aluminum oxide automatic absorbing impurity, styrene is purified), add demulsifier sodium chloride (generally styrene monomer total amount 2%
5%) and water, logical nitrogen 30min, adds initiator ammonium persulfate (generally styrene monomer total amount 0.1% 2%) afterwards,
Reaction certain time (24h) at 70 DEG C, you can obtain the homogeneous ps bead of size shape.
2), the configuration of ps suspension
The surfactant being configured to finite concentration (0.5mg/ml 10mg/ml) with lauryl sodium sulfate (sds) is molten
Liquid, then ps is scattered in activator solution, is prepared into suspension.
3), the preparation of photoetching array silicon column template and silicon chip substrate
By copying image and chemical attack, the array silicon column required for deep etching goes out on silicon chip.To silicon chip substrate
Processed, silicon chip is cut into the sheet material of 1cm × 1cm, and sequentially passed through the ultrasonic cleaning of acetone, ethanol and ultra-pure water, then
Silicon chip is placed in large beaker, adds a certain proportion of hydrogen peroxide and the concentrated sulfuric acid (the two volume ratio is 1:3), soak 1h.Finally
Take out silicon chip clear water repeatedly to rinse, dry up stand-by.
4), the hydrophilic treated of array silicon column and silicon chip substrate
Array silicon column and silicon chip substrate are put into plasma surface treatment instrument, set parameter, by high speed oxygen etc.
Gas ions are processed its surface hydrophilic.
5), the assembling of ps bead and nm of gold hybrid system
The ps hanging drop of 10 μ l is added in silicon chip substrate, is then covered by array silicon column template, composition " sandwich " knot
Structure, at a certain temperature (30 DEG C) be evaporated assembling formed array, then pass through physics Gold-plating technique by nm of gold cover exist
Micro-nano hybrid system is constituted on ps bead.
Step 1 described further), with emulsion polymerization synthesis hydrophilic ps bead, i.e. styrene addition chlorination after purification
Sodium logical nitrogen 30min, add afterwards and react 24h at 70 DEG C of initiator ammonium persulfate, you can obtain the homogeneous ps of size shape little
Ball.
Step 2 described further), the sodium dodecyl sulfate solution concentration of configuration is 3mg/ml.
Step 3 described further), the preparation of silicon chip substrate firstly the need of by the silicon chip of 15cm × 15cm be divided into 1cm ×
The sheet material of 1cm size.
Step 3 further) silicon chip substrate is positioned over " Piranha " solution (3:1 concentrated sulfuric acid: hydrogen peroxide) immersion 1h, then
It is cleaned by ultrasonic with acetone, second alcohol and water respectively, finally repeatedly cleaned with clear water afterwards, dried up with nitrogen stand-by.
Step 3 described further), prepare array silicon column needs and first photoresist is coated uniformly on the silicon chip of cleaning, profit
It is exposed with the optical mask plate preparing, obtained and mask plate identical patterning by developer solution, then carry out depth quarter
Erosion obtains required array silicon column structure.
Step 4 described further), stamp oxygen gas plasma in array silicon column and silicon chip surface, cleaned further
And obtain water-wetted surface.
Step 5 described further), after obtaining water-wetted surface, array silicon column, ps suspension, silicon to be completed within 5min
The structure of piece substrate sandwich interlayer, is so in order to ps suspension can be sprawled before silicon chip surface reinstatement well.
Solvent volatilization and template are combined by the present invention, by achieving to the regulation and control of capillary force to micro-and nano-particles essence
Determine position, sequencing assembling, obtain large-area one-dimensional micro-nanometer lines assembly array.And with rhodamine 6g molecule for detection
Molecule, carries out Raman test to the nano-array obtaining, and finds that array has obvious humidification to detection signal.
Brief description
Fig. 1 is the experimental principle figure of ps bead nano-array constructed by case study on implementation 1 of the present invention.Array silicon column, ps suspend
Liquid, silicon chip substrate form " sandwich " structure, and through evaporation after a while, ps ball is assembled into linear array
Fig. 2 be case study on implementation 1 of the present invention obtained by homogeneous hydrophilic ps bead SEM (sem) figure,
A diameter of 1.4 μm of bead.
Fig. 3/Fig. 4/Fig. 5 be case study on implementation 1 of the present invention obtained by the little ball array of ps SEM (sem)
Figure, the ps suspension of variable concentrations is arranged in the array of different size, and wherein, ps suspension concentration is respectively 2mg/ml, 3mg/
Ml, 4mg/ml.
Fig. 6/Fig. 7 Fig. 8 is the ps bead lines of case study on implementation 1 of the present invention zones of different in same p-type silicon chip substrate
Scanning electron microscope diagram.
The little ball array of ps obtained by Fig. 9/Figure 10/Figure 11 is case study on implementation 2 of the present invention carries out the curve map of Raman test,
Ps bead array sample with a collection of preparation is immersed in variable concentrations (10-6mol/l、10-9mol/l、10-12Mol/l sieve)
Soak 60min in red bright 6g solution, with Raman spectrometer, array is detected, find to have the place of array substantially Raman to be believed
Number there is humidification, in 613cm-1Near, there is obvious rhodamine 6g characteristic peak.Bead in array is more intensive, enhancement effect
Stronger.The corresponding concentration of wherein 9/10/11 figure is respectively 10-6mol/l、10-9mol/l、10-12mol/l.The a line of each in figure
Represent the Raman signal not having at ps bead array lines, b/c/d represents at one line/tri- bar line/five bar line of ps array respectively
Raman signal.
Specific embodiment
Embodiment further illustrates to technical scheme
Embodiment 1:
100mgnacl, 60g water, 6.8ml styrene (crossing pillar to purify) sequentially adds in 100ml single port bottle, logical nitrogen drum
Bubble stirring 30min, adds 70mg ammonium persulfate, 70 DEG C of condensing reflux 24h afterwards.After reaction terminates, product adds ethanol warp
8000rpm (5min) is centrifuged, and water/water/ethanol washs successively.The sediment (i.e. ps bead) obtaining is vacuum dried at 35 DEG C.
Weigh the lauryl sodium sulfate (sds) of 90mg, be dissolved in 30ml water, be configured to the surfactant that concentration is 3mg/ml molten
Liquid, then weighs the ps white powder of 6mg, is dissolved in 2ml surfactant solution.
Photoetching is the complex art that a kind of copying image and chemical attack combine, and first photoresist is coated uniformly on cleaning
Silicon chip on, be exposed using the optical mask plate preparing, obtained and mask plate identical patterning by developer solution, then
Carry out deep etching and obtain required array silicon column structure.
With acetone, ethanol, water, ultrasonically treated 15min is carried out to array silicon column and silicon chip substrate respectively.Afterwards at one
In the beaker of 100ml, it is firstly added the hydrogen peroxide of 10ml30%, be slowly added into 98% concentrated sulfuric acid of 30ml afterwards and repeatedly stir
Mix, be configured to Piranha solution.After its cooling, array silicon column and silicon chip substrate are soaked wherein 1h, deionized water is anti-afterwards
Multiple clean, and be contained in clear water deposit stand-by.
With dt-03 type plasma cleaning treatment array silicon chip and silicon chip substrate, arrange parameter is discharge time 600s,
Power 200w, gas flow is 200sccm, air pressure 65.2pa.After cleaning, 10 microlitres of ps hanging drop is added in cleaned
Silicon chip substrate surface, after solution after surface is uniformly sprawled, array silicon column is gently covered in silicon chip substrate surface, formed base
Bottom, solution, " sandwich " structure of array silicon column contact.Put into afterwards in 30 DEG C of drying box, stand 6h.Treat that solution is evaporated
Entirely, array silicon column is separated with substrate, ps bead assembly array can be obtained in silicon chip substrate surface.
Finally by physics Gold-plating technique, nm of gold is covered and micro-nano hybrid system, nanogold particle are constituted on ps bead
Size is 4nm.
Figure three is ps ball array of different shapes obtained by the array silicon column applying different size, can be seen that from right figure
If the silicon column length of side is less and spacing is excessive, when liquid is shunk back can not along pillar edge, have only reach in the middle of four pillars flat
The arrangement of weighing apparatus state, therefore ps ball is complex；If the pillar length of side is longer and spacing is less, when liquid is shunk back, both sides have edge to prop up
Support, ps ball is arranged with edge；When the pillar length of side and spacing are similar, unidirectional linear array can be formed.
Embodiment 2:
Select three preferable samples of arrangement from the silicon chip substrate with the little ball array of ps, seal up for safekeeping stand-by.Configuration 10-6m/
10-9m/10-12The rhodamine 6g solution of m, three samples are soaked 60min wherein, with Raman spectrometer, substrate are carried out afterwards
Test, test wavelength is chosen to be 633nm.
The ps lines of different in width can be found on same sample.Choose mono- line/tri- bar line/five bar line of ps respectively to enter
Row spectrum test, finds as shown in Fig. 5 Fig. 7, under same rhodamine 6g concentration, with increasing of ps lines, array pair
The humidification of detection signal is more obvious.
Claims (7)
1. the ordered fabrication method of the micro-nano hybrid system of a kind of ps bead and gold nano grain, concrete steps include: 1) synthesize
Hydrophilic ps ball；2) prepare ps suspension, the configuration of described ps suspension is: being configured to concentration with lauryl sodium sulfate is
The surfactant solution of 0.5mg/ml 10mg/ml, then ps is scattered in activator solution, is prepared into suspension；3)
Preparation photoetching array silicon column template；4) hydrophilic treated array silicon column template and silicon chip substrate, the process of described silicon chip substrate is: will
The silicon chip obtaining is cut into the sheet material of 1cm × 1cm, and sequentially passes through the ultrasonic cleaning of acetone, ethanol and ultra-pure water, then by silicon chip
It is placed in beaker, adds the hydrogen peroxide that volume ratio is 1:3 and the concentrated sulfuric acid, soak 1h, finally take out silicon chip clear water and repeatedly rinse,
Dry up stand-by；Array silicon column template and silicon chip substrate are put into plasma surface treatment instrument, sets parameter, by high speed oxygen
Corona treatment by its surface hydrophilic；5) assembling ps bead and nm of gold hybrid system.
2. the ordered fabrication method of the micro-nano hybrid system of a kind of ps bead and gold nano grain according to claim 1, its
It is characterised by: step 1) synthesis of described hydrophilic ps ball is:
The styrene crossing pillar purifying leads to nitrogen 30min, adds afterwards and reacts 24h at 70 DEG C of initiator ammonium persulfate, you can obtains
The homogeneous ps bead of size shape.
3. the ordered fabrication method of the micro-nano hybrid system of a kind of ps bead and gold nano grain according to claim 1, its
It is characterised by: step 3) preparation of described photoetching array silicon column template is:
By copying image and chemical attack, the array silicon column required for deep etching goes out on silicon chip.
4. the ordered fabrication method of the micro-nano hybrid system of a kind of ps bead and gold nano grain according to claim 1, its
It is characterised by: step 5) described ps bead with the assembling mode of nm of gold hybrid system is:
The ps hanging drop of 10 μ l is added in silicon chip substrate, is then covered by array silicon column template, form " sandwich " structure,
It is evaporated assembling at a temperature of 30 DEG C and forms array, then pass through physics Gold-plating technique and nm of gold is covered composition on ps bead
Micro-nano hybrid system.
5. the ordered fabrication method of the micro-nano hybrid system of a kind of ps bead according to claim 1 or claim 2 and gold nano grain,
It is characterized in that: step 1) described hydrophilic ps ball synthesis be with emulsion polymerization i.e. after purification styrene add sodium chloride and water
And lead to nitrogen 30min, add initiator ammonium persulfate synthesis afterwards, the addition of sodium chloride is the amount of styrene monomer total material
2% 5%, the addition of ammonium persulfate is 0.1% the 2% of the amount of styrene monomer total material.
6. according to claim 1 or 3 the micro-nano hybrid system of a kind of ps bead and gold nano grain ordered fabrication method,
It is characterized in that: step 3) described in prepare array silicon column needs first by photoresist be coated uniformly on cleaning silicon chip on, utilize
The optical mask plate preparing is exposed, and is obtained and mask plate identical patterning by developer solution, then carries out deep etching
Obtain required array silicon column structure.
7. according to claim 1 or 4 the micro-nano hybrid system of a kind of ps bead and gold nano grain ordered fabrication method,
It is characterized in that: step 5) described in assembling ps bead and nm of gold hybrid system be obtain water-wetted surface after, 5min it
Inside complete array silicon column, ps suspension, the structure of silicon chip substrate sandwich interlayer.
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| CN104876179B (en) * | 2015-04-16 | 2017-01-11 | 华中科技大学 | Large-area assembling method for non-contact type one-dimensional nano material |
| CN106935501B (en) * | 2016-10-19 | 2023-08-22 | 中国人民解放军国防科学技术大学 | Method for preparing single-electron transistor by assembling gold particles with polystyrene microsphere template |
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| CN113937182A (en) * | 2020-07-13 | 2022-01-14 | 中国科学院理化技术研究所 | Size-controllable zinc oxide-based photoelectric device with flexible substrate and preparation method thereof |
| CN112250033A (en) * | 2020-09-29 | 2021-01-22 | 江苏大学 | Super-oleophobic surface preparation method based on structure dipping-in-situ dragging forming |
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