CN106226283A - A kind of Raman strengthens the manufacture method of substrate - Google Patents
A kind of Raman strengthens the manufacture method of substrate Download PDFInfo
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- CN106226283A CN106226283A CN201610533715.2A CN201610533715A CN106226283A CN 106226283 A CN106226283 A CN 106226283A CN 201610533715 A CN201610533715 A CN 201610533715A CN 106226283 A CN106226283 A CN 106226283A
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- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
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Abstract
The present invention is the manufacture method that a kind of Raman strengthens substrate.Substrate (inorganic substrate) is put into the growth district in plasma chemical vapor deposition system by the present invention, is passed through the reaction source gas containing carbon, and the atmospheric pressure value controlling reaction source gas is 0.01Torr 760Torr；Control base reservoir temperature at 300 1200 DEG C, open plasma electrical source, set plasma power as 1 1000W, make reaction source gas molecular cleavage, active group reacts under the effect of plasma, at substrate surface, generates graphene quantum dot, by regulation and control growth temperature and growth time, prepare various sizes of graphene quantum dot Raman and strengthen substrate.Drip at prepared Raman enhancing substrate surface and need the solution of detection molecules, by LR laser raman instrument, record high-sensitive Raman enhancing signal.Raman prepared by the present invention strengthens substrate, pollution-free, highly sensitive, can large area prepare, and preparation process the most easily realizes.
Description
Technical field
The invention belongs to Raman and strengthen substrate manufacture technology field, be specifically related to a kind of Raman and strengthen the making side of substrate
Method.
Background technology
Raman spectrum is as the characteristic spectrum of sign molecular vibration energy level, in fields one such as physics, chemistry, biologys
Directly there is consequence.Raman spectrum is combined with confocal microscopy, is possible not only to realize the spectrographic detection to sample, also may be used
To realize the research of the three-dimensional visualization to biological sample.But owing to normal Raman scattered signal strength ratio is relatively low, and easily
Being flooded by some substrate fluorescence, therefore detection difficulty is bigger.Until 1974, Fleischmann et al. is in smooth silver electricity
After surface, pole is roughened, obtains absorption the high-quality of monolayer Pyridine Molecules in silver electrode surface first and draw
Graceful spectrum.But Fleishmann thiss is presumably because the roughening of electrode surface, electrode real table area increases and makes absorption
The amount increase of Pyridine Molecules causes, and does not recognize that the enhancing of the raman spectral signal of binding molecule is made by rough surface
With.1977, Van Duyne and Creighton Liang Ge seminar found independently of one another, and absorption is in coarse silver electrode surface
The Raman signal of single Pyridine Molecules is the strongest by 10 than in solution for the Raman signal of each Pyridine Molecules6Times, it is indicated that this is one
Plant the surface enhanced effect relevant to rough surface, be referred to as SERS effect.The discovery of surface enhanced raman spectroscopy (SERS),
Improve substrate and intermolecular energy transfer, it is to avoid the interference of fluorescence background, the precision making raman scattering spectrum detect is produced
Give birth to leap, be widely used at aspects such as biochemistry, biophysics and molecular biology.
Alkali metal that the substrate strengthened for Raman the earliest is mainly of little use with gold, silver, three kinds of metals of copper and minority pole (as
Lithium, sodium etc.) it is main, because these metals have strong Raman enhancement effect, and the metal system beyond gold, silver, copper is at Raman
Research in terms of enhancing does not obtain the progress with practical significance for a long time.Further, gold, silver, copper metallic face have to pass through slightly
Roughening just has high Raman and strengthens activity after processing, therefore, gold, silver and bronze are in addition to expensive, it is simply that production process compares
Complexity, the enhancing efficiency difference of different metal is bigger simultaneously, therefore finds more preferable surface Raman enhancement backing material to closing
Important.
The two dimensional crystal of only one layer of atomic thickness that Graphene is made up of carbon atom.2004, Manchester, England
College Physics scholar An Deliegaimu and Constantine's Nuo Woxiao love, Graphene is isolated in success from graphite, it was demonstrated that
It can be with individualism.2011, the Graphene of team's trial mechanical stripping of Peking University was as surface Raman enhancement
Backing material, successfully detects the Raman peaks of fluorescence molecule, and this also further illustrates Graphene and can apply in Raman enhancing
Aspect.In consideration of it, the Graphene Area comparison owing to peeling off is little, the bad control of the number of plies, our using plasma chemical gaseous phase
The quantum dot of deposition process growth Graphene, quantum dot is smaller due to size for Graphene, so can introduce more
Many borders, may improve the interaction of Graphene and molecular detection further, and then improve Raman enhancing efficiency.Experiment
Result also further demonstrates that quantum dot efficiency in terms of Raman enhancing is higher than the Graphene of stripping, and this based on graphite
The Raman of alkene quantum dot strengthens substrate and is easier to make.
Summary of the invention
It is an object of the invention to provide a kind of make simple, growth rate high, the measured Raman of matter strengthens the system of substrate
Make method.
The invention provides and prepare the method that graphite Raman strengthens substrate, use plasma activated chemical vapour deposition
(PECVD) equipment, it mainly includes the coil (plasma generation) of inductive coupling system, growth tube furnace and vacuum pumping section
Point.Specifically comprising the following steps that of preparation
(1) clean substrate, remove impurity and the Organic substance of substrate surface；
(2) in step (1) gained substrate surface growth graphene quantum dot:
The vitellarium in apparatus for plasma chemical vapor deposition cavity is put in cleaned substrate in step (1) being obtained
In territory, using plasma chemical gaseous phase depositing process, it is passed through the reaction source gas containing carbon, controls reaction source gas
Atmospheric pressure value is 0.01 Torr-760 Torr；Make substrate be warming up to growth temperature 300-1200 DEG C, when base reservoir temperature raises simultaneously
During to growth temperature, opening plasma electrical source, control plasma power is 1-1000W, makes reaction source gas crack, contains
The active group of carbon reacts under the effect of plasma, generates graphene quantum dot at substrate surface；
(3) taking and need the solution of molecular detection, dropping in step (2) gained length has in the substrate of graphene quantum dot；Need detection
The addition of the solution of molecule is 10 μ L, and concentration is between 10-3-10-11Between Mol/L；
(4) sample in step (3) does Raman characterize.
In the present invention, substrate described in step (1) is inorganic substrate, particularly as follows: silicon oxide/silicon, silicon dioxide, sapphire
Or in glass etc. any one.
In the present invention, described in step (2), reaction source gas is the gaseous molecular containing carbon or steam, particularly as follows:
Described gaseous molecular is any one in methane, ethylene or acetylene etc., and described steam is alcohol vapour.
In the present invention, described in step (2), the atmospheric pressure value of reaction source gas is 0.1Torr-10Torr.
In the present invention, needing molecular detection in described step (3) is luminescent dye molecule such as rhodamine, pyridine, amethyst,
Ppp, in Phthalocyanine etc. any one.
In the present invention, control plasma power is 10-100W.
The present invention utilizes plasma chemical vapor enhanced chemical vapor deposition (PECVD) equipment to make Graphene in inorganic substrate
Quantum dot Raman strengthens substrate, and its principle is, reaction source gas is when being heated to more than specified temp, in the effect of plasma
Under, resolve into containing hydrocarbon group and hydrogen, this material is diffused into growth substrates region, in the common effect of plasma
Under, it is deposited on substrate surface, forms graphene quantum dot.
The present invention is different from place of other Ramans strengthen substrate and is: (1) manufacture method is simple;(2) environmentally safe；
(3) cheap；(4) batch growth.Graphite Raman prepared by this new method strengthens substrate to be had Raman detection technology
The biggest impetus.
Accompanying drawing explanation
Fig. 1: using plasma chemical vapor depsotition equipment grows graphene quantum dot Raman at different temperatures to be strengthened
The scanning probe microscopy picture of substrate, scale 500 nm.Wherein, (1), (2), (3), (4) and (5) figure is growth temperature difference
It is at 605 DEG C, 615 DEG C, 620 DEG C, 625 DEG C and 635 DEG C of five temperature, growth time 10 min, plasma power 20 W feelings
Scanning probe microscopy figure under condition.(6) it is between growth temperature and the size of graphene quantum dot and nucleation density
Graph of a relation.
The x-ray photoelectron energy spectrogram of Fig. 2: graphene quantum dot.Wherein: (1) is the X-ray light of graphene quantum dot
The full spectrogram of electron spectrum, (2) are the C 1s spectrogram of graphene quantum dot.
The Raman peaks of Fig. 3: graphene quantum dot corresponding with Fig. 1 and drip and have the Raman peaks comparison diagram after rhodamine liquor.
Wherein: (1) is the Raman spectrogram of the graphene quantum dot of growth under different temperatures, (2) are the graphite of growth under different temperatures
Dripping of alkene quantum dot has the Raman spectrogram after rhodamine liquor.
The rhodamine molecule of Fig. 4: (1) variable concentrations drops in the Raman spectrogram on graphene quantum dot surface；(2) rhodamine
Solution concentration is diluted to 10-8During Mol/L, obvious rhodamine Raman peaks.
Fig. 5: using plasma chemical vapor depsotition equipment under 10W plasma power under grow graphene quantum dot
Raman strengthens the scanning probe microscopy picture of substrate.
Fig. 6: using plasma chemical vapor depsotition equipment is lower growth Graphene quantum under 100W plasma power
Point Raman strengthens the scanning probe microscopy picture of substrate.
Detailed description of the invention
Combine accompanying drawing below by embodiment and further illustrate the present invention.
Embodiment 1:
(1) choose silica-based silicon oxide substrate as growth substrate, clean with acetone, ethanol and isopropanol successively by ultrasonic method
Growth substrate, removes impurity and the Organic substance of substrate surface.
(2) growth district in plasma activated chemical vapour deposition cavity is put in silica-based silicon oxide substrate, be evacuated down to
10-3Torr, is passed through methane gas, and substrate is warmed up to 605 DEG C-635 DEG C.Control the atmospheric pressure value of methane gas at 0.12 Torr.When
When base reservoir temperature is increased to 605 DEG C-635 DEG C, open plasma electrical source, power 20W, methane gas cracking journey containing hydrocarbon group with
And hydrogen, these hydrocarbon active groups react under the effect of plasma, connect at edge, at substrate surface, according to
The mode of nucleation-grow up, generates graphene quantum dot, through 10 min, grows graphene quantum dot, see in silicon oxide substrate
Accompanying drawing 1.Wherein (1), (2), (3), (4) and (5) figure be growth temperature be 605 DEG C, 615 DEG C, 620 DEG C, 625 DEG C and 635 respectively
At DEG C five temperature, growth time 10 min, the scanning probe microscopy figure in the case of plasma power 20 W, (6) make a living
Graph of a relation between long temperature and the size of graphene quantum dot and nucleation density.
(3) graphene quantum dot grown does x-ray photoelectron power spectrum characterize, the C 1s of the Graphene grown
Peak position, at 284.4 eV, is classified as sp2The carbon peak position of hydridization, is shown in Fig. 2.Wherein (1) is the x-ray photoelectron of graphene quantum dot
The full spectrogram of power spectrum, (2) are the C 1s spectrogram of graphene quantum dot.
(4) graphene quantum dot to different temperatures growth does Raman sign, can see D, G of Graphene clearly
With 2D peak value, see Fig. 3 (1)；Taking rhodamine powder, dissolve in ethanol, being made into concentration is 10-5The solution of Mol/L, drops in difference
In the silica-based silicon oxide substrate of the graphene quantum dot of temperature growth, obtain Raman enhanced spectrum, see Fig. 3 (2).Wherein (1) is
The Raman spectrogram of the graphene quantum dot of growth under different temperatures, (2) are the graphene quantum dot of growth under different temperatures
Drip and have the Raman spectrogram after rhodamine liquor.
(4) take rhodamine powder, dissolve in ethanol, be made into variable concentrations (10 in five-5,10-7,10-8,10-9,10-10
Mol/L) solution, dropping in length has in the silica-based silicon oxide substrate of graphene quantum dot.Doing Raman to characterize, optical maser wavelength is chosen
532nm, laser intensity is 50%, and object lens select can detect easily the Raman enhancing signal of rhodamine at 50 times simultaneously,
Relatively the rhodamine liquor Raman reinforced effects of variable concentrations, is shown in Fig. 4, and wherein (1) is that the rhodamine molecule of variable concentrations drops in
The Raman spectrogram on graphene quantum dot surface, (2) rhodamine liquor concentration dilution is to 10-8During Mol/L, obvious Luo Dan
Bright Raman peaks.
Embodiment 2:
According to the method for embodiment (1), after cleaning, silicon oxide/silicon base is put into plasma activated chemical vapour deposition chamber
Growth district in body, is evacuated down to 10-3Torr, is passed through methane gas, controls the atmospheric pressure value of methane gas at 0.12 Torr.
When base reservoir temperature is increased to 700 C, opening plasma electrical source, power 10W, methane gas cracking journey is containing hydrocarbon group and hydrogen
Gas, these hydrocarbon active groups react under the effect of plasma, connect at edge, at substrate surface, according to nucleation-
The mode grown up, generates graphene quantum dot, through 30 min, grows graphene quantum dot in silicon oxide substrate.See Fig. 5.
Embodiment 3:
Also according to the method for embodiment (1), silicon oxide/silicon base put into plasma enhanced chemical vapor sink after cleaning
Growth district in long-pending cavity, is evacuated down to 10-3Torr, is passed through methane gas, controls the atmospheric pressure value of methane gas 0.12
Torr.When base reservoir temperature is increased to 500 C, opening plasma electrical source, power 100W, methane gas cracking journey is containing hydrocarbon group
And hydrogen, these hydrocarbon active groups react under the effect of plasma, connect at edge, at substrate surface, press
According to the mode of nucleation-grow up, generate graphene quantum dot, through 30 min, silicon oxide substrate grows graphene quantum dot.
See Fig. 6.
Embodiment 4:
According to the method for embodiment (1) growth graphene quantum dot, make Raman and strengthen substrate, take pyridine powder afterwards, in second
Alcohol dissolves, is made into five kinds of variable concentrations (10-5,10-7,10-8,10-9,10-10Mol/L) solution, dropping in length has Graphene amount
In the silica-based silicon oxide substrate of son point.Doing Raman equally to characterize, optical maser wavelength still chooses 532 nm, and laser intensity is 50%, simultaneously
Object lens select at 50 times, compare the pyridine solution Raman reinforced effects of variable concentrations, along with the reduction of concentration, to Pyridine Molecules
Detectivity can reduce.
Embodiment 5:
According to the method for embodiment (1) growth graphene quantum dot, make Raman and strengthen substrate, afterwards by thermal evaporation evaporation side
Method strengthens the CuPc being deposited with 0.5nm thickness on substrate at graphene quantum dot Raman.Doing Raman equally to characterize, optical maser wavelength is still
Choosing 532 nm, laser intensity is 50%, and object lens select at 50 times simultaneously, obtain Raman enhancing signal.
Claims (6)
1. a Raman strengthen probing substrate manufacture method, it is characterised in that specifically comprise the following steps that
(1) clean substrate, remove impurity and the Organic substance of substrate surface；
(2) in step (1) gained substrate surface growth graphene quantum dot:
In step (1) being obtained, the growth district in apparatus for plasma chemical vapor deposition cavity is put in cleaned substrate
In, using plasma chemical gaseous phase depositing process, it is passed through the reaction source gas containing carbon, substrate rises temperature control at 300-
1200 DEG C, the atmospheric pressure value controlling reaction source gas is 0.01Torr-760 Torr；Make substrate be warming up to growth temperature 300-simultaneously
1200 DEG C, when base reservoir temperature is increased to growth temperature, open plasma electrical source, control plasma power ranges for 1-
Between 1000W, making reaction source gas crack, the active group containing carbon reacts under the effect of plasma,
Substrate surface generates graphene quantum dot；
(3) taking and need the solution of molecular detection, dropping in step (2) gained length has in the substrate of graphene quantum dot；Need detection
The addition of the solution of molecule is 10 μ L, and concentration is between 10-3-10-11Between Mol/L；
(4) sample in step (3) does Raman characterize.
Method the most according to claim 1, it is characterised in that substrate described in step (1) is inorganic substrate, particularly as follows:
In silicon oxide/silicon, silicon dioxide, sapphire or glass any one.
Method the most according to claim 1, it is characterised in that described in step (2), reaction source gas is containing carbon
Gaseous molecular or steam, particularly as follows: described gaseous molecular is any one in methane, ethylene, ethanol or acetylene, described steam is
Alcohol vapour.
Method the most according to claim 1, it is characterised in that described in step (2), the atmospheric pressure value of reaction source gas is 0.1
Torr-10Torr。
Method the most according to claim 1, it is characterised in that needing molecular detection in described step (3) is fluorescent dye
In molecule, specially rhodamine, pyridine, amethyst, PPP or Phthalocyanine any one.
Method the most according to claim 1, it is characterised in that control plasma power is 10-100W.
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Cited By (3)
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| CN107161988A (en) * | 2017-05-19 | 2017-09-15 | 中国电子科技集团公司第十三研究所 | The method for preparing nanocrystalline graphene on a sapphire substrate |
| CN108033438A (en) * | 2017-12-28 | 2018-05-15 | 中国华能集团公司 | One kind visualization carbon material structure and preparation method thereof |
| CN113945518A (en) * | 2021-10-20 | 2022-01-18 | 云南师范大学 | Silicon quantum dot hydrogen detector |
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Cited By (4)
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| CN107161988A (en) * | 2017-05-19 | 2017-09-15 | 中国电子科技集团公司第十三研究所 | The method for preparing nanocrystalline graphene on a sapphire substrate |
| CN108033438A (en) * | 2017-12-28 | 2018-05-15 | 中国华能集团公司 | One kind visualization carbon material structure and preparation method thereof |
| CN113945518A (en) * | 2021-10-20 | 2022-01-18 | 云南师范大学 | Silicon quantum dot hydrogen detector |
| CN113945518B (en) * | 2021-10-20 | 2024-04-19 | 云南师范大学 | Silicon quantum dot hydrogen detector |
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