CN105954253B - Glucose SERS detection substrate and preparation method thereof based on Ag@Ag nano dot classification galaxy array - Google Patents
Glucose SERS detection substrate and preparation method thereof based on Ag@Ag nano dot classification galaxy array Download PDFInfo
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Abstract
The glucose SERS detection substrate and preparation method thereof based on Ag@Ag nano dot classification galaxy array that the present invention relates to a kind of.The substrate base is that the glucose SERS containing the Ag@Ag nano dot of silver nanoparticle point mother array of particles and sub- array of particles two-level configuration classification galaxy array deposited in surface of silicon detects substrate.The diameter of silver nanoparticle point mother's particle is 91 ~ 97 nm, and the silver nanoparticle idea particle diameter of silver nanoparticle point mother particle surface and surrounding distribution is 3 ~ 12 nm, and adjacent silver nano dot mother granular center is away from for 98 ~ 102 nm.The glucose SERS of Ag@Ag galaxy array provided by the invention detects substrate, structure-controllable, and galactic structure is highly coupled, and Raman signal enhancing is significant, and enhances signal stable homogeneous, and SERS test result shows that it has very strong response to concentration of glucose.The method of the present invention realizes the flexible modulation of female particle and sub- particle size, it is easier to realize large area, high sensitivity, low cost preparation, can be realized performance advantage of the SERS substrate in the application of the biological detections such as glucose.
Description
Technical field
The present invention relates to a kind of glucose SERS detection substrate and its preparation based on Ag@Ag nano dot classification galaxy array
Method.Especially a kind of Ag@Ag nano dot based on ultrathin alumina template (UTAM) nano surface technology of preparing is classified galaxy
Array glucose detection substrate and preparation method thereof.
Background technique
Nearest decades, along with the continuous development of modern life level, the dietetic life of eutrophication adds amount of exercise
The factors such as reduction, cause diabetes morbidity to rise year by year.The entire mankind are perplexed always in the diagnosis detection of the diseases such as diabetes,
And Surface enhanced Raman scattering (Surface Enhanced Raman Scattering, SERS) technology is because it is with highly sensitive
Property, high-resolution and the advantages that fast reaction, sent out in terms of chemistry, environment and biology are especially medical sensing detection in recent years
It opens up very fast.
SERS detection underlying structure how is designed and prepared, Raman signal can be greatlyd improve, even up to singly
Molecular Detection, for SERS technology in detection field using most important.Many researchers are done a lot of work, and electricity is proposed
Beamlet photoetching (electronbeam lithography), focused ion beam lithography (focused-ion-beam
Lithography) and nanosphere assists preparation methods such as photoetching (nanosphere-assisted lithography), so
And usually it is more difficult adjust surface nano-structure structural parameters, and due to low-yield and high cost constrain SERS technology into
One step application.Accuracy controlling and preparation SERS activity hot spot realize large area, low cost and expeditiously prepare high enhancing
SERS active-substrate is still a difficult point in current research.
UTAM nano surface technology of preparing is with its large area high-sequential, flexible controllable, ultra high density (1010-1012 cm-2), simple and quick unique advantage in conjunction with depositional modes such as thermal evaporation, electron beam evaporation or magnetron sputterings nanometer may be implemented
Structural parameters it is flexible controllable；Realization smaller (the structure list of spot size can be facilitated especially in conjunction with the multiple vapor deposition of UTAM mask
First spacing is smaller), the nanometer hierarchical array structure that Raman scattering signal is highly coupled between hierarchical structure, it is effectively guaranteed that
Large area, low cost and the realization for expeditiously preparing the SERS active-substrate that height enhances, signal is uniform.
Summary of the invention
One of the objects of the present invention is to provide a kind of glucose SERS inspections based on Ag@Ag nano dot classification galaxy array
Survey substrate.
The second object of the present invention is to provide the preparation method of the detection substrate.
To achieve the above object, the invention adopts the following technical scheme:
The one glucose SERS based on Ag@Ag nano dot classification galaxy array detects substrate, it is characterised in that the substrate is
It is obtained in surface of silicon by deposition, two-level configuration made of nested sub- array of particles in silver nanoparticle point mother's array of particles
Ag@Ag nano dot is classified galaxy array；The diameter of silver nanoparticle point mother's particle is 91 ~ 97 nm, adjacent two silver nanoparticles point mother
Grain center away from be 98 ~ 102 nm, the silver nanoparticle idea array of particles be distributed in described in silver nanoparticle point mother particle surface and
Around, particle diameter is 3 ~ 12 nm.
A method of it preparing the above-mentioned glucose SERS based on Ag@Ag nano dot classification galaxy array and detects substrate,
It is characterized in that the specific steps of this method are as follows:
A. the preparation of ultrathin alumina template (UTAM)；
B.UTAM aperture adjustment under the conditions of 30 DEG C of constant temperature；
C.UTAM is transferred on Si substrate；
D.UTAM aperture adjustment under constant temperature within the scope of 10 DEG C~15 DEG C；
E. female array of particles preparation in the glucose SERS detection substrate based on Ag@Ag nano dot classification galaxy array；
F. the glucose SERS detection substrate preparation based on Ag@Ag nano dot classification galaxy array.
The specific steps of the preparation of above-mentioned ultrathin alumina template (UTAM) are as follows:
A-1. aluminium flake after pretreatment is carried out first using 0.3 M oxalic acid solution as electrolyte under 40V constant voltage
Secondary anodized, time are 8 ~ 12 h；Then the phosphorus that mass percent concentration is 6% is dipped under the conditions of 60 DEG C of temperature
In the mixed liquor of acid and 1.8% chromic acid, wherein the volume ratio of phosphoric acid and chromic acid is 1:1；It impregnates to remove the once oxidation on surface
Resulting aluminium oxide, then using 0.3 M oxalic acid solution as electrolyte, second of anodic oxidation, 5 min is carried out under 40V constant voltage；
Inactive area around is cut off after dioxy and drips an attached layer photoresist in 60 DEG C of drying in oven.
A_2. alumina formwork obtained by step a_1 is put into the mixed liquor of copper chloride and hydrochloric acid by the volume ratio of 1:1,
To remove remaining aluminium, pure UTAM is obtained.
The specific steps of above-mentioned step b are as follows: the barrier layer of alumina formwork obtained by step a is swum in 30 DEG C downward,
In the dilute phosphoric acid solution that mass percent concentration is 5%, pore-enlargement is 70 min, obtains the UTAM that aperture is 83~87 nm.
The specific steps of above-mentioned step c are as follows: swim in step b resulting UTAM in acetone soln, the light to surface
Photoresist all after dissolution, UTAM is transferred on the Si substrate after cleaning up and making hydrophilic treated, and with 80 DEG C of heated at constant temperature
Platform drying.
The specific steps of above-mentioned step d are as follows: by the UTAM/Si sample arrived in step c, within the scope of 10 DEG C~15 DEG C
It under conditions of constant temperature, is placed in the dilute phosphoric acid solution that mass percent concentration is 5%, pore-enlargement is 30~50 min, is obtained
Aperture is the ultrathin alumina template of 91~97nm.
The specific steps of above-mentioned step e are as follows: be 8 × 10 in vacuum degree by UTAM/Si sample obtained by step d-4 Pa steams
Under the conditions of sending out 0.3~0.5 nm/s of rate, evaporated metal silver is with a thickness of 50 ~ 70 nm；Then UTAM is removed, obtaining diameter is 91
Ag nano dot mother's array of particles of~97 nm.
The specific steps of above-mentioned step f are as follows: be in vacuum degree by the resulting Ag nano dot mother array of particles sample of step e
8×10-4 Under the conditions of Pa, 0.3~0.5 nm/s of evaporation rate, Ag powder is evaporated again with a thickness of 3 ~ 12 nm to get to completely
The glucose SERS that Ag@Ag nano dot is classified galaxy array detects substrate.
Advantages of the present invention and effect are: the present invention compared with prior art, has the advantage that
1) present invention by it is very simple, be prepared in a manner of low cost large area, high density, structure-controllable Ag@Ag receive
The glucose SERS of rice point classification galaxy array detects substrate, and substrate has significant surface Raman enhancement effect, it can be achieved that right
0.08 m mol·L-1The Sensitive Detection of extremely low concentration glucose.
2) present invention carries out aperture control twice under high/low temperature to UTAM, conveniently realizes nanometer metallic silver particle size
Flexible modulation and the preparation of large scale (91~97 nm) nano-grain array, to realize the glucose of Ag@Ag galaxy array
Flexible modulation in SERS substrate detection performance.
3) present invention aperture can accuracy controlling on the basis of, carry out the metal thermal evaporation of different-thickness twice, Ke Yishi
Now to the accurate control of metallic particles hierarchical structure preparation, it is ensured that the height between the two-stage nano-dot matrix array structure of galactic structure
Coupling, and then ensure that the very big enhancing of SERS active-substrate Raman signal and the good homogeneity of signal, and then realize
Advantage of the SERS active-substrate in detection performance.
Detailed description of the invention
Fig. 1 be Ag@Ag nano dot be classified galaxy array glucose SERS detect substrate preparation process (such as Fig. 1 (a),
(b), (c), (d), (e)) and structural schematic diagram.
The SEM figure that Fig. 2 is prepared UTAM after two step reaming of high/low temperature.
Fig. 3 is second of deposition silver Ag@Ag nano dot classification galaxy battle array best with a thickness of detection performance made from 9 nm
The SEM of array structure schemes.
Fig. 4 is that the best Ag@Ag nano dot of detection performance is classified galaxy array detection substrate to physiological concentration (5~25 m
mol·L-1) glucose responding SERS spectrogram.
Fig. 5 is that the glucose detection response limit for the glucose SERS detection substrate that Ag@Ag nano dot is classified galaxy array is rung
It answers.
Fig. 6 is detected for the SERS that the best Ag Ag nano dot of performance is classified galaxy array and is arbitrarily selected 24 points in substrate
Response detection to the glucose of 15 m molL-1 concentration.
Specific embodiment
Embodiment 1: after this example carries out high/low temperature reaming twice to UTAM, vacuum thermal resistance deposition is made twice on UTAM
It is standby to go out to be classified the glucose SERS detection substrate of galaxy array containing the Ag@Ag nano dot of female particle and sub- particle two-stage array, system
Standby process is as shown in Figure 1.Concrete operations are as follows: first by with a thickness of 0.2 mm, purity be 99.999% aluminium flake in acetone, second
It is cleaned by ultrasonic 10 min in alcohol and water respectively, is then placed on aluminium flake in the solution of ethyl alcohol and perchloric acid, is carried out under condition of ice bath
Spare aluminium flake is made in electrochemical polish.By spare aluminium flake in 0.3 M oxalic acid 40 V voltages, aoxidize 10 h at 2 DEG C, take out,
It is put into the mixed solution of the phosphoric acid of 1.8w% chromic acid and 6w% that volume ratio is 1:1,10 h is impregnated at a temperature of 60 DEG C；With
It after deionized water repeated flushing, places into electrolytic cell, carries out 5 min of secondary oxidation using with once oxidation the same terms.It takes
After rinsing drying out, photoresist, baking molding, in copper chloride and salt acid-mixed are covered in remaining sample surfaces drop after removing inactive area
(1:1 is mixed the two by volume) 2 min of reaction are closed in liquid, aluminium are completely removed, to obtain pure UTAM.Aluminium substrate will be removed
UTAM sample barrier layer swim in downward 30 DEG C of constant temperature, mass fraction be 5% dilute phosphoric acid solution in, with remove bottom compared with
Thick barrier layer and adjustment aperture size.According to experiment needs, pore-enlargement is 70 min, obtains the bilateral that aperture is 85 nm
UTAM, wherein adjacent aperture centers are away from for 100 nm.UTAM is dipped in acetone and dissolves photoresist, the Si after being transferred to hydrophilic treated
On substrate, 80 DEG C of warm table drying.Then under conditions of 10 DEG C of constant temperature, it is placed on the phosphoric acid,diluted that mass percent concentration is 5%
In solution, pore-enlargement is 30 min, obtains the ultrathin alumina template that aperture is 95nm, as shown in Figure 2.UTAM is put into very
Reciprocal of duty cycle is 8 × 10-4 Under the conditions of Pa, 0.3~0.5 nm/s of evaporation rate, evaporation silver is with a thickness of 60 nm, then with 0.1M's
NaOH solution removes UTAM, obtains orderly aligned, silver nanoparticle point mother's array of particles that structure and morphology is uniform, diameter in silicon base and is
95 nm, with a thickness of 60 nm.Evaporation thickness is the silver of 9 nm again, and the Ag@Ag nano dot classification containing two-level configuration can be obtained
Galaxy array structure, as shown in Figure 3.The structure is used for physiological concentration (5~25 mmolL-1) glucose SERS respond survey
Examination, spectrogram is as shown in figure 4,893 cm in figure on each spectral line-1, 1124 cm-1, 1069 cm-1With 1437 cm-1Locate four grapes
The raman characteristic peak and intensity of sugar show that substrate is good to glucose responding.Structure is to extremely low concentration (0.08 mmol in Fig. 5
L-1) detection of glucose also shows that the excellent responding ability of substrate.It is any to select in order to illustrate the signal homogeneity of detection substrate
It selects 24 positions and tests substrate to 15 mmolL-1It is inclined to have obtained relative standard at characteristic peak for the response of concentration of glucose
Poor (RSD) is 3.11%, as a result as shown in fig. 6, showing good signal homogeneity.
Claims (5)
1. a kind of glucose SERS based on Ag@Ag nano dot classification galaxy array detects substrate, it is characterised in that the substrate is
It is obtained in surface of silicon by deposition, in silver nanoparticle point mother's array of particles two made of nested silver nanoparticle idea array of particles
The Ag@Ag nano dot of level structure is classified galaxy array；The diameter of silver nanoparticle point mother's particle is 91~97nm, adjacent two silver nanoparticles point
For female granular center away from for 98~102nm, the silver nanoparticle idea array of particles is distributed in silver nanoparticle point mother's particle table
Face and surrounding, particle diameter are 3~12nm；
The method of the preparation glucose SERS detection substrate based on Ag Ag nano dot classification galaxy array, specific steps are as follows:
A. the preparation of ultrathin alumina template UTAM；
B.UTAM aperture adjustment under the conditions of 30 DEG C of constant temperature；
C.UTAM is transferred on Si substrate；
D.UTAM aperture adjustment under constant temperature within the scope of 10 DEG C~15 DEG C；
E. female array of particles preparation in the glucose SERS detection substrate based on Ag@Ag nano dot classification galaxy array；
F. the glucose SERS detection substrate preparation based on Ag@Ag nano dot classification galaxy array；
Wherein, the barrier layer of the gained alumina formwork in step a is swum in 30 DEG C downward, mass percent concentration 5%
Dilute phosphoric acid solution in, pore-enlargement 70min, obtain aperture be 83~87nm UTAM；
Wherein, the UTAM/Si sample arrived in step c is placed on quality within the scope of 10 DEG C~15 DEG C under conditions of constant temperature
In the dilute phosphoric acid solution that percent concentration is 5%, pore-enlargement is 30~50min, obtains the ultra-thin oxygen that aperture is 91~97nm
Change aluminum alloy pattern plate；
Wherein, the specific steps of the step e are as follows: be 8 × 10 in vacuum degree by UTAM/Si sample obtained by step d-4Pa, evaporation
Under the conditions of 0.3~0.5nm/s of rate, evaporated metal silver is with a thickness of 60~70nm；Then remove UTAM, obtain diameter be 91~
Ag nano dot mother's array of particles of 97nm.
2. a kind of prepare the glucose SERS detection according to claim 1 based on Ag@Ag nano dot classification galaxy array
The method of substrate, it is characterised in that the specific steps of this method are as follows:
A. the preparation of ultrathin alumina template UTAM；
B.UTAM aperture adjustment under the conditions of 30 DEG C of constant temperature；
C.UTAM is transferred on Si substrate；
D.UTAM aperture adjustment under constant temperature within the scope of 10 DEG C~15 DEG C；
E. female array of particles preparation in the glucose SERS detection substrate based on Ag@Ag nano dot classification galaxy array；
F. the glucose SERS detection substrate preparation based on Ag@Ag nano dot classification galaxy array；
Wherein, the barrier layer of the gained alumina formwork in step a is swum in 30 DEG C downward, mass percent concentration 5%
Dilute phosphoric acid solution in, pore-enlargement 70min, obtain aperture be 83~87nm UTAM；
Wherein, the UTAM/Si sample arrived in step c is placed on quality within the scope of 10 DEG C~15 DEG C under conditions of constant temperature
In the dilute phosphoric acid solution that percent concentration is 5%, pore-enlargement is 30~50min, obtains the ultra-thin oxygen that aperture is 91~97nm
Change aluminum alloy pattern plate；
Wherein, the specific steps of the step e are as follows: be 8 × 10 in vacuum degree by UTAM/Si sample obtained by step d-4Pa, evaporation
Under the conditions of 0.3~0.5nm/s of rate, evaporated metal silver is with a thickness of 60~70nm；Then remove UTAM, obtain diameter be 91~
Ag nano dot mother's array of particles of 97nm.
3. according to the method described in claim 2, it is characterized in that preparing the preparation of the ultrathin alumina template UTAM
Specific steps are as follows:
A_1. by aluminium flake after pretreatment using 0.3M oxalic acid solution as electrolyte, first time anode is carried out under 40V constant voltage
Oxidation processes, time are 10~12h；Then be dipped under the conditions of temperature 60 C mass percent concentration be 6% phosphoric acid and
In the mixed liquor of 1.8% chromic acid, wherein the volume ratio of phosphoric acid and chromic acid is 1:1；It impregnates to remove obtained by the once oxidation on surface
Aluminium oxide, then using 0.3M oxalic acid solution as electrolyte, second of anodic oxidation 5min is carried out under 40V constant voltage；Carry out the
Inactive area around is cut off after two-step anodization and drips an attached layer photoresist in 60 DEG C of drying in oven；
A_2. alumina formwork obtained by step a_1 is put into the mixed liquor of copper chloride and hydrochloric acid by the volume ratio of 1:1, with removal
Remaining aluminium obtains pure UTAM.
4. according to the method described in claim 2, it is characterized in that the specific steps of the step c are as follows: step b is resulting
UTAM is swum in acetone soln, after the photoresist on surface all dissolves, UTAM is transferred to and cleans up and make hydrophilic place
On Si substrate after reason, and dried with 80 DEG C of heated at constant temperature platforms.
5. according to the method described in claim 2, it is characterized in that the specific steps of the step f are as follows: step e is resulting
Ag nano dot mother's array of particles sample is 8 × 10 in vacuum degree-4Under the conditions of Pa, 0.3~0.5nm/s of evaporation rate, evaporate again
Ag powder detects substrate with a thickness of 3~12nm to get the glucose SERS to complete Ag@Ag nano dot classification galaxy array.
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| CN107262735B (en) * | 2017-06-09 | 2019-05-03 | 吉林大学 | 2 area's fluorescent functional alloy nano point of near-infrared, preparation method and its application in terms of bioluminescence imaging |
| CN108375567B (en) * | 2018-02-24 | 2021-03-09 | 国家纳米科学中心 | Surface-enhanced Raman substrate and preparation method thereof |
| CN109504994B (en) * | 2018-12-13 | 2020-08-21 | 上海科技大学 | Novel anodic aluminum oxide template and preparation method of nano array |
| CN112630151A (en) * | 2020-12-18 | 2021-04-09 | 成都子之源绿能科技有限公司 | SERS substrate, preparation method thereof and method for measuring pesticide residues by SERS |
| CN113185144B (en) * | 2021-04-29 | 2022-06-21 | 安徽师范大学 | Preparation method of echinoid ordered micro-nano array structure |
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