CN107167834B - Detect the SERS active-substrate and its preparation method and application of thermoneutron radiation - Google Patents
Detect the SERS active-substrate and its preparation method and application of thermoneutron radiation Download PDFInfo
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Abstract
The invention discloses the SERS active-substrate of detection thermoneutron radiation, the SERS active-substrate of the detection thermoneutron radiation is to modify the surface reinforced Raman active substrate with thermoneutron radiation response molecule to amination slide surface and the substrate that obtains.The invention also discloses the preparation method and application of the SERS active-substrate of detection thermoneutron radiation.The present invention is effectively utilized the characteristic of nano material, is detected using Raman spectrometer, and testing cost is significantly reduced, and the present invention has many advantages, such as at low cost, quick, easy, sensitive and favorable repeatability.SERS variation is generated, it can be achieved that quickly detecting to thermoneutron radiation to thermal neutron sensitivity response based on the probe of surface modification thermoneutron radiation response molecule.
Description
Technical field
The invention belongs to SERS field of sensing technologies, and in particular to detect the SERS active-substrate and its system of thermoneutron radiation
Preparation Method and application.
Technical background
Neutron may have the charge for being difficult to detect of very little, it can be regarded as neutral particle, quality is bigger
In proton.Ultrafast neutron: energy is between 10MeV~50MeV.Wherein:
Fast neutron: energy is between 0.5MeV~10MeV.
Intermediate neutron: energy is between 1keV~0.5MeV.
Slow neutron: energy is between 0~1keV, including epithermal neutron, thermal neutron, cold neutrons and resonance neutron.Wherein can
Amount is about that the thermal neutron of 0.025eV is known as thermal neutron.Neutron irradiation flourishes with nuclear technology, gradually comes into human lives
In.One side nuclear technology is used for the radiotherapy of cancer, power generation etc.；On the other hand, organism and the Nature are deposited in nuclear radiation
In serious pollution and threat.Therefore it is precisely detected and is effectively controlled most important.
Measure thermal neutron it is most suitably used be boron trifluoride proportional counter, casing pack10BF3Gas, commonly referred to as10BF3
Counting tube.After neutron enters counting tube, (n, α) nuclear reaction occurs with boron；In addition,10The scintillator of boron scintillation counter is ZnS
(Ag) add boron compound, (n, α) nuclear reaction is utilized to detect neutron；Secondly also3He counting tube is the core using neutron and helium
It reacts made of (n, p) principle.
Surface enhanced Raman scattering (SERS) is as a kind of spectral analysis technique for having development potentiality, in chemistry, physics, life
The various aspects such as object, medicine, environmental monitoring, public safety have obtained certain application.Non-toxic, lossless, high sensitivity can weigh
Renaturation is its big advantage by force.Therefore, have in terms of the evaluation of thermoneutron radiation process in conjunction with Raman technology it is very big before
Scape.
Summary of the invention
Goal of the invention: technical problem to be solved by the invention is to provide the SERS active-substrates of detection thermal neutron.
There is provided the preparation methods of the SERS active-substrate of detection thermal neutron for the present invention also technical problems to be solved.
There is provided the SERS active-substrates of detection thermal neutron in detection thermal neutron for the present invention also technical problems to be solved
Radiate the application of aspect.
There is provided a kind of materials for detecting thermoneutron radiation for the present invention also technical problems to be solved.
There is provided a kind of methods for detecting thermoneutron radiation for the last technical problems to be solved of the present invention.
Technical solution: in order to solve the above-mentioned technical problems, the present invention provides the SERS active-substrates for detecting thermal neutron to be
Surface reinforced Raman active substrate with thermoneutron radiation response molecule.
Specifically, being by the above-mentioned surface reinforced Raman active substrate modification with thermoneutron radiation response molecule to amino
Glass carrier surface and the substrate obtained.
Wherein, above-mentioned thermoneutron radiation response molecule is 3- sulfydryl benzene10Boric acid, 4- sulfydryl benzene10Boric acid, 3- aminobenzene10Boron
Acid or 4- aminobenzene10One or more of boric acid.
Wherein, above-mentioned surface reinforced Raman active substrate is gold, silver, the single-element of copper or the compound liquid phase of multiple element
Suspension or modify gold, silver, the single-element of copper or the compound liquid phase suspension liquid of multiple element to surface of solid phase carriers obtain
The solid phase surface obtained enhances Raman active substrate.
Wherein, above-mentioned surface reinforced Raman active substrate is gold nanoshell probe, the Jenner in the gold nanoshell probe
Rice shell diameter is 100nm~300nm.
Preferably, the gold nanoshell diameter in above-mentioned gold nanoshell probe is 165~175nm.
The content of present invention further includes the preparation method of the SERS active-substrate of above-mentioned detection thermal neutron, including following step
It is rapid:
1) preparation of surface reinforced Raman active substrate: the surface reinforced Raman active substrate be gold, silver, copper it is single
Element or the compound liquid phase suspension liquid of multiple element or by gold, silver, the single-element of copper or the compound liquid phase suspension of multiple element
Liquid modification, which obtains solid phase surface to surface of solid phase carriers, enhances Raman active substrate；
2) preparation of the surface reinforced Raman active substrate of thermoneutron radiation is detected: in surface reinforced Raman active substrate
There is thermoneutron radiation to respond molecule for modification, obtain the SERS active-substrate of detection thermoneutron radiation.
Specifically, the preparation method of the active substrate of the gold nanoshell probe based on detection thermal neutron, including following step
It is rapid:
1) preparation of gold nanoshell；
2) preparation of probe: in gold nanoshell surface modification there is thermoneutron radiation to respond molecule, obtains detection thermal neutron
The gold nanoshell probe of radiation；
3) it detects the preparation of the SERS active-substrate of the gold nanoshell probe of thermoneutron radiation: will test thermoneutron radiation
Gold nanoshell probe modification is cleaned to amination slide surface, and sufficiently, prepares the Jenner of stand-by detection thermoneutron radiation
The SERS active-substrate of rice shell probe.
Specifically, detection thermoneutron radiation gold nanoshell probe SERS active-substrate the preparation method comprises the following steps: prepare not
With the suspension of the gold nanoshell probe with thermoneutron radiation response molecule of concentration, respectively by various concentration probe suspension
Respectively with amidized glass slide, after being incubated for altogether, after sufficiently being cleaned with deionized water, spontaneously dries, then carries out SERS detection,
Select most stable of one group of the ratio of SERS feature peak intensity as optimal condition.
Wherein, the ratio of this feature peak intensity is 1574cm-1With 1585cm-1Locate the ratio of intensity.
Wherein, above-mentioned thermoneutron radiation response molecule is 3- sulfydryl benzene10Boric acid, 4- sulfydryl benzene10Boric acid, 3- aminobenzene10Boron
Acid or 4- aminobenzene10One or more of boric acid.
The content of present invention further includes the SERS active-substrate of above-mentioned detection thermal neutron in terms of detecting thermoneutron radiation
Using.
The content of present invention further includes a kind of material for detecting thermoneutron radiation, and the material includes the detection thermal neutron
The SERS active-substrate of radiation.
The content of present invention further includes a kind of method for detecting thermoneutron radiation, and the detection method is by the detection heat
The SERS active-substrate of neutron irradiation is exposed to paraffin and lead to the radiating aperture slowing down and gamma-rays of neutron emitter
Absorption after neutron source aperture in, take out measure its Surface enhanced Raman spectroscopy, according to the ratio of characteristic spectral line intensity
The intensity or dosage of neutron irradiation is calculated.
Wherein, above-mentioned environment to be measured is that different time or radiation different distance are radiated in neutron emitter.
Wherein, the above-mentioned method based on SERS detection neutron irradiation process are as follows: obtain substrate SERS spectrogram and probe
SERS spectrogram, and compare proof its there is no otherness；According to the ratio of feature peak intensity in the substrate SERS spectrogram and heat
The corresponding relationship of neutron irradiation time and radiation length carry out data processing, and summarize the SERS spectrogram phase of substrate during this
To the relationship of intensity rate.
Working principle of the present invention: the present invention utilizes the signaling molecule of the thermoneutron radiation sensitivity with obvious SERS signal,
It is modified on gold nanoshell surface, obtains probe.The diameter of gold nanoshell is 165~175nm, and diameter is in the range
Gold nanoshell has strong resonance to the laser of 785nm.Wherein, it is based on surface modification 4- sulfydryl benzene10The probe of boric acid, to heat
Neutron irradiation sensitivity response generates SERS and changes the evaluation, it can be achieved that thermoneutron radiation intensity；Based on this principle, then tie
The cheap and quick preparation of SERS active-substrate is closed, the two combines, and realizes the inspection of quick and high performance-price ratio thermoneutron radiation
It surveys.By the evaluation to different radiated times and radiation length, a series of variation of the relative intensity of SERS characteristic peaks is obtained, it is real
Now to the detection of neutron radiative process.
The utility model has the advantages that compared with the existing technology, the invention has the following advantages that
(1) present invention utilizes gold nanoshell probe after the surface-assembled of function glass carrier, with the thermal neutron given off
Interaction, at any time and significant change occurs for the variation of sample, SERS signal, realizes the spectrum detection method of thermal neutron detection
Evaluation, by paraffin and lead to the radiating aperture slowing down and gamma-ray absorption of neutron emitter, to improve thermal neutron
The accuracy of detection.
(2) present invention is effectively utilized the characteristic of nano material, is detected, is significantly reduced using Raman spectrometer
Testing cost, the present invention have many advantages, such as at low cost, quick, easy, sensitive and favorable repeatability.Based on surface modification thermal neutron
The probe of rdaiation response molecule generates SERS variation, it can be achieved that the evaluation radiated to heating seed to thermal neutron sensitivity response；Base
In this principle, in conjunction with the cheap and quick preparation of SERS active-substrate, the two is combined, and is realized quick and high performance-price ratio
The detection of neutron irradiation.By the evaluation to different radiated times and radiation length, a series of the opposite of SERS characteristic peaks is obtained
The detection to neutron radiative process is realized in the variation of intensity.
Detailed description of the invention
Fig. 1 shows the schematic diagram of the detection thermoneutron radiation of the SERS active-substrate based on gold nanoshell probe.It is explained in figure
The preparation process and detection process of substrate are stated；
Fig. 2 shows the scanning electron microscope diagram piece of prepared golden shell, the scanning electron microscope (SEM) photograph of constructed substrate, thermal neutron
Respond the Raman characterization figure of SERS substrate preparation process, prepared base Evaluation for Uniformity figure；
Probe is by completely anti-after Fig. 3 shows the SERS spectrogram of the probe based on gold nanoshell substrate and idealizes radiation
SERS spectrogram comparison diagram after answering；
Fig. 4 show thermal neutron detection substrate radiated in neutron emitter the SERS testing result after different time and
The variation line chart of corresponding relative intensity；
Fig. 5 shows thermal neutron detection substrate different radiation lengths in neutron emitter, radiates SERS after twenty minutes
The variation line chart of testing result and corresponding relative intensity；
Probe is complete after Fig. 6 shows the SERS spectrogram of the probe molecule based on silver nanoparticle shell substrate and idealizes radiation
SERS spectrogram comparison diagram after full response；
Fig. 7 show thermal neutron detection suspension radiated in neutron emitter the SERS testing result after different time with
And the variation line chart of corresponding relative intensity.
Specific embodiment
The synthesis of 1 gold nanoshell of embodiment and solid phase surface enhance constructing for Raman active substrate
1, the synthesis of gold nanoshell:
The SiO for being about first 110nm in diameter2Surface carries out amination modification and adsorbs the gold nano grain shape of 2-3nm
At composite particles, being formed by composite particles is gold nanoshell growth precursors object；Again using hydrogen peroxide as reducing agent, in precursor
Gold chloride is constantly restored under the catalysis on surface and is constantly deposited on its surface, to form certain thickness complete gold nano
Shell.Then 3000rpm is centrifuged 10min, abandons supernatant, collects precipitating, and resuspension obtains gold nanoshell suspension (OD700nm=1.0) it, keeps away
Light saves backup.The diameter of the gold nanoshell is 165~175nm, and the gold nanoshell of diameter in the range swashs 785nm
Light has strong resonance (in addition to the present embodiment, other methods can also prepare the nano material).
2, the preparation of solid phase surface enhancing Raman active substrate:
Taking a volume is the volumetric flask of 100mL, and 15.4g 4- sulfydryl benzene is added thereto10Boric acid is dissolved in 100mL's
In 10% ethanol water, ultrasound is mixed.Common commercial glass carrier is cleaned three times with ethyl alcohol, 30 minutes every time；Later
After drying, it is immersed into the ethanol solution of the aminopropyl triethoxysilane of 1% (v/v), after processing 24 hours, then uses ethyl alcohol
Cleaning is three times.Then dry, obtain amino glass carrier, by the amino glass carrier with glass cutter be cut into area be 0.5cm ×
The fritter of 0.5cm.Take out 10 μ L (OD700nm=2.0) the gold nanoshell suspension of above-mentioned preparation, being added dropwise in area is 0.5cm
The amino glass carrier of × 0.5cm, substrate constructs completion after 30 minutes.Every piece of the substrate is individually positioned in equipped with 1mL 4- mercapto
Base benzene10In the centrifuge tube of boric acid solution, impregnate 24 hours.Glass slide is taken out later, is respectively washed 3 with deionized water and ethyl alcohol
It is secondary, obtain active substrate.
Proof-Of Principle:
Taking a volume is the volumetric flask of 100mL, and 13.2g benzenethiol sodium is added thereto and is dissolved in the aqueous solution of 100mL,
Ultrasound mixes.Common commercial glass carrier is cleaned three times with ethyl alcohol, 30 minutes every time；After drying later, it is immersed into 1%
(v/v) ethanol solution of aminopropyl triethoxysilane after processing 24 hours, then is cleaned three times with ethyl alcohol.Then it dries, obtains
Amino glass carrier is obtained, which is cut into the fritter that area is 0.5cm × 0.5cm with glass cutter.Take out 10 μ L
(OD700nm=2.0) gold nanoshell suspension is added dropwise in the amino glass carrier that area is 0.5cm × 0.5cm, after 30 minutes
Substrate constructs completion.Every piece of the substrate is individually positioned in the centrifuge tube equipped with 1mL benzenethiol sodium solution, is impregnated 24 hours.
Glass slide is taken out later, is respectively washed 3 times with deionized water and ethyl alcohol, is obtained the substrate of benzenethiol sodium.By comparing benzenethiol
Sodium and 4- sulfydryl benzene10The SERS spectrogram of boric acid compares, the feasibility of judgment experiment.Concrete outcome is as shown in Figure 3.
The test experience of the different neutron irradiation times of embodiment 2
Neutron irradiation responds the synthesis of substrate referring to the method for embodiment 1, and this embodiment is not repeated.
The evaluation of solid phase surface enhancing Raman active substrate: substrate is attached to paraffin and lead packaged block rear, is placed in
In radiant tunnel, the substrate that same treatment obtains is placed in the same position in duct, radiates the different time every time.Radiated time
It is respectively as follows: 10 seconds, 20 seconds, 40 seconds, 60 seconds, 120 seconds, 180 seconds, 300 seconds, 600 seconds, 1200 seconds.
Experimental result: 10 test points that each substrate randomly selects are recorded respectively using surface-enhanced Raman spectroscopy
SERS spectra seeks averaged spectrum, and records and be depicted as integration map, as shown in Figure 4 A.It is corresponding in turn to blank group from top to bottom,
10 seconds, 20 seconds, 40 seconds, 60 seconds, 120 seconds, 180 seconds, 300 seconds, 600 seconds, 1200 seconds groups.And according to spectrum change situation, choose
Reference peak 1574cm-1With 1585cm-1The relative ratio of intensity draw line chart as shown in Figure 4 B.It can from result
Out, under different radiated times, the 4- sulfydryl benzene of natural component10The content that boric acid raying is partially converted into benzenethiol is different.
The result can intuitively be found out from spectrogram and line chart.In addition, when radiated time reach 300 seconds and after, spectrum
Significant change no longer occurs, corresponding relative intensity also tends towards stability, this shows contained in the substrate to occur with thermal neutron
Effect10Boron is by fully reacting.
The test experience of the different neutron irradiation distances of embodiment 3
The substrate synthesis of neutron irradiation response is referring to the method for embodiment 1, and this embodiment is not repeated.
The evaluation of solid phase surface enhancing Raman active substrate: substrate is attached to paraffin and lead packaged block rear, is placed in
In radiant tunnel, the substrate that same treatment obtains is placed in the different location in duct, Distance Layout point distance be successively 0cm,
2cm, 4cm, 6cm, 8cm, 10cm, the time radiated every time are 1200 seconds.
Experimental result: 10 test points that each substrate randomly selects are recorded respectively using surface-enhanced Raman spectroscopy
SERS spectra seeks averaged spectrum, and records and be depicted as integration map, as shown in Figure 5A.Corresponding radiation length from top to bottom
It is successively 0cm, 2cm, 4cm, 6cm, 8cm, 10cm, and according to spectrum change situation, chooses reference peak 1574cm-1With 1585cm-1
The relative ratio of intensity draw line chart as shown in Figure 5 B.As can be seen from the results, natural under different radiation lengths
The 4- sulfydryl benzene of ingredient10The content that boric acid raying is partially converted into benzenethiol is different.The result can be intuitively from spectrogram
And find out in line chart.With the expansion of distance, the content of substrate surface benzenethiol is gradually reduced, and decrease speed by becoming fastly
Slowly.The feasibility and sensitivity of the result further instruction this method.
The synthesis of 4 silver nanoparticle shell of embodiment and solid phase surface enhance constructing for Raman active substrate
1, the synthesis of silver nanoparticle shell:
The SiO for being first 110 ± 5nm by 25mg diameter2Nanosphere is evenly dispersed to be in 13mL ethyl alcohol；Then 1g is gathered
Vinylpyrrolidone is dissolved in above-mentioned solution；Then 0.1g silver nitrate is dissolved in ammonium hydroxide dilution to (0.2ml ammonium hydroxide is dissolved in
In 2mL water)；And then a few minutes are mixed in two kinds of solution；Finally mixed liquor is dispensed into reaction kettle, 120 DEG C of reactions
12h.After reaction, after reaction kettle natural cooling, 5000rpm is centrifuged 2min, is cleaned multiple times with ethyl alcohol up to silver nanoparticle shell
Suspension, and collect into 1mL.The diameter of the silver nanoparticle shell is 165~175nm.
2, the preparation of solid phase surface enhancing Raman active substrate:
Taking a volume is the volumetric flask of 100mL, and 15.4g 4- sulfydryl benzene is added thereto10Boric acid is dissolved in 100mL's
In 10% ethanol water, ultrasound is mixed.Common commercial glass carrier is cleaned three times with ethyl alcohol, 30 minutes every time；Later
After drying, it is immersed into the ethanol solution of the aminopropyl triethoxysilane of 1% (v/v), after processing 24 hours, then uses ethyl alcohol
Cleaning is three times.Then dry, obtain amino glass carrier, by the amino glass carrier with glass cutter be cut into area be 0.5cm ×
The fritter of 0.5cm.The above-mentioned silver nanoparticle shell suspension of 10 μ L is taken out, is added dropwise and carries glass in the amination that area is 0.5cm × 0.5cm
Piece, substrate constructs completion after 30 minutes.Every piece of the substrate is individually positioned in equipped with 1mL 4- sulfydryl benzene10The centrifugation of boric acid solution
Guan Zhong impregnates 24 hours.Glass slide is taken out later, is respectively washed 3 times with deionized water and ethyl alcohol, obtains active substrate (except this
Except embodiment, other methods can also prepare the nano material).
Every piece of the substrate is individually positioned in the centrifuge tube equipped with 1mL benzenethiol sodium solution, is impregnated 24 hours.It takes later
Glass slide out is respectively washed 3 times with deionized water and ethyl alcohol, obtains the substrate of benzenethiol sodium.Pass through comparison benzenethiol sodium and 4-
Sulfydryl benzene10The SERS spectrogram of boric acid compares, the feasibility of judgment experiment.Concrete outcome is as shown in Figure 6.The result can be seen that
On the one hand illustrate the SERS result after such probe molecule adsorbs on silver nanoparticle shell and its knot after adsorbing on gold nanoshell
Apparent otherness is not present in fruit；On the other hand also demonstrating the substrate based on silver nanoparticle shell can be used in the test.
The experiment of the different radiated times of the suspended surface enhancing Raman active substrate of 5 liquid phase of embodiment
The suspended surface enhancing Raman active substrate evaluation of liquid phase: each centrifuge tube contains the 4- sulfydryl of the 1mM of 200 μ L
Benzene1010% (v/v) ethanol water of boric acid, the gold nanoshell suspension for then taking 10 μ L embodiments 1 to prepare are mixed with 24
Hour.After centrifuge tube to be attached to paraffin and lead packaged block respectively, it is put into radiation channel, same position is placed in and radiation is different
Time.Radiated time is 0,1 minute, 2 minutes, 3 minutes, 5 minutes, 10 minutes and 20 minutes.
Experimental result: by treated, precipitating is collected by centrifugation in sample respectively.Then repeatedly centrifugation resuspension is not inhaled with removing
Attached residue is finally distributed in 10 μ L water, solid phase slide or silicon wafer etc. is then added dropwise above, then pass through SERS spectra
10 random selection points of each substrate are recorded, obtain averaged spectrum, as shown in Figure 7 A.Correspond to control group from top to bottom,
1min, 2min, 3min, 5min, 10min, 20min group.According to spectrum change, 1574cm is selected-1And 1585cm-1Locate reference peak
The relative scale of intensity draws line chart shown in Fig. 7 B.It can be seen that by the result of comparison diagram 4 and examined using solid phase substrate
The sensitivity of survey is higher, and the time of required detection is shorter.
Claims (9)
1. detecting the SERS active-substrate of thermoneutron radiation, which is characterized in that the SERS active group of the detection thermoneutron radiation
Bottom is the surface reinforced Raman active substrate with thermoneutron radiation response molecule, and the thermoneutron radiation response molecule is 3- mercapto
Base benzene10Boric acid, 4- sulfydryl benzene10Boric acid, 3- aminobenzene10Boric acid or 4- aminobenzene10One or more of boric acid.
2. the SERS active-substrate of detection thermoneutron radiation according to claim 1, which is characterized in that the surface enhanced
Raman active substrate is gold, silver, the suspension of the single-element of copper or the compound liquid phase of multiple element or by gold, silver, the list of copper
The solid phase surface enhancing Raman active that one element or the compound liquid phase suspension liquid modification of multiple element are obtained to surface of solid phase carriers
Substrate.
3. the SERS active-substrate of detection thermoneutron radiation according to claim 1, which is characterized in that the surface enhanced
Raman active substrate is gold nanoshell probe, and the gold nanoshell diameter in the gold nanoshell probe is the nm of 100 nm ~ 300.
4. the preparation method of the SERS active-substrate of the described in any item detection thermoneutron radiations of claim 1 ~ 3, feature exist
In, comprising the following steps:
1) preparation of surface reinforced Raman active substrate: the surface reinforced Raman active substrate is the single-element of gold, silver, copper
Or the compound liquid phase suspension liquid of multiple element or gold, silver, the single-element of copper or the compound liquid phase suspension liquid of multiple element are repaired
It adorns surface of solid phase carriers and obtains solid phase surface enhancing Raman active substrate；
2) it detects the preparation of the surface reinforced Raman active substrate of thermoneutron radiation: being modified in surface reinforced Raman active substrate
Molecule is responded with thermoneutron radiation, obtains the SERS active-substrate of detection thermoneutron radiation.
5. the preparation method of the SERS active-substrate of detection thermoneutron radiation according to claim 4, which is characterized in that institute
Stating thermoneutron radiation response molecule is 3- sulfydryl benzene10Boric acid, 4- sulfydryl benzene10Boric acid, 3- aminobenzene10Boric acid or 4- aminobenzene10Boron
One or more of acid.
6. the SERS active-substrate of the described in any item detection thermoneutron radiations of claim 1 ~ 3 is in terms of detecting thermoneutron radiation
Application.
7. a kind of material for detecting thermoneutron radiation, which is characterized in that the material includes that claim 1 ~ 3 is described in any item
Detect the SERS active-substrate of thermoneutron radiation.
8. it is a kind of detect thermoneutron radiation method, which is characterized in that the detection method be by claim 1 ~ 3 any one institute
The SERS active-substrate for the detection thermoneutron radiation stated is exposed in environment to be measured, is taken out and is measured its Surface enhanced Raman spectroscopy,
According to the ratio of characteristic spectral line intensity, it can the intensity or dosage of thermoneutron radiation is calculated.
9. the method for detection thermoneutron radiation according to claim 8, which is characterized in that the environment to be measured is thermal neutron
Different time or radiation different distance are radiated in radiation source.
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