CN108997592A - SERS substrate based on MOFs and the preparation method and application thereof - Google Patents
SERS substrate based on MOFs and the preparation method and application thereof Download PDFInfo
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Abstract
The present invention discloses a kind of preparation method of SERS substrate based on MOFs comprising: at least make metal salt and organic ligand hybrid reaction in a solvent, reaction temperature is 25~120 DEG C, and the time in 2h or more, forms the SERS substrate based on MOFs；The metal salt is selected from transition metal salt, and the organic ligand is selected from the organic matter containing functional group, and the functional group includes any one of aromatic rings, carboxyl and pyridine nitrogen or two or more combinations.Compared with the prior art, the present invention constructs SERS substrate by MOFs, is related to various metals-organic framework material, has good general applicability and adjustability；And the Raman response detection limit of detected organic molecule can greatly be reduced using enrichment effect in Raman detection by the method for acid corrosion expansion duct；And by metal-organic framework materials surface modification, it can detect that aldehyde material and reduce the detectable limit of aldehyde material, expand molecular detection range again.
Description
Technical field
The present invention relates to a kind of surface enhanced Raman scattering substrates and preparation method thereof, and in particular to one kind is based on metal-
Organic framework material and its surface enhanced Raman scattering substrate of derivative and preparation method thereof belong to molecular recognition technology neck
Domain.
Background technique
Surface enhanced Raman scattering (SERS) is a kind of powerful Analytical Methods of Trace, can effectively pass through molecule
With the interaction of base material, chemical structure and composition in relation to molecule are provided, there is highly sensitive, fingerprint, quick, lossless
Etc. features.Thus being with a wide range of applications in fields such as food inspection complete, chemical analysis, biological medicines.SERS substrate
There is vital effect for SERS detection.Traditional SERS substrate is generally two classes: noble metal substrate and semiconductor material
Expect substrate.Noble metal substrate, such as Au, Ag bring powerful coupled plasma, and Raman enhancement factor is up to 104-109The order of magnitude
[Science 1997,275,1102-1106.], but such substrate is expensive；Semiconductor base material, such as W18O49、
CuO2, due to strong electric charge transfer, Raman enhancement factor can achieve 106Magnitude [Chem.Commun.2016,52,2893-
2896], but the adjustability of semiconductor material is not strong.
Currently, the type limitation based on existing SERS substrate, develops the novel SERS base material based on MOFs, tool
There are excellent adjustability and being modified property and good enrichment effect, it will push the development of SERS technology significantly.
Summary of the invention
SERS (the surface increasing based on MOFs (metal-organic framework materials) that the main purpose of the present invention is to provide a kind of
Strong Raman scattering) substrate and preparation method thereof, to overcome deficiency in the prior art.
Use of the SERS substrate based on MOFs that it is another object of the present invention to provide described in detection aldehyde material
On the way.
It is another object of the present invention to provide a kind of detection methods of aldehyde material.
For achieving the above object, present invention employs following technical solutions:
The preparation method for the SERS substrate based on MOFs that the embodiment of the invention provides a kind of, comprising:
At least make metal salt and organic ligand hybrid reaction in a solvent, reaction temperature is 25~120 DEG C, the time 2h with
On, form the SERS substrate based on MOFs；
The metal salt is selected from transition metal salt, and the organic ligand is selected from the organic matter containing functional group, the function
Group includes any one of aromatic rings, carboxyl and pyridine nitrogen or two or more combinations.
The embodiment of the invention also provides the SERS substrates based on MOFs prepared by preceding method.
Purposes of the SERS substrate based on MOFs that the embodiment of the invention also provides above-mentioned in detection aldehyde material.
The embodiment of the invention also provides a kind of detection methods of aldehyde material, comprising:
SERS substrate based on MOFs is prepared using method above-mentioned；
Using the SERS substrate, aldehyde material is detected by enhancing Raman detection method.
Compared with the prior art, the beneficial effects of the present invention are:
1) embodiment of the present invention constructs surface enhanced Raman scattering substrate by metal-organic framework materials, is related to a variety of
Metal-organic framework materials cover multiple material system, increase existing surface enhanced Raman scattering substrate type, make up existing
The deficiency of surface enhanced Raman scattering substrate has good general applicability and adjustability.
2) embodiment of the present invention provides one kind based on same metal-organic framework materials as Surface enhanced Raman scattering base
Bottom, the method for reducing detectable limit.Duct transformation including MOFs is expanded duct by the method for acid corrosion, is imitated using enrichment
It answers, the Raman response detection limit of detected organic molecule can be greatly reduced in Raman detection, this method is simple, is easy to
Implement.
3) embodiment of the present invention provides one kind based on same metal-organic framework materials as Surface enhanced Raman scattering base
Bottom, the method being surface modified, increase or the interaction of supplement substrate and aldehyde radical, the further expansion detection kind of substrate
Class can detect that aldehyde material and reduce the detectable limit of aldehyde material, expands molecular detection range.
Detailed description of the invention
Fig. 1 a is SERS substrate (ZIF-67) scanning electron microscope (SEM) photograph in the embodiment of the present invention 1；
Fig. 1 b is SERS substrate in the embodiment of the present invention 3 " (acid treated) ZIF-67 after acid processing " transmission electron microscope
Figure；
Fig. 1 c is SERS substrate in the embodiment of the present invention 6 (APTES@ZIF-67) scanning electron microscope (SEM) photograph.
Fig. 1 d is SERS substrate in the embodiment of the present invention 2 (Co-TCPP MOFs) scanning electron microscope (SEM) photograph.
Fig. 2 be in the embodiment of the present invention 1 SERS substrate (ZIF-67) to the Surface enhanced Raman spectroscopy of probe molecule；
Fig. 3 is surface-enhanced Raman light of the SERS substrate in the embodiment of the present invention 2 (Co-TCPP MOFs) to probe molecule
Spectrum；
Fig. 4 is SERS substrate in the embodiment of the present invention 3 " (acid treated) ZIF-67 after acid processing " to probe molecule
Surface enhanced Raman spectroscopy；
Fig. 5 is SERS substrate in the embodiment of the present invention 6 (APTES@ZIF-67) to the surface-enhanced Raman light of probe molecule
Spectrum；
Fig. 6 a, Fig. 6 b, Fig. 6 c, Fig. 6 d are the repeatability and homogeneity of SERS substrate (ZIF-67) in the embodiment of the present invention 1
Experimental result.
Specific embodiment
For many defects of the prior art, inventor is studied for a long period of time and is largely practiced, and is able to propose the present invention
Technical solution.The technical solution, its implementation process and principle etc. will be further explained as follows.But it should
Understand, within the scope of the present invention, each technology specifically described in above-mentioned each technical characteristic of the invention and below (embodiment)
It can be combined with each other between feature, to constitute new or preferred technical side's scheme.As space is limited, herein no longer one by one
It is tired to state.
As the one aspect of technical solution of the present invention, involved in be a kind of SERS substrate based on MOFs preparation
Method, comprising:
At least make metal salt and organic ligand hybrid reaction in a solvent, reaction temperature is 25~120 DEG C, the time 2h with
On, form the SERS substrate based on MOFs；
The metal salt is selected from transition metal salt, and the organic ligand is selected from the organic matter containing functional group, the function
Group includes any one of aromatic rings, carboxyl and pyridine nitrogen or two or more combinations.
Wherein, organic ligand and central metallic ions are coordinated to form porous polycomplexation zoarium.
In some embodiments, the metal salt includes any one in nitrate, chlorate and sulfate or two
Kind or more combination, and the metal salt includes iron, cobalt, nickel, copper, any one element in zinc or two or more elements
Combination.
In some embodiments, the organic ligand includes methylimidazole, porphyrin and 2,5-Dihydroxyterephthalic acid
In any one or two or more combinations.
Wherein, organic ligand includes the organic matter containing aromatic rings, carboxyl and pyridine nitrogen functional group.
In some embodiments, the solvent includes any one in water, n,N-Dimethylformamide (DMF) and methanol
Kind or two or more combinations, but not limited to this.
In some embodiments, the time of the reaction is 2h~for 24 hours.
Thus, it is possible to obtain the MOFs (metal-organic framework materials) of different size and pattern.
In some specific embodiments, after hybrid reaction is sufficiently reacted, lower layer's washing of precipitate is taken, it is dry, obtain base
In SERS (Surface enhanced Raman scattering) substrate of MOFs (metal-organic framework materials).
In some embodiments, further includes: acid etch, the acid etch are carried out to the SERS substrate based on MOFs
For the reaction temperature used for 45~75 DEG C, the reaction time is 0.5h~3h.
Using the method for acid etch, the pore size of MOFs can be expanded, to reduce detection limit.
Further, the acid that the acid etch uses includes any one or two kinds in phosphoric acid, acetic acid, hydrochloric acid and sulfuric acid
Above combination.
Further, the concentration for the acid that the acid etch uses is 30mmol/L~60mmol/L.
In some embodiments, further includes: the SERS substrate based on MOFs is surface modified, the surface modification
Mode include any one or two or more combinations in phosphatization, amination and vulcanization.
Its object is to detect aldehyde material.
In some more preferred embodiments, the organic matter that the surface modification uses at least contain amido and/or
Sulfydryl.
In some more preferred embodiments, the solvent that the surface modification uses includes organic solvent, described to have
Solvent includes n,N-Dimethylformamide (DMF) and/or toluene, but not limited to this.
Further, the organic matter that the surface modification uses includes 3- aminopropyl triethoxysilane (APTES), thio
Any one in acetamide (TAA) and p-aminophenyl thiophenol or two or more combinations.
In some more preferred embodiments, the reaction time that the surface modification uses, temperature was for 5-20h
80-120℃。
Purpose is to be modified the surface MOFs sufficiently.
The embodiment of the present invention also provides a kind of SERS substrate based on MOFs prepared by preceding method.
The embodiment of the present invention also provides a kind of purposes of the SERS substrate based on MOFs in detection aldehyde material.
The embodiment of the present invention also provides a kind of detection method of aldehyde material, comprising:
SERS substrate based on MOFs is prepared using method above-mentioned；
Using the SERS substrate, aldehyde material is detected by surface enhanced Raman detection method.
Wherein, SERS (Surface enhanced Raman scattering) base based on MOFs (metal-organic framework materials) and its derivative
Bottom preparation method, comprising: fixed center metal ion and organic ligand respectively constantly design cvdmetallorganiccvd ligand topological structure
Different MOFs are prepared, most suitable MOFs substrate is found, greatly enhance the Raman signal of organic molecule；Based on same metal-
Organic framework material expands duct, increases enrichment effect, reduces detectable limit；Based on same metal-organic framework materials, adopt
With means such as surface modifications, aldehyde material is detected.Compared with similar substrate, MOFs and its derivative have as SERS substrate
Excellent adjustability, good enrichment effect and huge modify potentiality.
Below with reference to several preferred embodiments and attached drawing, further details of the technical solution of the present invention, it is clear that
Described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on the implementation in the present invention
Example, those of ordinary skill in the art's every other embodiment obtained without making creative work, all belongs to
In the scope of protection of the invention.The implementation condition used in following embodiment can do further adjustment according to actual needs,
The implementation condition being not specified is usually the condition in routine experiment.
Embodiment 1
Co(NO3)2For center metal ion Co2+, it is the different organic ligand of adaptation respectively: methylimidazole (functional group:
Pyridine nitrogen, aromatic rings), porphyrin (functional group: carboxyl, aromatic rings) and 2,5-Dihydroxyterephthalic acid (functional group: carboxyl,
Aromatic rings), ZIF-67, Co-TCPP MOFs, Co-MOF-74 are obtained, the SERS substrate of MOFs is obtained.The wherein reaction of ZIF-67
Time is 12h, and reaction temperature is 25 DEG C；The Co-TCPP MOFs reaction time is that for 24 hours, reaction temperature is 80 DEG C；Co-MOF-74 is anti-
For for 24 hours, reaction temperature is 120 DEG C between seasonable.If Fig. 1 a is SERS substrate (ZIF-67) scanning electron microscope (SEM) photograph, if Fig. 2 is SERS base
Bottom (ZIF-67) is to the enhancing Raman spectrum of probe molecule, by taking R6G as an example, optical maser wavelength 532nm, and detectable limit 10-7M,
Such as Fig. 6 a, 6b, 6c, 6d, it is the repeatability and homogeneity experimental result of SERS substrate (ZIF-67), it is good shows that the SERS substrate has
Good repeatability and homogeneity, RSD refers to relative standard deviation in figure.
Embodiment 2
TCPP (functional group: carboxyl, pyridine nitrogen, aromatic rings) is organic ligand, be the different central metal of adaptation respectively from
Son: Co ion, Cu ion, Zn ion obtain Co-TCPP MOFs, Cu-TCPP MOFs, Zn-TCPP MOFs, obtain MOFs's
SERS substrate, wherein the reaction temperature of these three TCPP bases MOFs is 80 DEG C, and the reaction time is for 24 hours.Wherein central metal
Ion is originated from metal salt, can be nitrate salts or sulphate form.If Fig. 1 d is SERS substrate (Co-TCPP MOFs)
Scanning electron microscope (SEM) photograph by taking R6G as an example, swashs if Fig. 3 is enhancing Raman spectrum of the SERS substrate (Co-TCPP MOFs) to probe molecule
The a length of 532nm of light wave, detectable limit 10-6M。
Embodiment 3
ZIF-67 in embodiment 1 is placed in the phosphoric acid of 40mmol/L, 60 DEG C, reacts 2h, obtain the widened ZIF- in duct
67 SERS substrate.If Fig. 1 b is SERS substrate " (acid treated) ZIF-67 after acid processing " transmission electron microscope picture, as Fig. 4 is
SERS substrate " (acid treated) ZIF-67 after acid processing " is to the enhancing Raman spectrum of probe molecule, by taking R6G as an example, laser
Wavelength is 532nm, and treated that SERS substrate detectable limit is down to 10 for acid-8M。
Embodiment 4
ZIF-67 in embodiment 1 is placed in the phosphoric acid of 30mmol/L, 75 DEG C, reacts 3h, obtain the widened ZIF- in duct
67 SERS substrate.
Embodiment 5
ZIF-67 in embodiment 1 is placed in the phosphoric acid of 60mmol/L, 45 DEG C, reacts 0.5h, it is widened to obtain duct
The SERS substrate of ZIF-67.
Embodiment 6
ZIF-67 in embodiment 1 is placed in 3- aminopropyl triethoxysilane, 120 DEG C, reacts 20h, obtain surface amine
The SERS substrate of the ZIF-67 of change.If Fig. 1 c is SERS substrate (APTES@ZIF-67) scanning electron microscope (SEM) photograph, if Fig. 5 is SERS substrate
(ZIF-67 (unmodified) and APTES@ZIF-67 (modification)) to the enhancing Raman spectrum of probe molecule, by taking benzaldehyde as an example,
Optical maser wavelength is 532nm.
Embodiment 7
ZIF-67 in embodiment 1 is placed in thioacetamide, 80 DEG C, reacts 5h, obtain the ZIF-67's of surface sulfide
SERS substrate.
In conclusion constructing SERS substrate by above-mentioned technical proposal of the invention by MOFs, being related to various metals-
Organic framework material has good general applicability and adjustability.Expand duct by the method for acid corrosion, is imitated using enrichment
It answers, the Raman response detection limit of detected organic molecule can be greatly reduced in Raman detection；By metal-organic framework
Material surface modification can detect that aldehyde material and reduction aldehyde material detection limit using modes such as such as amination, vulcanization, phosphatizations,
Molecular detection range is expanded again.
In addition, inventor also utilize it is corresponding in the alternate embodiments 1-7 such as above listed other process conditions
Process conditions have carried out corresponding test, the content of required verifying and close with embodiment 1-7 product.So herein not to each
The verifying content of a embodiment is explained one by one, and only illustrates the excellent place of the present patent application using Examples 1 to 7 as representative.
It should be noted that, in this document, under normal circumstances, the element limited by sentence " including ... ", not
There is also other identical elements in including the steps that the element, process, method or experimental facilities for exclusion.
It should be appreciated that the technical concepts and features of example described above only to illustrate the invention, it is familiar its object is to allow
The people of technique is to can understand the content of the present invention and implement it accordingly, and it is not intended to limit the scope of the present invention.
It is all any equivalent transformation or modification made according to the spirit of the present invention, should be covered by the protection scope of the present invention.
Claims (12)
1. a kind of preparation method of the SERS substrate based on MOFs, characterized by comprising:
At least make metal salt and organic ligand hybrid reaction in a solvent, reaction temperature is 25~120 DEG C, the time in 2h or more,
Form the SERS substrate based on MOFs；
The metal salt is selected from transition metal salt, and the organic ligand is selected from the organic matter containing functional group, functional group's packet
Include any one of aromatic rings, carboxyl and pyridine nitrogen or two or more combinations.
2. preparation method according to claim 1, it is characterised in that: the metal salt includes nitrate, chlorate and sulphur
Any one in hydrochlorate or two or more combinations, and the metal salt includes any one in iron, cobalt, nickel, copper, zinc
The combination of element or two or more elements；And/or the organic ligand includes methylimidazole, porphyrin and 2,5- dihydroxy is to benzene
Any one in dioctyl phthalate or two or more combinations；And/or the solvent includes water, n,N-Dimethylformamide and first
Any one in alcohol or two or more combinations.
3. preparation method according to claim 1, it is characterised in that: the time of the reaction is 2h~for 24 hours.
4. preparation method according to claim 1, it is characterised in that further include: to the SERS substrate based on MOFs into
Row acid etch, for the reaction temperature that the acid etch uses for 45~75 DEG C, the reaction time is 0.5h~3h.
5. the preparation method according to claim 4, it is characterised in that: the acid that the acid etch uses include phosphoric acid, acetic acid,
Any one in hydrochloric acid and sulfuric acid or two or more combinations；And/or the acid etch use acid concentration for
30mmol/L~60mmol/L.
6. preparation method according to any one of claims 1-5, it is characterised in that further include: to the SERS based on MOFs
Substrate is surface modified, and the mode of the surface modification includes any one or two kinds in phosphatization, amination and vulcanization
Above combination.
7. preparation method according to claim 6, it is characterised in that: the organic matter that the surface modification uses at least contains
Amido and/or sulfydryl；And/or the solvent that the surface modification uses includes organic solvent, the organic solvent includes N, N- bis-
Methylformamide and/or toluene.
8. preparation method according to claim 7, it is characterised in that: the organic matter that the surface modification uses includes 3- ammonia
Any one in propyl-triethoxysilicane, thioacetamide and p-aminophenyl thiophenol or two or more combinations.
9. preparation method according to claim 6, it is characterised in that: the reaction time that the surface modification uses is 5-
20h, temperature are 80-120 DEG C.
10. the SERS substrate based on MOFs prepared by any one of claim 1-9 the method.
11. purposes of the SERS substrate based on MOFs in detection aldehyde material as claimed in claim 10.
12. a kind of detection method of aldehyde material, characterized by comprising:
SERS substrate based on MOFs is prepared using method described in any one of claim 6-9；
Using the SERS substrate, aldehyde material is detected by surface enhanced Raman detection method.
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Cited By (5)
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| CN109799220A (en) * | 2018-12-21 | 2019-05-24 | 中国科学院合肥物质科学研究院 | Method based on histamine in metallo-chelate Raman tag technology detection tissue fluid |
| CN109926578A (en) * | 2019-02-26 | 2019-06-25 | 中国科学院化学研究所 | A kind of surface enhanced Raman scattering substrate material, preparation method and application |
| CN112051255A (en) * | 2020-09-07 | 2020-12-08 | 中国科学院苏州纳米技术与纳米仿生研究所 | Application of nano copper-based semiconductor compound in Sudan red specificity detection |
| CN113603894A (en) * | 2021-07-23 | 2021-11-05 | 上海应用技术大学 | Ag-MOF/AuNRs nano composite material and preparation and application thereof |
| CN114133582A (en) * | 2021-11-20 | 2022-03-04 | 桂林理工大学 | Preparation of three-dimensional structure Co-MOF-74 material and application of VOCs (volatile organic Compounds) of material |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109799220A (en) * | 2018-12-21 | 2019-05-24 | 中国科学院合肥物质科学研究院 | Method based on histamine in metallo-chelate Raman tag technology detection tissue fluid |
| CN109799220B (en) * | 2018-12-21 | 2021-03-26 | 中国科学院合肥物质科学研究院 | Method for detecting histamine in tissue fluid based on metal chelate Raman label technology |
| CN109926578A (en) * | 2019-02-26 | 2019-06-25 | 中国科学院化学研究所 | A kind of surface enhanced Raman scattering substrate material, preparation method and application |
| CN109926578B (en) * | 2019-02-26 | 2020-08-21 | 中国科学院化学研究所 | Surface-enhanced Raman scattering substrate material, and preparation method and application thereof |
| CN112051255A (en) * | 2020-09-07 | 2020-12-08 | 中国科学院苏州纳米技术与纳米仿生研究所 | Application of nano copper-based semiconductor compound in Sudan red specificity detection |
| CN113603894A (en) * | 2021-07-23 | 2021-11-05 | 上海应用技术大学 | Ag-MOF/AuNRs nano composite material and preparation and application thereof |
| CN113603894B (en) * | 2021-07-23 | 2022-08-16 | 上海应用技术大学 | Ag-MOF/AuNRs nano composite material and preparation and application thereof |
| CN114133582A (en) * | 2021-11-20 | 2022-03-04 | 桂林理工大学 | Preparation of three-dimensional structure Co-MOF-74 material and application of VOCs (volatile organic Compounds) of material |
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