CN104668580A - Preparation of ferroferric oxide/gold nanometer composite material and method for rapidly detecting rhodamine molecules by using ferroferric oxide/gold nanometer composite material - Google Patents
Preparation of ferroferric oxide/gold nanometer composite material and method for rapidly detecting rhodamine molecules by using ferroferric oxide/gold nanometer composite material Download PDFInfo
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- CN104668580A CN104668580A CN201510100521.9A CN201510100521A CN104668580A CN 104668580 A CN104668580 A CN 104668580A CN 201510100521 A CN201510100521 A CN 201510100521A CN 104668580 A CN104668580 A CN 104668580A
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Abstract
The invention discloses a method for rapidly detecting rhodamine molecules by using a ferroferric oxide/gold nanometer composite material. The method comprises the following steps: mechanically mixing the rhodamine molecules serving as probe molecules and the ferroferric oxide/gold nanometer composite material serving as an SERS (Surface Enhanced Raman Scattering) substrate with probe molecules of different concentrations for a certain time period; separating a substrate material of which the surface adsorbs the probe molecules out with a magnetic separation method; coating the substrate material on a glass slide, and airing for use in Raman detection. Meanwhile, the invention further provides preparation of the ferroferric oxide/gold nanometer composite material. The ferroferric oxide/gold nanometer composite material has the rapid magnetic response of ferroferric oxide, so that the detection of rhodamine by taking a pure gold nanometer material as the substrate is simplified, and the detection limit can be up to the order of magnitude 10<-8>. The SERS substrate has a wide application prospect in the fields of foods additives, heavy metal detection and the like.
Description
Technical field
The invention belongs to the preparation of nano composite material and the application in surface Raman enhancement field thereof, relate to a kind of preparations and applicatio of surface Raman enhancement (SERS) substrate of quick detection rhodamine molecule.
Background technology
Rhodamine is that one has fresh pinkish Prof. Du Yucang dyestuff, belongs to non-food raw material, and in vitro cell fluorescence dyeing and the field such as coloured glass, characteristic fireworks and firecrackers obtain certain application.In addition, it is also used as food additives, proved that rhodamine can be carcinogenic owing to testing afterwards, so do not allowed it for food colouring art now, but still have the bad retailer of part to it can be used as the substitute of tonyred, very large threat is caused to the healthy diet of people, various simultaneously along with food variety, cause its experiment testing conditions requirement also to become very harsh.
The method of current detection rhodamine mainly contains liquid chromatographic detection and Raman strengthens detection, and the substrate wherein for Raman detection is more, such as detects rhodamine using proof gold nano material as substrate, but its cost is higher, operation is relatively loaded down with trivial details.In view of shortcoming many above, be so necessary to work out a kind of substrate that fast and conveniently can detect rhodamine content.
Summary of the invention
For problems of the prior art, the invention provides the preparation method of a kind of tri-iron tetroxide/gold nano composite, using this composite as surface Raman enhancement (SERS) substrate quick and precisely detecting rhodamine molecule content.Detecting rhodamine molecule content object fast to reach, present invention also offers the method being used for this composite to detect fast rhodamine molecule.Simplify traditional operating process detecting rhodamine molecule using proof gold nano material as substrate, and its detectable limit can reach 10
-8the order of magnitude.Composite of the present invention, as surface Raman enhancement (SERS) substrate quick and precisely detecting rhodamine molecule content, will have broad application prospects in the field such as food additives, heavy metal analysis.
In order to solve the problems of the technologies described above, the preparation method of a kind of tri-iron tetroxide/gold nano composite that the present invention proposes, comprises the following steps:
Step one, obtain by hydro-thermal method the ferroferric oxide nano granules that particle diameter is 120 ~ 170nm, for subsequent use;
Step 2, according to absolute ethyl alcohol, water and mass concentration are the volume ratio of the ammoniacal liquor of 28% is that 60:15:1 obtains mixed solution A, the ferroferric oxide nano granules taking step one obtained is dissolved in mixed solution A, quality-the volumetric concentration of ferroferric oxide nano granules and mixed solution A is 1 ~ 5mg/ml, ultrasonic 30min, be that 2:1 adds ethyl orthosilicate according to the mol ratio of tri-iron tetroxide and ethyl orthosilicate, 10 ~ 12h is reacted under room temperature, thus in the surface of ferroferric oxide nano granules parcel layer of silicon dioxide, the shell thickness of described silica is 5 ~ 6nm,
Step 3, be that 15:1 adds two amino silicane coupling agent and reacts 10 ~ 13h according to the volume ratio of two amino silicane coupling agent and ethyl orthosilicate, with deionized water and absolute ethanol washing repeatedly, isolate the tri-iron tetroxide of surface amination;
Step 4, be that 1:1 prepares mixed solution B according to the volume ratio of 0.075wt% sodium borohydride and 1wt% natrium citricum, for subsequent use; According to volume ratio 1:99 by soluble in water for 1wt% aqueous solution of chloraurate, magnetic agitation 15min mixes; At room temperature, add isopyknic 1wt% natrium citricum with 1wt% aqueous solution of chloraurate, then add the mixed solution B doubling 1wt% aqueous solution of chloraurate volume; Magnetic agitation reaction 30-60min, prepares gold nano seed solution;
Step 5, the preparation of golden salting liquid of reducing: be that 0.25mg/ml adds sodium carbonate in deionized water according to quality-volumetric concentration, mechanical agitation 10min, add 1wt% aqueous solution of chloraurate afterwards, the volume ratio of 1wt% aqueous solution of chloraurate and deionized water is 3:200, under lucifuge, mechanical agitation 10 ~ 12h, stand-by;
Step 6, be 2 ~ 6mg/ml according to quality-volumetric concentration, in the tri-iron tetroxide of the surface amination that step 3 is obtained and the obtained gold nano seed solution of step 4, mechanical agitation 2-3h, then with water and the washing of absolute ethyl alcohol magnetism separate method repeatedly;
Step 7, the product that step 6 obtains is joined in the obtained reduction gold salting liquid of step 5, wherein, gold nano seed solution is 1.7 ~ 3.4:1 with the volume ratio of the golden salting liquid of reduction, stirring is that 400:1 adds formaldehyde according to the volume ratio of reduction golden salting liquid and formaldehyde again, reacts 10min;
Step 8, be that 1.7 ~ 3.4:1 continues to add and reduce golden salting liquid according to gold nano seed solution and the volume ratio of the golden salting liquid of reduction, stirring is that 400:1 adds formaldehyde according to the volume ratio of the golden salting liquid of reduction and formaldehyde again, reacts 10min;
The operation of step 9, repetition N step 8, wherein N is 5 ~ 10; By deionized water repeatedly washed product, until remove solvent completely, finally obtain tri-iron tetroxide/gold nano composite.
The invention allows for the method utilizing tri-iron tetroxide/gold nano composite to detect rhodamine molecule fast, it is characterized in that, using tri-iron tetroxide/gold nano composite as SERS base material, the saturation magnetization of described SERS base material is 48.7-50emu/g, rhodamine molecule is Raman probe molecule, and comprises the following steps:
Step one, by described SERS base material respectively with 10
-8, 10
-7m, 10
-6, 10
-5, 10
-4the rhodamine liquor of mol/l concentration fully mixes, and the SERS base material of the Raman probe molecule that utilized magnetism separate method by adsorption is separated, and is coated on slide and dries, obtained test samples, stand-by;
Step 2, test samples obtained for step one is placed in Reinshaw laser Raman spectrometer, wherein: frequency range is 2500cm
-1-0cm
-1, wavelength is 532nm, and laser attenuation power is 0.01-0.05%, and in a continuous mode, adopt the 1-3s time for exposure, multi collect, completes the Raman detection of rhodamine.
Compared with prior art, the invention has the beneficial effects as follows:
1, using the tri-iron tetroxide prepared by the present invention/gold nano composite as SERS substrate, there is the spectral characteristic of noble metal, and sample preparation is fast, low cost and other advantages.
2, tri-iron tetroxide of the present invention/gold nano composite has magnetic as SERS substrate, compared to traditional proof gold nano material as SERS substrate, is conducive to discrete testing thing, makes to detect easy and simple to handleization.
3, the detection method provided in the present invention, compared with the detection method of existing rhodamine, has highly sensitive feature, and its detectability can reach 10
-8mol/l.
4, tri-iron tetroxide/gold nano composite of preparing of the present invention is as SERS substrate, and also can be used for heavy metal Hg, the detection of food additives melamine, detection method is similar to detection rhodamine.
Accompanying drawing explanation
Fig. 1 is the synthesis mechanism schematic diagram of tri-iron tetroxide of the present invention/gold nano composite;
Fig. 2 is the Fe of preparation in the embodiment of the present invention 1
3o
4nano particle and Fe
3o
4-SiO
2the TEM photo of Nano composite granules, wherein, (a) is Fe
3o
4the TEM photo of nano particle, (b) is Fe
3o
4-SiO
2the TEM photo of Nano composite granules;
Fig. 3 is the nanogold particle of preparation in the embodiment of the present invention 1 and final Fe
3o
4the TEM photo of-SiO2-Au nano particle, wherein, the TEM photo that (a) is nanogold particle, (b) is Fe
3o
4the TEM photo of-SiO2-Au nano particle;
Fig. 4 is the Fe of preparation in the embodiment of the present invention 3
3o
4and Fe
3o
4-SiO
2-Au nano particle magnetic hysteresis the tropic at room temperature.
Fig. 5 is the HAuCl of different quality ratio
4and Au-Fe
3o
4-SiO
2with the graph of a relation of SERS detectable limit.
Detailed description of the invention
Be described in further detail technical solution of the present invention below in conjunction with the drawings and specific embodiments, described specific embodiment only explains the present invention, not in order to limit the present invention.
Fig. 1 shows the synthesis mechanism of tri-iron tetroxide of the present invention/gold nano composite, preparation process comprises the synthesis of tri-iron tetroxide, tri-iron tetroxide surface parcel silica, particle surface amination process, seed mediated growth method prepares magnetic core gold shell Nano composite granules.
The preparation method of embodiment 1, a kind of tri-iron tetroxide/gold nano composite, comprises the following steps:
Step one, obtain ferroferric oxide nano granules by hydro-thermal method: be dissolved in 30ml ethylene glycol by 1.0g Iron trichloride hexahydrate, 4.0g anhydrous sodium acetate and 2ml ethylenediamine respectively, vigorous stirring 30min, then be transferred in polytetrafluoroethyllining lining reactor, 7h is reacted at 200 DEG C, the product deionized water obtained and the washing of ethanol magnetism separate method are repeatedly, stand-by;
Step 2, in the surface of ferroferric oxide nano granules parcel layer of silicon dioxide: taking the obtained ferriferrous oxide nanometer material of 0.4g step one, to be dissolved in 120ml absolute ethyl alcohol, 30ml water and 2ml mass concentration be in the mixed liquor of the ammoniacal liquor of 28%, add 0.2ml ethyl orthosilicate (TEOS) after ultrasonic 30min, under room temperature, react 10h; Thus in the surface of ferroferric oxide nano granules parcel layer of silicon dioxide, the shell thickness of described silica is about 5nm;
Step 3, the particle surface that step 2 obtains is carried out amination modification: on the basis of step 2, add 3ml two amino silicane coupling agent reaction 12h again, with deionized water and absolute ethanol washing repeatedly, isolate the tri-iron tetroxide of surface amination, stand-by;
The preparation of step 4, gold nano seed: be dissolved in 99ml water by 1ml1wt% aqueous solution of chloraurate, magnetic agitation 15min mixes; At room temperature add 1ml1wt% natrium citricum again, finally add the mixed liquor of 1ml0.075wt% sodium borohydride and 1ml1wt% natrium citricum, then magnetic agitation reaction 50min, prepare gold nano seed solution, stand-by;
Step 5, the preparation of golden salting liquid of reducing: in 200ml deionized water, add 50mg sodium carbonate, machinery stirs 10min soon, adds 3ml1wt% aqueous solution of chloraurate afterwards, and lucifuge mechanical agitation 12h is stand-by;
In the gold nano seed solution that step 6, the tri-iron tetroxide of surface amination step 3 obtained and step 4 are obtained, mechanical agitation 2h, with water and the washing of absolute ethyl alcohol magnetism separate method repeatedly;
Step 7, the 40ml that product is added step 5 obtained reduce in golden salting liquid, stir and add 0.1ml formaldehyde again, reaction 10min;
Step 8, continue to add 40ml and reduce golden salting liquid, stir and add 0.1ml formaldehyde again, reaction 10min;
The operation of step 9, repetition step 85 times, finally by deionized water repeatedly washed product, until remove solvent completely, finally obtains tri-iron tetroxide/gold nano composite.
The Fe that (a) in Fig. 2 prepares for step one in embodiment 1
3o
4the TEM photo of nano particle, this Fe
3o
4the particle size of nano particle comparatively evenly and have excellent magnetic property; (b) in Fig. 2 is the Fe that step 2 prepares
3o
4-SiO
2the TEM photo of Nano composite granules, this Fe
3o
4-SiO
2the silica shell layer thickness of Nano composite granules parcel is about 5nm.The TEM photo of the nanogold particle that the step 4 that (a) in Fig. 3 is preparation in embodiment 1 prepares, the tri-iron tetroxide that (b) in Fig. 3 finally prepares for embodiment 1/gold nano composite Fe
3o
4-SiO
2the TEM photo of-Au nano particle, this Fe
3o
4-SiO
2the load capacity of the golden nanometer particle of-Au nano grain surface is less.
Embodiment 2, the Fe utilizing embodiment 1 to prepare
3o
4-SiO2-Au nano particle is as SERS substrate, and the saturation magnetization of this SERS base material is 50emu/g, with rhodamine molecule for Raman probe molecule, detects rhodamine molecule content and comprises the following steps:
Step one, by SERS base material respectively with 10
-8, 10
-7m, 10
-6, 10
-5, 10
-4the rhodamine liquor of mol/l concentration fully mixes, and the SERS base material of the Raman probe molecule that utilized magnetism separate method by adsorption is separated, and is coated on slide and dries, obtained test samples, stand-by;
Step 2, test samples obtained for step one is placed in laser Raman spectrometer, wherein, frequency range is 2500cm
-1-0cm
-1, wavelength is 532nm, and laser attenuation power is 0.01-0.05%, and in a continuous mode, adopt the 1-3s time for exposure, multi collect, completes the Raman detection of rhodamine.With Fe
3o
4+ SiO
2it is 10 that+Au nano particle makes the detection line that SERS substrate records rhodamine
-7mol/l.
The preparation method of embodiment 3, a kind of tri-iron tetroxide/gold nano composite, compared with embodiment 1, difference is only in step 9, repeats step 8 and continue to add the golden salting liquid of reduction---the operation of---adding 0.1ml formaldehyde again---reaction 10min that stirs 10 times.
Due to, embodiment 3, compared with embodiment 1, adds the golden salting liquid of reduction---and the number of operations of---adding 0.1ml formaldehyde again---reaction 10min that stirs, makes repeatedly reduction reaction to occur, therefore, the Fe finally obtained
3o
4-SiO
2the load capacity of the golden nanometer particle on the surface of-Au nano particle comparatively embodiment 1 increases.
Embodiment 4, the Fe utilizing embodiment 3 to prepare
3o
4-SiO
2-Au nano particle is as SERS substrate, the saturation magnetization of this SERS base material is 49.2emu/g, with rhodamine molecule for Raman probe molecule, detect rhodamine molecule content to comprise the following steps: the application of SERS substrate when detecting rhodamine content, detecting step is identical with embodiment 2, with this Fe
3o
4-SiO
2it is 10 that-Au nano particle makes the detection line that SERS substrate records rhodamine
-8mol/l.
The preparation method of embodiment 5, a kind of tri-iron tetroxide/gold nano composite, comprises the following steps:
Step one, obtains Fe by hydro-thermal method
3o
4nano particle: identical with embodiment 1;
Step 2, in the surface of ferroferric oxide nano granules parcel layer of silicon dioxide: difference from Example 1 is, change the ferriferrous oxide nanometer material taking 0.4g step one obtained into 0.6g, 0.2ml ethyl orthosilicate (TEOS) will be added and change 0.3ml into, thus wrap up one deck shell thickness on the surface of ferroferric oxide nano granules and be about 6.1nm silica.
Step 3, the particle surface that step 2 obtains is carried out amination modification: difference from Example 1 is, will add the two amino silicane coupling agent of 3ml and change 4.5ml pair of amino silicane coupling agent into;
The preparation of step 4, gold nano seed: identical with embodiment 1;
Step 5, the preparation of golden salting liquid of reducing: identical with embodiment 1;
Step 6 is to step 9, identical with embodiment 1.
Because, embodiment 5 is compared with embodiment 1, to Fe
3o
4-SiO
2particle surface carries out in amination modification, makes the SiO wrapped up
2thickness increase, the amino of surperficial keyed jointing increases, therefore, the Fe finally obtained
3o
4-SiO
2the load capacity of the golden nanometer particle on the surface of-Au nano particle comparatively embodiment 1 increases.
Fig. 4 is the Fe prepared in embodiment 5
3o
4nano particle and final obtained Fe
3o
4-SiO
2the magnetic property of-Au nano particle is characterized by vibrating specimen magnetometer under room temperature (VSM).Result shows, Fe
3o
4the saturation magnetization value of nano particle is about 107.5emu/g, after its surface parcel layer of silicon dioxide and golden nanometer particle, and Fe
3o
4-SiO
2the saturation magnetization value of-Au nano particle drops to 48.7emu/g.The minimizing of saturation magnetization value can be summed up as the silica of parcel and golden shell also has diamagnetism while adding the distance between magnetic-particle.This nano composite material still has the stronger intensity of magnetization.
Embodiment 6,
Utilize the Fe that embodiment 5 prepares
3o
4-SiO2-Au nano particle is as SERS substrate, the saturation magnetization of this SERS base material is 48.7emu/g, with rhodamine molecule for Raman probe molecule, detect rhodamine molecule content to comprise the following steps: the application of SERS substrate when detecting rhodamine content, detecting step is identical with embodiment 2, with this Fe
3o
4-SiO
2it is 10 that-Au nano particle makes the detection line that SERS substrate records rhodamine
-8mol/l.
Fig. 5 shows the HAuCl of different quality ratio
4and Au-Fe
3o
4-SiO
2with the graph of a relation of SERS detectable limit.Result shows, and initial abscissa is directly proportional to ordinate, when
hAuCl 4 and Au-Fe 3 o 4 -SiO 2 mass ratio when being 1:3.3, SERS inspectionsurveying the limit is 10
-7mol/l.If continue to increase HAuCl
4and Au-Fe
3o
4-SiO
2mass ratio, SERS detectable limit start decline, when mass ratio reaches a certain numerical value, ordinate no longer changes with the change of abscissa.The load capacity of analysis result display golden nanometer particle strengthens Raman material impact.
It is important to point out at this; above embodiment is only limitted to be further elaborated and understanding concrete operations scheme of the present invention and the technique effect that can reach; the further restriction to content of the present invention and technical scheme can not be interpreted as; the essential characteristics of the non-protruding that those skilled in the art make on this basis and the improvement of marked improvement, all belong to protection category of the present invention.
Claims (2)
1. a preparation method for tri-iron tetroxide/gold nano composite, is characterized in that, comprise the following steps:
Step one, obtain by hydro-thermal method the ferroferric oxide nano granules that particle diameter is 120 ~ 170nm, for subsequent use;
Step 2, according to absolute ethyl alcohol, water and mass concentration are the volume ratio of the ammoniacal liquor of 28% is that 60:15:1 obtains mixed solution A, the ferroferric oxide nano granules taking step one obtained is dissolved in mixed solution A, quality-the volumetric concentration of ferroferric oxide nano granules and mixed solution A is 1 ~ 5mg/ml, ultrasonic 30min, be that 2:1 adds ethyl orthosilicate according to the mol ratio of tri-iron tetroxide and ethyl orthosilicate, 10 ~ 12h is reacted under room temperature, thus in the surface of ferroferric oxide nano granules parcel layer of silicon dioxide, the shell thickness of described silica is 5 ~ 6nm,
Step 3, be that 15:1 adds two amino silicane coupling agent and reacts 10 ~ 13h according to the volume ratio of two amino silicane coupling agent and ethyl orthosilicate, with deionized water and absolute ethanol washing repeatedly, isolate the tri-iron tetroxide of surface amination;
Step 4, be that 1:1 prepares mixed solution B according to the volume ratio of 0.075wt% sodium borohydride and 1wt% natrium citricum, for subsequent use; According to volume ratio 1:99 by soluble in water for 1wt% aqueous solution of chloraurate, magnetic agitation 15min mixes; At room temperature, add isopyknic 1wt% natrium citricum with 1wt% aqueous solution of chloraurate, then add the mixed solution B doubling 1wt% aqueous solution of chloraurate volume; Magnetic agitation reaction 30-60min, prepares gold nano seed solution;
Step 5, the preparation of golden salting liquid of reducing: be that 0.25mg/ml adds sodium carbonate in deionized water according to quality-volumetric concentration, mechanical agitation 10min, add 1wt% aqueous solution of chloraurate afterwards, the volume ratio of 1wt% aqueous solution of chloraurate and deionized water is 3:200, under lucifuge, mechanical agitation 10 ~ 12h, stand-by;
Step 6, be 2 ~ 6mg/ml according to quality-volumetric concentration, in the tri-iron tetroxide of the surface amination that step 3 is obtained and the obtained gold nano seed solution of step 4, mechanical agitation 2-3h, then with water and the washing of absolute ethyl alcohol magnetism separate method repeatedly;
Step 7, the product that step 6 obtains is joined in the obtained reduction gold salting liquid of step 5, wherein, gold nano seed solution is 1.7 ~ 3.4:1 with the volume ratio of the golden salting liquid of reduction, stirring is that 400:1 adds formaldehyde according to the volume ratio of reduction golden salting liquid and formaldehyde again, reacts 10min;
Step 8, be that 1.7 ~ 3.4:1 continues to add and reduce golden salting liquid according to gold nano seed solution and the volume ratio of the golden salting liquid of reduction, stirring is that 400:1 adds formaldehyde according to the volume ratio of the golden salting liquid of reduction and formaldehyde again, reacts 10min;
The operation of step 9, repetition N step 8, wherein N is 5 ~ 10; By deionized water repeatedly washed product, until remove solvent completely, finally obtain tri-iron tetroxide/gold nano composite.
2. tri-iron tetroxide/gold nano the composite utilizing the preparation method of tri-iron tetroxide/gold nano composite as claimed in claim 1 to obtain detects the method for rhodamine molecule fast, it is characterized in that, using tri-iron tetroxide/gold nano composite as SERS base material, the saturation magnetization of described SERS base material is 48.7-50emu/g, rhodamine molecule is Raman probe molecule, and comprises the following steps:
Step one, by described SERS base material respectively with 10
-8, 10
-7m, 10
-6, 10
-5, 10
-4the rhodamine liquor of mol/l concentration fully mixes, and the SERS base material of the Raman probe molecule that utilized magnetism separate method by adsorption is separated, and is coated on slide and dries, obtained test samples, stand-by;
Step 2, test samples obtained for step one is placed in Reinshaw laser Raman spectrometer, wherein: frequency range is 2500cm
-1-0cm
-1, wavelength is 532nm, and laser attenuation power is 0.01-0.05%, and in a continuous mode, adopt the 1-3s time for exposure, multi collect, completes the Raman detection of rhodamine.
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