CN113777092B - Preparation method of three-dimensional wool-shaped potassium titanate surface-enhanced Raman scattering substrate material - Google Patents
Preparation method of three-dimensional wool-shaped potassium titanate surface-enhanced Raman scattering substrate material Download PDFInfo
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- 238000004416 surface enhanced Raman spectroscopy Methods 0.000 title claims abstract description 59
- 239000000463 material Substances 0.000 title claims abstract description 52
- 239000000758 substrate Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- NJLLQSBAHIKGKF-UHFFFAOYSA-N dipotassium dioxido(oxo)titanium Chemical compound [K+].[K+].[O-][Ti]([O-])=O NJLLQSBAHIKGKF-UHFFFAOYSA-N 0.000 title claims abstract description 14
- 238000009940 knitting Methods 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 17
- 239000006185 dispersion Substances 0.000 claims abstract description 14
- 239000000725 suspension Substances 0.000 claims abstract description 14
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 claims description 7
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 239000000243 solution Substances 0.000 claims description 5
- 238000003760 magnetic stirring Methods 0.000 claims description 4
- 239000001508 potassium citrate Substances 0.000 claims description 2
- 229960002635 potassium citrate Drugs 0.000 claims description 2
- QEEAPRPFLLJWCF-UHFFFAOYSA-K potassium citrate (anhydrous) Chemical compound [K+].[K+].[K+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O QEEAPRPFLLJWCF-UHFFFAOYSA-K 0.000 claims description 2
- 235000011082 potassium citrates Nutrition 0.000 claims description 2
- 239000001509 sodium citrate Substances 0.000 claims description 2
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical group O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 2
- 210000002268 wool Anatomy 0.000 abstract description 14
- 238000001514 detection method Methods 0.000 abstract description 10
- 239000002086 nanomaterial Substances 0.000 abstract description 5
- 239000012535 impurity Substances 0.000 abstract description 4
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- FVIGODVHAVLZOO-UHFFFAOYSA-N Dixanthogen Chemical compound CCOC(=S)SSC(=S)OCC FVIGODVHAVLZOO-UHFFFAOYSA-N 0.000 abstract 1
- 231100001261 hazardous Toxicity 0.000 abstract 1
- 239000010936 titanium Substances 0.000 description 46
- 239000002585 base Substances 0.000 description 6
- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-UHFFFAOYSA-N 0.000 description 3
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 230000007246 mechanism Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 230000035945 sensitivity Effects 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000003837 high-temperature calcination Methods 0.000 description 2
- CXKWCBBOMKCUKX-UHFFFAOYSA-M methylene blue Chemical compound [Cl-].C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 CXKWCBBOMKCUKX-UHFFFAOYSA-M 0.000 description 2
- 229960000907 methylthioninium chloride Drugs 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 229910003077 Ti−O Inorganic materials 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000004454 trace mineral analysis Methods 0.000 description 1
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
- G01N21/658—Raman scattering enhancement Raman, e.g. surface plasmons
Abstract
A preparation method of a three-dimensional wool-shaped potassium titanate surface-enhanced Raman scattering substrate material belongs to the technical field of preparation of surface-enhanced Raman scattering substrate materials. It aims to solve the problems of the existing preparation K 2 Ti 8 O 17 The method of (2) has problems of high temperature operation and use of hazardous reagents. The method comprises the following steps: 1. preparation of Ti 2 An AlN dispersion suspension; 2. ti (Ti) 2 The AlN dispersion suspension reacts at 120-200 ℃, and is cooled, washed and dried to finish the preparation. The three-dimensional knitting wool cluster K obtained by the invention 2 Ti 8 O 17 The material has regular morphology, a porous three-dimensional structure, no impurities, controllable structure and good surface enhanced Raman scattering performance, and can be used in the fields of trace detection and the like. The invention avoids a great deal of energy consumption, has simple operation, good result repeatability and low cost, and is easy to realize industrial production. In the invention, the three-dimensional knitting wool is shaped like a group K 2 Ti 8 O 17 The surface-enhanced Raman scattering substrate material is used as a nonmetallic nanomaterial.
Description
Technical Field
The invention belongs to the technical field of preparation of surface-enhanced Raman scattering substrate materials; in particular to a three-dimensional knitting wool cluster K 2 Ti 8 O 17 A preparation method of a surface enhanced Raman scattering substrate material.
Background
Surface Enhanced Raman Scattering (SERS) is a method of characterizing the structure of surface molecules using raman spectroscopy. The principle is that the scattered laser intensity is improved by 2-8 orders of magnitude by utilizing an electromagnetic enhancement mechanism of the electronic vibration of the substrate material and chemical enhancement mechanisms such as charge transfer between the substrate material and molecules to be detected, so that the molecular information under low concentration is obtained. Since 1974, the method is discovered by Fleischmann, and has great application potential in trace analysis, water environment detection and food safety detection due to the advantages of good circularity, high sensitivity and the like, and is widely studied. The SERS substrate material has great significance in improving detection sensitivity and the like, and becomes an important point in the field of SERS research.
In view of development of SERS substrate materials, the traditional noble metal-based SERS substrate materials have high sensitivity and are the first SERS substrate materials, but have the defects of poor dispersibility, certain biotoxicity and the like. The novel nonmetallic nanomaterials overcome these disadvantages to some extent and have advantages not possessed by noble metal-based materials. For example, graphene can quench fluorescence, eliminating molecular resonance interference; moS (MoS) 2 Dipole acting force can be generated with a specific group, so that the electron transfer probability is improved; tiO (titanium dioxide) 2 The Ti-O bond of the (C) has excellent charge transmission capability and strong adsorption force on some groups. These unique properties make nonmetallic based nanomaterials a very promising class of SERS substrate materials, which has become the focus of research in recent years.
Recently, one study will be K 2 Ti 8 O 17 Brings the research field of SERS. They prepared a composite structure of potassium titanate with MXene and MAX phases, and obtained 3.98X10 when crystal violet was detected 5 Enhancement factor of 10 -6 The lowest detection limit of M indicates K 2 Ti 8 O 17 Is a nonmetallic nanomaterial with SERS potential. Its SERS mechanism is then attributed by the author to K 2 Ti 8 O 17 Is expected to be new due to the charge transmission capability and electrostatic action of the polymerNonmetallic based SERS substrate material.
And at K 2 Ti 8 O 17 In the preparation of (a) the prior art, high-temperature calcination or high-temperature hydrothermal is commonly used, and in a slightly mild scheme, the problems of using dangerous reagents (such as hydrofluoric acid) and the like exist, which are unfavorable for energy conservation and experimental security and are in favor of K 2 Ti 8 O 17 As a widely studied nonmetallic-based SERS substrate material, there is a great room for optimization.
Disclosure of Invention
The invention aims to solve the problems of the prior preparation of K 2 Ti 8 O 17 The method has the problems of high-temperature operation and dangerous reagent use, and provides a three-dimensional knitting wool-like K 2 Ti 8 O 17 A preparation method of a (potassium titanate) surface enhanced Raman scattering substrate material.
Three-dimensional knitting wool cluster-shaped K 2 Ti 8 O 17 The preparation method of the surface enhanced Raman scattering substrate material is realized by the following steps:
1. according to the mass volume ratio of (1-10) g (50-150) ml (0-28.8) g, ti is added 2 AlN is added into KOH aqueous solution, then citric acid or citrate is added, and Ti is obtained after stirring 2 An AlN dispersion suspension;
2. the Ti is mixed with 2 Transferring AlN dispersion suspension into a reaction kettle, reacting for 12-48 h at 120-200 ℃, cooling to room temperature after the reaction is finished, washing the product by deionized water, and drying at 50-80 ℃ for 8-16 h to obtain three-dimensional knitting wool-like K 2 Ti 8 O 17 The preparation method is completed by the surface enhanced Raman scattering substrate material.
The three-dimensional knitting wool cluster K prepared by the invention 2 Ti 8 O 17 By K 2 Ti 8 O 17 Molecular [ TiO ] 2 ]The structure improves the charge transfer capability and enhances the surface enhanced Raman scattering function; the three-dimensional knitting wool cluster K 2 Ti 8 O 17 The material has regular morphology and good surface enhanced Raman scattering performance. The hydrothermal temperature used in the invention is about 150 ℃, which is the same as the prior artSynthetic methods such as high temperature calcination of TiO 2 Preparation of K by the method 2 Ti 8 O 17 Compared with the prior art, the method has the advantages of avoiding a large amount of energy consumption, along with simple operation, low cost and easy realization of industrial production.
The invention adopts a simple one-step hydrothermal alkali corrosion method, the method is simple and easy to operate, only one-step simple hydrothermal method is needed, other experimental operations are not needed, and the result repeatability is good and the control is easy. Preparing the three-dimensional knitting wool cluster K 2 Ti 8 O 17 Surface-enhanced Raman scattering base material with coil size dependent on Ti 2 The particle size of AlN raw material, hole size can be adjusted through alkali concentration or citric acid (salt) additive amount, the line diameter is 30-200 nm, single line length is less than 100 mu m, the material has porous three-dimensional structure, no impurity, controllable structure, high surface enhanced Raman scattering capability, and can be used in the fields of trace detection and the like.
The three-dimensional wool cluster K prepared by the invention 2 Ti 8 O 17 The surface enhanced Raman scattering substrate material is used as a nonmetallic nano material.
Drawings
FIG. 1 is a three-dimensional loop K of example 1 2 Ti 8 O 17 SEM spectrogram of surface enhanced raman scattering base material;
FIG. 2 is a three-dimensional loop K of example 1 2 Ti 8 O 17 SEM spectrogram of surface enhanced raman scattering base material;
FIG. 3 is a three-dimensional loop K of example 1 2 Ti 8 O 17 A lowest detection limit diagram of the surface enhanced Raman scattering substrate material on crystal violet;
FIG. 4 is a three-dimensional loop K of example 2 2 Ti 8 O 17 SEM spectrogram of surface enhanced raman scattering base material;
FIG. 5 is a three-dimensional loop K of example 2 2 Ti 8 O 17 SEM spectrogram of surface enhanced raman scattering base material;
FIG. 6 is a three-dimensional loop K of example 2 2 Ti 8 O 17 Surface enhanced RamanMinimum detection limit diagram of scattering base material versus methylene blue.
Detailed Description
The technical scheme of the invention is not limited to the specific embodiments listed below, and also includes any combination of the specific embodiments.
The first embodiment is as follows: in this embodiment, a three-dimensional loop shape K 2 Ti 8 O 17 The preparation method of the surface enhanced Raman scattering substrate material is realized by the following steps:
1. according to the mass volume ratio of (1-10) g (50-150) ml (0-28.8) g, ti is added 2 AlN is added into KOH aqueous solution, then citric acid or citrate is added, and Ti is obtained after stirring 2 An AlN dispersion suspension;
2. the Ti is mixed with 2 Transferring AlN dispersion suspension into a reaction kettle, reacting for 12-48 h at 120-200 ℃, cooling to room temperature after the reaction is finished, washing the product by deionized water, and drying at 50-80 ℃ for 8-16 h to obtain three-dimensional knitting wool-like K 2 Ti 8 O 17 The preparation method is completed by the surface enhanced Raman scattering substrate material.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is that in the first step, ti is added according to a mass/volume ratio of 5g to 100ml to 10g 2 AlN is added to an aqueous KOH solution, and citric acid or citrate is added. Other steps and parameters are the same as in the first embodiment.
And a third specific embodiment: this embodiment differs from the first or second embodiments in that the Ti is as described in the first step 2 The particle size of AlN is 300-800 meshes. Other steps and parameters are the same as in the first or second embodiment.
The specific embodiment IV is as follows: this embodiment differs from one to three embodiments in that the molar concentration of the aqueous KOH solution in step one is 1 to 20M. Other steps and parameters are the same as in one to three embodiments.
Fifth embodiment: this embodiment differs from one to four embodiments in that the citrate in step one is sodium citrate or potassium citrate. Other steps and parameters are the same as in one to four embodiments.
Specific embodiment six: this embodiment differs from one of the first to fifth embodiments in that the stirring in the first step: the magnetic stirring speed is 100-1000 rpm, and the stirring time is 5-10 min. Other steps and parameters are the same as in one of the first to fifth embodiments.
Seventh embodiment: this embodiment differs from the first to sixth embodiments in that in the second step, ti is as described above 2 The AlN dispersion suspension was transferred to a reaction vessel and reacted at 150℃for 24 hours. Other steps and parameters are the same as in one of the first to sixth embodiments.
Eighth embodiment: the difference between the present embodiment and the first to seventh embodiments is that the number of deionized water washes in the second step is 2 to 5. Other steps and parameters are the same as those of one of the first to seventh embodiments.
Detailed description nine: the difference between the embodiment and one of the first to eighth embodiments is that the second step is drying at 50-80 deg.c for 10 hr. Other steps and parameters are the same as in one to eight of the embodiments.
The beneficial effects of the invention are verified by the following examples:
example 1:
three-dimensional knitting wool cluster-shaped K 2 Ti 8 O 17 The preparation method of the surface enhanced Raman scattering substrate material is realized by the following steps:
1. ti is added according to the mass volume ratio of 1g to 100ml 2 AlN is added into KOH aqueous solution, and Ti is obtained after stirring 2 An AlN dispersion suspension;
2. the Ti is mixed with 2 Transferring AlN dispersion suspension into a reaction kettle, reacting for 24 hours at 150 ℃, cooling to room temperature after the reaction is finished, washing a product by deionized water, and drying for 10 hours at 60 ℃ to obtain a three-dimensional knitting wool-shaped K 2 Ti 8 O 17 The preparation method is completed by the surface enhanced Raman scattering substrate material.
The Ti as described in step one of this embodiment 2 AlN has a particle size of 300 meshes。
The molar concentration of the aqueous KOH solution in step one of this example was 5M.
Stirring in step one of this example: the magnetic stirring speed was 500rpm and the stirring time was 5min.
The number of deionized water washes in step two of this example was 4.
The three-dimensional loop shape K prepared in this example 2 Ti 8 O 17 The surface enhanced Raman scattering substrate material is in powder form, and is subjected to scanning electron microscope and surface enhanced Raman scattering performance test, and the result shows that a three-dimensional knitting wool cluster structure K is formed 2 Ti 8 O 17 The wire is formed by intertwining a plurality of fine wire structures, the coil size is 20-40 mu m, the wire diameter is 100nm, the length of a single wire is about 70 mu m, the surface of the single wire is free of impurities, and the reaction degree is high (see fig. 1 and 2, and fig. 2 is a partial enlargement of fig. 1). Three-dimensional knitting wool cluster K 2 Ti 8 O 17 The surface enhanced Raman scattering substrate material has excellent surface enhanced Raman scattering performance, and the enhancement factor of crystal violet can reach 1.99 multiplied by 10 5 The lowest detection limit can reach 10 -8 M (see FIG. 3).
Example 2:
three-dimensional knitting wool cluster-shaped K 2 Ti 8 O 17 The preparation method of the surface enhanced Raman scattering substrate material is realized by the following steps:
1. ti was added in a mass/volume ratio of 1g to 150ml to 19.213g 2 AlN is added into KOH aqueous solution, citric acid is added, and Ti is obtained after stirring 2 An AlN dispersion suspension;
2. the Ti is mixed with 2 Transferring AlN dispersion suspension into a reaction kettle, reacting for 24 hours at 150 ℃, cooling to room temperature after the reaction is finished, washing a product by deionized water, and drying for 10 hours at 60 ℃ to obtain a three-dimensional knitting wool-shaped K 2 Ti 8 O 17 The preparation method is completed by the surface enhanced Raman scattering substrate material.
The Ti as described in step one of this embodiment 2 The AlN has a particle size of 300 meshes.
The molar concentration of the aqueous KOH solution in step one of this example was 13M.
Stirring in step one of this example: the magnetic stirring speed was 700rpm and the stirring time was 5min.
In the second example, the number of deionized water washes was 5.
The three-dimensional loop shape K prepared in this example 2 Ti 8 O 17 The surface enhanced Raman scattering substrate material is in powder form, and is subjected to scanning electron microscope and surface enhanced Raman scattering performance test, and the result shows that a three-dimensional knitting wool cluster structure K is formed 2 Ti 8 O 17 The device is formed by interlacing a plurality of fine linear structures, the coil size is 5-20 mu m, the line diameter is 70nm, the length of a single line is 100 mu m, the surface of the single line is free of impurities, and the reaction degree is high (see fig. 4 and 5, and fig. 5 is a partial enlargement of fig. 4). Three-dimensional knitting wool cluster K 2 Ti 8 O 17 The surface enhanced Raman scattering substrate material has excellent surface enhanced Raman scattering performance, and the enhancement factor of the surface enhanced Raman scattering substrate material to methylene blue can reach 9.61 multiplied by 10 4 The lowest detection limit can reach 10 -8 M (FIG. 6).
Claims (9)
1. The preparation method of the three-dimensional wool-shaped potassium titanate surface-enhanced Raman scattering substrate material is characterized by comprising the following steps of:
1. according to the mass volume ratio of (1-10) g (50-150) ml (0-28.8) g, ti is added 2 AlN is added into KOH aqueous solution, then citric acid or citrate is added, and Ti is obtained after stirring 2 An AlN dispersion suspension;
2. the Ti is mixed with 2 Transferring AlN dispersion suspension into a reaction kettle, reacting for 12-48 h at 120-200 ℃, cooling to room temperature after the reaction is finished, washing the product by deionized water, and drying at 50-80 ℃ for 8-16 h to obtain three-dimensional knitting wool-like K 2 Ti 8 O 17 The preparation method is completed by the surface enhanced Raman scattering substrate material.
2. A three-dimensional wool-like potassium titanate surface-enhanced raman scattering substrate according to claim 1The preparation method of the base material is characterized in that in the first step, ti is added according to the mass volume ratio of 5g to 100ml to 10g 2 AlN is added to an aqueous KOH solution, and citric acid or citrate is added.
3. The method for preparing a three-dimensional haired-shaped potassium titanate surface-enhanced raman scattering substrate material according to claim 1, wherein in the step one, the Ti is as follows 2 The particle size of AlN is 300-800 meshes.
4. The method for preparing a three-dimensional wool-like potassium titanate surface-enhanced raman scattering substrate material according to claim 1, wherein the molar concentration of the KOH aqueous solution in the step one is 1-20M.
5. The method for preparing a three-dimensional wool-shaped potassium titanate surface-enhanced raman scattering substrate material according to claim 1, wherein in the step one, the citrate is sodium citrate or potassium citrate.
6. The method for preparing a three-dimensional wool-like potassium titanate surface-enhanced raman scattering substrate material according to claim 1, wherein in the step one, the stirring is performed: the magnetic stirring speed is 100-1000 rpm, and the stirring time is 5-10 min.
7. The method for preparing a three-dimensional wool-like potassium titanate surface-enhanced Raman scattering substrate material according to claim 1, wherein in the second step, ti is as follows 2 The AlN dispersion suspension was transferred to a reaction vessel and reacted at 150℃for 24 hours.
8. The method for preparing a three-dimensional wool-like potassium titanate surface-enhanced raman scattering substrate material according to claim 1, wherein the number of times of deionized water washing in the second step is 2-5 times.
9. The method for preparing the three-dimensional wool-like potassium titanate surface-enhanced Raman scattering substrate material according to claim 1, wherein in the second step, the substrate material is dried at 50-80 ℃ for 10 hours.
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| 低能耗制备钛酸钾晶须的方法研究;王慧等;应用化工;第39卷(第12期);第1878-1881页 * |
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