CN111551533A - Surface enhanced substrate, preparation method thereof and detection method of methanol in insulating oil - Google Patents
Surface enhanced substrate, preparation method thereof and detection method of methanol in insulating oil Download PDFInfo
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- CN111551533A CN111551533A CN202010391212.2A CN202010391212A CN111551533A CN 111551533 A CN111551533 A CN 111551533A CN 202010391212 A CN202010391212 A CN 202010391212A CN 111551533 A CN111551533 A CN 111551533A
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 title claims abstract description 171
- 239000000758 substrate Substances 0.000 title claims abstract description 117
- 238000001514 detection method Methods 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title abstract description 30
- 238000001069 Raman spectroscopy Methods 0.000 claims abstract description 40
- 239000002184 metal Substances 0.000 claims abstract description 39
- 229910052751 metal Inorganic materials 0.000 claims abstract description 39
- 239000011888 foil Substances 0.000 claims abstract description 38
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000004140 cleaning Methods 0.000 claims abstract description 19
- 238000001035 drying Methods 0.000 claims abstract description 16
- SLAMLWHELXOEJZ-UHFFFAOYSA-N 2-nitrobenzoic acid Chemical compound OC(=O)C1=CC=CC=C1[N+]([O-])=O SLAMLWHELXOEJZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 11
- 229910021642 ultra pure water Inorganic materials 0.000 claims abstract description 11
- 239000012498 ultrapure water Substances 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims description 41
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 29
- 239000011889 copper foil Substances 0.000 claims description 29
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 15
- 238000001291 vacuum drying Methods 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims 1
- 238000001237 Raman spectrum Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 239000007788 liquid Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 230000002708 enhancing effect Effects 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 230000035945 sensitivity Effects 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 230000001133 acceleration Effects 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000011810 insulating material Substances 0.000 description 2
- 230000010354 integration Effects 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 239000011344 liquid material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910001868 water Inorganic materials 0.000 description 1
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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
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- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
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- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
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- Pathology (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention relates to the technical field of Raman detection, and discloses a surface-enhanced substrate, a preparation method thereof and a detection method of methanol in insulating oil. The preparation method comprises the steps of preparing a reaction solution, wherein the reaction solution is prepared from silver nitrate, o-nitrobenzoic acid and ultrapure water; placing the metal foil in a reaction solution to react for a preset time to obtain a surface enhanced substrate; and taking the surface enhanced substrate out for cleaning and drying. According to the preparation method of the surface enhanced substrate for detecting the methanol in the insulating oil, provided by the invention, the steps for preparing the surface enhanced substrate are simple, and the preparation cost is lower. On the other hand, the surface enhanced substrate prepared by the preparation method of the surface enhanced substrate provided by the invention is used for detecting the content of methanol in the insulating oil, can overcome the problems of complex steps, complex operation and the like of the conventional detection method for detecting the content of methanol in the insulating oil, and is suitable for field detection.
Description
Technical Field
The invention relates to the technical field of Raman detection, in particular to a surface enhanced substrate, a preparation method thereof and a detection method of methanol in insulating oil.
Background
The power transformer belongs to an important component part of a power system, and the safe and stable operation of the power transformer is directly related to the safe state of the power system. Most of the transformers put into use at present rely on insulating oil paper as an insulating material, and methanol is generated due to long-term high-voltage operation and is dissolved in the insulating oil. At present, the method for detecting the methanol dissolved in the insulating oil is complex and complicated to operate, and can only be completed in a laboratory. The Raman spectroscopy technology has great advantages in the detection of liquid materials as a fast-developing new multidisciplinary detection technology. The Raman spectrum technology is used for measuring the content of the dissolved methanol in the oil, and the method has the advantages of high detection speed, simple operation, nondestructive detection and little influence from environmental factors. However, the raman spectroscopy detection directly performed on the insulating oil cannot accurately detect the content of methanol in the low-concentration insulating oil.
Disclosure of Invention
Based on the above, it is necessary to provide a surface enhanced substrate for detecting methanol in insulating oil, a preparation method thereof and a method for detecting methanol in insulating oil, aiming at the problem that the methanol content in low-concentration insulating oil cannot be accurately detected by raman spectroscopy.
A preparation method of a surface enhanced substrate comprises the steps of preparing a reaction solution, wherein the reaction solution is prepared from silver nitrate, o-nitrobenzoic acid and ultrapure water; placing the metal foil in a reaction solution to react for a preset time to obtain a surface enhanced substrate; and taking the surface enhanced substrate out for cleaning and drying.
In one embodiment, the method for preparing the reaction solution comprises the step of dissolving 0.5-1.5 mmol of silver nitrate and 1-2 mmol of o-nitrobenzoic acid in 200-400 mL of ultrapure water to obtain the reaction solution.
In one embodiment, the metal foil is a copper foil.
In one embodiment, the reaction time is 4-8 min.
In one embodiment, before the metal foil is placed in the reaction solution for reaction, the method further comprises the following steps of cleaning the metal foil, and drying the cleaned metal foil.
In one embodiment, the metal foil and the surface enhancing substrate are cleaned using an ultrasonic cleaning technique.
In one embodiment, the metal foil and the surface enhanced substrate are alternately cleaned a predetermined number of times using ethanol and deionized water as the media for the ultrasonic cleaning.
In one embodiment, the metal foil and the surface enhanced substrate are dried using a vacuum drying oven, and the dried surface enhanced substrate is placed in a vacuum oven for standby.
A surface enhanced substrate prepared using the method of preparing a surface enhanced substrate as described in any one of the preceding embodiments.
A method for detecting methanol in insulating oil, a surface enhanced substrate for detecting methanol in insulating oil is prepared by adopting the method for preparing the surface enhanced substrate in any embodiment; placing the surface enhanced substrate in insulating oil to be detected for a preset time; and taking out the surface enhanced substrate, carrying out Raman detection on the surface enhanced substrate, and analyzing the content of the methanol in the insulating oil according to the detection result.
According to the preparation method of the surface enhanced substrate, a reaction solution is prepared by silver nitrate, o-nitrobenzoic acid and ultrapure water, and the prepared metal foil is placed in the reaction solution for reaction for a preset time to obtain the surface enhanced substrate. And taking out the obtained surface enhanced substrate, cleaning to remove the reaction solution remained on the surface, and finally drying the surface enhanced substrate for later use. According to the preparation method of the surface enhanced substrate for detecting the methanol in the insulating oil, provided by the invention, the steps for preparing the surface enhanced substrate are simple, and the preparation cost is lower. On the other hand, by detecting the raman signal of methanol in the insulating oil using the prepared surface enhanced substrate, the raman peak of methanol in the insulating oil can be rapidly detected, and the raman peak of methanol in the insulating oil cannot be detected by directly performing raman spectroscopy. The surface enhanced substrate for detecting the methanol in the insulating oil, which is prepared by the preparation method of the surface enhanced substrate provided by the invention, can overcome the problems of complex method, complex operation and the like of the conventional method for detecting the methanol in the insulating oil, and is suitable for field detection.
Drawings
FIG. 1 is a flow chart of a method for preparing a surface enhanced substrate according to one embodiment of the present invention;
FIG. 2 is a flow chart of a method for pre-testing a metal foil according to one embodiment of the present invention;
FIG. 3 is a scanning electron micrograph of a surface enhanced substrate according to one embodiment of the present invention;
FIG. 4 is a flow chart of a method for detecting methanol in insulating oil according to an embodiment of the present invention;
FIG. 5 shows three Raman spectra according to one embodiment of the present invention.
Detailed Description
To facilitate an understanding of the invention, the invention will now be described more fully with reference to the accompanying drawings. Preferred embodiments of the present invention are shown in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
It will be understood that when an element is referred to as being "secured to" another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present. As used herein, the terms "vertical," "horizontal," "left," "right," "upper," "lower," "front," "rear," "circumferential," and the like are based on the orientation or positional relationship shown in the drawings for ease of description and simplicity of description, and do not indicate or imply that the referenced device or element must have a particular orientation, be constructed and operated in a particular orientation, and are therefore not to be considered limiting of the present invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The power transformer belongs to an important component part of a power system, and the safe and stable operation of the power transformer is directly related to the safe state of the power system. Most of the transformers put into use at present rely on insulating oil paper as an insulating material, and methanol is generated due to long-term high-voltage operation and is dissolved in the insulating oil. The Raman spectrum technology is utilized to measure the content of the dissolved methanol in the insulating oil, and the method has the advantages of high detection speed, simple operation, nondestructive detection and little influence from environmental factors. However, the direct use of raman spectroscopy has the disadvantage of low detection sensitivity and therefore requires the incorporation of surface enhancement techniques for the detection of the methanol content of low concentrations of insulating oil. The surface enhancement mechanism is mainly based on the principle of metal surface local electric field enhancement, and the incident light irradiates a rough metal surface to enhance the surface Raman scattering intensity. The detection limit of Raman detection can be further expanded by combining a surface enhancement technology, and the method can be used for rapidly detecting the content of methanol in the transformer oil on site.
The preparation of the surface enhanced substrate is an important link for detecting the content of methanol in the insulating oil. Different materials, different reagent concentrations and deposition times will have different effects on the enhancement of the surface enhanced substrate. Fig. 1 is a flowchart illustrating a method for manufacturing a surface enhanced substrate according to an embodiment of the present invention, wherein the method for manufacturing a surface enhanced substrate includes the following steps S100 to S300.
S100: preparing a reaction solution, wherein the reaction solution is prepared from silver nitrate, o-nitrobenzoic acid and ultrapure water.
S200: and placing the metal foil in the reaction solution to react for a preset time to obtain the surface enhanced substrate.
S300: and taking the surface enhanced substrate out for cleaning and drying.
Specifically, silver nitrate, o-nitrobenzoic acid and ultrapure water are used to prepare a reaction solution according to a preset ratio, and the prepared metal foil is placed in the reaction solution to react for a preset time to obtain the surface enhanced substrate. And removing the surface enhanced substrate, cleaning to remove the residual reaction solution on the surface, finally drying the cleaned surface enhanced substrate, and placing for later use after drying. According to the preparation method of the surface enhanced substrate for detecting the methanol in the insulating oil, provided by the invention, the steps for preparing the surface enhanced substrate are simple, and the preparation cost is lower. On the other hand, the prepared surface enhanced substrate is used for detecting the Raman signal of the methanol in the insulating oil, so that the Raman peak of the methanol in the insulating oil can be quickly detected, and the Raman peak of the methanol in the insulating oil can not be detected by directly performing Raman spectrum detection, so that the surface enhanced substrate is suitable for field detection.
In one embodiment, the method for preparing the reaction solution comprises the step of dissolving 0.5-1.5 mmol of silver nitrate and 1-2 mmol of o-nitrobenzoic acid in 200-400 mL of ultrapure water to obtain the reaction solution. Different materials and different reagent concentrations can affect the enhancement effect of the surface enhancement substrate, and in the embodiment, the reaction solution is prepared by selecting the preparation ratio of 0.5mmol of silver nitrate and 1.5mmol of o-nitrobenzoic acid dissolved in 300mL of ultrapure water, and is prepared at normal temperature for standby.
In one embodiment, the metal foil is a copper foil. Since the surface enhanced substrate made of different materials has different enhancing effects, the copper foil is selected as a material for the surface enhanced substrate for detecting methanol in the insulating oil in the present embodiment. The commercially available copper foil is cut before the copper foil is placed in the reaction solution. In the embodiment, the metal foil is obtained by cutting a copper foil, and the shape and size of the metal foil can be set according to actual needs, for example, the metal foil can be a square foil of 0.8cm × 0.8 cm; of course, in other examples, the metal foil may also be circular, triangular or rectangular, etc., and the size of the metal foil is not limited by the above data.
In one embodiment, the reaction time is 4-8 min. In this embodiment, the copper foil after being cleaned and dried is placed in the reaction solution and reacted for 6min to obtain the surface enhanced substrate for detecting methanol in the insulating oil.
Fig. 2 is a flowchart of a method for pre-testing a metal foil according to an embodiment of the present invention, wherein the method further includes the following steps S110 and S120 before the metal foil is placed in the reaction solution for reaction.
S110: and cleaning the metal foil.
S120: and drying the cleaned metal foil.
After cutting a copper foil into a size of 0.8cm × 0.8cm, the copper foil was placed in an ethanol solution and subjected to ultrasonic cleaning. And then, cleaning the copper foil for several times alternately by using ethanol and deionized water as ultrasonic cleaning media in sequence so as to remove impurities on the surface of the copper foil and prevent the impurities on the surface of the copper foil from influencing the preparation effect of the surface-enhanced substrate. And after the copper foil is cleaned, placing the copper foil in a vacuum drying oven for drying treatment so as to prevent cleaning media on the surface of the copper foil from being brought into the reaction solution when the copper foil is placed in the reaction solution, and influencing the preparation effect of the surface-enhanced substrate.
In one embodiment, the metal foil and the surface enhancing substrate are cleaned using an ultrasonic cleaning technique. The ultrasonic cleaning is to utilize the cavitation, acceleration and direct current action of ultrasonic waves in liquid to directly and indirectly act on the liquid and dirt, so that the dirt layer is dispersed, emulsified and stripped to achieve the purpose of cleaning. The ultrasonic cleaning technology is used, the cleaning speed of the copper foil is high, the quality is high, the automatic control is easy, and the cleaning method is not limited by the complex shape of the surface of a cleaning piece.
In one embodiment, the metal foil and the surface enhanced substrate are alternately cleaned a predetermined number of times using ethanol and deionized water as the media for the ultrasonic cleaning. Ultrasonic cleaning utilizes cavitation, acceleration and straight-through flow of ultrasonic waves in liquid, so that a liquid medium is required for ultrasonic cleaning. In this embodiment, when the metal foil and the surface enhanced substrate are ultrasonically cleaned, ethanol and deionized water are respectively used as media for the ultrasonic cleaning, and the metal foil and the surface enhanced substrate are alternately cleaned for several times until stains or residual reaction solution are thoroughly cleaned.
In one embodiment, the metal foil and the surface enhanced substrate are dried using a vacuum drying oven, and the dried surface enhanced substrate is placed in a vacuum oven for standby. And drying the metal foil by using a vacuum drying oven, wherein the vacuum drying oven is used for preventing cleaning media remained on the surface from being brought into the reaction solution when the copper foil is placed in the reaction solution after the copper foil is cleaned, so that the preparation effect of the surface enhanced substrate is influenced. And drying the surface enhanced substrate by using a vacuum drying box, and placing the dried surface enhanced substrate in a vacuum furnace for later use, wherein the surface enhanced substrate is used for preventing the copper foil of the surface enhanced substrate from rusting under the condition that oxygen, water and carbon dioxide exist on the surface so as to influence the application effect of the surface enhanced substrate.
The invention also provides a surface enhanced substrate, which is prepared by adopting the preparation method of the surface enhanced substrate in any embodiment.
The following examples, which are included to further illustrate and not to limit the invention, provide specific details for the preparation of the surface enhanced substrates of the present invention. The instruments and reagents used in the examples are all commercially available.
The preparation process steps of the surface enhanced substrate by the preparation method provided by the invention are as follows.
Test step 1: a commercially available copper foil was cut into a copper foil of about 0.8cm × 0.8cm size, and the copper foil was placed in an ethanol solution and subjected to ultrasonic cleaning. And then, cleaning the copper foil for several times alternately by using ethanol and deionized water as ultrasonic cleaning media in sequence so as to remove impurities on the surface of the copper foil. And after the copper foil is cleaned, placing the copper foil in a vacuum drying oven for drying treatment.
Test step 2: 1mmol of silver nitrate and 1.5mmol of o-nitrobenzoic acid were precisely measured and dissolved in 300mL of ultrapure water to prepare a reaction solution, which was prepared at normal temperature for use.
Test step 3: and placing the copper foil subjected to cleaning and drying treatment in the reaction solution, and reacting for 6min to obtain the surface enhanced substrate. After the reaction was completed, the surface-enhanced substrate was taken out of the reaction solution with tweezers. And (3) cleaning the surface enhanced substrate for several times by using ethanol and deionized water as ultrasonic cleaning media in sequence after the reaction so as to remove the residual reaction solution on the surface of the surface enhanced substrate. After the surface enhanced substrate is cleaned, the surface enhanced substrate is placed in a vacuum drying oven for drying treatment. And after the surface enhanced substrate is cleaned and dried, placing the surface enhanced substrate in a vacuum furnace for standby.
Fig. 3 is a scanning electron microscope image of the surface enhanced substrate according to an embodiment of the present invention, and the prepared surface enhanced substrate for detecting the content of methanol in insulating oil is detected and analyzed by using a field emission scanning electron microscope. The detection result is shown in FIG. 3, in which the particle size of the nano-block is mainly distributed in the range of 100-300nm, and the average diameter of the nano-block is 208 nm.
The invention also provides a method for detecting methanol in insulating oil, and fig. 4 is a flow chart of the method for detecting methanol in insulating oil according to one embodiment of the invention, and in one embodiment, the method for detecting methanol in insulating oil comprises the following steps S10 to S30.
S10: the surface enhanced substrate for detecting methanol in insulating oil is prepared by adopting the preparation method of the surface enhanced substrate in any embodiment.
S20: and placing the surface enhanced substrate in insulating oil to be detected for a preset time.
S30: and taking out the surface enhanced substrate, carrying out Raman detection on the surface enhanced substrate, and analyzing the content of the methanol in the insulating oil according to the detection result.
The surface enhanced substrate for detecting the methanol in the insulating oil is prepared by adopting the preparation method of the surface enhanced substrate. And placing the prepared surface enhanced substrate in insulating oil to be detected for a preset time. And taking out the surface enhanced substrate and then carrying out Raman detection on the surface enhanced substrate. The Raman spectrum detection of the insulating oil to be detected can not detect the Raman peak of the methanol in the insulating oil directly, and the detection sensitivity is low; the surface enhanced substrate prepared by the preparation method is used for detecting the Raman signal of the methanol in the insulating oil, so that the Raman peak of the methanol in the insulating oil can be quickly detected, the detection sensitivity is improved, and the detection method is used for detecting the content of the methanol in the insulating oil with low concentration.
Fig. 5 is three raman spectrograms of one embodiment of the present invention, and the surface enhanced substrate obtained by the above preparation method is used for raman detection of the methanol content in the insulating oil. When Raman detection is carried out, a solid laser with the wavelength of 532nm is adopted, the output power of laser generated by the solid laser is 10mW, the slit width of a spectrometer is 100 micrometers, the Raman detection integration frequency is 50 times, and the integration time is 0.2 s. The results of raman spectroscopy on the surface enhanced substrate are shown in fig. 5.
From the waveform (c) in FIG. 5, it can be seen that the Raman spectroscopy of liquid pure methanol before the surface enhancement technique was combined gave a spectrum in the range of 1036cm-1And 1453cm-1Has obvious Raman peak, but the peak width of the Raman peak is wide, and the Raman peak is not easy to carry out quantitative analysis. The waveform (b) in FIG. 5 is the Raman spectrum of a 600. mu.L/L methanol-insulating oil solution obtained by Raman spectroscopy via a surface-enhanced substrate, at 789, as compared to the Raman signal obtained by Raman spectroscopy on the surface-enhanced substrate itself, as shown in waveform (a) in FIG. 5-1、1041-1And 1446cm-1There is a significant change. Wherein, 789cm-1The enhancement at the peak may be caused by other substances dissolved in the insulating oil.
In summary, 1041cm of the waveform in FIG. 5b (b) can be determined-1The raman-enhanced peak at (a) is derived from the c waveform of fig. 5 at 1036cm-1The methanol peak at (c). It can be seen that the raman peak of methanol in 600 μ L/L of methanol-insulating oil can be detected by using the raman spectroscopy technique in combination with the surface enhanced substrate obtained in the above preparation method. The surface enhanced substrate is combined to carry out Raman detection on the insulating oil with low methanol content concentration, and a Raman signal of the methanol in the insulating oil can be detected, so that a tester can analyze the content of the methanol dissolved in the insulating oil according to the Raman signal conveniently, the problems of complex detection method and complex operation of the conventional method for detecting the methanol in the insulating oil can be solved, and the surface enhanced substrate is suitable for field detection.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. A method of preparing a surface enhanced substrate, comprising:
preparing a reaction solution, wherein the reaction solution is prepared from silver nitrate, o-nitrobenzoic acid and ultrapure water;
placing the metal foil in a reaction solution to react for a preset time to obtain a surface enhanced substrate;
and taking the surface enhanced substrate out for cleaning and drying.
2. The method of preparing a surface enhanced substrate according to claim 1, wherein the method of preparing the reaction solution is:
dissolving 0.5-1.5 mmol of silver nitrate and 1-2 mmol of o-nitrobenzoic acid in 200-400 mL of ultrapure water to obtain the reaction solution.
3. The method of claim 1 or 2, wherein the metal foil is a copper foil.
4. The method for preparing a surface-enhanced substrate according to claim 1, wherein the predetermined reaction time is 4 to 8 min.
5. The method of claim 1, wherein the step of placing the metal foil in the reaction solution for reaction further comprises the steps of:
cleaning the metal foil;
and drying the cleaned metal foil.
6. The method of preparing a surface enhanced substrate according to claim 5, wherein the metal foil and the surface enhanced substrate are cleaned using an ultrasonic cleaning technique.
7. The method of preparing a surface enhanced substrate according to claim 6, wherein the metal foil and the surface enhanced substrate are alternately washed a predetermined number of times using ethanol and deionized water as the medium for the ultrasonic washing.
8. The method of claim 5, wherein the metal foil and the surface enhanced substrate are dried using a vacuum drying oven, and the dried surface enhanced substrate is placed in a vacuum oven for standby.
9. A surface-enhanced substrate, characterized in that it is produced by a process for the production of a surface-enhanced substrate according to any one of claims 1 to 8.
10. A method for detecting methanol in insulating oil is characterized by comprising the following steps:
preparing a surface enhanced substrate for detecting methanol in insulating oil by using the method for preparing a surface enhanced substrate according to any one of claims 1 to 8;
placing the surface enhanced substrate in insulating oil to be detected for a preset time;
and taking out the surface enhanced substrate, carrying out Raman detection on the surface enhanced substrate, and analyzing the content of the methanol in the insulating oil according to the detection result.
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| CN114200164A (en) * | 2021-12-10 | 2022-03-18 | 深圳职业技术学院 | Method for removing trace impurities on surface of copper foil by using dichloromethane/methanol mixed solvent under AFM-IR monitoring |
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