CN113588746B - Method for preparing carbide material at low temperature by plasma one-step method - Google Patents
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Abstract
The invention relates to a method for preparing a carbide material at low temperature by a plasma one-step method, which comprises the following steps: 1) Adding a carbon material into water, stirring, adding a metal salt, fully stirring, standing, and drying to obtain a dried sample; 2) And (3) placing the dried sample in plasma equipment for treatment to obtain the carbide material. Compared with the prior art, the method has the advantages that the carbide material is prepared at a low temperature by a one-step method by using a plasma treatment method and taking a carbon material as a carbon source and a template and loading metal salt, the preparation method is simple and environment-friendly, and compared with the traditional carbide material preparation method, the method is safer, the particle size of the material is smaller, the dispersity is better, the method has a better glucose detection application prospect, and the advantages are obvious.
Description
Technical Field
The invention belongs to the technical field of nano materials and glucose detection and preparation, and relates to a method for preparing a carbide material at a low temperature by a plasma one-step method.
Background
With the improvement of living standard of people, more and more people suffer from diabetes due to unreasonable dietary structure and lack of necessary exercise. Diabetes is a disease which is very easy to cause related complications, and the diabetes is unconscious in onset and has no symptoms in the early stage, or only patients with mild hypodynamia, thirst and unobvious blood sugar increase can be diagnosed by systematic examination such as blood sugar detection. Therefore, it is important to detect abnormal blood glucose conditions by the blood glucose monitoring device as early and accurate as possible. Blood glucose monitoring is always an important component in the medical field, the detection accuracy of the blood glucose monitoring is a core problem, and a general circuit element system cannot meet the requirement of the measurement accuracy of the blood glucose monitoring. Researchers have found that electrochemical sensors are expected to solve this problem.
The carbon nano tube is considered as a good carrier material, has high electrocatalytic effect, high electron transfer rate and large working surface area, and can be used for preparing a glucose detection material. Liu et al (Guodong Liu, yuehe Lin. Enzymatic glucose biosensor based on self-assembling glucose oxidase on carbon nanotubes. Electrochemical communication.2006.8.2.251-256.) disclose a flow injection amperometric glucose biosensor modified glassy carbon sensor based on electrostatic self-assembling glucose oxidase (GOx) oil and carbon nanotubes, which has a linear response range of 15 μ M to 6mM for glucose detection and a detection limit of 7 μ M. Although the sensitivity of the technology can meet the requirement, the technology has the defects of complex preparation process and materials, use of non-environment-friendly substances (substances such as sulfuric acid, nitric acid, N-dimethylformamide and the like), generation of a large amount of waste liquid and the like, and the final detection depends on glucose oxidase and needs a special salt solution detection system.
Chinese patent publication No. CN108088881A discloses a method for preparing a glucose sensor by using an amphiphilic polymer modified carbon nanotube hybrid as a carrier, loading metal nano catalyst particles thereon, and applying the same. The method uses toxic organic solvent and dialysis equipment, and needs to prepare precursor, and has complex process and low preparation efficiency.
Therefore, the traditional method for preparing the carbon nanotube material needs high temperature and high pressure, has obvious energy consumption, is easy to cause environmental pollution, has complex process and low yield, and the prepared material has poor performance and cannot meet the requirement of practical application.
Disclosure of Invention
The invention aims to provide a method for preparing a carbide material at a low temperature by a plasma one-step method. The method adopts plasma treatment, prepares the carbide material at low temperature, does not use toxic organic solvent, does not use a dialysis device, does not relate to precursor preparation, and has the characteristics of simple process, safety, reliability, environmental friendliness and the like.
The purpose of the invention can be realized by the following technical scheme:
a method for preparing carbide material at low temperature by a plasma one-step method comprises the following steps:
1) Adding a carbon material into water, stirring, adding a metal salt, fully stirring, standing, and drying to obtain a dried sample;
2) And (3) placing the dried sample in plasma equipment for treatment to obtain the carbide material.
Further, in step 1), adding the carbon material into water, and stirring to form a paste.
Further, in the step 1), the standing time is 11 to 20 hours, so that the metal salt is uniformly impregnated on the carbon material.
Further, in the step 1), the drying temperature is 100-140 ℃, and the drying time is 10-16 hours. Preferably vacuum drying.
Further, in step 1), the carbon material includes one or more of carbon nanotubes, carbon microspheres, carbon fibers or graphene, and the metal salt includes one or more of tungstate (e.g., ammonium metatungstate, ammonium paratungstate, sodium tungstate, etc.), molybdate (e.g., ammonium molybdate), nickel salt (e.g., nickel acetate), or indium salt (e.g., indium acetate).
Further, in the step 1), the mass ratio of the metal salt to the carbon material is (1.5-2.5) to 1, and the dosage ratio of the carbon material to water is 0.2g (3-8) mL.
Further, in the step 2), the treatment process is carried out under the air condition, the treatment temperature is normal temperature (preferably 10-30 ℃), the treatment pressure is normal pressure, and the treatment time is 0.5-1.5h.
Further, in the treatment process, the process parameters of the plasma equipment are as follows: 100-150V, 1.5-3A and 150-400W.
The carbide material is prepared by the method. The carbide material can be used in the fields of electrocatalysis, photocatalysis, thermocatalysis and the like.
The application of a carbide material, wherein the carbide material is used in blood sugar monitoring equipment, for example, as a medical appliance element such as a glucose detection sensor electrode or a blood sugar detection element.
The carbide material is prepared by taking the carbon material and the metal salt as raw materials and utilizing a plasma device to perform a high-voltage discharge one-step method at a low temperature, has excellent glucose detection performance, can be used for glucose detection when being made into an electrode, has the characteristics of high sensitivity, strong anti-interference performance, large measurement range and the like, can be used in the fields of human blood glucose monitoring and the like, has good practical applicability, and is easy to commercialize.
Compared with the prior art, the invention has the following characteristics:
1) According to the invention, the carbide material is prepared at a low temperature by a one-step method by using a plasma treatment method and taking a carbon material as a carbon source and a template and loading metal salt, the preparation method is simple and environment-friendly, and compared with the traditional carbide material preparation method, the method is safer, the material particle size is smaller, the dispersity is better, the glucose detection application prospect is better, and the advantages are obvious;
2) In the process of preparing the carbide material by the plasma method, any toxic reagent and hazardous gas are not used, so the preparation process is green and environment-friendly;
3) The carbide material prepared by the method has good shape consistency, good particle size uniformity, high catalytic activity, good dispersibility and stability, and is suitable for batch production;
4) The raw materials used by the invention have rich resources, low price and low preparation cost;
5) The carbide material prepared by the invention has better glucose detection performance, the measurement range covers the concentration range of human blood glucose, and the carbide material is hopeful to be prepared into a sensor electrode and applied to the detection of the human blood glucose content in medicine.
Drawings
FIG. 1 is an XRD pattern of a general tungsten oxide material prepared by a conventional calcination method in a comparative example and a carbide material prepared by a plasma method in example 1;
FIG. 2 is a TEM spectrum of a carbide material prepared by the plasma method in example 1, wherein b and c are partially enlarged views of a;
FIG. 3 is a Mapping chart of elements C, O and W of a general tungsten oxide material prepared by a conventional calcination method in a comparative example and a carbide material prepared by a plasma method in example 1;
FIG. 4 is a plot of cyclic voltammetry for different glucose concentration measurements after the electrodes were made of the carbide material made by plasma in example 1;
FIG. 5 is a graph showing comparison of data obtained by measuring glucose after electrodes are formed on a general tungsten oxide material prepared by a conventional calcination method in a comparative example and a carbide material prepared by a plasma method in example 1, respectively;
FIG. 6 is a graph of current versus time for glucose measurements taken after forming electrodes of the carbide material formed by the plasma process of example 1;
FIG. 7 is a graph showing the AC impedance of the plasma-processed carbide material used in example 1 after forming an electrode for glucose measurement;
FIG. 8 is a graph showing the stability test of glucose test conducted after the electrode was made of the carbide material obtained by the plasma method in example 1;
FIG. 9 is a graph showing the interference results of different substances when glucose measurement is performed after the electrode is made of the carbide material prepared by the plasma method in example 1;
the carbon nano tube CNT is a carbon nano tube, the CNT @ W-C is a common tungsten oxide material prepared by a conventional roasting method in a comparative example, the CNT @ W-P is a carbide material prepared by a plasma method in example 1, OA is Oxalic acid (Oxalic acid), CA is Citric acid (Citric acid), PS is Potato starch (Potatto starch), CTS is Chitosan (Chitosan), UREA is UREA, and GLU is glucose.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments. The present embodiment is implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, but the scope of the present invention is not limited to the following embodiments.
The invention provides a method for preparing a carbide material at low temperature by a plasma one-step method, which comprises the following steps:
1) Adding a carbon material into water, stirring, adding a metal salt, fully stirring, standing, and drying to obtain a dried sample;
2) And (3) placing the dried sample in plasma equipment for treatment to obtain the carbide material.
In the step 1), adding the carbon material into water, and stirring into paste. The standing time is 11-20 hours. The drying temperature is 100-140 deg.C, and the drying time is 10-16 hr. The carbon material includes one or more of carbon nanotubes, carbon microspheres, carbon fibers, or graphene, and the metal salt includes one or more of tungstate, molybdate, nickel salt, or indium salt. The mass ratio of the metal salt to the carbon material is (1.5-2.5): 1, and the dosage ratio of the carbon material to water is 0.2g (3-8) mL.
In the step 2), the treatment process is carried out under the air condition, the treatment temperature is normal temperature, the treatment pressure is normal pressure, and the treatment time is 0.5-1.5h. In the treatment process, the process parameters of the plasma equipment are as follows: 100-150V, 1.5-3A and 150-400W.
The invention also provides a carbide material which is prepared by the method.
The invention also provides application of the carbide material, and the carbide material is used in blood sugar monitoring equipment.
Comparative example:
the common tungsten oxide material is prepared by adopting a conventional roasting method, and the preparation process comprises the following steps:
weighing 0.2g of carbon nano tube, adding 5ml of water, and stirring into paste; then 0.37g of ammonium metatungstate is weighed and added into the pasty carbon nano tube, and the mixture is fully stirred for 1 hour and then stands for 11 hours to be fully impregnated; the impregnated sample was dried at 120 ℃ for 12 hours to obtain a preliminarily dried sample. And then roasting the dried sample at 400 ℃ for 2 hours under the atmosphere of argon protective gas to obtain a common tungsten oxide sample.
Example 1:
the carbide material is prepared by adopting a plasma method, and the preparation process comprises the following steps:
weighing 0.2g of carbon nano tube, adding 5ml of water, and stirring into paste; then 0.37g of ammonium metatungstate is weighed and added into the pasty carbon nano tube, and the mixture is fully stirred for 1 hour and then is kept stand for 11 hours to be fully impregnated; the impregnated sample was dried at 120 ℃ for 12 hours. And then placing the dried sample in a plasma device for plasma treatment under the air condition, normal temperature and normal pressure, 100V, 2A, 200W and 1 hour. Finally, the carbide material is prepared.
Structural characterization and performance testing:
1. phase analysis of the material was performed using a 3 kW/D8 ADVANCE Da Vinci multifunctional X-ray diffractometer (XRD), corresponding XRD patterns are shown in figure 1. As can be seen from FIG. 1, the carbide material produced by the plasma method in example 1 corresponds to standard X-ray diffraction powder diffraction cards (PDF #41-1035 and PDF # 39-0186), confirming the presence of tungsten carbide in the material.
Compared with the prior art, when the material is prepared, because the roasting mode only has high temperature and does not have active energy, the ammonium metatungstate is decomposed by the high temperature, and carbon and tungsten molecules are not sufficiently active in the decomposition process, and no chemical bond is formed, so that tungsten carbide is not formed; in the embodiment 1, the internal temperature of the plasma is up to several hundreds to thousands of degrees centigrade, and the ammonium metatungstate forms chemical bonds between carbon and tungsten molecules by virtue of active high-energy electron groups in the plasma in the decomposition process, so that tungsten carbide molecules are formed.
2. The morphology and element distribution of the material were observed with a TALOS F200X field emission Transmission Electron Microscope (TEM) as shown in fig. 2 and fig. 3, respectively. As can be seen from fig. 2, the main morphology of the carbide material prepared by the plasma method in example 1 is tubular, which is determined by the morphology of the carbon nanotube itself; tungsten carbide is embedded and grown on the carbon nano tube, and existence of lattice tungsten carbide and unsaturated tungsten oxide is observed on the surface of the carbon nano tube; the grain size of the carbide material is about 10 nm. As can be seen from fig. 3, the carbide material is composed of three elements, C, W, and O, and has different element distributions.
3. The preparation process of the electrode comprises the following steps: dispersing 4mg of the prepared carbide material powder in a mixed solution of 40 mu L of ethanol and 6 mu L of naphthol serving as a binder with good conductivity, carrying out ultrasonic treatment for 1 minute under the condition of 80% power, then dropwise adding 10 mu L of the obtained carbide material powder on a polished Glassy Carbon Electrode (GCE for short), and drying for 30 minutes under the condition of room temperature to obtain the detection Electrode for glucose detection. The detection Electrode, a reference Electrode platinum (Pt) and a Saturated Calomel Electrode (SCE for short) form an electrochemical detection device, an electrolyte is an alkali solution with a proper concentration, and data such as a cyclic voltammetry curve, an alternating current impedance curve and a current-time curve are obtained by using a CHI760E electrochemical workstation in Shanghai Chenghua through a conventional cyclic voltammetry method, a linear voltammetry method and the like, so that the detection effect of the carbide material on glucose is verified.
The detection parameters of the electrochemical workstation are set as follows:
cyclic Voltammetry (CV for Cyclic Voltammetry), the parameters are as follows: under the condition of 0.1M NaOH solution, the voltage range is 0.2-0.6V, the scanning speed is 0.02V/s, the number of scanning turns is 2, the sample interval time is 0.001V, the pause time is 2 seconds, the sensitivity is 0.001A/V, and glucose current values with the concentrations of 0.2mM, 0.4mM, 0.6mM, 0.8mM, 1.0mM, 1.2mM, 1.4mM, 1.6mM, 1.8mM and 2.0mM are respectively measured.
Current-time curves (Amperometric i-t Curve) with the following parameters: voltage 0.5V, sample interval 0.1 sec, pause time 0 sec, sensitivity 0.1A/V, time 1200 sec.
AC Impedance curve (AC Impedance), parameters are as follows: voltage 0.2V, dwell time 2 seconds, amplitude 0.005V.
The electrochemical detection results are shown in fig. 4 to 9, which comprehensively illustrate that the carbide material prepared by the plasma method in example 1 has lower resistance, better lower detection limit and more stable detection performance.
FIG. 4 is a plot of cyclic voltammograms at different glucose concentrations at the same sweep rate, illustrating that the oxidation and reduction peaks of the amperometric data change regularly with regular changes in glucose concentration.
FIG. 5 shows that the carbide material prepared by the plasma method in example 1 has a more sensitive detection capability.
FIG. 6 shows that the lower limit of detection of glucose by the carbide material prepared by the plasma method in example 1 is 5. Mu.M, and the detection result is visible to the naked eye.
FIG. 7 shows that the carbide material obtained by the plasma method in example 1 has a smaller resistance value.
FIG. 8 illustrates the long term stable performance of the carbide material produced by the plasma process in example 1.
FIG. 9 illustrates that the carbide material prepared by plasma in example 1 is sensitive only to glucose in blood, but not to other substances in blood such as oxalic acid, citric acid and urea, which do not interfere with glucose detection.
Example 2:
the carbide material is prepared by adopting a plasma method, and the preparation process comprises the following steps:
weighing 0.2g of carbon nano tube, adding about 5ml of proper amount of water, and stirring the carbon nano tube into paste; weighing 0.37g of ammonium metatungstate, adding the ammonium metatungstate into the pasty carbon nanotube, fully stirring for 1 hour, and standing for 11 hours to fully soak the ammonium metatungstate; drying the impregnated sample at 110 ℃ for 12 hours; and (3) treating the dried sample by plasma under the air condition of 100V, 2A, 200W and 1 hour. Finally obtaining the carbide material obtained by the plasma method.
Example 3:
the carbide material is prepared by adopting a plasma method, and the preparation process comprises the following steps:
weighing 0.2g of carbon nano tube, adding about 5ml of proper amount of water, and stirring the carbon nano tube into paste; weighing 0.37g of ammonium metatungstate, adding the ammonium metatungstate into the pasty carbon nanotube, fully stirring for 1 hour, and standing for 11 hours to fully soak the ammonium metatungstate; drying the dipped sample at 100 ℃ for 12 hours; and (3) treating the dried sample by plasma under the air condition of 100V, 2A, 200W and 1 hour. Finally obtaining the carbide material obtained by the plasma method.
Example 4:
the carbide material is prepared by adopting a plasma method, and the preparation process comprises the following steps:
weighing 0.2g of carbon nano tube, adding about 5ml of proper amount of water, and stirring the carbon nano tube into paste; weighing 0.37g of ammonium metatungstate, adding the ammonium metatungstate into the pasty carbon nanotube, fully stirring for 1 hour, and standing for 11 hours to fully soak the ammonium metatungstate; drying the impregnated sample at 120 ℃ for 11 hours; and (3) treating the dried sample by plasma under the air condition of 100V, 2A, 200W and 1 hour. Finally obtaining the carbide material obtained by the plasma method.
Example 5:
the carbide material is prepared by adopting a plasma method, and the preparation process comprises the following steps:
weighing 0.2g of carbon nano tube, adding about 5ml of proper amount of water, and stirring the carbon nano tube into paste; weighing 0.37g of ammonium metatungstate, adding the ammonium metatungstate into the pasty carbon nanotube, fully stirring for 1 hour, and standing for 11 hours to fully soak the ammonium metatungstate; drying the impregnated sample at 120 ℃ for 10 hours; and (3) treating the dried sample by plasma under the air condition of 100V, 2A, 200W and 1 hour. Finally obtaining the carbide material obtained by the plasma method.
Example 6:
the carbide material is prepared by adopting a plasma method, and the preparation process comprises the following steps:
weighing 0.2g of carbon nano tube, adding about 5ml of proper amount of water, and stirring the carbon nano tube into paste; weighing 0.37g of ammonium metatungstate, adding the ammonium metatungstate into the pasty carbon nanotube, fully stirring for 1 hour, and standing for 11 hours to fully impregnate the ammonium metatungstate; drying the impregnated sample at 120 ℃ for 11 hours; and (3) treating the dried sample by plasma under the air condition of 110V, 2A, 220W and 1 hour. Finally obtaining the carbide material obtained by the plasma method.
Example 7:
the carbide material is prepared by adopting a plasma method, and the preparation process comprises the following steps:
weighing 0.2g of carbon nano tube, adding about 5ml of proper amount of water, and stirring the carbon nano tube into paste; weighing 0.37g of ammonium metatungstate, adding the ammonium metatungstate into the pasty carbon nanotube, fully stirring for 1 hour, and standing for 11 hours to fully soak the ammonium metatungstate; drying the dipped sample at 120 ℃ for 12 hours; and (3) treating the dried sample by plasma under the air condition of 120V, 2A, 240W and 1 hour. Finally obtaining the carbide material obtained by the plasma method.
Example 8:
the carbide material is prepared by adopting a plasma method, and the preparation process comprises the following steps:
weighing 0.2g of carbon nano tube, adding about 5ml of proper amount of water, and stirring the carbon nano tube into paste; weighing 0.37g of ammonium tungstate, adding the ammonium tungstate into the pasty carbon nano tube, fully stirring for 1 hour, and standing for 12 hours to fully impregnate the ammonium tungstate; drying the dipped sample at 120 ℃ for 12 hours; and (3) treating the dried sample by plasma under the air condition of 120V, 2A, 240W and 1 hour. Finally obtaining the carbide material obtained by the plasma method.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make modifications and alterations without departing from the scope of the present invention.
Claims (3)
1. A method for preparing carbide material at low temperature by a plasma one-step method is characterized by comprising the following steps:
1) Adding a carbon material into water, stirring the mixture into paste, then adding metal salt, fully stirring the mixture, standing the mixture to fully impregnate the mixture, and then drying the mixture to obtain a dried sample;
2) Placing the dried sample in plasma equipment for processing to obtain the carbide material;
the carbon material is a carbon nano tube, and the metal salt is ammonium metatungstate;
in the step 1), the standing time is 11-20 hours; in the step 1), the drying temperature is 100-140 ℃, and the drying time is 10-16 hours;
in the step 1), the mass ratio of the metal salt to the carbon material is (1.5-2.5) to 1, and the dosage ratio of the carbon material to water is 0.2g (3-8) mL;
in the step 2), the treatment process is carried out under the air condition, the treatment temperature is normal temperature, the treatment pressure is normal pressure, and the treatment time is 0.5-1.5h;
in the treatment process, the process parameters of the plasma equipment are as follows: 100-150V, 1.5-3A and 150-400W.
2. A carbide material prepared by the method of claim 1.
3. Use of the carbide material of claim 2 in a blood glucose monitoring device.
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| CN106492863A (en) * | 2016-10-31 | 2017-03-15 | 合肥工业大学 | The method that base metal molybdenum carbide catalyst is prepared using cold plasma |
| CN107069052A (en) * | 2017-01-05 | 2017-08-18 | 中国科学院合肥物质科学研究院 | A kind of method that CNT platinum-nickel alloys composite nano materials are prepared with ammonia plasma treatment |
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