CN111285411A - Preparation method of binary metal oxide nano material - Google Patents
Preparation method of binary metal oxide nano material Download PDFInfo
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- CN111285411A CN111285411A CN202010117668.XA CN202010117668A CN111285411A CN 111285411 A CN111285411 A CN 111285411A CN 202010117668 A CN202010117668 A CN 202010117668A CN 111285411 A CN111285411 A CN 111285411A
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- metal oxide
- binary metal
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- niwo
- sodium polyacrylate
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
- G01N27/308—Electrodes, e.g. test electrodes; Half-cells at least partially made of carbon
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
- G01N27/327—Biochemical electrodes, e.g. electrical or mechanical details for in vitro measurements
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
- G01N27/327—Biochemical electrodes, e.g. electrical or mechanical details for in vitro measurements
- G01N27/3275—Sensing specific biomolecules, e.g. nucleic acid strands, based on an electrode surface reaction
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
- G01N27/327—Biochemical electrodes, e.g. electrical or mechanical details for in vitro measurements
- G01N27/3275—Sensing specific biomolecules, e.g. nucleic acid strands, based on an electrode surface reaction
- G01N27/3278—Sensing specific biomolecules, e.g. nucleic acid strands, based on an electrode surface reaction involving nanosized elements, e.g. nanogaps or nanoparticles
Abstract
The invention discloses a preparation method of a binary metal oxide nano material. Mixing nickel salt and Na2WO4·2H2Adding O into deionized water, respectively adding sodium polyacrylate and a cross-linking agent after ultrasonic dispersion is uniform, and uniformly stirring to obtain a mixed solution; transferring the mixed solution into a stainless steel reaction kettle, and reacting at the temperature of 120-160 ℃ for 12-24 h; after the reaction is finished, naturally cooling to room temperature, filtering the obtained product, washing with distilled water and drying to obtain the binary metal oxide NiWO4A nanocrystal. The invention adopts hydrophilic high molecular polymer sodium polyacrylate and a cross-linking agent to form gel by cross-linking in aqueous solution, thereby limiting NiWO4Growth of material to obtain a rulerBinary metal oxide NiWO with small size and good dispersibility4Nano material and has excellent glucose sensing performance.
Description
Technical Field
The invention belongs to the field of electrochemical material preparation, and particularly relates to a binary metal oxide NiWO4A preparation method of a glucose sensing nano electrode material.
Background
Diabetes mellitus, a metabolic disease, has become a serious health problem for humans, and thus further improvement of the performance of glucose sensors is a very important problem. Since glucose oxidase is easily affected by environmental factors, the enzyme immobilization process is also complicated, and its application is limited, high-performance non-enzymatic glucose sensors have received much attention. Metal oxides are considered useful non-enzymatically because of their low cost, high stability and excellent propertiesGlucose sensing detects promising materials. Particularly, binary metal oxides have better conductivity and more excellent electrochemical properties than single metal oxides, and thus are widely used in many fields. Among these binary metal oxides, NiWO4Due to high conductivity, structural stability and inherent good electrochemical performance of Ni, the material is widely applied to enzyme-free glucose electrochemical sensing active materials.Mani,SivakumarEtc. (Hydrothermal synthesis of 4NiWOcrystals forhigh performance non-enzymatic glucose biosensorsSCIENTIFIC REPORTS 2016, Vol 6: 24128) with Na2WO4·2H2O and NiCl2·6H2Synthesizing nano NiWO by taking O as raw material and adopting hydrothermal method4Application of the obtained NiWO as a non-enzymatic glucose sensor4The crystal is about 2 mu particles formed by the agglomeration of nano-scale particles.Kumar,MohitEtc. (Morphology-controlled synthesis of3D flower-like 4NiWOmicrostructure viasurfactant-free wet chemical methodJOURNAL OF ALLOYS AND COMPOUNDS,2018, Vol: 753, p: 791-798) with Na2WO4·2H2O is tungsten source, Ni (NO)3)2·6H2O is used as a nickel source, and NiWO with the size of more than 3 microns is prepared by a surfactant-free wet chemical method4Flower-like crystals. NiWO obtained as described above4The crystals are large sized particles, which severely limits their glucose sensing performance.
Disclosure of Invention
The invention aims to solve the problem of the existing NiWO prepared4Large size, poor dispersibility and easy agglomeration, and provides a binary metal oxide NiWO4A method for preparing nano material.
The invention relates to a binary metal oxide NiWO4The preparation method of the nano material specifically comprises the following steps:
1) mixing nickel salt and Na2WO4·2H2Adding O into deionized water, and ultrasonically dispersing uniformlyThen respectively adding sodium polyacrylate and a cross-linking agent, and uniformly stirring to obtain a mixed solution;
2) and transferring the mixed solution into a stainless steel reaction kettle, and reacting at the temperature of 120-160 ℃ for 12-24 h.
3) After the reaction is finished, naturally cooling to room temperature, filtering the obtained product, washing with distilled water and drying to obtain the binary metal oxide NiWO4A nanocrystal.
The nickel salt and Na2WO4·2H2The molar ratio of O is 1: 1;
the adding amount ratio of the nickel salt, the sodium polyacrylate and the cross-linking agent is (0.01-0.02) mmol: (0.5-1.0) g: (0.01-0.03) g;
the nickel salt is Ni (NO)3)2·6H2O、NiCl2·6H2O or NiCl2；
The cross-linking agent is dodecyl trimethyl ammonium bromide, tetradecyl trimethyl ammonium bromide or hexadecyl trimethyl ammonium bromide;
the molecular weight of the sodium polyacrylate is 500-700 ten thousand.
The invention adopts hydrophilic high molecular polymer sodium polyacrylate and a cross-linking agent to form gel by cross-linking in aqueous solution, thereby limiting NiWO4The growth of the material can obtain the binary metal oxide NiWO with small size and good dispersibility4Nano material and has excellent glucose sensing performance.
Detailed Description
The present invention is further analyzed with reference to the following specific examples.
Example 1.
Weighing 0.01mmol of Ni (NO)3)2·6H2O and 0.01mmol of Na2WO4.2H2O, added to 50ml of deionized water. After the ultrasonic dispersion is uniform, 1.0g of sodium polyacrylate and 0.01g of dodecyl trimethyl ammonium bromide are respectively added and stirred uniformly. The obtained solution is transferred to a stainless steel reaction kettle and reacted for 12 hours at the temperature of 160 ℃. After the reaction is finished, naturally cooling to room temperature, filtering the obtained product, washing with distilled water and dryingDry to obtain binary metal oxide NiWO4A nanocrystal.
Example 2.
Weighing 0.01mmol NiCl2·6H2O and 0.01mmol Na2WO4.2H2O, added to 50ml of deionized water. After the ultrasonic dispersion is uniform, 0.5g of sodium polyacrylate and 0.01g of tetradecyl trimethyl ammonium bromide are respectively added and stirred uniformly. Transferring the obtained solution into a stainless steel reaction kettle, and reacting at the temperature of 120 ℃ for 24 hours. After the reaction is finished, naturally cooling to room temperature, filtering the obtained product, washing with distilled water and drying to obtain the binary metal oxide NiWO4A nanocrystal.
Example 3.
Weighing 0.02mmol NiCl2And 0.02mmol Na2WO4.2H2O, added to 100ml of deionized water. After the ultrasonic dispersion is uniform, 1.0g of sodium polyacrylate and 0.03g of hexadecyl trimethyl ammonium bromide are respectively added and stirred uniformly. Transferring the obtained solution into a stainless steel reaction kettle, and reacting at the temperature of 160 ℃ for 12 h. After the reaction is finished, naturally cooling to room temperature, filtering the obtained product, washing with distilled water and drying to obtain the binary metal oxide NiWO4A nanocrystal.
Example 4.
Weighing 0.015mmol Ni (NO)3)2·6H2O and 0.015mmol Na2WO4.2H2O, added to 80ml of deionized water. After the ultrasonic dispersion is uniform, 0.8g of sodium polyacrylate and 0.02g of dodecyl trimethyl ammonium bromide are respectively added and stirred uniformly. The resulting solution was transferred to a stainless steel reaction kettle and reacted at a temperature of 140 ℃ for 18 h. After the reaction is finished, naturally cooling to room temperature, filtering the obtained product, washing with distilled water and drying to obtain the binary metal oxide NiWO4A nanocrystal.
Example 5.
Weighing 0.012mmolNi (NO)3)2·6H2O and 0.012mmol Na2WO4.2H2O, added to 60ml of deionized water. After the ultrasonic dispersion is uniform, 0.6g of sodium polyacrylate and 0.015g of ten sodium polyacrylate are respectively addedDialkyl trimethyl ammonium bromide and stirring uniformly. The obtained solution was transferred to a stainless steel reaction vessel and reacted at a temperature of 130 ℃ for 20 h. After the reaction is finished, naturally cooling to room temperature, filtering the obtained product, washing with distilled water and drying to obtain the binary metal oxide NiWO4A nanocrystal.
Example 6.
Weighing 0.016mmol NiCl2·6H2O and 0.016mmol Na2WO4.2H2O, added to 70ml of deionized water. After the ultrasonic dispersion is uniform, 0.7g of sodium polyacrylate and 0.017g of dodecyl trimethyl ammonium bromide are respectively added and stirred uniformly. The resulting solution was transferred to a stainless steel reaction kettle and reacted at a temperature of 145 ℃ for 17 h. After the reaction is finished, naturally cooling to room temperature, filtering the obtained product, washing with distilled water and drying to obtain the binary metal oxide NiWO4A nanocrystal.
Performance analysis experiments:
glucose sensing performance was tested using the three-electrode system of the CHI630D electrochemical analysis workstation. 5mg of the above example NiWO4And dissolving the nanocrystal sample in 5mL of absolute ethyl alcohol, adding 20 mu L of Nafion solution, and carrying out ultrasonic oscillation until the sample is completely dispersed in the solution to obtain a sample dispersion liquid. And (3) coating 20 mu L of sample dispersion liquid on the cleaned bare glassy carbon electrode, and airing to obtain the working electrode. The counter electrode is a platinum electrode and the reference electrode is a silver/silver chloride electrode. The electrolyte solution was 0.1M sodium hydroxide solution. All solutions used in electrochemical tests need to be deoxidized by high-purity nitrogen for at least 15min to remove dissolved oxygen in the solutions and improve the catalytic oxidation efficiency of glucose, and a constant voltage of 0.5V is set by a chronoamperometry method. The pipette was manually operated to complete the continuous addition of glucose. The particle size of the sample was analyzed using a laser particle size analyzer.
TABLE 1 particle size and glucose sensing Performance of each example sample
The above embodiments are not intended to limit the present invention, and the present invention is not limited to the above embodiments, and all embodiments are within the scope of the present invention as long as the requirements of the present invention are met.
Claims (6)
1. A preparation method of a binary metal oxide nano material is characterized by comprising the following steps:
1) mixing nickel salt and Na2WO4·2H2Adding O into deionized water, respectively adding sodium polyacrylate and a cross-linking agent after ultrasonic dispersion is uniform, and uniformly stirring to obtain a mixed solution;
2) transferring the mixed solution into a stainless steel reaction kettle, and reacting at the temperature of 120-160 ℃ for 12-24 h;
3) after the reaction is finished, naturally cooling to room temperature, filtering the obtained product, washing with distilled water and drying to obtain the binary metal oxide NiWO4A nanocrystal.
2. The method of claim 1, wherein the nickel salt and Na salt are selected from the group consisting of sodium, potassium, magnesium, and sodium2WO4·2H2The molar ratio of O is 1: 1.
3. The method for preparing a binary metal oxide nano material as claimed in any one of claims 1 to 2, wherein the adding amount ratio of the nickel salt, the sodium polyacrylate and the cross-linking agent is (0.01-0.02) mmol: (0.5-1.0) g: (0.01-0.03) g.
4. The method for preparing a binary metal oxide nanomaterial according to any one of claims 1 to 3, wherein the nickel salt is Ni (NO)3)2·6H2O、NiCl2·6H2O or NiCl2。
5. The method according to any one of claims 1 to 4, wherein the crosslinking agent is dodecyl trimethyl ammonium bromide, tetradecyl trimethyl ammonium bromide or hexadecyl trimethyl ammonium bromide.
6. The method for preparing a binary metal oxide nano material as claimed in any one of claims 1 to 5, wherein the molecular weight of the sodium polyacrylate is 500 to 700 ten thousand.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009117863A1 (en) * | 2008-03-28 | 2009-10-01 | 中国科学院大连化学物理研究所 | A complex metal oxide catalyst and its preparation and application |
| CN106379949A (en) * | 2016-11-10 | 2017-02-08 | 洛阳理工学院 | Preparation method of nickel tungsten tetraoxide nanowire |
| CN106449175A (en) * | 2016-11-14 | 2017-02-22 | 江苏大学 | Method for preparing nickel tungstate/polyaniline super-capacitor electrode material by taking foamed nickel as substrate |
| CN109054444A (en) * | 2018-06-29 | 2018-12-21 | 江苏师范大学 | A kind of preparation method of yellow nickel tungstate ceramic paint |
| CN109461590A (en) * | 2018-09-30 | 2019-03-12 | 江苏理工学院 | A kind of porous g-C3N4/NiWO4The preparation method of composite material |
| CN109806902A (en) * | 2019-02-28 | 2019-05-28 | 陕西科技大学 | A kind of W18O49/NiWO4The preparation method of/NF self-supporting electrocatalysis material |
-
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- 2020-02-25 CN CN202010117668.XA patent/CN111285411B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009117863A1 (en) * | 2008-03-28 | 2009-10-01 | 中国科学院大连化学物理研究所 | A complex metal oxide catalyst and its preparation and application |
| CN106379949A (en) * | 2016-11-10 | 2017-02-08 | 洛阳理工学院 | Preparation method of nickel tungsten tetraoxide nanowire |
| CN106449175A (en) * | 2016-11-14 | 2017-02-22 | 江苏大学 | Method for preparing nickel tungstate/polyaniline super-capacitor electrode material by taking foamed nickel as substrate |
| CN109054444A (en) * | 2018-06-29 | 2018-12-21 | 江苏师范大学 | A kind of preparation method of yellow nickel tungstate ceramic paint |
| CN109461590A (en) * | 2018-09-30 | 2019-03-12 | 江苏理工学院 | A kind of porous g-C3N4/NiWO4The preparation method of composite material |
| CN109806902A (en) * | 2019-02-28 | 2019-05-28 | 陕西科技大学 | A kind of W18O49/NiWO4The preparation method of/NF self-supporting electrocatalysis material |
Non-Patent Citations (3)
| Title |
|---|
| MANI, SIVAKUMAR ET AL.: ""Hydrothermal synthesis of NiWO4 crystals for high performance non-enzymatic glucose biosensors"", 《SCIENTIFIC REPORTS》 * |
| MASTERI-FARAHANI ET AL.: ""Microemulsion-mediated synthesis, characterization and optical properties of spherical nickel tungstate nanocrystals"", 《JOURNAL OF MATERIALS SCIENCE: MATERIALS IN ELECTRONICS 》 * |
| MEIFENG HAO ET AL.: ""Synthesis of NiWO4 powder crystals of polyhedron for photocatalytic degradation of Rhodamine"", 《SOLID STATE SCIENCES》 * |
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