CN107082455B - A kind of nickel doped cobaltic-cobaltous oxide nano flower and preparation method thereof - Google Patents
A kind of nickel doped cobaltic-cobaltous oxide nano flower and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of nickel doped cobaltic-cobaltous oxide nano flowers and preparation method thereof.The form of the nickel doped cobaltic-cobaltous oxide nano flower of the present invention is a large amount of nanometer rods flower-like structure made of a center, and nanorod length is 500-350 nanometers.The Ni of the present invention is adulterated into Co3O4Nano flower is used in modified electrode, has good catalytic performance, low detection limit and the wide range of linearity to glucose, and the Ni of the present invention adulterates Co3O4The preparation method of nano flower is easy to operate.
Description
Technical field
The present invention relates to inorganic nano materials to adulterate field, and in particular to nickel（Ni）Doped cobaltic-cobaltous oxide（Co3O4）Nanometer
Flower and preparation method thereof.
Background technology
Metal oxide plays an important role in terms of chemistry, physics and material science, and metallic element can form
A variety of metal oxides, they can be formed it is numerous possess the geometry of different electronics structures, therefore show not
Same metal, semiconductor and insulation bulk properties.In application aspect, metal oxide be used for manufacture microelectronic circuit, sensor,
Piezoelectric device, fuel cell, and it is used for etch-proof surface passivating treatment, or it is used as catalyst.In field of electrochemical detection,
Nano material has a wide range of applications, and although nano-carbon material has high conductivity, but its electro catalytic activity is relatively low, and
Nano-noble metal material fancy price hinders the progress further applied.In contrast, transition metal oxide both has
Excellent electro catalytic activity and cheap, one-dimensional nano structure, due to its interesting characteristic and unique application, all the time
All it is the theme that scholars further investigate.Cobaltosic oxide suffers from many aspects as a kind of magnetic semiconductor of p-type
Be widely applied, for example, in terms of catalyst, energy storage and conversion, sensor and device etc..Cobaltosic oxide is in these sides
The application in face depends primarily on electricity, magnetics, optics and the catalytic performance of its own, these performances mainly depend on four oxygen again
Change the crystal structure and surface state that three bore.
On the other hand, in recent years, the incidence of diabetes is in rapid increase trend.The normal life of more and more people
The threat of diabetes is received, has millions of diabetic to need to detect the content of its blood glucose daily.In addition, glucose
Sensor is also widely used in fields such as bioanalysis, environmental monitoring and food security industry.City huge in this way
Field demand makes glucose sensor achieve quick development, while also to glucose sensor, more stringent requirements are proposed：More
High sensitivity, lower detection limit, better stability and stronger anti-interference ability etc..Electrochemical glucose sensor has
Have the advantages that of low cost, manufacturing process is simple and response is rapid, however but there is sensitivity low, detection limit for height and linear model
Enclose the problems such as small.Therefore, applicant consider, how by modified cobaltosic oxide material excellently be applied to electrochemistry grape
In terms of sugared sensor.
Invention content
To solve above-mentioned problems of the prior art, the present invention provides a kind of Ni doping Co3O4Nano flower, feature
It is, the Ni adulterates Co3O4The form of nano flower is a large amount of nanometer rods flower-like structure, nanometer rods made of a center
Length is 300-350 nanometers.Specifically, Ni of the invention adulterates Co3O4The form of nano flower is that a large amount of nanometer rods surround one
Flower-like structure made of the self assembly of center.
The present invention also provides a kind of Ni as described above to adulterate Co3O4The preparation method of nano flower comprising following steps：It will
Nickel salt, cobalt salt, urea are added to the in the mixed solvent of water and ethyl alcohol, 10-12h are reacted at 120-180 DEG C, later in 400 DEG C of skies
It is calcined 2 hours in gas, obtains Ni doping Co3O4Nano flower.
According to Co as described above3O4The molar ratio of the preparation method of nano flower, the nickel salt, cobalt salt and urea is 1:2-
3:10-11。
According to Co as described above3O4The preparation method of nano flower, the cobalt salt are Co (NO3)2ˑ6H2O, the nickel salt is
Ni(NO3)2ˑ6H2O。
Co is adulterated according to Ni as described above3O4The preparation method of nano flower, the volume ratio of the in the mixed solvent water and ethyl alcohol
It is 1:1-2.
Co is adulterated according to Ni as described above3O4The preparation method of nano flower, heating rate when calcining are 1-2 DEG C/min.
The present invention also provides a kind of modified electrodes comprising Ni as described above adulterates Co3O4Nano flower.
The present invention also provides a kind of preparation methods of modified electrode as described above, and the Ni is adulterated Co3O4Nano flower
In organic solvent, then drop coating obtains modified electrode on glass-carbon electrode for dispersion.
The present invention also provides a kind of glucose sensors comprising modified electrode as described above.
The Ni of the present invention adulterates Co3O4The preparation method of nano flower is easy to operate, and the wherein incorporation of Ni can improve four oxidations
The electric conductivity of three cobalts, the glass-carbon electrode through material modification have good catalytic performance, low detection limit and width to glucose
The range of linearity, to glucose detection high sensitivity.
Description of the drawings
Fig. 1 is the Ni doping Co of the embodiment of the present invention 13O4Nano flower scanning electron microscope diagram.
Fig. 2 is the Ni doping Co of the embodiment of the present invention 13O4Nano flower scanning electron microscope diagram.
Fig. 3 is the modified electrode of the present invention at 1mMFe (CN)6 3-/4-Cyclic voltammogram in solution.
Fig. 4 is the modified electrode of the present invention at 5mMFe (CN)6 3-/4-AC impedance figure in solution.
Fig. 5 is differential pulse figure of the nano-modified glass-carbon electrode to different glucose of the present invention.
Fig. 6 is the XRD diagram for the Co3O4 nano flowers that Ni made from embodiment 1 is adulterated.
Specific implementation mode
In order to illustrate more clearly of present disclosure, the present invention is made into one with specific embodiment below in conjunction with the accompanying drawings
The explanation of step.
The water used in experimentation is redistilled water（Abbreviation secondary water）, it is analysis to test reagent used
It is pure.
（1）, instrument and reagent used in the present embodiment
CHI832 electrochemical analysers（Shanghai Chen Hua instrument company）It is tested for cyclic voltammetric, differential pulse；It is saturated sweet
Mercury reference electrode（Shanghai Dao scientific instrument Co., Ltd）, electronic balance（Beijing Sai Duolisi Instrument Ltd.）For claiming
Measure drug；JSM-6701F cold field emission type scanning electron microscope (Jeol Ltd.) is used for morphology characterization；Ultrasonic wave is clear
Wash device（Kunshan Ultrasonic Instruments Co., Ltd.）；Alundum (Al2O3) polishing powder（0.30 mm, 0.05 mm, the examination of Shanghai Chen Hua instrument
Agent company）For handling glass-carbon electrode；Cabaltous nitrate hexahydrate, Nickelous nitrate hexahydrate, urea, absolute ethyl alcohol, potassium hydroxide（Tianjin
Kai Xin chemical industry Co., Ltd of city）High pure nitrogen（Purity is 99.999%, O2≤ 0.001%）.
One, Ni adulterates Co3O4The preparation of nano flower
Embodiment 1
a）By 0.8731g Co (NO3)2ˑ6H2O is put into the beaker of 100mL, and 0.4362g Ni (NO are added3)2ˑ6H2O adds
It is 1 to enter 80mL volume ratios：1 water and the mixed solution of ethyl alcohol stir 15min, and 0.9g urea then is being added, is waiting being completely dissolved
Form the solution of aubergine.
B) reaction solution is moved into 100mL autoclaves, is put into baking oven, reacts 12h under the conditions of 180 DEG C.
C) by autoclave natural cooling, the solution after reaction is filtered, ethyl alcohol and secondary water cleaning is used in combination for several times,
It is dried at 60 DEG C, obtains the precursor powder of aubergine.
D) gained presoma is calcined into 2h in 400 DEG C of air, heating rate when calcining is 1 DEG C/min, is finally obtained
The powder of black, i.e. Ni adulterate Co3O4Nano flower.
Fig. 1 and Fig. 2 is the Ni doping Co of the embodiment of the present invention 13O4Nano flower scanning electron microscope diagram.From Fig. 1 and Fig. 2
Electronic Speculum (SEM) characterization can be seen that, synthesized material be flowers shape.In addition, taking 10 flowers shape Ni doping Co3O4Nano flower,
It is 1.5 μm, nanorod length 350nm to measure diameter average value.In addition, Fig. 6, which is Ni made from embodiment 1, adulterates Co3O4Nano flower
XRD diagram, by Fig. 6 it can be seen that at 18.9 °, 31.1 °, 36.7 °, 44.5 °, 59.1 ° and 64.7 ° have 5 angles of diffraction,
These peaks both correspond to 111,220,311,400,511,400 crystal faces of cobalt acid nickel.Can learn in material obtained has Ni to mix
It is miscellaneous.
Embodiment 2
a）By 0.8731g Co (NO3)2ˑ6H2O is put into the beaker of 100mL, and 0.2908g Ni (NO are added3)2ˑ6H2O adds
It is 1 to enter 80mL volume ratios：2 water and the mixed solution of ethyl alcohol stir 15min, and 0.66g urea then is being added, and wait for completely molten
Solution forms the solution of aubergine.
B) reaction solution is moved into 100mL autoclaves, is put into baking oven, reacts 12h under the conditions of 120 DEG C.
C) by autoclave natural cooling, the solution after reaction is filtered, ethyl alcohol and secondary water cleaning is used in combination for several times,
It is dried at 60 DEG C, obtains the precursor powder of aubergine.
D) gained presoma is calcined into 2h in 400 DEG C of air, heating rate when calcining is 2 DEG C/min, is finally obtained
The powder of black, i.e. Ni adulterate Co3O4Nano flower.
Take 10 flowers shape Ni doping Co3O4Nano flower, it is 1.3 μm, nanorod length 336nm to measure diameter average value.
Embodiment 3
a）By 0.7275g Co (NO3)2ˑ6H2O is put into the beaker of 100mL, and 0.2908g Ni (NO are added3)2ˑ6H2O adds
It is 1 to enter 80mL volume ratios：1 water and the mixed solution of ethyl alcohol stir 15min, and 0.63g urea then is being added, and wait for completely molten
Solution forms the solution of aubergine.
B) reaction solution is moved into 100mL autoclaves, is put into baking oven, reacts 10h under the conditions of 150 DEG C.
C) by autoclave natural cooling, the solution after reaction is filtered, ethyl alcohol and secondary water cleaning is used in combination for several times,
It is dried at 60 DEG C, obtains the precursor powder of aubergine.
D) gained presoma is calcined into 2h in 400 DEG C of air, heating rate when calcining is 1 DEG C/min, is finally obtained
The powder of black, i.e. Ni adulterate Co3O4Nano flower.
Take 10 flowers shape Ni doping Co3O4Nano flower, it is 1.0 μm, length 300nm to measure diameter average value.
Two, Ni adulterates Co3O4The preparation of nano flower modified electrode and to glucose chemical property measure
Glass-carbon electrode is polished to minute surface with the alundum (Al2O3) suspension of 0.3 μm, 0.05 μm successively, then successively through volume
After the ethyl alcohol, 95%-99.5% acetone, redistilled water that score is 95%-99.5% are cleaned by ultrasonic, the glass carbon after processing totally is obtained
Electrode.Ni made from embodiment 1 is adulterated into Co3O4Nano flower disperses in ethanol, then drop coating on glass-carbon electrode to get to repairing
Adorn electrode.
Fig. 3 is the modified electrode of the present invention at 1mMFe (CN)6 3-/4-Cyclic voltammogram in solution.Fig. 4 is of the invention
Modified electrode is at 5mMFe (CN)6 3-/4-AC impedance figure in solution.In shown in Fig. 3 and Fig. 4,（a）The line mark present invention is real
Apply the Ni doping Co of example 13O4Nano flower modified electrode,（b）Indicate cobaltosic oxide modified electrode.It can from Fig. 3 and Fig. 4
To with cobaltosic oxide modified electrode（b）It compares, Ni adulterates Co3O4Nano flower modified electrode（a）Electric conductivity have prodigious carry
It is high.
Fig. 5 is differential pulse figure of the nano-modified glass-carbon electrode to different glucose of the present invention.It can from Fig. 5
To see that Ni adulterates Co3O4Nano flower modified electrode has very high sensitivity to the electrochemical oxidation of glucose, detects linear model
It encloses for 0.05mM to 0.45mM, detection is limited to 0.012mM.
The experimental results showed that the nanometer material modified electrode has very high sensitivity to the electrochemical oxidation of glucose,
Low detection line and good stability.
Finally it should be noted that：The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention,
Although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art, still may be used
With technical scheme described in the above embodiments is modified or equivalent replacement of some of the technical features.
All within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in the present invention's
Within protection domain.
Claims (9)
1. a kind of nickel doped cobaltic-cobaltous oxide nano flower, which is characterized in that the form of the nickel doped cobaltic-cobaltous oxide nano flower
For a large amount of nanometer rods flower-like structure made of a center, nanorod length is 300-350 nanometers.
2. the preparation method of nickel doped cobaltic-cobaltous oxide nano flower described in claim 1, which is characterized in that including walking as follows
Suddenly：Nickel salt, cobalt salt, urea are added to the in the mixed solvent of water and ethyl alcohol, autoclave is moved into after dissolving, in 120-180
DEG C reaction 10-12h, calcined 2 hours in 400 DEG C of air later, obtain nickel doped cobaltic-cobaltous oxide nano flower.
3. the preparation method of nickel doped cobaltic-cobaltous oxide nano flower according to claim 2, which is characterized in that the nickel
The molar ratio of salt, cobalt salt and urea is 1:2-3:10-11.
4. the preparation method of nickel doped cobaltic-cobaltous oxide nano flower according to claim 3, which is characterized in that the cobalt salt
For Co (NO3)2·6H2O, the nickel salt is Ni (NO3)2·6H2O。
5. the preparation method of nickel doped cobaltic-cobaltous oxide nano flower according to claim 2, which is characterized in that the mixing is molten
The volume ratio of water and ethyl alcohol is 1 in agent:1-2.
6. the preparation method of nickel doped cobaltic-cobaltous oxide nano flower according to claim 2, which is characterized in that liter when calcining
Warm rate is 1-2 DEG C/min.
7. a kind of modified electrode, which is characterized in that including any one of the claim 1-6 nickel doped cobaltic-cobaltous oxide nanometers
Flower.
8. a kind of preparation method of modified electrode as claimed in claim 7, which is characterized in that by four oxidation three of nickel doping
Cobalt nano flower disperses in organic solvent, and then drop coating obtains modified electrode on glass-carbon electrode.
9. a kind of glucose sensor, which is characterized in that including the modified electrode of claim 7 or 8.
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| CN109580737A (en) * | 2018-11-13 | 2019-04-05 | 云南大学 | A kind of preparation method of non-enzymatic glucose electrolytic catalysis material |
| CN110015698B (en) * | 2019-04-24 | 2021-06-15 | 湖南雅城新材料有限公司 | Flower-like aluminum-doped cobaltosic oxide and preparation method and application thereof |
| CN111072073A (en) * | 2019-12-20 | 2020-04-28 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of Ni monatomic doped cobaltosic oxide nano material, product and application thereof |
| CN112723423A (en) * | 2020-12-30 | 2021-04-30 | 西南大学 | Nickel-doped cobaltosic oxide nanosheet, preparation method thereof and application thereof in dopamine detection |
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| CN102332576A (en) * | 2011-10-20 | 2012-01-25 | 上海应用技术学院 | Chrysanthemum-shaped cobaltosic oxide (Co3O4) material and preparation method and application thereof |
| CN102502889A (en) * | 2011-10-20 | 2012-06-20 | 上海应用技术学院 | Co3O4 microsphere flower-like material as well as preparation method and application thereof |
| CN102903533A (en) * | 2012-11-06 | 2013-01-30 | 东华大学 | Method for preparing porous hybridization NiO/Co3O4 electrode material of super capacitor |
| CN103224258A (en) * | 2013-04-26 | 2013-07-31 | 吉林化工学院 | Simple method for preparing Co3O4 nano-spheres and beta-Co(OH)2 micron-flowers |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102332576A (en) * | 2011-10-20 | 2012-01-25 | 上海应用技术学院 | Chrysanthemum-shaped cobaltosic oxide (Co3O4) material and preparation method and application thereof |
| CN102502889A (en) * | 2011-10-20 | 2012-06-20 | 上海应用技术学院 | Co3O4 microsphere flower-like material as well as preparation method and application thereof |
| CN102903533A (en) * | 2012-11-06 | 2013-01-30 | 东华大学 | Method for preparing porous hybridization NiO/Co3O4 electrode material of super capacitor |
| CN103224258A (en) * | 2013-04-26 | 2013-07-31 | 吉林化工学院 | Simple method for preparing Co3O4 nano-spheres and beta-Co(OH)2 micron-flowers |
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