CN110441362A - A kind of nanometer of NbN/graphite composite paste electrode sensor preparation method - Google Patents
A kind of nanometer of NbN/graphite composite paste electrode sensor preparation method Download PDFInfo
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Abstract
The invention discloses the preparation methods of a kind of nanometer of NbN/ graphite composite paste electrode sensor, which is characterized in that uses sulfuric acid: and potassium metaperiodate pre-processes nano graphite powder, obtains pretreatment nano graphite powder；Composite adhesive is made using 1- vinyl -3- butyl imidazole fluoroform sulphonate dissolution luffa；Then, in the agate mortar, it is added by following mass percent, nano silicon nitride niobium: 42 ~ 46%, pretreatment nano graphite powder: 22 ~ 26%, composite adhesive: 14 ~ 18%, atoleine: 16 ~ 20%, then the loading of its carbon paste is connected in the interior glass tube passed through as Φ 6mm of conducting wire uniformly at carbon paste shape, obtains a nanometer NbN/ graphite composite paste electrode sensor by grinding.The advantages that carbon paste electrode prepared by the application improves 6 ~ 8 times than common carbon paste electrode electric conductivity, and electrochemical window mouth width, preparation method are simple, at low cost, surface easily updates, aftercurrent is small.Astaxanthin high sensitivity is detected, selectivity is good.
Description
Technical field
The present invention relates to a kind of preparation methods of electrochemical sensor, in particular to a kind of nanometer of NbN/graphite composite paste
The preparation method and application of electrode sensor.Belong to electrochemical analysis field.
Background technique
Nitride is the binary compound that nitrogen is formed with electronegativity element less than that.By transition elements and the direct chemical combination of nitrogen
The nitride of generation is also known as metal mold nitride.They belong to " fill compound ", because nitrogen-atoms is in occupation of in metal lattice
Interstitial site and gain the name.This compound metallike in terms of appearance, hardness and electric conductivity, typically hardness is big, fusing point is high,
Chemical property is stablized, and conductive.Niobium nitride (NbN) is typical B-1 type compound.Sodium chloride crystal structure.Thermostabilization
Property and chemical stability it is high, anti-neutron irradiation, excellent superconducting film material, and electric conductivity with higher and superconductivity and
Wide potential window.
Graphite is a kind of transiens crystal between atomic crystal, metallic crystal and molecular crystal.The same layer carbon in crystal
Covalent bond is formed with sp2 hydridization between atom, each carbon atom is connected with the other three carbon atom, and six carbon atoms are in same plane
The upper ring for forming regular hexagon, stretching, extension form lamellar structure.Next p track is remained conplane carbon atom is also each, they
It overlaps each other, the pi bond electronics for forming delocalization can move freely in lattice, can be excited, so graphite has metallic luster, energy
Conductive, heat transfer.The electric conductivity of graphite is 100 times higher than general nonmetallic ore.Thermal conductivity is more than the metal materials work stones such as steel, iron, lead
Ink.Thermal coefficient is increased with temperature and is reduced, or even at very high temperatures, graphite has good at normal temperature at heat guard, graphite
Good chemical stability and wide potential window, acidproof, alkaline-resisting and organic solvent-resistant the corrosion of energy, graphite use at normal temperature
When be able to take the acute variation of temperature and will not destroy.But in many cases graphite be all multiple-layer stacked together, layer with
Area between layer is not utilized effectively, and actual capacity is low.How to realize that effective dispersion of graphite is to improve and change
The important channel of kind graphite electrochemistry performance.In addition, graphite is overlapping with the compound also inhibition graphite flake layer of other nanostructures.
It is compound that the transition metal nitride of high capacity or conducting polymer and graphite are subjected to lamination, one side graphite by other substances every
Leave, reunion can be reduced, increase the mobility of electrolyte, on the other hand, graphite be it is compound after fake capacitance substance provide
The three-dimensional network of electronics conduction.Composite material exhibits based on graphite go out synergistic effect, maintain while obtaining high capacity
Good high rate performance.
Carbon paste electrode is the Carbon Materials using electric conductivity, if the adhesive of graphite powder and hydrophobicity is mixed and made into paste,
Then it is coated in the surface of electrode bar or is packed into electrode tube and manufactured a kind of electrode.Since carbon paste electrode is nontoxic, electric
The advantages that chemical window is wide, preparation method is simple, at low cost, surface easily updates, aftercurrent is small, is widely used to electrochemistry
In analysis, biosensor preparation and environment measuring, food and medicine analysis.But there is also some disadvantages for carbon paste electrode, such as conductive
Performance is poor, and sensitivity is low, stability difference etc..In order to improve the performance of carbon paste electrode, using titanium nitride/carbon nanotube composite
Expect the conductive material as carbon paste electrode, improves electrode sensitivity and selectivity.
Astaxanthin has a variety of physiological functions, such as inoxidizability, antitumor, pre- anti-cancer, strengthen immunity, prevent
Cardiovascular and cerebrovascular disease, improvement eyesight etc. have certain effect.Astaxanthin in vivo can be in conjunction with protein and in green, blue
Color, effect.For astaxanthin from the microalgae of referred to as haematococcus clothing, this kind of seaweed is extremely rich in polar ocean environment
Richness, and be a kind of natural carotenoid.Antioxidant effect is 10 times stronger than beta carotene, 100 times stronger than vitamin E.
The method for having reported measurement astaxanthin is high performance liquid chromatography.It is that one kind is accurate using carbon paste electrode method measurement astaxanthin,
Sensitive and effectively analysis method.
Summary of the invention
The purpose of the present invention is melt luffa as compound adhesive using 1- vinyl -3- butyl imidazole fluoroform sulphonate
Stick prepares a kind of nanometer of NbN/graphite composite paste electrode sensor, provides the compound paste electrode of a kind of nanometer of NbN/graphite and passes
The preparation method of sensor, and application detection astaxanthin.
Instrument and reagent
CHI660B electrochemical workstation (Shanghai Chen Hua instrument company), experiment use three-electrode system: platinum electrode is auxiliary electricity
Pole, Ag/AgCl are reference electrode (SCE), and nano silicon nitride niobium/compound paste electrode of graphite is working electrode；KQ-250E type ultrasound
Wave washer (Kun Feng ultrasonic instrument Co., Ltd).
Nano silicon nitride niobium, nano graphite powder, 1- vinyl -3- butyl imidazole fluoroform sulphonate, dehydrated alcohol, sulfuric acid,
Potassium metaperiodate, astaxanthin, silicone oil, agents useful for same are that analysis is pure, and water is deionized water.
The purpose of the present invention is achieved through the following technical solutions.
A kind of nanometer of NbN/graphite composite paste electrode sensor preparation method, which is characterized in that this method has following
Processing step:
(1) nano graphite powder pre-processes: in the reactor, it is added by following mass percent, deionized water: 54 ~ 57%, slowly
The addition concentrated sulfuric acid: 30 ~ 34%, it stirs evenly, is cooled to room temperature, potassium metaperiodate: 3 ~ 5%, stirring and dissolving, addition nano graphite powder: 8 ~
12%, the sum of each component mass percent is absolutely, in 18 ~ 20h of soaking at room temperature, then to boil 20min, be cooled to room temperature, solid-liquid
Separation is washed with deionized to neutrality, dry, and grinding is to get pretreatment nano graphite powder；
(2) prepared by composite adhesive: in a kettle, being added by following mass percent, 1- vinyl -3- butyl imidazole trifluoro
Mesylate: 72 ~ 76%, pretreatment Loofah powder: 24 ~ 28%, sealing cover is covered, is placed in insulating box, temperature is at 160 ± 2 DEG C
Constant temperature reacts 15 ~ 18h, obtains viscous light yellow transparency liquid, is composite adhesive；
(3) nanometer NbN/graphite composite paste electrode sensor preparation: in the agate mortar, being added by following mass percent,
Nano silicon nitride niobium: 42 ~ 46%, pretreatment nano graphite powder: 22 ~ 26%, composite adhesive: 14 ~ 18%, atoleine: 16 ~ 20%,
The sum of each component mass percent is absolutely, to grind uniformly at carbon paste shape, and then the loading of its carbon paste is connected in conducting wire
Through in the glass tube for Φ 6mm, be compacted, it is dry, polished, polished with abrasive paper for metallograph, deionized water washing to get nanometer NbN/
Graphite composite paste electrode sensor.
Pretreatment Loofah powder described in step (2) is that mature loofah peeling removes son, is handled respectively with soda acid, goes to deacidify
Alkali soluble matter is crushed, and be sieved 200 mesh.
Atoleine described in step (3) is medical grade.
Nanometer NbN/steps are as follows for graphite composite paste electrode sensor measurement astaxanthin:
(1) standard solution is prepared: preparing the astaxanthin standard solution of one group of various concentration including blank standard specimen, bottom liquid is
PH=4.00B-R buffer solution；
It (2) is reference electrode by Ag/AgCl, platinum electrode is auxiliary electrode, nanometer NbN/graphite composite paste prepared by the present invention
Electrode sensor is that working electrode forms three-electrode system, connects CHI660B electrochemical workstation, and bottom liquid is pH=4.00B-R
Then buffer solution scans the solution using chronoamperometry in the potential range of -0.1 ~ 1.2V, operating voltage 0.50V,
The peak point current of astaxanthin and astaxanthin concentration is taken under various concentration to work curve；This method shows very highly selective and clever
The concentration of quick property, response current and astaxanthin is 6.0 × 10-8~2.0×10-4It is in good linear relationship, phase within the scope of mol/L
Coefficients R=0.9962 is closed, detection is limited to 2.21 × 10-8mol/L；
(3) detection of astaxanthin: the astaxanthin standard solution in step (1) is replaced with sample to be tested, according to the method for step (2)
It is detected, according to response the difference of current reduction△IAnd working curve, obtain the content of astaxanthin in sample to be tested.Its time
Yield is between 95.02 ~ 105.12%.
Advantages of the present invention and effect are:
(1) present invention preparation nanometer NbN/graphite composite paste electrode sensor, is added nanometer NbN, using 1- in carbon paste electrode
Vinyl -3- butyl imidazole fluoroform sulphonate melts luffa as composite adhesive, and atoleine will be received as adjuvant
The carbon paste electrode that rice NbN and pretreatment nano graphite powder are mixed with improves 6 ~ 8 times than common carbon paste electrode electric conductivity,
The advantages that electrochemical window mouth width, preparation method are simple, at low cost, surface easily updates, aftercurrent is small；
(2) nanometer NbN/graphite composite paste electrode sensor prepared by the present invention does not use toxic examination during preparation
Agent, environment-friendly and green are prepared simple and easy；
(3) nanometer NbN prepared by the present invention/graphite composite paste electrode sensor is used successfully to drug, biological sample astaxanthin
Detection in, solve astaxanthin detection difficult, improve the sensitivity of detection.
Specific embodiment
Embodiment 1
(1) nano graphite powder pre-processes: in the reactor, be separately added into, deionized water: 55 mL are slowly added to the concentrated sulfuric acid: 18
ML is stirred evenly, and is cooled to room temperature, potassium metaperiodate: 6g, stirring and dissolving, and nano graphite powder: 7g is added, in soaking at room temperature 19h, then
20min is boiled, room temperature is cooled to, is separated by solid-liquid separation, is washed with deionized to neutrality, dry, grinding is to get pretreatment nano-graphite
Powder；
(2) prepared by composite adhesive: it in a kettle, is separately added into, 1- vinyl -3- butyl imidazole fluoroform sulphonate:
74g, pre-process Loofah powder: 26g covers sealing cover, is placed in insulating box, and temperature is reacted 16h, obtained in 160 ± 2 DEG C of constant temperature
It is composite adhesive to viscous light yellow transparency liquid；
(3) it nanometer NbN/graphite composite paste electrode sensor preparation: in the agate mortar, is separately added into, nano silicon nitride niobium:
44g pre-processes nano graphite powder: 24g, composite adhesive: 16g, atoleine: 16g, then grinding will uniformly at carbon paste shape
Its carbon paste is packed into the interior glass tube through being Φ 6mm for being connected with conducting wire, is compacted, dry, is polished, is polished with abrasive paper for metallograph, gone from
Sub- water washing is to get nanometer NbN/graphite composite paste electrode sensor.
Embodiment 2
(1) nano graphite powder pre-processes: it in the reactor, is separately added into, deionized water: 57mL and is slowly added to the concentrated sulfuric acid:
17mL is stirred evenly, and is cooled to room temperature, potassium metaperiodate: 7g, stirring and dissolving, and nano graphite powder: 6g is added, in soaking at room temperature 18h,
20min is boiled again, is cooled to room temperature, is separated by solid-liquid separation, is washed with deionized to neutrality, and dry, grinding is to get pretreatment nanometer stone
Ink powder；
(2) prepared by composite adhesive: it in a kettle, is separately added into, 1- vinyl -3- butyl imidazole fluoroform sulphonate:
72g, pre-process Loofah powder: 28g covers sealing cover, is placed in insulating box, and temperature is reacted 17h, obtained in 160 ± 2 DEG C of constant temperature
It is composite adhesive to viscous light yellow transparency liquid；
(3) it nanometer NbN/graphite composite paste electrode sensor preparation: in the agate mortar, is separately added into, nano silicon nitride niobium:
42g pre-processes nano graphite powder: 26g, composite adhesive: 14g, atoleine: 18g, then grinding will uniformly at carbon paste shape
Its carbon paste is packed into the interior glass tube through being Φ 6mm for being connected with conducting wire, is compacted, dry, is polished, is polished with abrasive paper for metallograph, gone from
Sub- water washing is to get nanometer NbN/graphite composite paste electrode sensor.
Embodiment 3
(1) nano graphite powder pre-processes: in the reactor, be separately added into, deionized water: 54 mL are slowly added to the concentrated sulfuric acid:
17.5mL is stirred evenly, and is cooled to room temperature, potassium metaperiodate: 5g, stirring and dissolving, nano graphite powder: 10g is added, in soaking at room temperature
20h, then 20min is boiled, it is cooled to room temperature, is separated by solid-liquid separation, be washed with deionized to neutrality, dry, grinding is received to get pretreatment
Rice graphite powder；
(2) prepared by composite adhesive: it in a kettle, is separately added into, 1- vinyl -3- butyl imidazole fluoroform sulphonate:
76g, pre-process Loofah powder: 24g covers sealing cover, is placed in insulating box, and temperature is reacted 15h, obtained in 160 ± 2 DEG C of constant temperature
It is composite adhesive to viscous light yellow transparency liquid；
(3) it nanometer NbN/graphite composite paste electrode sensor preparation: in the agate mortar, is separately added into, nano silicon nitride niobium:
46g pre-processes nano graphite powder: 22g, composite adhesive: 15g, atoleine: 17g, then grinding will uniformly at carbon paste shape
Its carbon paste is packed into the interior glass tube through being Φ 6mm for being connected with conducting wire, is compacted, dry, is polished, is polished with abrasive paper for metallograph, gone from
Sub- water washing is to get nanometer NbN/graphite composite paste electrode sensor.
Embodiment 4
(1) nano graphite powder pre-processes: in the reactor, be separately added into, deionized water: 54 mL are slowly added to the concentrated sulfuric acid: 19
ML is stirred evenly, and is cooled to room temperature, potassium metaperiodate: 5g, stirring and dissolving, and nano graphite powder: 7g is added, in soaking at room temperature 18.5h,
20min is boiled again, is cooled to room temperature, is separated by solid-liquid separation, is washed with deionized to neutrality, and dry, grinding is to get pretreatment nanometer stone
Ink powder；
(2) prepared by composite adhesive: it in a kettle, is separately added into, 1- vinyl -3- butyl imidazole fluoroform sulphonate:
75g, pre-process Loofah powder: 25g covers sealing cover, is placed in insulating box, and temperature is reacted 18h, obtained in 160 ± 2 DEG C of constant temperature
It is composite adhesive to viscous light yellow transparency liquid；
(3) it nanometer NbN/graphite composite paste electrode sensor preparation: in the agate mortar, is separately added into, nano silicon nitride niobium:
43g pre-processes nano graphite powder: 25g, composite adhesive: 18g, atoleine: 14g, then grinding will uniformly at carbon paste shape
Its carbon paste is packed into the interior glass tube through being Φ 6mm for being connected with conducting wire, is compacted, dry, is polished, is polished with abrasive paper for metallograph, gone from
Sub- water washing is to get nanometer NbN/graphite composite paste electrode sensor.
By the NbN of nanometer prepared by above-described embodiment 1 ~ 4/graphite composite paste electrode sensor, for astaxanthin in sample
Detection, by detecting step carry out.Nanometer NbN prepared by the present invention/graphite composite paste electrode sensor be used successfully to drug,
In biological sample in the detection of astaxanthin, thus molecular engram sensor prepared by the present invention can be widely applied to biological medicine,
The related fieldss such as biology sample detection solve the difficulty of astaxanthin detection.
Claims (4)
1. a kind of nanometer of NbN/graphite composite paste electrode sensor preparation method, which is characterized in that this method has following
Processing step:
(1) nano graphite powder pre-processes: in the reactor, it is added by following mass percent, deionized water: 54 ~ 57%, slowly
The addition concentrated sulfuric acid: 30 ~ 34%, it stirs evenly, is cooled to room temperature, potassium metaperiodate: 3 ~ 5%, stirring and dissolving, addition nano graphite powder: 8 ~
12%, the sum of each component mass percent is absolutely, in 18 ~ 20h of soaking at room temperature, then to boil 20min, be cooled to room temperature, solid-liquid
Separation is washed with deionized to neutrality, dry, and grinding is to get pretreatment nano graphite powder；
(2) prepared by composite adhesive: in a kettle, being added by following mass percent, 1- vinyl -3- butyl imidazole trifluoro
Mesylate: 72 ~ 76%, pretreatment Loofah powder: 24 ~ 28%, sealing cover is covered, is placed in insulating box, temperature is at 160 ± 2 DEG C
Constant temperature reacts 15 ~ 18h, obtains viscous light yellow transparency liquid, is composite adhesive；
(3) nanometer NbN/graphite composite paste electrode sensor preparation: in the agate mortar, being added by following mass percent,
Nano silicon nitride niobium: 42 ~ 46%, pretreatment nano graphite powder: 22 ~ 26%, composite adhesive: 14 ~ 18%, atoleine: 16 ~ 20%,
The sum of each component mass percent is absolutely, to grind uniformly at carbon paste shape, and then the loading of its carbon paste is connected in conducting wire
Through in the glass tube for Φ 6mm, be compacted, it is dry, polished, polished with abrasive paper for metallograph, deionized water washing to get nanometer NbN/
Graphite composite paste electrode sensor.
2. a kind of nanometer of NbN according to claim 1/graphite composite paste electrode sensor preparation method, feature
It is, pretreatment Loofah powder described in step (2) is that mature loofah peeling removes son, is handled respectively with soda acid, removes soda acid
Soluble matter is crushed, and be sieved 200 mesh.
3. a kind of nanometer of NbN according to claim 1/graphite composite paste electrode sensor preparation method, feature
It is, atoleine described in step (3) is medical grade.
4. prepared by a kind of nanometer of NbN according to claim 1/graphite composite paste electrode sensor preparation method
Nanometer NbN/graphite composite paste electrode sensor.
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Cited By (1)
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Application publication date: 20191112 |