CN107658145B - A kind of three-dimensional " nanometer pearl-decorated curtain shape " composition metal nitrogen/oxide and the preparation method and application thereof - Google Patents
A kind of three-dimensional " nanometer pearl-decorated curtain shape " composition metal nitrogen/oxide and the preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a kind of three-dimensional " nanometer pearl-decorated curtain shape " composition metal nitrogen/oxide, it is to use using conducting bracket material as electrode and support, in the growing mixed metal oxide precursor in its surface, then by heat treatment and nitridation, the composition metal nitrogen/oxide method formed on load conducting bracket material is made;Composition metal nitrogen/the oxide is to form three-dimensional " nanometer pearl-decorated curtain " shape on conducting bracket material with the composite metal nitride nanosphere that metal composite oxide nanometer sheet connects, wherein metal composite oxide nanometer sheet is having a size of 100~500nm, composite metal nitride nanosphere diameter is 5~50nm, and composition metal nitrogen/load capacity of the oxide on conducting bracket is 0.1~0.5mg/cm2.Operation of the present invention simple process, lower cost and higher capacitive property make the combination of composition metal nitrogen/oxide have broad application prospects in terms of energy storage.
Description
Technical field
The present invention relates to a kind of three-dimensional " nanometer pearl-decorated curtain shape " composition metal nitrogen/oxide and preparation method thereof in preparation electricity
Application in container electrode material.
Background technique
Supercapacitor and electrochemical capacitor are concerned in recent years with advantages such as its high-energy density and power densities.
The key of acquirement high-energy density and power density is largely dependent upon the selection and preparation of electrode material.In addition to traditional
Outside double layer capacitor, the capacitor of fake capacitance also attracts attention.Traditional fake capacitance capacitor electrode material is mainly Mn,
The mixing of the metal oxides such as Ni, Co, hydroxide or both.But such electrode material leads to electricity due to the problems such as electric conductivity
Container there are high rate performances poor, the more low drawback of capacitive property.
To improve disadvantages mentioned above, by metal oxide hetero atom or Heteroatom doping to introduce functional group abundant with reality
Now improve the performance of fake capacitance capacitor.Metal nitride causes the discussion interest of numerous scientific research personnel at present.Metal nitride
There is many advantageous characteristics, such as high reaction activity, excellent electronic characteristic and good catalysis effect compared with metal oxide
Fruit etc..Additionally due to the price of metal nitride is lower, therefore it also has biggish potential in energy storage field, is ideal
Anode material.Traditional metal nitride is CoN, CrN, VN or nitrided iron etc., but such nitride is because of its stability and synthesis
Complex process etc., when being used as electrode material, capacitor high rate performance is low, and cyclical stability is poor, it is still necessary to further improve.Therefore
There is an urgent need to develop novel nitride materials as high-performance fake capacitance material, to solve the defect of current material and technology.Through
Retrieval in relation to three-dimensional " nanometer pearl-decorated curtain shape " composition metal nitrogen/oxide and preparation method thereof and is preparing capacitor electrode material
In application have not been reported.
Summary of the invention
The preparation of deficiency and nitride material for current fake capacitance material property and performance limitation, the present invention mention
Supply one kind that there is three-dimensional " nanometer pearl-decorated curtain shape " composition metal nitrogen/oxide of high-performance fake capacitance and preparation method thereof and preparing
Application in capacitor electrode material.
To obtain above-mentioned three-dimensional " nanometer pearl-decorated curtain shape " composition metal nitrogen/oxide material with high-performance fake capacitance, this
It invents the technical solution used and reaction mechanism is: using constant voltage electrochemical deposition method, being prepared in conductive substrates point
The uniform metal composite oxide presoma of cloth obtains metal composite oxide by calcining, then by corresponding atmosphere
Further heat treatment, realizes the nitridation process of metal composite oxide, to obtain target composition metal nitrogen/oxide.Pass through
Realize that there are the three-dimensional " nano-beads of high-performance fake capacitance in conjunction with the stability of metal oxide and the high reaction activity of metal nitride
The preparation of curtain shape " composition metal nitrogen/oxide.
Specifically, three-dimensional " nanometer pearl-decorated curtain shape " composition metal nitrogen/oxide of the present invention, is used with conducting bracket
Material is electrode and support, in the growing mixed metal oxide precursor in its surface, then by heat treatment and nitridation, is formed negative
Composition metal nitrogen/oxide the method carried on conducting bracket material is made;It is characterized by: the three-dimensional " nanometer pearl-decorated curtain shape "
Composition metal nitrogen/oxide is the composite metal nitride connected on conducting bracket material with metal composite oxide nanometer sheet
Nanosphere forms three-dimensional " nanometer pearl-decorated curtain " shape, and wherein metal composite oxide nanometer sheet is having a size of 100~500nm, compound gold
Category nitride nano microsphere diameter be 5~50nm, composition metal nitrogen/load capacity of the oxide on conducting bracket be 0.1~
0.5mg/cm2;Metal composite oxide is that the two-dimentional cobalt acid nickel that nanometer sheet is representative is received in the composition metal nitrogen/oxide structure
Rice piece, composite metal nitride be nanosphere be the three-dimensional nickel cobalt nitrogen represented and/or be nano particle as representative two-dimentional nickel
Cobalt nitrogen;The conducting bracket material is porous metal material, selects one of nickel foam, titanium foam, foam copper, conducting bracket material
The size of material is 1 × 4cm2~4 × 8cm2, depositional area is 1 × 1cm2~1 × 4cm2。
In above-mentioned three-dimensional " nanometer pearl-decorated curtain shape " composition metal nitrogen/oxide: the metal composite oxide nanometer sheet ruler
Very little preferably 200~400nm, composite metal nitride nanosphere diameter is preferably 10~30nm, composition metal nitrogen/oxide
Load capacity on conducting bracket is 0.2~0.4mg/cm2, the conducting bracket material preferred foams nickel is preferably dimensioned to be 1
×4cm2~1 × 6cm2, depositional area is preferably 1 × 1cm2~1 × 3cm2。
Three-dimensional " nanometer pearl-decorated curtain shape " composition metal nitrogen/oxide preparation method of the present invention, step is:
(1) electrochemical deposition of metal composite oxide presoma;
(2) calcining of electrochemical deposition object, prepares metal composite oxide;
(3) three-dimensional " nanometer pearl-decorated curtain shape " composition metal nitrogen/oxide is made in the nitridation of metal composite oxide;
It is characterized by:
The method of the electrochemical deposition of step (1) the metal composite oxide presoma is: according to molar ratio 1:1~5:
1 is dissolved in water two kinds of salt in manganese nitrate, cobalt nitrate, nickel nitrate or ferric nitrate, is stirred continuously complete to dissolution;Measure 10
The mixed solution that~50mL is prepared is placed in electrolytic cell, will be having a size of 1 × 4cm2~4 × 8cm2Conducting bracket material suspend leaching
In mixing salt solution, 2~20min is deposited with -0.2~-1V with constant voltage electrochemical deposition method, depositional area is 1 × 1~1
×4cm2;Product after electrochemical deposition is cleaned up with deionized water, is placed in a vacuum drying oven, at 50~100 DEG C
Dry 5~for 24 hours;
The method that the calcining of step (2) the electrochemical deposition object prepares metal composite oxide is: by the electricity after drying
Chemical sediment is placed in silica crucible, then crucible is placed in tube furnace, under nitrogen and/or argon atmosphere protection, with 1~
10 DEG C/min heating rate is warming up to 300~350 DEG C, calcines 1~5h;Air velocity is 50~100scc;It is cooled to room temperature
Product obtained is metal composite oxide afterwards;
Step (3) method by metal composite oxide nitridation is: will obtain metal composite oxide in step (2)
It is placed in silica crucible, then crucible is placed in tube furnace, then pass to nitrogen, ammonia, nitrogen/hydrogen or Nitrogen, Ammonia,
300~800 DEG C are warming up to 1~10 DEG C/min, calcines 1~5h;Air velocity is 20~100scc;It is cooled to institute after room temperature
The product obtained is three-dimensional " nanometer pearl-decorated curtain shape " composition metal nitrogen/oxide.
In above-mentioned three-dimensional " nanometer pearl-decorated curtain shape " composition metal nitrogen/oxide preparation method: step (1) described conducting bracket
One of material preferred foams nickel, titanium foam, foam copper, conducting bracket material is preferably dimensioned to be 1 × 4cm2~1 × 6cm2,
Depositional area is preferably 1 × 1cm2~1 × 3cm2, with constant voltage electrochemical deposition method preferably with -0.8~-1V deposition 10~
12min。
In above-mentioned three-dimensional " nanometer pearl-decorated curtain shape " composition metal nitrogen/oxide preparation method: step (2) preferred embodiment party
Formula is to be warming up to 320 DEG C under nitrogen or argon atmosphere protection with 1~2 DEG C/min heating rate, calcine 2~4h.
In above-mentioned three-dimensional " nanometer pearl-decorated curtain shape " composition metal nitrogen/oxide preparation method: step (3) preferred embodiment party
Formula is to be warming up to 400 DEG C under ammonia or Nitrogen, Ammonia atmosphere protection with 1~2 DEG C/min heating rate, calcine 2~4h.
Three-dimensional " nanometer pearl-decorated curtain shape " composition metal nitrogen/oxide of the present invention is preparing answering in capacitor electrode material
With.
The present invention selects metal composite oxide that can overcome self-supporting electrode material conduction base as the matrix of nitridation
The disadvantage that combination degree is poor between electrode material, electric conductivity is low, the part of simultaneous oxidation object, which retains, can effectively improve electrode material
Stability;The formation of nitride can provide more reactivity sites, improve the compatibility of compound and electrolyte, reduce electricity
The resistivity of pole material improves the high rate performance and cyclical stability of pseudocapacitors simultaneously.Experiment confirms: three-dimensional of the invention " is received
Measle curtain shape " composition metal nitrogen/oxide has good electric conductivity and chemical property (see Fig. 4~Fig. 6), higher electricity
Capacitive can make the combination of composition metal nitrogen/oxide be widely used in terms of energy storage, indicate that it is preparing capacitor electricity
It has broad application prospects in the material of pole.
Present invention has the advantage that
(1) present invention synthesizes metal composite oxide presoma using electrochemical deposition method one-step method, and with
Collector does substrate, it is not necessary that binder is added.Simple process is effective, and save the cost avoids binder to the shadow of capacitor performance
It rings.
(2) present invention is nitrogenized using metal composite oxide, can be participated in more compared with monometallic compound first
More redox reactions provides higher fake capacitance, and secondly the introducing of nitrogen is so that complex metal compound metal oxide
Overcome the defects of multiplying power is low, resistivity is high and cyclical stability is poor, metal composite oxide part is left composition metal nitrogen
Compound provides bigger reference area and provides more active sites, while composition metal nitrogen/higher chemical stability of oxide
Be conducive to the capacitive property of capacitor.
Detailed description of the invention
Fig. 1 is the XPS spectrum figure (a) and XRD diagram (b) of metal composite oxide nitridation front and back.
Fig. 2 be different amplification under metal composite oxide (a) to (c), metal composite oxide nitridation after (d) extremely
(f) SEM schemes.
Fig. 3 be different amplification under metal composite oxide (a), (b), metal composite oxide nitridation after (c),
(d) TEM schemes.
Fig. 4 is the impedance operator spectrogram before composition metal nitrogen/oxide nitride and after nitridation.
Fig. 5 is the cyclic voltammetry curve of (a) and (b) after nitridation before composition metal nitrogen/oxide nitride.
Fig. 6 is the charging and discharging curve of (a) and (b) after nitridation before composition metal nitrogen/oxide nitride.
Specific embodiment
Combined with specific embodiments below and attached drawing the invention will be further elaborated, but embodiments of the present invention are not
It is only limitted to this, further includes any combination between each specific embodiment.Routine techniques can refer to for the technological parameter being not specified
It carries out.
Embodiment 1
Three-dimensional " nanometer pearl-decorated curtain shape " composition metal nitrogen/oxide preparation method, step is:
(1) by cobalt nitrate and nickel nitrate according to molar ratio be 2:1 ratio mixed dissolution in water, and be stirred continuously to mixing
Completely.
(2) it measures the mixed solution that 40mL is prepared to be placed in electrolytic cell, cuts 1 × 5cm2Nickel foam be suspended in mixing it is molten
In liquid, the wetted area of nickel foam is 1 × 1cm2.Circuit is connected in a manner of three-electrode system, it is heavy using constant voltage electrochemistry
Area method, deposition voltage are -1V, deposit 10min.Post-depositional nickel foam is cleaned repeatedly with deionized water to remove surface attachment
Object and the ion of attachment.Nickel foam after cleaning is placed in a vacuum drying oven, and is dried for 24 hours at 50 DEG C.
(3) nickel foam after drying is placed in silica crucible, is placed it in tube furnace under argon atmosphere with 1
DEG C/min is warming up to 320 DEG C, keep the temperature 2h.Calcined nickel foam is placed again into tube furnace, with 1 DEG C/min in ammonia atmosphere
Heating rate is warming up to 400 DEG C, keeps the temperature 2h.Air velocity control is 50scc.Resulting product is multiple after being cooled to room temperature
Close metal nitrogen/oxide.
By the nitrogen of composition metal obtained in above-described embodiment/oxide PHI 5000X X-ray photoelectron spectroscopy X (XPS) and
Nitrogen element content obviously increases in product after BrukerD8X x ray diffraction (XRD) (Fig. 1) analysis sample discovery nitridation and oxygen is first
Cellulose content reduces obviously, and most of oxygen element is successfully replaced to form Ni by nitrogen in metal composite oxide after calcining3N and
CoN, and retain NiCo2O4。
With HTACHI S-4800 Flied emission Scanning Electron microscope (Fig. 2) and JEOL company of Japan JEM2100 type transmission electricity
It is equally distributed porous NiCo that sub- microscope (Fig. 3), which carries out the metal composite oxide that observation discovery obtains,2O4Nanometer sheet.Nitrogen
After change porous nano-sheet become be with a small amount of nanometer sheet connection size be about 5-10nm nanosphere.Wherein a small amount of nanometer
Piece is metal composite oxide NiCo2O4, nanosphere is the product Ni after nitridation3N and CoN, nanometer sheet play connection nanometer
Conducting wire effect between microballoon.
Nitridation front and back composition metal chemical combination is tested with the CHI600E electrochemical workstation of Shanghai Chen Hua Instrument Ltd.
The impedance characteristic and cyclic voltammetry curve of object, the complex metal compound after discovery nitridation have good electric conductivity and electricity
Chemical property (Fig. 4~Fig. 6).Indicate that it has a wide range of applications in preparing capacitor electrode material.
To sum up, the nitrogen of composition metal obtained in above-described embodiment/oxide be three-dimensional " nanometer pearl-decorated curtain shape " composition metal nitrogen/
Oxide is the composite metal nitride nanosphere connected on conducting bracket material with metal composite oxide nanometer sheet
Three-dimensional " nanometer pearl-decorated curtain " shape is formed, wherein metal composite oxide nanometer sheet is having a size of 100~500nm, composite metal nitride
Nanosphere diameter is 5~50nm, and composition metal nitrogen/load capacity of the oxide on conducting bracket is 0.1~0.5mg/cm2;
Metal composite oxide is the two-dimentional cobalt acid nickel nano film that nanometer sheet is representative in the composition metal nitrogen/oxide structure, compound
Metal nitride be nanosphere be the three-dimensional nickel cobalt nitrogen represented and/or be nano particle as representative two-dimentional nickel cobalt nitrogen, it is described
Conducting bracket material is nickel foam.
Embodiment 2
(1) by cobalt nitrate and nickel nitrate according to molar ratio be 1:1 ratio mixed dissolution in water, and be stirred continuously to mixing
Completely.
(2) it measures the mixed solution that 40mL is prepared to be placed in electrolytic cell, cuts 1 × 4cm2Nickel foam be suspended in mixing it is molten
In liquid, the wetted area of nickel foam is 1 × 2cm2.Circuit is connected in a manner of three-electrode system, it is heavy using constant voltage electrochemistry
Area method, deposition voltage are -0.8V, deposit 5min.Post-depositional nickel foam is cleaned with deionized water repeatedly attached to remove surface
The ion of object and attachment.Nickel foam after cleaning is placed in a vacuum drying oven, the dry 20h at 60 DEG C.
(3) nickel foam after drying is placed in silica crucible, is placed it in tube furnace under argon atmosphere with 2
DEG C/min is warming up to 300 DEG C, keep the temperature 2h.Calcined nickel foam is placed again into tube furnace, in ammonia and nitrogen with the mixed of 4:1
It closes in gas and is warming up to 300 DEG C with 1 DEG C/min heating rate, keep the temperature 2h.Air velocity control is 50scc.It is cooled to room temperature
Resulting product is three-dimensional " nanometer pearl-decorated curtain shape " composition metal nitrogen/oxide afterwards.
Embodiment 3
(1) by cobalt nitrate and nickel nitrate according to molar ratio be 4:1 ratio mixed dissolution in water, and be stirred continuously to mixing
Completely.
(2) it measures the mixed solution that 50mL is prepared to be placed in electrolytic cell, cuts 1 × 8cm2Nickel foam be suspended in mixing it is molten
In liquid, the wetted area of nickel foam is 1 × 3cm2.Circuit is connected in a manner of three-electrode system, it is heavy using constant voltage electrochemistry
Area method, deposition voltage are -1V, deposit 15min.Post-depositional nickel foam is cleaned repeatedly with deionized water to remove surface attachment
Object and the ion of attachment.Nickel foam after cleaning is placed in a vacuum drying oven, the dry 10h at 80 DEG C.
(3) nickel foam after drying is placed in silica crucible, is placed it in tube furnace under argon atmosphere with 2
DEG C/min is warming up to 350 DEG C, keep the temperature 3h.Calcined nickel foam is placed again into tube furnace, in ammonia and nitrogen mixed proportion
To be warming up to 500 DEG C in the gaseous mixture of 3:1 with 1 DEG C/min heating rate, 2h is kept the temperature.Air velocity control is 50scc.It is to be cooled
Resulting product is three-dimensional " nanometer pearl-decorated curtain shape " composition metal nitrogen/oxide after to room temperature.
Claims (3)
1. a kind of three-dimensional " nanometer pearl-decorated curtain shape " composition metal nitrogen/oxide, is to use using conducting bracket material as electrode and support,
In the growing mixed metal oxide precursor in its surface, then by heat treatment and nitridation, formed on load conducting bracket material
Composition metal nitrogen/oxide method be made;It is characterized by: described three-dimensional " nanometer pearl-decorated curtain shape " composition metal nitrogen/oxidation
Object is to form three on conducting bracket material with the composite metal nitride nanosphere of metal composite oxide nanometer sheet connection
" nanometer pearl-decorated curtain " shape is tieed up, wherein for metal composite oxide nanometer sheet having a size of 100~500nm, composite metal nitride nanometer is micro-
Bulb diameter is 5~50nm, and composition metal nitrogen/load capacity of the oxide on conducting bracket is 0.1~0.5mg/cm2;This is compound
Metal composite oxide is the two-dimentional cobalt acid nickel nano film that nanometer sheet is representative, composition metal nitrogen in metal nitrogen/oxide structure
Compound be nanosphere be the three-dimensional nickel cobalt nitrogen represented and/or be nano particle as representative two-dimentional nickel cobalt nitrogen;The conductive branch
Frame material is porous metal material, selects one of nickel foam, titanium foam, foam copper, the size of conducting bracket material is 1 ×
4cm2~4 × 8cm2, depositional area is 1 × 1cm2~1 × 4cm2。
2. three-dimensional " nanometer pearl-decorated curtain shape " composition metal nitrogen/oxide according to claim 1, it is characterised in that: described multiple
Metal oxide nano-sheet is closed having a size of 200~400nm, composite metal nitride nanosphere diameter is 10~30nm, compound
Load capacity of the metal nitrogen/oxide on conducting bracket is 0.2~0.4mg/cm2, the conducting bracket material is nickel foam,
Having a size of 1 × 4cm2~1 × 6cm2, depositional area is 1 × 1cm2~1 × 3cm2。
3. three-dimensional " nanometer pearl-decorated curtain shape " composition metal nitrogen/oxide as claimed in claim 1 or 2 is in preparing capacitor electrode material
Application.
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