CN106927513A - A kind of method that nano bar-shape electrode material is prepared based on tin oxide nickel molybdate - Google Patents
A kind of method that nano bar-shape electrode material is prepared based on tin oxide nickel molybdate Download PDFInfo
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Abstract
The invention belongs to electrode material preparing technical field, and in particular to a kind of method that nano bar-shape electrode material is prepared based on tin oxide nickel molybdate.The present invention is using hydro-thermal method and the synthetic method of high-temperature calcination, pass through hydro-thermal method at a lower temperature, molybdic acid nickel nano film is directly obtained, nanometer tin dioxide rod is grown in its surface again by hydro-thermal method after drying, one-step calcination of going forward side by side obtains nickel molybdate tin ash hierarchy composite.The material has unique bar-shaped multistage package assembly of corn, and has specific surface area and good electrical conductivity higher, is expected to be used for preparing the electrode material of lithium ion battery or solar cell.The inventive method experiment condition is gently controllable, practical, and favorable reproducibility, environmental protection, and raw material be easy to get, low cost.The material has great application potential in electrochemical energy storage with the field such as conversion art and electrochemical sensing, detection.The preparation method is simple and easy to apply, general, is expected to realize industrialized application.
Description
Technical field
The invention belongs to electrochemical electrode technical field of material, and in particular to one kind is based on tin oxide-nickel molybdate system
The method of standby nano bar-shape electrode material.
Background technology
The regulation and control of the structure and pattern of inorganic nano material are always the emphasis of scientists concern.In recent years, transition gold
Category oxide material, especially manganate, the metal oxide of molybdate etc., its research report are numerous, especially photoelectrocatalysis,
The fields such as bio-sensing, microelectronic component, ultracapacitor, lithium ion battery show huge application prospect.Nickel molybdate material
Material being widely used in fields such as sensor, hydrogen reduction, electro-catalysis and lithium ion batteries, the nickel molybdate nanometer material of various patterns
Material has been synthesized.However, to meet growing energy and material demand, its specific surface area, electrolyte wellability are still
Needs are increased substantially.And the performance of electrode material depends on the arrangement of construction unit, the specific surface area of material and the electricity of material
The factors such as the wellability of pole material and electrolyte, the electric conductivity of electrode material, the quantity in electro-chemical activity site.Therefore, pass through
Increase its specific surface area, attempt the composite of the complicated hierarchy of preparation so as to effectively improve the chemical property of material
It is the hot issue for being currently needed for urgent solution.
Research shows that the composite of hierarchy can greatly improve its chemical property.Its advantage is summarized as follows：1, point
The composite of level structure has big specific surface area, can improve effective contact area of electrolyte and active material；2, point
The composite of level structure can improve the diffusion path of electrolyte；3, the composite of hierarchy is conducive to filling for electrolyte
Sub-dip is moistened.In sum, the chemical property of the composite of hierarchy is expected to be not fully exerted.
The content of the invention
The purpose of the present invention aims to provide a kind of bar-shaped nano composite material based on nickel molybdate-tin ash of corn
Preparation method.
To achieve the above object, the technical solution adopted by the present invention is to add the powder of a certain amount of nickel nitrate, sodium molybdate
Enter distilled water, be well mixed, hydro-thermal reaction is carried out at low temperature and obtains solid precursor, it is scrubbed, dry last in tube furnace
Middle calcining is obtained nickel molybdate.Then further, add in butter of tin, the solution of NaOH, drying is washed after hydro-thermal reaction
Obtain nickel molybdate-tin ash hierarchy composite.
Concrete technical scheme is as follows：
A kind of preparation method based on nickel molybdate-tin ash hierarchy composite, step is as follows：
The preparation of step 1, molybdic acid nickel nano film precursor solution：
Nickel nitrate and sodium molybdate are dissolved in distilled water and are mixed, temperature constant magnetic stirring, and be transferred in a polytetrafluoroethylene (PTFE)
It is then stand-by in the stainless steel autoclave of lining, obtain molybdic acid nickel nano film precursor solution.
The preparation of step 2, molybdic acid nickel nano film presoma electrode material：
Foam nickel sheet is cut into the fritter of 5 centimetres of 1 cm x, then it is respectively placed in acetone soln, watery hydrochloric acid successively molten
It is in liquid, the aqueous solution and ultrasonically treated；Vacuum drying is placed in after being disposed, it is stand-by；
Then above-mentioned foam nickel sheet is immersed in the solution of step 2.And be sealed in stainless steel autoclave, it is maintained at
180oC reacts 12 h, is then cooled to room temperature.After reaction terminates, cleaned with deionized water, and use acetone soak a few minutes, with
Remaining granular debris are removed, 12 h are then dried in 60 DEG C of baking ovens.
The preparation of step 3, molybdic acid nickel nano film electrode material：
Step 2 gained molybdic acid nickel nano film presoma electrode material is put into tube furnace and is calcined, after the completion of calcining, obtained
Molybdic acid nickel nano film；Last high annealing 1 hour under air conditionses, obtains molybdic acid nickel nano film.
The preparation of step 4, nickel molybdate-tin ash hierarchy composite：
By butter of tin and NaOH dissolving in deionized water.After the min of strong agitation about 5, translucent solution is obtained.
The above-mentioned molybdic acid nickel nano film being grown in nickel sheet in step 3 is transferred to the stainless steel reaction under high pressure of polytetrafluoroethyllining lining
In kettle, room temperature is heated and naturally cooled in an oven and is taken out, absolute ethyl alcohol cleaning down is used, then 80oOne is dried under C
At night, obtain nickel molybdate-tin ash hierarchy composite.
In step 1, the concentration of the nickel nitrate and sodium molybdate is 5 ~ 50 mmol/L.
In step 1, described soluble nickel salt is any one in nickel chloride, nickel nitrate, nickel acetate, soluble molybdenum salt
It is any one in sodium molybdate, amine molybdate.
In step 2, the reaction temperature in described stainless steel autoclave is 100oC~250oC, is incubated 3 ~ 24 h.
In step 3, described calcining heat is 200oC~600oC is incubated 2 ~ 5 h；Calcining programming rate is 1 ~ 5 DEG C/min.
In step 4, the concentration of described butter of tin is 1 ~ 10 mmol/L and the concentration of NaOH is 20 ~ 200
mmol/L。
In step 4, described baking oven heating-up temperature is 150oC~250oC, is incubated 3 ~ 24 hours.
Beneficial effect：
The inventive method experiment condition is gently controllable, practical, and favorable reproducibility, environmental protection, and raw material be easy to get, cost
It is low.The material is expected to be applied to the fields such as lithium ion battery, ultracapacitor field and electrochemical sensing, detection.The preparation
Method is simple and easy to apply, general, is expected to realize industrialized application.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph (SEM) of the gained nickel molybdate of the embodiment of the present invention 1-tin ash.
Specific embodiment
The present invention is expanded on further below by example, but protection scope of the present invention is not limited to these examples.This
Raw material in invention example is purchased from Shanghai Chinese medicines group, is analysis pure.
Embodiment 1
By the sodium molybdate of the nickel nitrate of 2.5mmol and 2.5mmol in 45 milliliters of distilled water, ultrasound 5 minutes in Ultrasound Instrument are put into,
It is well mixed 30 minutes it with magnetic stirrer.Temperature constant magnetic stirring, and above-mentioned solution is poured into 50 ml polytetrafluoroethyl-nes
In the reactor of alkene substrate, take out a piece of nickel foam for weighing up quality in advance and be added in aforesaid reaction vessel, seal, be placed in baking oven
In, control the temperature of baking oven for 130 DEG C, react 16 hours, room temperature is cooled to, repeatedly washing, vacuum drying, before obtaining final product nickel molybdate
Drive body；It is grown in the nickel molybdate presoma of foam nickel surface and is put into tube furnace to be calcined in 450 DEG C of air by above-mentioned, forges
It is 2 degree per minute to burn speed, is incubated 3 hours.Obtain molybdic acid nickel nano film.By 2 mmol butters of tin and 15 mmol hydroxides
Sodium is dissolved in 60 ml deionized waters.After strong agitation about 5 minutes, translucent solution is obtained.It is transferred into polytetrafluoro
In the stainless steel autoclave of ethene liner, while the above-mentioned molybdic acid nickel nano film being grown in nickel sheet is entered into instead together
Answer in kettle, be incubated 7 hours in 190 DEG C of baking ovens and naturally cool to room temperature.The nickel foam of the inside is taken out, it is thorough with absolute ethyl alcohol
Bottom is rinsed, then 80oIt is dried overnight under C, obtain nickel molybdate-tin ash hierarchy composite.As can be seen from Figure 1
The nickel molybdate of preparation-tin ash hierarchy composite includes molybdic acid nickel nano film and elongated nanometer tin dioxide rod two
Part, and the two is assembled into the corn club shaped structure of uniqueness.
Embodiment 2
By the sodium molybdate of the nickel nitrate of 6 mmol and 6 mmol in 45 milliliters of distilled water, ultrasonic 5 minutes, use in Ultrasound Instrument is put into
Magnetic stirrer is well mixed 30 minutes it.Temperature constant magnetic stirring, and above-mentioned solution is poured into 50 ml polytetrafluoroethylene (PTFE)
In the reactor of substrate, take out a piece of nickel foam for weighing up quality in advance and be added in aforesaid reaction vessel, seal, be placed in baking oven
In, control the temperature of baking oven for 150 DEG C, react 13 hours, room temperature is cooled to, repeatedly washing, vacuum drying, before obtaining final product manganese molybdate
Drive body；It is grown in the manganese molybdate presoma of foam nickel surface and is put into tube furnace to be calcined in 350 DEG C of air by above-mentioned, forges
It is 1 degree per minute to burn speed, is incubated 4 hours.Obtain molybdic acid nickel nano film.By 2.5 mmol butters of tin and 30 mmol hydrogen-oxygens
Change sodium to be dissolved in 60 ml deionized waters.After strong agitation about 5 minutes, translucent solution is obtained.It is transferred into poly- four
In the stainless steel autoclave of PVF liner, while the above-mentioned molybdic acid nickel nano film being grown in nickel sheet is entered into together
In reactor, it is incubated 5 hours in 230 DEG C of baking ovens and naturally cools to room temperature.The nickel foam of the inside is taken out, absolute ethyl alcohol is used
Cleaning down, then 80oIt is dried overnight under C, obtain nickel molybdate-tin ash hierarchy composite.
Embodiment 3
By the sodium molybdate of the nickel nitrate of 9 mmol and 9 mmol in 80 milliliters of distilled water, ultrasonic 5 minutes, use in Ultrasound Instrument is put into
Magnetic stirrer is well mixed 30 minutes it.Temperature constant magnetic stirring, and above-mentioned solution is poured into 100 ml polytetrafluoroethyl-nes
In the reactor of alkene substrate, take out a piece of nickel foam for weighing up quality in advance and be added in aforesaid reaction vessel, seal, be placed in baking oven
In, control the temperature of baking oven for 210 DEG C, react 5 hours, room temperature is cooled to, repeatedly washing, vacuum drying, before obtaining final product nickel molybdate
Drive body；It is grown in the nickel molybdate presoma of foam nickel surface and is put into tube furnace to be calcined in 300 DEG C of air by above-mentioned, forges
It is 1 degree per minute to burn speed, is incubated 5 hours.Obtain molybdic acid nickel nano film.By 3.5 mmol butters of tin and 35 mmol hydrogen-oxygens
Change sodium to be dissolved in 60 ml deionized waters.After strong agitation about 5 minutes, translucent solution is obtained.It is transferred into poly- four
In the stainless steel autoclave of PVF liner, while the above-mentioned molybdic acid nickel nano film being grown in nickel sheet is entered into together
In reactor, it is incubated 4 hours in 250 DEG C of baking ovens and naturally cools to room temperature.The nickel foam of the inside is taken out, absolute ethyl alcohol is used
Cleaning down, then 80oIt is dried overnight under C, obtain nickel molybdate-tin ash hierarchy composite.
Claims (7)
1. a kind of method that nano bar-shape electrode material is prepared based on tin oxide-nickel molybdate, it is characterised in that step is as follows：
Step 1 --- the preparation of molybdic acid nickel nano film precursor solution：Nickel nitrate and sodium molybdate are dissolved in distilled water and are mixed,
Temperature constant magnetic stirring, and be transferred in a stainless steel autoclave for polytetrafluoroethyllining lining, it is then stand-by, obtain nickel molybdate and receive
Rice piece precursor solution；Step 2 --- the preparation of molybdic acid nickel nano film presoma electrode material：Foam nickel sheet is cut into 1 li
, then be respectively placed in acetone soln, dilute hydrochloric acid solution, the aqueous solution successively for it by rice × 5 centimetres of fritter, and ultrasonically treated；
Vacuum drying is placed in after being disposed, it is stand-by；Then above-mentioned foam nickel sheet is immersed in the solution of step 2, and is sealed in not
In rust steel autoclave, 180oC reacts 12 hours, is then cooled to room temperature；Taking-up cleans several with deionized water, acetone soak
Minute, to remove the granular debris of remnants, then dried 12 hours in 60 DEG C of baking ovens；Step 3 --- molybdic acid nickel nano film electricity
The preparation of pole material：Step 2 gained molybdic acid nickel nano film presoma electrode material is put into tube furnace into high temperature in atmosphere to move back
Fire 1 hour, obtains molybdic acid nickel nano film；The preparation of step 4 --- nickel molybdate-tin ash hierarchy composite：By four
Stannic chloride and NaOH dissolving are in deionized water；After strong agitation about 5 minutes, translucent solution is obtained；By in step 3
The above-mentioned molybdic acid nickel nano film being grown in nickel sheet is transferred in the stainless steel autoclave of polytetrafluoroethyllining lining, is being dried
Certain hour is heated in case and is taken out after naturally cooling to room temperature, absolute ethyl alcohol cleaning down is used, then 80oDried under C, obtained
The nickel molybdate for arriving-tin ash hierarchy composite.
2. the preparation method based on nickel molybdate-tin ash hierarchy composite according to claim 1, its feature
It is that in step 1, the concentration of the nickel nitrate and sodium molybdate is 5 ~ 50 mmol/L.
3. the preparation method based on nickel molybdate-tin ash hierarchy composite according to claim 1, its feature
It is that in step 1, described soluble nickel salt is any one in nickel chloride, nickel nitrate, nickel acetate, and soluble molybdenum salt is
Any one in sodium molybdate, amine molybdate.
4. the preparation method based on nickel molybdate-tin ash hierarchy composite according to claim 1, its feature
It is that in step 2, the reaction temperature in described stainless steel autoclave is 100oC~250oC, is incubated 3 ~ 24 hours.
5. the preparation method based on nickel molybdate-tin ash hierarchy composite according to claim 1, its feature
It is that in step 3, described calcining heat is 200oC~600oC is incubated 2 ~ 5h；Calcining programming rate is 1 ~ 5 DEG C/min.
6. the preparation method based on nickel molybdate-tin ash hierarchy composite according to claim 1, its feature
It is that in step 4, the concentration of described butter of tin is 1 ~ 10 mmol/L and the concentration of NaOH is 20 ~ 200 mmol/
L。
7. the preparation method based on nickel molybdate-tin ash hierarchy composite according to claim 1, its feature
It is that in step 4, described baking oven heating-up temperature is 150oC~250oC, is incubated 3 ~ 24 hours.
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Cited By (2)
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| CN108597907A (en) * | 2018-06-14 | 2018-09-28 | 福建宸琦新材料科技有限公司 | A kind of preparation method and application of nickel molybdenum selenides/nickel foam combination electrode material |
| CN108754526A (en) * | 2018-04-12 | 2018-11-06 | 中国科学院合肥物质科学研究院 | A kind of manganese tungstate nanometer sheet material and the preparation method and application thereof |
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Cited By (2)
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| CN108754526A (en) * | 2018-04-12 | 2018-11-06 | 中国科学院合肥物质科学研究院 | A kind of manganese tungstate nanometer sheet material and the preparation method and application thereof |
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