CN102757101A - Method for preparing large-specific-surface-area porous nickel oxide microspheres - Google Patents
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- CN102757101A CN102757101A CN2012100486082A CN201210048608A CN102757101A CN 102757101 A CN102757101 A CN 102757101A CN 2012100486082 A CN2012100486082 A CN 2012100486082A CN 201210048608 A CN201210048608 A CN 201210048608A CN 102757101 A CN102757101 A CN 102757101A
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Abstract
The invention discloses a method for preparing large-specific-surface-area porous nickel oxide microspheres. The method comprises the following steps of: preparing and synthesizing a mixed solution by taking nickel nitrate and urine as raw materials, taking hexadecyl trimethyl ammonium bromide as a surfactant, taking absolute ethanol and deionized water as washing agents and refining raw materials; heating in a reaction kettle for preparing hydrogen nickel carbonate; and washing, performing suction filtration, drying in vacuum, and baking to obtain large-specific-surface-area porous nickel oxide microspheres. The preparation method has the advantages of advanced process, short process flow, small using amount of raw materials, detailed and accurate data, high product yield which can be up to 95 percent and high product purity, which can be up to 98.5 percent; the specific surface area of the product, i.e., nickel oxide microspheres is 748.25m<2>/g, microsphere particles are less than or equal to 10 mum, irregular hexagonal nano-sheets are distributed on the surfaces of the microspheres and are less than or equal to 40 nanometers in diameter, and the microspheres can be matched with a plurality of chemical substances; and the method is very ideal method for preparing large-specific-surface-area porous nickel oxide microspheres.
Description
Technical field
The present invention relates to a kind of preparation method of bigger serface porous nickel oxide microballoon, the technical field that belongs to the mineral compound preparation and use.
Background technology
Along with the development of nano science with technology, the material with special appearance nanostructure arises at the historic moment, and is applied in fields such as optics, electronics, catalysis; Semiconductor oxide micro-nano rice structured material because of having special construction and complex topography, often is applied in the optical electron device; The porous pattern is owing to have equally distributed micropore and hole; Porosity is high; Volume density is little, has high specific surface area and unique physical surface properties, and different porousness can change the physics and the chemical property of material; Therefore bigger serface porous structure material function is good, can use in biotechnology, fine chemistry industry, environmental engineering, catalyzer and sensor field.
Nano-nickel oxide is a kind of important functional material; Because its unique electricity, magnetics and catalysis characteristics; Be widely used as electrode, catalyzer, magneticsubstance and the gas sensor etc. of battery, because the peculiar property of nano-nickel oxide depends on their pattern and size, so its compound method of the nano-nickel oxide of different-shape structure also has various ways; For example: in water and glycerine mixed solvent, hydrolysis has prepared the nano-nickel oxide of carnation shape to Yang etc. through nickel acetate; Kuang etc. under the effect of AS, through Hydrothermal Preparation the nickel oxide micron ball of laminate structure; Employing Hydrazine Hydrate 80 methods such as Zhou have prepared the concave polyhedron nickel oxide nano particle that nanometer sheet is formed; Banerjee etc. are that soft template, urea are that precipitation agent has prepared ordered porous NiO nano-multicrystal body with the sodium lauryl sulphate; Feng etc. are that template has prepared nickel oxide material bimodal distribution, order mesoporous with KIT-6; Though these methods have prepared the nickel oxide material of different structure, the specific surface area of NiO is little, and its application has received great limitation; Also all there are some technology drawbacks, the processing parameter out of true that has, product purity is low, and the product structure characteristic that has is not obvious, is difficult to and other chemical substance couplings, and the process method that has is complicated, and preparation cost is high, is difficult to carry out suitability for industrialized production.
Summary of the invention
Goal of the invention
The objective of the invention is situation to background technology; Adopt sluggish precipitation; The preparation mixing solutions, hydrothermal preparation hydrogen-carbonate nickel is through filtration, washing, vacuum-drying, high-temperature roasting; Process bigger serface porous nickel oxide microballoon, with purity and the physical and chemical performance that increases substantially the nickel oxide microballoon.
Technical scheme:
The chemical substance material that the present invention uses is: nickelous nitrate, urea, cetyl trimethylammonium bromide, absolute ethyl alcohol, deionized water, it is following that consumption is prepared in its combination: with gram, milliliter is measure unit
Nickelous nitrate: Ni (NO
3)
26H
2O 14.55g ± 0.01g
Urea: CO (NH
2)
23g ± 0.01g
Cetyl trimethylammonium bromide: C
16H
33(CH
3)
3NBr 9.1g ± 0.01g
Absolute ethyl alcohol: C
2H
5OH 1000mL ± 50mL
Deionized water: H
2O 2000mL ± 50mL
The preparation method is following:
(1) selected chemical substance material
The chemical substance material that preparation is used will carry out selected, and carries out quality purity control:
Nickelous nitrate: solid-state solid >=99%
Urea: solid-state solid >=99%
Cetyl trimethylammonium bromide: solid-state solid >=99%
Absolute ethyl alcohol: liquid liquid 99.7%
Deionized water: liquid liquid 99.7%
(2) preparation nickel nitrate aqueous solution
Take by weighing nickelous nitrate 14.55g ± 0.01g, measure deionized water 200mL ± 0.01mL, add in the beaker, magnetic agitation 60min becomes: the nickel nitrate aqueous solution of 0.25mol/L;
(3) the preparation cetyl trimethylammonium bromide aqueous solution
Take by weighing cetyl trimethylammonium bromide 9.1g ± 0.01g, measure deionized water 200mL ± 0.01mL and add in the beaker, magnetic agitation 60min becomes: the cetyl trimethylammonium bromide aqueous solution of 0.125mol/L;
(4) preparation carbonate synthesis hydrogen nickel mixing solutions
Nickel nitrate aqueous solution 100mL, cetyl trimethylammonium bromide aqueous solution 100mL are added in the polytetrafluoroethylcontainer container;
Take by weighing urea 3g ± 0.01g, add in the polytetrafluoroethylcontainer container, and sealing;
Polytetrafluoroethylcontainer container is placed on the magnetic stirring apparatus, and magnetic agitation 60min becomes: transparence blue-greenish colour ternary mixing solutions;
(5) hydrogen-carbonate nickel building-up reactions
The building-up reactions of hydrogen-carbonate nickel is in stainless steel cauldron, in electrical heater, to carry out;
The polytetrafluoroethylcontainer container that fills the ternary mixing solutions is placed in the stainless steel cauldron, and seal with kettle cover;
Then reaction kettle is placed the electrical heater internal heating, 150 ℃ ± 2 ℃ of Heating temperatures, heat-up time 240min ± 5min;
Mixing solutions will carry out chemical reaction under heated condition in reaction kettle, reaction equation is following:
In the formula: Ni (HCO
3)
2: hydrogen-carbonate nickel, NH
4NO
3: an ammonium nitrate, H
2O: water vapour, Ni (NH
3)
6(NO
3)
2: nitric acid hexamine nickel (II), CO
2: carbonic acid gas;
After reaction finishes, for containing the sedimentary turbid solution of hydrogen-carbonate nickel, stop heating in the polytetrafluoroethylcontainer container, make it naturally cool to 20 ℃ ± 2 ℃;
After the cooling, open reaction kettle, take out and contain the sedimentary turbid solution of hydrogen-carbonate nickel;
(6) suction filtration
The sedimentary turbid solution of carbonated hydrogen nickel is placed the B on the filter flask, carry out suction filtration with millipore filtration, retain the product filter cake on the filter membrane, waste liquid is evacuated in the filter flask;
(7) deionized water wash, suction filtration
The product filter cake is placed beaker, add deionized water 100mL, agitator treating 5min; Then washings is placed the B on the filter flask, carry out suction filtration with millipore filtration, retain the product filter cake on the filter membrane, washings is evacuated in the filter flask; Deionized water wash, suction filtration repeat 5 times;
(8) absolute ethanol washing, suction filtration
The product filter cake is placed beaker, add absolute ethyl alcohol 100mL, agitator treating 5min; Then washings is placed the B on the filter flask, carry out suction filtration with millipore filtration, retain the product filter cake on the filter membrane, washings is evacuated in the filter flask; Absolute ethanol washing, suction filtration repeat 5 times;
(9) vacuum-drying
Product filter cake behind washing, the suction filtration is placed quartzy product boat, place vacuum drying oven to carry out drying then, 60 ℃ ± 2 ℃ of drying temperatures, vacuum tightness 15Pa, time of drying, 480min ± 5min got hydrogen-carbonate nickel presoma after the drying;
(10) hydrogen-carbonate nickel presoma roasting
Exsiccant hydrogen-carbonate nickel presoma is placed quartz crucible, place stoving oven to carry out roasting then, 600 ℃ ± 2 ℃ of maturing temperatures, roasting time 120min ± 5min, under the reaction equation:
In the formula: NiO: nickel oxide;
Stop heating after the roasting, make it naturally cool to 20 ℃ ± 2 ℃ with stoving oven;
Open stoving oven, take out quartz crucible, promptly get: porous nickel oxide microballoon product;
(11) detect, chemically examine, analyze, characterize
Color and luster, composition, pattern, the physical and chemical performance of porous nickel oxide microballoon to preparation detects, chemically examines, analyzes, characterizes;
Carrying out crystalline phase with Rigaku/max-2500 type X-ray diffractometer identifies;
Carry out the product morphology analysis with JSM-6700F sem and JEOL JEM-100f high resolving power transmission electron microscope;
Carry out sreen analysis with the LA-300 Laser Scattering Particle Size Distribution Analyzer;
Carry out the specific surface area measuring and calculating with the full-automatic physics of ASAP2020, chemisorption appearance;
Conclusion: the nickel oxide microballoon is a black crystals, microsphere particle diameter≤10 μ m, and vesicular structure, the surface is made up of irregular hexagon nanometer sheet, hexagon diameter≤40nm, specific surface area is 748.25m
2/ g;
(12) product stores
The porous nickel oxide microballoon is placed brown transparent Glass Containers, and airtight lucifuge stores in dry, cool place, clean environment, waterproof, protection against the tide, sun-proof, acid-proof alkali salt erosion, 20 ℃ ± 2 ℃ of storing temps, relative humidity≤10%.
Beneficial effect
The present invention compares with background technology has tangible advance, is to be raw material with nickelous nitrate, urea, is tensio-active agent with the cetyl trimethylammonium bromide, is washing composition with absolute ethyl alcohol, deionized water; Through picking of raw material, the synthetic mixed solution of preparation, the reaction kettle internal heating is produced hydrogen-carbonate nickel, after bigger serface porous nickel oxide microballoon is processed in washing, suction filtration, vacuum-drying, high-temperature roasting; This preparing method's technology is advanced, and technical process is short, uses raw material few; Informative data is accurate, and production yield rate is high, reaches 95%; Product purity is good, reaches 98.5%, and the specific surface area of product nickel oxide microballoon is 748.25m
2/ g, microsphere particle diameter≤10 μ m, microsphere surface is distributed with irregular hexagon nanometer sheet, and hexagon nanometer sheet diameter≤40nm can mate with the number of chemical material, is the very good method for preparing bigger serface porous nickel oxide microballoon.
Description of drawings
Fig. 1 is the state graph of hydrogen-carbonate nickel building-up reactions
Fig. 2 is hydrogen-carbonate nickel maturing temperature and time coordinate graph of a relation
Fig. 3 is that nickel oxide microballoon ESEM amplifies 10000 times product shape appearance figure
Fig. 4 is that nickel oxide microballoon transmission electron microscope amplifies 200000 times of product shape appearance figures
Fig. 5 is a nickel oxide microballoon X-ray diffraction intensity collection of illustrative plates
Fig. 6 is a nickel oxide microspherulite diameter distribution plan
Fig. 7 is a nickel oxide microballoon adsorption isotherm line chart
Shown in the figure, list of numerals is following:
1. power switch, 2. temperature regulator, 3. stove seat, 4. image display, 5. reaction solution, 6. process furnace, 7. bell, 8. kettle cover, 9. container cover, 10. reaction kettle, 11. polytetrafluoroethylcontainer container, 12. worktable, 13. PL.
Embodiment
Below in conjunction with accompanying drawing the present invention is further specified:
Shown in Figure 1, be the state graph of hydrogen-carbonate nickel building-up reactions, it is correct that each location is wanted, according to quantity proportioning, operation according to the order of sequence.
The value of the chemical substance that preparation is used is to confirm by the scope that is provided with in advance, is measure unit with gram, milliliter, when industriallization is produced with kilogram, be upgraded to measure unit.
The building-up reactions of hydrogen-carbonate nickel is carried out in reaction kettle, in process furnace, under 150 ℃ ± 2 ℃ states of Heating temperature;
Process furnace is rectangular, and the bottom of process furnace 6 is a stove seat 3, and top is bell 7, on stove seat 3, is provided with image display 4, PL 13, power switch 1, temperature regulator 2; Being worktable 12 at process furnace 6 inner bottom parts, on worktable 12, putting reaction kettle 10 and kettle cover 8, be polytetrafluoroethylcontainer container 11 and container cover 9 reaction kettle 10 in, and polytetrafluoroethylcontainer container 11 is interior to be reaction solution 5, and reaction kettle 10 tops are sealed by kettle cover 8.
Shown in Figure 2, be hydrogen-carbonate nickel maturing temperature and time coordinate graph of a relation, the roasting of hydrogen-carbonate nickel is carried out in stoving oven, and maturing temperature begins to heat up by 20 ℃; Be the A point, rise to 600 ℃ ± 2 ℃ with 10 ℃/min speed, i.e. the B point; At this temperature constant temperature, insulation, roasting 120min, promptly the B-C section stops heat temperature raising then; Make it naturally cool to 20 ℃ ± 2 ℃ with stove, i.e. D point, the roasting heat-up rate was directly proportional with the time.
Shown in Figure 3, for nickel oxide microballoon ESEM amplifies 10000 times of product shape appearance figures, product is loose powder, spherical shape, and there is irregular hole on the ball surface, ball particle diameter≤10 μ m.
Shown in Figure 4, for nickel oxide microballoon transmission electron microscope amplifies 200000 times of shape appearance figures, can know among the figure: the nickel oxide microsphere surface is distributed with irregular hexagon nanometer sheet, hexagon nanometer sheet diameter≤40nm.
Shown in Figure 5; Be nickel oxide microballoon X-ray diffraction intensity collection of illustrative plates; Can know among the figure: the diffraction crystal face is (111), (200), (220), (311) and (222), and consistent with the NiO standard value, diffraction peak is more sharp-pointed; Explain that crystal property is good, from diffractogram, do not observe the existence at other crystal characteristic peaks.
Shown in Figure 6, be nickel oxide microspherulite diameter distribution plan, can know among the figure: synthetic nickel oxide microspherulite diameter homogeneous, concentrate to be distributed in the 10 μ m.
Shown in Figure 7, be the adsorption isotherm line chart of nickel oxide microballoon, calculated and can be known by figure: the specific surface area of synthetic nickel oxide microballoon is 748.25m
2/ g.
Claims (4)
1. the preparation method of a bigger serface porous nickel oxide microballoon; It is characterized in that: the chemical substance material of use is: nickelous nitrate, urea, cetyl trimethylammonium bromide, absolute ethyl alcohol, deionized water, it is following that consumption is prepared in its combination: with gram, milliliter is measure unit
Nickelous nitrate: Ni (NO
3)
26H
2O 14.55g ± 0.01g
Urea: CO (NH
2)
23g ± 0.01g
Cetyl trimethylammonium bromide: C
16H
33(CH
3)
3NBr 9.1g ± 0.01g
Absolute ethyl alcohol: C
2H
5OH 1000mL ± 50mL
Deionized water: H
2O 2000mL ± 50mL
The preparation method is following:
(1) selected chemical substance material
The chemical substance material that preparation is used will carry out selected, and carries out quality purity control:
Nickelous nitrate: solid-state solid >=99%
Urea: solid-state solid >=99%
Cetyl trimethylammonium bromide: solid-state solid >=99%
Absolute ethyl alcohol: liquid liquid 99.7%
Deionized water: liquid liquid 99.7%
(2) preparation nickel nitrate aqueous solution
Take by weighing nickelous nitrate 14.55g ± 0.01g, measure deionized water 200mL ± 0.01mL, add in the beaker, magnetic agitation 60min becomes: the nickel nitrate aqueous solution of 0.25mol/L;
(3) the preparation cetyl trimethylammonium bromide aqueous solution
Take by weighing cetyl trimethylammonium bromide 9.1g ± 0.01g, measure deionized water 200mL ± 0.01mL and add in the beaker, magnetic agitation 60min becomes: the cetyl trimethylammonium bromide aqueous solution of 0.125mol/L;
(4) preparation carbonate synthesis hydrogen nickel mixing solutions
Nickel nitrate aqueous solution 100mL, cetyl trimethylammonium bromide aqueous solution 100mL are added in the polytetrafluoroethylcontainer container;
Take by weighing urea 3g ± 0.01g, add in the polytetrafluoroethylcontainer container, and sealing;
Polytetrafluoroethylcontainer container is placed on the magnetic stirring apparatus, and magnetic agitation 60min becomes: transparence blue-greenish colour ternary mixing solutions;
(5) hydrogen-carbonate nickel building-up reactions
The building-up reactions of hydrogen-carbonate nickel is in stainless steel cauldron, in electrical heater, to carry out;
The polytetrafluoroethylcontainer container that fills the ternary mixing solutions is placed in the stainless steel cauldron, and seal with kettle cover;
Then reaction kettle is placed the electrical heater internal heating, 150 ℃ ± 2 ℃ of Heating temperatures, heat-up time 240min ± 5min;
Mixing solutions will carry out chemical reaction under heated condition in reaction kettle, reaction equation is following:
In the formula: Ni (HCO
3)
2: hydrogen-carbonate nickel, NH
4NO
3: an ammonium nitrate, H
2O: water vapour, Ni (NH
3)
6(NO
3)
2: nitric acid hexamine nickel (II), CO
2: carbonic acid gas;
After reaction finishes, for containing the sedimentary turbid solution of hydrogen-carbonate nickel, stop heating in the polytetrafluoroethylcontainer container, make it naturally cool to 20 ℃ ± 2 ℃;
After the cooling, open reaction kettle, take out and contain the sedimentary turbid solution of hydrogen-carbonate nickel;
(6) suction filtration
The sedimentary turbid solution of carbonated hydrogen nickel is placed the B on the filter flask, carry out suction filtration with millipore filtration, retain the product filter cake on the filter membrane, waste liquid is evacuated in the filter flask;
(7) deionized water wash, suction filtration
The product filter cake is placed beaker, add deionized water 100mL, agitator treating 5min; Then washings is placed the B on the filter flask, carry out suction filtration with millipore filtration, retain the product filter cake on the filter membrane, washings is evacuated in the filter flask; Deionized water wash, suction filtration repeat 5 times;
(8) absolute ethanol washing, suction filtration
The product filter cake is placed beaker, add absolute ethyl alcohol 100mL, agitator treating 5min; Then washings is placed the B on the filter flask, carry out suction filtration with millipore filtration, retain the product filter cake on the filter membrane, washings is evacuated in the filter flask; Absolute ethanol washing, suction filtration repeat 5 times;
(9) vacuum-drying
Product filter cake behind washing, the suction filtration is placed quartzy product boat, place vacuum drying oven to carry out drying then, 60 ℃ ± 2 ℃ of drying temperatures, vacuum tightness 15Pa, time of drying, 480min ± 5min got hydrogen-carbonate nickel presoma after the drying;
(10) hydrogen-carbonate nickel presoma roasting
Exsiccant hydrogen-carbonate nickel presoma is placed quartz crucible, place stoving oven to carry out roasting then, 600 ℃ ± 2 ℃ of maturing temperatures, roasting time 120min ± 5min, under the reaction equation:
In the formula: NiO: nickel oxide;
Stop heating after the roasting, make it naturally cool to 20 ℃ ± 2 ℃ with stoving oven;
Open stoving oven, take out quartz crucible, promptly get: porous nickel oxide microballoon product;
(11) detect, chemically examine, analyze, characterize
Color and luster, composition, pattern, the physical and chemical performance of porous nickel oxide microballoon to preparation detects, chemically examines, analyzes, characterizes;
Carrying out crystalline phase with Rigaku/max-2500 type x-ray powder diffraction instrument identifies;
Carry out the product morphology analysis with JSM-6700F sem and JEOL JEM-100f high resolving power transmission electron microscope;
Carry out sreen analysis with the LA-300 Laser Scattering Particle Size Distribution Analyzer;
Carry out the specific surface area measuring and calculating with the full-automatic physics of ASAP2020, chemisorption appearance;
Conclusion: the nickel oxide microballoon is a black crystals, microsphere particle diameter≤10 μ m, and vesicular structure, the surface is made up of irregular hexagon nanometer sheet, hexagon diameter≤40nm, specific surface area is 748.25m
2/ g;
(12) product stores
The porous nickel oxide microballoon is placed brown transparent Glass Containers, and airtight lucifuge stores in dry, cool place, clean environment, waterproof, protection against the tide, sun-proof, acid-proof alkali salt erosion, 20 ℃ ± 2 ℃ of storing temps, relative humidity≤10%.
2. the preparation method of a kind of bigger serface porous nickel oxide microballoon according to claim 1 is characterized in that: the building-up reactions of hydrogen-carbonate nickel is in reaction kettle, in process furnace, under 150 ℃ ± 2 ℃ states of Heating temperature, carries out; Process furnace is rectangular, and the bottom of process furnace (6) is stove seat (3), and upper part bell (7) is provided with image display (4), PL (13), power switch (1), temperature regulator (2) on stove seat (3); At process furnace (6) inner bottom part is worktable (12); Go up storing reaction kettle (10) and kettle cover (8) at worktable (12); In reaction kettle (10) polytetrafluoroethylcontainer container (11) and container cover (9), the built-in reaction solution (5) of putting of polytetrafluoroethylcontainer container (11), reaction kettle (10) top is sealed by kettle cover (8).
3. according to the preparation method who requires 1 described a kind of bigger serface porous nickel oxide microballoon of right, it is characterized in that: the roasting of hydrogen-carbonate nickel is carried out in stoving oven, and maturing temperature and time coordinate relation are: maturing temperature begins to heat up by 20 ℃; Be the A point, rise to 600 ℃ ± 2 ℃ with 10 ℃/min speed, i.e. the B point; At this temperature constant temperature, insulation, roasting 120min ± 5min; Be the B-C section, stop heat temperature raising then, make it cool to 20 ℃ ± 2 ℃ with the furnace; Be the D point, the roasting heat-up rate was directly proportional with the time.
4. according to the preparation method who requires 1 described a kind of bigger serface porous nickel oxide microballoon of right; It is characterized in that: the nickel oxide microballoon is loose powder, and particle is a spherical shape, and there is irregular hole on the ball surface; Be vesicular structure; The ball surface is made up of irregular hexagon nanometer sheet, hexagon diameter≤40nm, and specific surface area is 748.25m
2/ g.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103880093A (en) * | 2014-04-15 | 2014-06-25 | 山东大学 | Hollow spherical nickel bicarbonate aggregate |
| CN104030371A (en) * | 2014-06-08 | 2014-09-10 | 吕仁江 | Method for synthesizing NiO microsphere consisting of mesoporous sheet structures by soft template process |
| CN105481026A (en) * | 2015-12-17 | 2016-04-13 | 宁波繁盛商业管理有限公司 | Preparation method of nickel bicarbonate |
| JP2017030994A (en) * | 2015-07-29 | 2017-02-09 | 公立大学法人首都大学東京 | Inorganic monodisperse spherical fine particle, electrode for cell, and cell |
| CN106711419A (en) * | 2017-01-05 | 2017-05-24 | 山东理工大学 | Core-shell NiO/C porous composite lithium ion battery negative electrode material |
| CN106865628A (en) * | 2017-03-10 | 2017-06-20 | 长春理工大学 | One kind is used for room temperature H2S gas sensing materials nickel oxide and preparation method thereof |
| CN108144616A (en) * | 2018-01-18 | 2018-06-12 | 太原理工大学 | A kind of low-temperature catalyzed decomposition N2The preparation method of the porous NiO nano flakes catalyst of O |
| CN111653768A (en) * | 2020-05-25 | 2020-09-11 | 海南大学 | Preparation method of NiO/Ni porous microspheres |
| CN117843046A (en) * | 2024-01-04 | 2024-04-09 | 兰州兰石中科纳米科技有限公司 | Preparation method of high-purity nano nickel oxide |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103880093A (en) * | 2014-04-15 | 2014-06-25 | 山东大学 | Hollow spherical nickel bicarbonate aggregate |
| CN103880093B (en) * | 2014-04-15 | 2015-03-11 | 山东大学 | Hollow spherical nickel bicarbonate aggregate |
| CN104030371A (en) * | 2014-06-08 | 2014-09-10 | 吕仁江 | Method for synthesizing NiO microsphere consisting of mesoporous sheet structures by soft template process |
| CN104030371B (en) * | 2014-06-08 | 2016-01-13 | 吕仁江 | The method of the NiO microballoon of the synthesising mesoporous sheet structure composition of a kind of soft template method |
| JP2017030994A (en) * | 2015-07-29 | 2017-02-09 | 公立大学法人首都大学東京 | Inorganic monodisperse spherical fine particle, electrode for cell, and cell |
| CN105481026A (en) * | 2015-12-17 | 2016-04-13 | 宁波繁盛商业管理有限公司 | Preparation method of nickel bicarbonate |
| CN106711419A (en) * | 2017-01-05 | 2017-05-24 | 山东理工大学 | Core-shell NiO/C porous composite lithium ion battery negative electrode material |
| CN106711419B (en) * | 2017-01-05 | 2019-06-07 | 山东理工大学 | The porous composite lithium ion battery cathode material of the NiO/C of core-shell structure copolymer shape |
| CN106865628A (en) * | 2017-03-10 | 2017-06-20 | 长春理工大学 | One kind is used for room temperature H2S gas sensing materials nickel oxide and preparation method thereof |
| CN108144616A (en) * | 2018-01-18 | 2018-06-12 | 太原理工大学 | A kind of low-temperature catalyzed decomposition N2The preparation method of the porous NiO nano flakes catalyst of O |
| CN108144616B (en) * | 2018-01-18 | 2020-11-06 | 太原理工大学 | Low-temperature catalytic decomposition of N2Preparation method of porous NiO nano flake catalyst of O |
| CN111653768A (en) * | 2020-05-25 | 2020-09-11 | 海南大学 | Preparation method of NiO/Ni porous microspheres |
| CN111653768B (en) * | 2020-05-25 | 2023-03-24 | 海南大学 | Preparation method of NiO/Ni porous microspheres |
| CN117843046A (en) * | 2024-01-04 | 2024-04-09 | 兰州兰石中科纳米科技有限公司 | Preparation method of high-purity nano nickel oxide |
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