CN102757101B - Method for preparing large-specific-surface-area porous nickel oxide microspheres - Google Patents
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- CN102757101B CN102757101B CN201210048608.2A CN201210048608A CN102757101B CN 102757101 B CN102757101 B CN 102757101B CN 201210048608 A CN201210048608 A CN 201210048608A CN 102757101 B CN102757101 B CN 102757101B
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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, belong to the technical field of mineral compound preparation and application.
Background technology
Along with the development of Nanometer scale science and 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 having special construction and complex topography, often be applied in the optical electron device; The porous pattern is owing to having equally distributed micropore and hole, porosity is high, volume density is little, there is high specific surface area and unique physical surface properties, different porousness can change the physics and chemistry character of material, therefore bigger serface porous structure material function is good, can be in biotechnology, fine chemistry industry, environmental engineering, catalyzer and sensor field application.
Nano-nickel oxide is a kind of important functional materials, due to 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, therefore its synthetic method of nano-nickel oxide of different-shape structure also has various ways, such as: Yang etc. are by nickel acetate in water and glycerine mixed solvent, and hydrolysis has prepared the nano-nickel oxide of carnation shape; Kuang etc., under the effect of anion surfactant, have prepared the nickel oxide micron ball of laminate structure by hydrothermal method; Zhou etc. adopt the hydrazine hydrate legal system for the concave polyhedron nickel oxide nanoparticle of nanometer sheet composition; Banerjee etc. be take sodium lauryl sulphate as soft template, the urea NiO nanocrystals ordered porous as prepared by precipitation agent; Feng etc. take KIT-6 as prepared by template nickel oxide material bimodal distribution, order mesoporous; Although these methods have prepared the nickel oxide material of different structure, the specific surface area of NiO is little, and its application has been subject to great limitation; Also all there are some technique drawbacks, some processing parameter out of true, product purity is low, and some product structure features are not obvious, are difficult to and other chemical substance couplings, and some processing methodes are more 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 the situation for background technology, adopt sluggish precipitation, the preparation mixing solutions, hydro-thermal prepares hydrogen-carbonate nickel, washing after filtration,, vacuum-drying, high-temperature roasting, make 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, dehydrated alcohol, deionized water, it is as follows that consumption is prepared in its combination: take 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
Dehydrated alcohol: C
2h
5oH 1000mL ± 50mL
Deionized water: H
2o 2000mL ± 50mL
The preparation method is as follows:
(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%
Dehydrated alcohol: liquid liquid 99.7%
Deionized water: liquid liquid 99.7%
(2) preparation nickel nitrate aqueous solution
Take nickelous nitrate 14.55g ± 0.01g, measure deionized water 200mL ± 0.01mL, add in beaker, magnetic agitation 60min, become: the nickel nitrate aqueous solution of 0.25mol/L;
(3) the preparation cetyl trimethylammonium bromide aqueous solution
Take cetyl trimethylammonium bromide 9.1g ± 0.01g, measure deionized water 200mL ± 0.01mL and add in beaker, magnetic agitation 60min, become: 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 polytetrafluoroethylcontainer container;
Take urea 3g ± 0.01g, add in polytetrafluoroethylcontainer container, and sealing;
Polytetrafluoroethylcontainer container is placed on magnetic stirring apparatus, and magnetic agitation 60min, become: transparence blue-greenish colour ternary mixing solutions;
(5) hydrogen-carbonate nickel building-up reactions
The building-up reactions of hydrogen-carbonate nickel is to carry out in stainless steel cauldron, in electrical heater;
The polytetrafluoroethylcontainer container that fills the ternary mixing solutions is placed in stainless steel cauldron, and seals with kettle cover;
Then reactor is placed in electrical heater and heats, 150 ℃ ± 2 ℃ of Heating temperatures, heat-up time 240min ± 5min;
Mixing solutions, in reactor, will carry out chemical reaction under heated condition, and reaction equation is as follows:
In formula: Ni (HCO
3)
2: hydrogen-carbonate nickel, NH
4nO
3: 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, in polytetrafluoroethylcontainer container, for containing the sedimentary turbid solution of hydrogen-carbonate nickel, stop heating, make it naturally cool to 20 ℃ ± 2 ℃;
After cooling, open reactor, take out and contain the sedimentary turbid solution of hydrogen-carbonate nickel;
(6) suction filtration
To be placed in the Büchner funnel on filter flask containing the sedimentary turbid solution of hydrogen-carbonate nickel, and with millipore filtration, carry out suction filtration, and retain the product filter cake on filter membrane, waste liquid is evacuated in filter flask;
(7) deionized water wash, suction filtration
The product filter cake is placed in to beaker, adds deionized water 100mL, agitator treating 5min; Then washings is placed in to the Büchner funnel on filter flask, with millipore filtration, carries out suction filtration, retain the product filter cake on filter membrane, washings is evacuated in filter flask; Deionized water wash, suction filtration repeat 5 times;
(8) absolute ethanol washing, suction filtration
The product filter cake is placed in to beaker, adds dehydrated alcohol 100mL, agitator treating 5min; Then washings is placed in to the Büchner funnel on filter flask, with millipore filtration, carries out suction filtration, retain the product filter cake on filter membrane, washings is evacuated in filter flask; Absolute ethanol washing, suction filtration repeat 5 times;
(9) vacuum-drying
Product filter cake after washing, suction filtration is placed in to quartzy product boat, then is placed in vacuum drying oven and carries out drying, 60 ℃ ± 2 ℃ of drying temperatures, vacuum tightness 15Pa, time of drying, 480min ± 5min, obtained hydrogen-carbonate nickel presoma after drying;
(10) hydrogen-carbonate nickel presoma roasting
Dry hydrogen-carbonate nickel presoma is placed in to quartz crucible, then is placed in stoving oven and carries out roasting, 600 ℃ ± 2 ℃ of maturing temperatures, roasting time 120min ± 5min, under reaction equation:
In formula: NiO: nickel oxide;
Stop heating after roasting, make it with stoving oven, naturally cool to 20 ℃ ± 2 ℃;
Open stoving oven, take out quartz crucible, obtain: 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 detected, chemically examined, analyzed, characterized;
Carry out the crystalline phase evaluation with Rigaku/max-2500 type X-ray diffractometer;
Carry out the product morphology analysis with JSM-6700F scanning electronic microscope 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 ASAP2020 Full-automatic physical, chemical adsorption instrument;
Conclusion: the nickel oxide microballoon is black crystals, microsphere particle diameter≤10 μ m, and vesicular structure, surface consists of irregular hexagonal nanosheet, hexagon diameter≤40nm, specific surface area is 748.25m
2/ g;
(12) product stores
The porous nickel oxide microballoon is placed in to brown transparent Glass Containers, and in dry, cool place, clean environment, airtight lucifuge stores, and waterproof, protection against the tide, sun-proof, anti-acid-alkali salt to corrode, 20 ℃ ± 2 ℃ of storing temps, relative humidity≤10%.
Beneficial effect
The present invention compares with background technology has obvious advance, with nickelous nitrate, urea is raw material, take cetyl trimethylammonium bromide as tensio-active agent, with dehydrated alcohol, deionized water is washing composition, through picking of raw material, the synthetic mixed solution of preparation, in reactor, hydrogen-carbonate nickel is produced in heating, by washing, suction filtration, vacuum-drying, high-temperature roasting, make bigger serface porous nickel oxide microballoon, this preparation method's technique advanced person, technical process is short, the use raw material is few, informative data is accurate, production yield rate is high, reach 95%, product purity is good, reach 98.5%, 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 hexagonal nanosheet, and hexagonal nanosheet diameter≤40nm can mate with the number of chemical material, is the very good method for preparing bigger serface porous nickel oxide microballoon.
The accompanying drawing explanation
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 scanning electron microscope is amplified the product shape appearance figure of 10000 times
Fig. 4 is that nickel oxide microballoon transmission electron microscope amplifies 200000 times of product shape appearance figures
Fig. 5 is nickel oxide microballoon X-ray diffraction intensity collection of illustrative plates
Fig. 6 is nickel oxide microspherulite diameter distribution plan
Fig. 7 is nickel oxide microballoon adsorption isotherm line chart
Shown in figure, list of numerals is as follows:
1. power switch, 2. temperature regulator, 3. stove seat, 4. display screen, 5. reaction solution, 6. process furnace, 7. bell, 8. kettle cover, 9. container cover, 10. reactor, 11. polytetrafluoroethylcontainer container, 12. worktable, 13. pilot lamp.
Embodiment
Below in conjunction with accompanying drawing, the present invention will be further described:
Shown in Fig. 1, be the state graph of hydrogen-carbonate nickel building-up reactions, it is correct that want each position, according to quantity proportioning, operation according to the order of sequence.
The value of the chemical substance that preparation is used is to determine by the scope set in advance, and take gram, milliliter is measure unit, when industrialization is produced with kilogram, be upgraded to measure unit.
The building-up reactions of hydrogen-carbonate nickel is carried out in reactor, in process furnace, under 150 ℃ ± 2 ℃ states of Heating temperature;
Process furnace is rectangular, and the bottom of process furnace 6 is stove seat 3, and top is bell 7, is provided with display screen 4, pilot lamp 13, power switch 1, temperature regulator 2 on stove seat 3; Be worktable 12 at process furnace 6 inner bottom parts, put reactor 10 and kettle cover 8 on worktable 12, be polytetrafluoroethylcontainer container 11 and container cover 9 in reactor 10, in polytetrafluoroethylcontainer container 11, is reaction solution 5, and reactor 10 tops are by kettle cover 8 sealings.
Shown in Fig. 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, maturing temperature starts 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, be the B-C section, then stop heat temperature raising, make it with stove, naturally cool to 20 ℃ ± 2 ℃, be the D point, the roasting heat-up rate was directly proportional to the time.
Shown in Fig. 3, for nickel oxide microballoon scanning electron microscope is amplified 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 Fig. 4, for nickel oxide microballoon transmission electron microscope amplifies 200000 times of shape appearance figures, known in figure: the nickel oxide microsphere surface is distributed with irregular hexagonal nanosheet, hexagonal nanosheet diameter≤40nm.
Shown in Fig. 5, for nickel oxide microballoon X-ray diffraction intensity collection of illustrative plates, known in figure: the diffraction crystal face is (111), (200), (220), (311) and (222), consistent with the NiO standard value, diffraction peak is more sharp-pointed, illustrate that crystal property is good, do not observe other crystal characteristic peaks from diffractogram.
Shown in Fig. 6, be nickel oxide microspherulite diameter distribution plan, known in figure: synthetic nickel oxide microspherulite diameter homogeneous, concentrate and be distributed in 10 μ m.
Shown in Fig. 7, be the adsorption isotherm line chart of nickel oxide microballoon, from figure, calculated: 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, dehydrated alcohol, deionized water, it is as follows that consumption is prepared in its combination: take 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
Dehydrated alcohol: C
2h
5oH 1000mL ± 50mL
Deionized water: H
2o 2000mL ± 50mL
The preparation method is as follows:
(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%
Dehydrated alcohol: liquid liquid 99.7%
Deionized water: liquid liquid 99.7%
(2) preparation nickel nitrate aqueous solution
Take nickelous nitrate 14.55g ± 0.01g, measure deionized water 200mL ± 0.01mL, add in beaker, magnetic agitation 60min, become: the nickel nitrate aqueous solution of 0.25mol/L;
(3) the preparation cetyl trimethylammonium bromide aqueous solution
Take cetyl trimethylammonium bromide 9.1g ± 0.01g, measure deionized water 200mL ± 0.01mL and add in beaker, magnetic agitation 60min, become: 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 polytetrafluoroethylcontainer container;
Take urea 3g ± 0.01g, add in polytetrafluoroethylcontainer container, and sealing;
Polytetrafluoroethylcontainer container is placed on magnetic stirring apparatus, and magnetic agitation 60min, become: transparence blue-greenish colour ternary mixing solutions;
(5) hydrogen-carbonate nickel building-up reactions
The building-up reactions of hydrogen-carbonate nickel is to carry out in stainless steel cauldron, in electrical heater;
The polytetrafluoroethylcontainer container that fills the ternary mixing solutions is placed in stainless steel cauldron, and seals with kettle cover;
Then reactor is placed in electrical heater and heats, 150 ℃ ± 2 ℃ of Heating temperatures, heat-up time 240min ± 5min;
Mixing solutions, in reactor, will carry out chemical reaction under heated condition, and reaction equation is as follows:
In formula: Ni (HCO
3)
2: hydrogen-carbonate nickel, NH
4nO
3: 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, in polytetrafluoroethylcontainer container, for containing the sedimentary turbid solution of hydrogen-carbonate nickel, stop heating, make it naturally cool to 20 ℃ ± 2 ℃;
After cooling, open reactor, take out and contain the sedimentary turbid solution of hydrogen-carbonate nickel;
(6) suction filtration
To be placed in the Büchner funnel on filter flask containing the sedimentary turbid solution of hydrogen-carbonate nickel, and with millipore filtration, carry out suction filtration, and retain the product filter cake on filter membrane, waste liquid is evacuated in filter flask;
(7) deionized water wash, suction filtration
The product filter cake is placed in to beaker, adds deionized water 100mL, agitator treating 5min; Then washings is placed in to the Büchner funnel on filter flask, with millipore filtration, carries out suction filtration, retain the product filter cake on filter membrane, washings is evacuated in filter flask; Deionized water wash, suction filtration repeat 5 times;
(8) absolute ethanol washing, suction filtration
The product filter cake is placed in to beaker, adds dehydrated alcohol 100mL, agitator treating 5min; Then washings is placed in to the Büchner funnel on filter flask, with millipore filtration, carries out suction filtration, retain the product filter cake on filter membrane, washings is evacuated in filter flask; Absolute ethanol washing, suction filtration repeat 5 times;
(9) vacuum-drying
Product filter cake after washing, suction filtration is placed in to quartzy product boat, then is placed in vacuum drying oven and carries out drying, 60 ℃ ± 2 ℃ of drying temperatures, vacuum tightness 15Pa, time of drying, 480min ± 5min, obtained hydrogen-carbonate nickel presoma after drying;
(10) hydrogen-carbonate nickel presoma roasting
Dry hydrogen-carbonate nickel presoma is placed in to quartz crucible, then is placed in stoving oven and carries out roasting, 600 ℃ ± 2 ℃ of maturing temperatures, roasting time 120min ± 5min, under reaction equation:
In formula: NiO: nickel oxide;
Stop heating after roasting, make it with stoving oven, naturally cool to 20 ℃ ± 2 ℃;
Open stoving oven, take out quartz crucible, obtain: 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 detected, chemically examined, analyzed, characterized;
Carry out the crystalline phase evaluation with Rigaku/max-2500 type x-ray powder diffraction instrument;
Carry out the product morphology analysis with JSM-6700F scanning electronic microscope 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 ASAP2020 Full-automatic physical, chemical adsorption instrument;
Conclusion: the nickel oxide microballoon is black crystals, microsphere particle diameter≤10 μ m, and vesicular structure, surface consists of irregular hexagonal nanosheet, hexagon diameter≤40nm, specific surface area is 748.25m
2/ g;
(12) product stores
The porous nickel oxide microballoon is placed in to brown transparent Glass Containers, and in dry, cool place, clean environment, airtight lucifuge stores, and waterproof, protection against the tide, sun-proof, anti-acid-alkali salt to corrode, 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, it is characterized in that: the building-up reactions of hydrogen-carbonate nickel is in reactor, 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 display screen (4), pilot lamp (13), power switch (1), temperature regulator (2) on stove seat (3); At process furnace (6) inner bottom part, be worktable (12), at upper reactor (10) and the kettle cover (8) put of worktable (12), in reactor (10), be polytetrafluoroethylcontainer container (11) and container cover (9), the built-in reaction solution (5) of putting of polytetrafluoroethylcontainer container (11), reactor (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, maturing temperature and time coordinate close: maturing temperature starts to heat up by 20 ℃, it is the A point, rise to 600 ℃ ± 2 ℃ with 10 ℃/min speed, it is the B point, at this temperature constant temperature, insulation, roasting 120min ± 5min, it is the B-C section, then stop heat temperature raising, make it cool to 20 ℃ ± 2 ℃ with the furnace, i.e. D point, the roasting heat-up rate was directly proportional to 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, particle is spherical shape, there is irregular hole on the ball surface, for vesicular structure, the ball surface consists of irregular hexagonal nanosheet, hexagon diameter≤40nm, and specific surface area is 748.25m
2/ g.
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| CN103880093B (en) * | 2014-04-15 | 2015-03-11 | 山东大学 | Hollow spherical nickel bicarbonate aggregate |
| 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 |
| JP6749574B2 (en) * | 2015-07-29 | 2020-09-02 | 東京都公立大学法人 | Inorganic monodisperse spherical fine particles, method for producing inorganic monodisperse spherical fine particles, battery electrode and battery |
| 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 |
| 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 |
| 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 |
| 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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| CN101857279A (en) * | 2010-06-29 | 2010-10-13 | 上海大学 | Method for preparing nano-nickel oxide power for surface alloying of carbon steel |
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