CN115465902A - Reaction solvent for preparing superfine nickel oxide nanoparticles and method for preparing superfine nickel oxide by using reaction solvent - Google Patents
Reaction solvent for preparing superfine nickel oxide nanoparticles and method for preparing superfine nickel oxide by using reaction solvent Download PDFInfo
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- CN115465902A CN115465902A CN202211199174.6A CN202211199174A CN115465902A CN 115465902 A CN115465902 A CN 115465902A CN 202211199174 A CN202211199174 A CN 202211199174A CN 115465902 A CN115465902 A CN 115465902A
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- nickel oxide
- nickel
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- 229910000480 nickel oxide Inorganic materials 0.000 title claims abstract description 146
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 title claims abstract description 106
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 23
- 239000007810 chemical reaction solvent Substances 0.000 title claims abstract description 18
- 239000002245 particle Substances 0.000 claims abstract description 47
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 40
- 150000002815 nickel Chemical class 0.000 claims description 34
- 239000000243 solution Substances 0.000 claims description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 28
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 239000011259 mixed solution Substances 0.000 claims description 21
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 18
- 239000002608 ionic liquid Substances 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 11
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 9
- -1 1-aminoethyl-2-ethylpyridinium bromide Chemical compound 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 7
- 239000007864 aqueous solution Substances 0.000 claims description 5
- KARARXAWCRQROT-UHFFFAOYSA-M CC(N)[N+]1=CC=CC=C1.[Br-] Chemical compound CC(N)[N+]1=CC=CC=C1.[Br-] KARARXAWCRQROT-UHFFFAOYSA-M 0.000 claims description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 3
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 2
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 2
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 2
- 239000001099 ammonium carbonate Substances 0.000 claims description 2
- 239000004202 carbamide Substances 0.000 claims description 2
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000012716 precipitator Substances 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000002086 nanomaterial Substances 0.000 abstract description 3
- 230000001105 regulatory effect Effects 0.000 abstract description 3
- 239000002904 solvent Substances 0.000 abstract description 3
- 230000008859 change Effects 0.000 abstract description 2
- 239000006185 dispersion Substances 0.000 description 39
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 26
- 238000009826 distribution Methods 0.000 description 19
- 230000000052 comparative effect Effects 0.000 description 16
- 239000008367 deionised water Substances 0.000 description 13
- 229910021641 deionized water Inorganic materials 0.000 description 13
- 239000007788 liquid Substances 0.000 description 13
- 238000002360 preparation method Methods 0.000 description 13
- 238000010586 diagram Methods 0.000 description 12
- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 description 12
- 239000000725 suspension Substances 0.000 description 12
- 238000001556 precipitation Methods 0.000 description 10
- 230000000694 effects Effects 0.000 description 9
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 9
- 239000007787 solid Substances 0.000 description 7
- 238000003756 stirring Methods 0.000 description 7
- 230000002776 aggregation Effects 0.000 description 6
- 238000004528 spin coating Methods 0.000 description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 4
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 description 4
- 235000019441 ethanol Nutrition 0.000 description 4
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 3
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 3
- MCEWYIDBDVPMES-UHFFFAOYSA-N [60]pcbm Chemical compound C123C(C4=C5C6=C7C8=C9C%10=C%11C%12=C%13C%14=C%15C%16=C%17C%18=C(C=%19C=%20C%18=C%18C%16=C%13C%13=C%11C9=C9C7=C(C=%20C9=C%13%18)C(C7=%19)=C96)C6=C%11C%17=C%15C%13=C%15C%14=C%12C%12=C%10C%10=C85)=C9C7=C6C2=C%11C%13=C2C%15=C%12C%10=C4C23C1(CCCC(=O)OC)C1=CC=CC=C1 MCEWYIDBDVPMES-UHFFFAOYSA-N 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 3
- 238000004220 aggregation Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical group Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000000137 annealing Methods 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- BAONHUZQTANSBI-UHFFFAOYSA-N formic acid;methanamine Chemical compound [NH3+]C.[O-]C=O BAONHUZQTANSBI-UHFFFAOYSA-N 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000005525 hole transport Effects 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- GJAAJNMURIECJS-UHFFFAOYSA-N CC(C1=NC=CC=C1)N.Br Chemical compound CC(C1=NC=CC=C1)N.Br GJAAJNMURIECJS-UHFFFAOYSA-N 0.000 description 1
- 229910021585 Nickel(II) bromide Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000011899 heat drying method Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 1
- IPLJNQFXJUCRNH-UHFFFAOYSA-L nickel(2+);dibromide Chemical compound [Ni+2].[Br-].[Br-] IPLJNQFXJUCRNH-UHFFFAOYSA-L 0.000 description 1
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 1
- BFSQJYRFLQUZKX-UHFFFAOYSA-L nickel(ii) iodide Chemical compound I[Ni]I BFSQJYRFLQUZKX-UHFFFAOYSA-L 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000013618 particulate matter Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000000284 resting effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000004729 solvothermal method Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000002207 thermal evaporation Methods 0.000 description 1
- 230000005641 tunneling Effects 0.000 description 1
- 239000011882 ultra-fine particle Substances 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/04—Oxides; Hydroxides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The invention relates to the technical field of nano materials, and particularly discloses a reaction solvent for preparing superfine nickel oxide nano particles and a method for preparing superfine nickel oxide by using the reaction solvent. The reaction solvent for preparing the superfine nickel oxide can change the viscosity and the surface energy of the reaction solvent, so that the morphology and the particle size of the prepared nickel oxide nanoparticles are effectively regulated, the particle size of the prepared nickel oxide nanoparticles is concentrated to 5-15 nm, the dispersibility of the nickel oxide nanoparticles in various solvents is improved, the nickel oxide nanoparticles can be rapidly and uniformly dispersed in subsequent application, the application field of the nickel oxide nanoparticles is favorably expanded, and the application prospect is high.
Description
Technical Field
The invention relates to the technical field of nano materials, in particular to a reaction solvent for preparing superfine nickel oxide nano particles and a method for preparing superfine nickel oxide by using the reaction solvent.
Background
The nano material is a material which is prepared by regulating and controlling a substance structure in a nano scale (0.1-100 nm) and has specific performance, and has a surface effect, a small-size effect and a macroscopic quantum tunneling effect. When a macroscopic object is subdivided into ultrafine particles (nanoscale), it will exhibit many unusual characteristics, i.e., its optical, thermal, electrical, magnetic, mechanical and chemical properties will appear significantly different when compared to large particulate matter.
Nickel oxide (NiO) is a green to dark green solid powdery substance, and is widely used in the fields of catalysis, ceramics, sensors, batteries, and the like. It is worth noting that nickel oxide is a typical P-type semiconductor material, and the forbidden band width of nickel oxide is 3.6-4.0eV, and the application of nickel oxide in the photovoltaic field is more and more extensive due to the characteristic.
The preparation method of nickel oxide is divided into a liquid phase method and a solid phase method, wherein the solid phase method has the defects of high energy consumption, low efficiency, large particle size and the like. The liquid phase method can be further classified into a sol-gel method, a precipitation method, a solvothermal method, and the like. The conventional precipitation method is simple in preparation process and is a method for preparing nickel oxide which is widely applied at present, however, a heating and drying step is generally required in the precipitation process, nanoparticles are close to each other under the action of interfacial tension, the particles are compact due to the existence of surface hydroxyl groups and the formation of crystal bridges due to dissolution-precipitation, and the crystal bridges are combined with each other to form a larger block-shaped aggregate with the extension of drying time. Therefore, the nickel oxide particles prepared by the conventional precipitation method generally have larger particle size, are easy to agglomerate and are not beneficial to dispersion in a medium during application. Therefore, the development of a novel preparation method of the superfine nickel oxide has very important significance for expanding the application range of the nickel oxide.
Disclosure of Invention
Aiming at the problems that the nickel oxide prepared by a precipitation method in the prior art has larger grain diameter, is easy to agglomerate and is not beneficial to be dispersed in a medium, the invention provides a preparation method of ultrafine nickel oxide nano-particles. The method prepares the nickel oxide in the ethanol and pyridine ionic liquid by a precipitation method to obtain the ultrafine nano nickel oxide particles, has concentrated particle size distribution and has very important significance for expanding the application field of the nickel oxide.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a reaction solvent for preparing superfine nickel oxide comprises an ethanol aqueous solution and pyridine type ionic liquid.
Compared with the prior art, the reaction solvent for preparing the superfine nickel oxide provided by the invention can change the viscosity and the surface energy of the reaction solvent, so that the appearance and the particle size of the prepared nickel oxide nanoparticles are effectively regulated, the particle size of the prepared nickel oxide nanoparticles is concentrated to 5nm-15nm, the dispersibility of the nickel oxide nanoparticles in various solvents is improved, the nickel oxide nanoparticles can be rapidly and uniformly dispersed in subsequent applications, the application field of the nickel oxide nanoparticles is favorably expanded, and the application prospect is high.
Preferably, the pyridine type ionic liquid is at least one of 1-aminoethyl-pyridine bromide salt, 1-aminoethyl-2-ethylpyridine bromide salt or 1-aminoethyl-3-ethylpyridine bromide salt.
The ethanol aqueous solution in the reaction solvent can reduce the agglomeration problem of nickel oxide particles during drying, and meanwhile, the preferred pyridine ionic liquid can be anchored on the surfaces of the nickel oxide particles to reduce the hydroxyl content of the surfaces of the nickel oxide particles, so that the agglomeration problem of the nickel oxide particles caused by dehydration condensation of hydroxyl groups is effectively reduced, and the preferred pyridine ionic liquid covers the surfaces of the nickel oxide particles to increase the steric hindrance among the nickel oxide particles, thereby further effectively preventing the agglomeration of the nickel oxide particles.
The invention also provides a method for preparing superfine nickel oxide nano-particles by using the reaction solvent, which comprises the following steps:
step a, dissolving soluble nickel salt in an ethanol water solution to obtain a nickel salt mixed solution;
b, adding pyridine type ionic liquid into the nickel salt mixed solution, and uniformly mixing to obtain a nickel salt reaction solution;
and c, adding a precipitator into the nickel salt reaction solution, reacting, centrifuging, washing, drying and roasting to obtain the superfine nickel oxide nano particles.
Preferably, in step a, the volume percentage of the absolute ethyl alcohol in the ethanol aqueous solution is 25-50%.
Preferably, in the step a, the concentration of the nickel salt in the nickel salt mixed solution is 0.5mol/L-1.5mol/L.
In step a, the soluble nickel salt is nickel chloride, nickel nitrate, nickel sulfate, nickel iodide or nickel bromide.
Preferably, in the step b, the addition amount of the pyridine-type ionic liquid is 0.01-0.06% of the mass of the soluble nickel salt.
Preferably, in step c, the precipitant is at least one of ammonia water, urea solution, sodium hydroxide solution, potassium hydroxide solution or ammonium bicarbonate solution.
Preferably, in step c, the molar ratio of the precipitant to the soluble nickel salt is 1.
Preferably, in the step c, the roasting temperature is 270-300 ℃, and the roasting time is 2-5 h.
In step c, the drying is performed by a heat drying method or a vacuum drying method.
The invention also provides superfine nickel oxide nanoparticles prepared by any one of the methods for preparing the superfine nickel oxide nanoparticles.
Preferably, the particle size of the nano nickel oxide particles is 5nm-15nm.
The preparation method of the superfine nano nickel oxide provided by the invention effectively reduces the particle size of the prepared nickel oxide and improves the dispersibility of the nickel oxide in various solvents, so that the nickel oxide can be better applied to various fields, and the preparation method is simple, has easily available raw materials, is suitable for industrial production and application, is beneficial to expanding the application range of the nano nickel oxide particles, and has higher popularization and application values.
Drawings
FIG. 1 is an XRD pattern of nickel oxide nanoparticles prepared in example 1 of the present invention;
FIG. 2 is a FT-IR diagram of nickel oxide nanoparticles prepared in example 1 of the present invention;
FIG. 3 is a comparison graph of the nickel oxide nanodispersion in example 1 of the present invention after standing for 24h, wherein the left graph is 0h and the right graph is 24h;
FIG. 4 is a distribution diagram of the particle size of nano nickel oxide in the nano nickel oxide dispersion liquid in example 1 of the present invention;
FIG. 5 is a comparison graph of the nickel oxide nanodispersion in example 2 of the present invention after standing for 24h, wherein the left graph is 0h and the right graph is 24h;
FIG. 6 is a distribution diagram of the particle size of nano nickel oxide in the nano nickel oxide dispersion liquid in example 2 of the present invention;
FIG. 7 is a comparative diagram of the nickel oxide nano-dispersion liquid in example 3 of the present invention after standing for 24h, wherein the left diagram is 0h, and the right diagram is 24h;
FIG. 8 is a distribution diagram of the particle size of nano nickel oxide in the nano nickel oxide dispersion liquid in example 3 of the present invention;
FIG. 9 is a comparative graph of a nickel oxide nanodispersion of the present invention in comparative example 1, which was left for 0h and right for 24h;
FIG. 10 is a graph showing a distribution of particle sizes of nano nickel oxide in a nano nickel oxide dispersion in comparative example 1 according to the present invention;
FIG. 11 is a comparative graph of nickel oxide nano-dispersion liquid of comparative example 2 of the present invention, which was left for 0h and right for 24h, left after standing;
FIG. 12 is a graph showing a distribution of particle sizes of nano nickel oxide in a nano nickel oxide dispersion liquid in comparative example 2 of the present invention;
FIG. 13 is a comparative graph of a nickel oxide nanodispersion of the present invention resting for 24 hours in comparative example 3, wherein the left graph is 0 hours and the right graph is 24 hours;
FIG. 14 is a graph showing the distribution of the particle size of nano nickel oxide in the nano nickel oxide dispersion in comparative example 3 according to the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In order to better illustrate the invention, the following examples are given by way of further illustration.
Example 1
The embodiment of the invention provides a preparation method of superfine nano nickel oxide, which comprises the following steps:
dissolving nickel nitrate in a mixed solution of absolute ethyl alcohol and deionized water in a volume ratio of 1;
step two, adding 1-aminoethyl-pyridinium bromide into 50mL of the nickel salt mixed solution, wherein the adding amount of the 1-aminoethyl-pyridinium bromide is 0.03wt% of the nickel nitrate to obtain a nickel salt reaction solution;
step three, adding 7.5mL of 10mol/L sodium hydroxide solution into the nickel salt reaction solution quickly, and stirring at the room temperature at the rotating speed of 800rpm for 30min to obtain a nickel hydroxide suspension;
and step four, centrifuging the nickel hydroxide suspension for 5min under the condition of 6800r/min, washing the obtained solid for 3 times by using a mixed solution of absolute ethyl alcohol and deionized water with the volume ratio of 1.
The XRD pattern of the nano nickel oxide nanoparticles of this example is shown in fig. 1, from which it can be seen that the three diffraction angles of the nickel oxide nanoparticles prepared in this example were 37.24 °, 43.27 ° and 62.87 ° in accordance with standard card #47-1049, indicating that the product is free of impurity phases. The three diffraction peaks correspond to three crystal faces (111), (200) and (220), and the prepared nickel oxide is proved to be in a cubic phase structure.
FIG. 2 is a FT-IR chart of the nickel oxide nanoparticles prepared in this example, from which it can be seen that-NH is present in the spectrum 2 And C = N, indicating that the pyridine-type ionic liquid was successfully adsorbed on the nickel oxide surface.
Fig. 3 is a graph of the effect of the prepared nickel oxide dispersion liquid (2 mg of nickel oxide nanoparticles dispersed in 10mL of water) after standing for 24 hours, and it can be seen from the graph that the nano nickel oxide dispersion liquid still has no aggregation and precipitation phenomenon after standing for 24 hours, which illustrates that the nano nickel oxide prepared in this example has good dispersion stability.
Fig. 4 is a distribution diagram of the particle size of nano nickel oxide in a nickel oxide dispersion (2 mg of nickel oxide nanoparticles dispersed in 10mL of water), and it can be seen that the particle size distribution of the nano nickel oxide dispersion prepared in this example is more concentrated, mainly around 10 nm.
Example 2
The embodiment of the invention provides a preparation method of superfine nano nickel oxide, which comprises the following steps:
step one, dissolving nickel nitrate into a mixed solution of absolute ethyl alcohol and deionized water with a volume ratio of 1;
step two, adding 1-aminoethyl-2-ethylpyridine bromide salt into 50mL of the nickel salt mixed solution, wherein the adding amount of the 1-aminoethyl-2-ethylpyridine bromide salt is 0.06wt% of nickel nitrate, so as to obtain a nickel salt reaction solution;
step three, quickly adding 3mL of 10mol/L sodium hydroxide solution into the nickel salt reaction solution, and stirring at the room temperature at the rotating speed of 800rpm for 30min to obtain a nickel hydroxide suspension;
and step four, centrifuging the nickel hydroxide suspension for 5min under the condition of 6800r/min, washing the obtained solid for 3 times by using a mixed solution of absolute ethyl alcohol and deionized water with the volume ratio of 1.
Fig. 5 is a graph showing the effect of the prepared nickel oxide dispersion liquid (2 mg of nickel oxide nanoparticles dispersed in 10mL of water) after standing for 24 hours, and it can be seen from the graph that the nano nickel oxide dispersion liquid still has no aggregation and precipitation phenomenon after standing for 24 hours, which illustrates that the nano nickel oxide prepared in this example has good dispersion stability.
Fig. 6 is a distribution diagram of the particle size of the nano nickel oxide in the nickel oxide dispersion (2 mg of nickel oxide nanoparticles dispersed in 10mL of water), and it can be seen from the diagram that the particle size distribution of the nano nickel oxide dispersion prepared in this example is concentrated, mainly around 10 nm.
Example 3
The embodiment of the invention provides a preparation method of superfine nano nickel oxide, which comprises the following steps:
dissolving nickel chloride in a mixed solution of absolute ethyl alcohol and deionized water in a volume ratio of 1;
step two, adding 1-aminoethyl-3-ethylpyridine bromide into 50mL of the nickel salt mixed solution, wherein the adding amount of the 1-aminoethyl-3-ethylpyridine bromide is 0.01wt% of nickel chloride, so as to obtain a nickel salt reaction solution;
step three, quickly adding 10mL of 10mol/L potassium hydroxide solution into the nickel salt reaction solution, and stirring at the room temperature at the rotating speed of 800rpm for 30min to obtain a nickel hydroxide suspension;
and step four, centrifuging the nickel hydroxide suspension for 5min under the condition of 6800r/min, washing the obtained solid for 3 times by using a mixed solution of absolute ethyl alcohol and deionized water with the volume ratio of 1.
Fig. 7 is a graph showing the effect of the prepared nickel oxide dispersion liquid (2 mg of nickel oxide nanoparticles dispersed in 10mL of water) after standing for 24 hours, and it can be seen from the graph that the nano nickel oxide dispersion liquid still has no aggregation and precipitation phenomenon after standing for 24 hours, which illustrates that the nano nickel oxide prepared in this example has good dispersion stability.
Fig. 8 is a graph showing the distribution of the particle size of nano nickel oxide in a nickel oxide dispersion (2 mg of nickel oxide nanoparticles dispersed in 10mL of water), and it can be seen that the particle size distribution of the nano nickel oxide dispersion prepared in this example is concentrated, mainly around 10 nm.
Comparative example 1
The comparative example provides a preparation method of superfine nano nickel oxide, which comprises the following steps:
step one, dissolving nickel nitrate in deionized water to obtain 0.75mol/L nickel salt solution;
step two, adding 7.5mL of 10mol/L sodium hydroxide solution into the 50mL of nickel salt solution quickly, and stirring at the room temperature at the rotating speed of 800rpm for 30min to obtain a nickel hydroxide suspension;
and step three, centrifuging the nickel hydroxide suspension for 5min under the condition of 6800r/min, washing the obtained solid for 3 times by using deionized water, drying for 12h under the condition of 80 ℃, and then roasting for 2h at 270 ℃ to obtain black nickel oxide powder.
Fig. 9 is a graph showing the effect of the prepared nickel oxide dispersion (2 mg of nickel oxide nanoparticles dispersed in 10mL of water) after standing for 24 hours, and it can be seen that the nickel oxide dispersions after standing for 0 hour and 24 hours can not be kept stable.
Fig. 10 is a graph showing the distribution of the particle size of nano nickel oxide in a nickel oxide dispersion (2 mg of nickel oxide nanoparticles dispersed in 10mL of water), and it can be seen from the graph that the particle size distribution of the nickel oxide dispersion is concentrated, but the particle size is large, so that the settling rate of the particles is high.
Comparative example 2
The comparative example provides a preparation method of superfine nano nickel oxide, which comprises the following steps:
dissolving nickel nitrate in a mixed solution of absolute ethyl alcohol and deionized water in a volume ratio of 1;
step two, adding 7.5mL of 10mol/L sodium hydroxide solution into the 50mL of nickel salt mixed solution quickly, and stirring at the room temperature at the rotating speed of 800rpm for 30min to obtain a nickel hydroxide suspension;
and step three, centrifuging the nickel hydroxide suspension for 5min under the condition of 6800r/min, washing the obtained solid for 3 times by using a mixed solution of absolute ethyl alcohol and deionized water with the volume ratio of 1.
FIG. 11 is a graph showing the effect of the prepared nickel oxide dispersion (2 mg of nickel oxide nanoparticles dispersed in 10mL of water) after standing for 24 hours, and it can be seen that none of the nickel oxide dispersions after standing for 24 hours was stable.
Fig. 12 is a distribution diagram of the particle size of nano nickel oxide in a nickel oxide dispersion (2 mg of nickel oxide nanoparticles dispersed in 10mL of water), and it can be seen from the diagram that although the particle size distribution of the nickel oxide dispersion is concentrated, the particle size is large, so that the particle settling rate is fast.
Comparative example 3
The comparative example provides a preparation method of superfine nano nickel oxide, which comprises the following steps:
step one, dissolving nickel nitrate into a mixed solution of absolute ethyl alcohol and deionized water with a volume ratio of 1;
step two, adding methylamine formate ionic liquid into 50mL of the nickel salt mixed solution, wherein the addition amount of methylamine formate ionic liquid is 0.03wt% of nickel nitrate, so as to obtain nickel salt reaction liquid;
step three, adding 7.5mL of 10mol/L sodium hydroxide solution into the nickel salt reaction solution quickly, and stirring at the room temperature at the rotating speed of 800rpm for 30min to obtain a nickel hydroxide suspension;
and step four, centrifuging the nickel hydroxide suspension for 5min under the condition of 6800r/min, washing the obtained solid for 3 times by using a mixed solution of absolute ethyl alcohol and deionized water with the volume ratio of 1.
Fig. 13 is a graph showing the effect of the prepared nickel oxide dispersion (2 mg of nickel oxide nanoparticles dispersed in 10mL of water) after standing for 24 hours, and it can be seen that none of the nickel oxide dispersions after standing for 24 hours was stable.
Fig. 14 is a graph showing the distribution of the particle size of nano nickel oxide in a nickel oxide dispersion (2 mg of nickel oxide nanoparticles dispersed in 10mL of water), and it can be seen from the graph that the particle size distribution of the nickel oxide dispersion is concentrated, but the particle size is large, so that the settling rate of the particles is high.
Application example
The nano nickel oxide dispersion liquid prepared in the example 1 is applied to the preparation of the perovskite solar cell, and the steps are as follows:
an ITO glass substrate (2X 2 cm) 2 ) In thatAnd respectively ultrasonically cleaning deionized water, acetone and isopropanol for 30min, and then treating in an ultraviolet cleaning machine for 20min to obtain the pretreated ITO glass.
Dispersing the nickel oxide prepared in example 1 in water to obtain a nickel oxide dispersion of 20 mg/mL; and (3) spin-coating the nickel oxide dispersion on the surface of the pretreated ITO glass, wherein the spin-coating amount is 80 mu L, and annealing at 120 ℃ for 20min to obtain the hole transport layer.
509.4mg of PbI 2 、71.6mg PbBr 2 179.7mg of FAI,20.2mg of MABr, 1mL of a mixed solvent (DMF: DMSO = 4; and spin-coating the precursor solution onto the surface of the hole transport layer at 3000r/min for 35s, quickly dropwise adding 200 mu L chlorobenzene when spin-coating for 10s, and quickly transferring the sample onto a heating plate at 100 ℃ for annealing treatment for 30min to form the perovskite thin film.
Adding 20mg of PCBM into a reagent bottle, adding 1mL of chlorobenzene, and stirring at 60 ℃ for 2 hours to obtain a PCBM solution; and (3) taking 50 mu L of PCBM solution, spin-coating to the surface of the perovskite thin film at the speed of 2000r/min, and spin-coating for 30s to obtain the electron transport layer.
2.5mg of BCP is dissolved in 5mL of isopropanol, 80 mu L of the solution is taken to be spin-coated on the surface of the electron transport layer, and the solution is spin-coated for 30s at the speed of 4000r/min to obtain the BCP barrier layer.
And evaporating an Au electrode with the thickness of 80nm on the surface of the BCP barrier layer by using vacuum thermal evaporation equipment to obtain the perovskite solar cell.
The perovskite solar cell is subjected to an I-V test, and the highest efficiency is 17.5%.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents or improvements made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. A reaction solvent for preparing superfine nickel oxide is characterized by comprising an ethanol aqueous solution and pyridine ionic liquid.
2. The reaction solvent for preparing ultrafine nickel oxide according to claim 1, wherein the pyridine type ionic liquid is at least one of 1-aminoethyl-pyridinium bromide, 1-aminoethyl-2-ethylpyridinium bromide, or 1-aminoethyl-3-ethylpyridinium bromide.
3. A method for preparing ultrafine nickel oxide nanoparticles using the reaction solvent of any one of claims 1 or 2, comprising the steps of:
step a, dissolving soluble nickel salt in an ethanol water solution to obtain a nickel salt mixed solution;
b, adding pyridine type ionic liquid into the nickel salt mixed solution, and uniformly mixing to obtain a nickel salt reaction solution;
and c, adding a precipitator into the nickel salt reaction solution, reacting, centrifuging, washing, drying and roasting to obtain the superfine nickel oxide nano-particles.
4. The method for preparing ultrafine nickel oxide nanoparticles as claimed in claim 3, wherein in the step a, the absolute ethanol content of the ethanol aqueous solution is 25 to 50% by volume.
5. The method for preparing ultrafine nickel oxide nanoparticles as claimed in claim 3, wherein the concentration of the nickel salt in the nickel salt mixed solution in the step a is 0.5mol/L to 1.5mol/L.
6. The method for preparing ultrafine nickel oxide nanoparticles according to claim 3, wherein the pyridine-type ionic liquid is added in an amount of 0.01 to 0.06% by mass of the soluble nickel salt in step b.
7. The method for preparing ultrafine nickel oxide nanoparticles according to claim 3, wherein in step c, the precipitant is at least one of aqueous ammonia, urea solution, sodium hydroxide solution, potassium hydroxide solution, or ammonium bicarbonate solution.
8. The method for preparing ultrafine nickel oxide nanoparticles according to claim 3 or 7, wherein in step c, the molar ratio of the precipitant to the soluble nickel salt is 1; and/or
In the step c, the roasting temperature is 270-300 ℃, and the roasting time is 2-5 h.
9. An ultrafine nickel oxide nanoparticle produced by the method for producing an ultrafine nickel oxide nanoparticle according to any one of claims 3 to 8.
10. The ultrafine nickel oxide nanoparticles of claim 9, wherein the nano-nickel oxide particles have a particle size of 5nm to 15nm.
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| CN101302040A (en) * | 2008-06-13 | 2008-11-12 | 辽宁石油化工大学 | Method for preparing particle diameter-controllable nano-nickel oxide particle |
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| CN108529690A (en) * | 2018-04-17 | 2018-09-14 | 广东普加福光电科技有限公司 | A kind of preparation method and applications of nickel oxide nano crystal |
| CN109004189A (en) * | 2018-07-10 | 2018-12-14 | 河北师范大学 | A method of nickel compound of the calcining containing ionic liquid prepares lithium cell cathode material |
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| CN101302040A (en) * | 2008-06-13 | 2008-11-12 | 辽宁石油化工大学 | Method for preparing particle diameter-controllable nano-nickel oxide particle |
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| CN116282958A (en) * | 2023-03-20 | 2023-06-23 | 中国科学技术大学 | Nickel oxide film and preparation method and application thereof |
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