CN115465902B - Reaction solvent for preparing superfine nickel oxide nano particles and method for preparing superfine nickel oxide by using reaction solvent - Google Patents
Reaction solvent for preparing superfine nickel oxide nano particles and method for preparing superfine nickel oxide by using reaction solvent Download PDFInfo
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- CN115465902B CN115465902B CN202211199174.6A CN202211199174A CN115465902B CN 115465902 B CN115465902 B CN 115465902B CN 202211199174 A CN202211199174 A CN 202211199174A CN 115465902 B CN115465902 B CN 115465902B
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- 229910000480 nickel oxide Inorganic materials 0.000 title claims abstract description 138
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 title claims abstract description 102
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 21
- 239000007810 chemical reaction solvent Substances 0.000 title abstract description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 27
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000002608 ionic liquid Substances 0.000 claims abstract description 14
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 150000002815 nickel Chemical class 0.000 claims description 39
- 239000000243 solution Substances 0.000 claims description 31
- 239000011259 mixed solution Substances 0.000 claims description 26
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 238000001035 drying Methods 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 9
- -1 1-amino ethyl-2-ethyl pyridine bromide Chemical compound 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- GJAAJNMURIECJS-UHFFFAOYSA-N CC(C1=NC=CC=C1)N.Br Chemical compound CC(C1=NC=CC=C1)N.Br GJAAJNMURIECJS-UHFFFAOYSA-N 0.000 claims description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 3
- 239000012295 chemical reaction liquid Substances 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
- 235000011114 ammonium hydroxide Nutrition 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
- 239000002245 particle Substances 0.000 abstract description 48
- 239000007864 aqueous solution Substances 0.000 abstract description 4
- 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
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 41
- 239000006185 dispersion Substances 0.000 description 36
- 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 18
- 238000002360 preparation method Methods 0.000 description 15
- 239000008367 deionised water Substances 0.000 description 13
- 229910021641 deionized water Inorganic materials 0.000 description 13
- 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
- 239000007788 liquid Substances 0.000 description 8
- 238000003756 stirring Methods 0.000 description 8
- 239000007787 solid Substances 0.000 description 7
- 238000004528 spin coating Methods 0.000 description 7
- 238000005054 agglomeration Methods 0.000 description 6
- 230000002776 aggregation Effects 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 5
- 239000011521 glass Substances 0.000 description 5
- 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
- 239000013078 crystal Chemical group 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
- 230000000284 resting effect Effects 0.000 description 3
- 238000004062 sedimentation Methods 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
- 239000003153 chemical reaction reagent Substances 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
- 239000002243 precursor Substances 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- 229910021585 Nickel(II) bromide Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000008859 change Effects 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
- 238000004090 dissolution 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
- 230000008569 process Effects 0.000 description 1
- 239000002994 raw material Substances 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
- 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
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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Organic Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Composite Materials (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
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 comprises ethanol aqueous solution and pyridine type ionic liquid, and the viscosity and the surface energy of the reaction solvent can be changed, so that the morphology and the particle size of the prepared nickel oxide nanoparticles are effectively regulated and controlled, the particle size of the prepared nickel oxide nanoparticles is concentrated at 5-15 nm, the dispersibility of the nickel oxide nanoparticles in various solvents is improved, and the nickel oxide nanoparticles can be rapidly and uniformly dispersed in subsequent application, so that the application field of the nickel oxide nanoparticles is favorably enlarged, and the nickel oxide nanoparticles have a higher application prospect.
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 with specific performance, which is prepared by regulating and controlling a substance structure in a nano scale (0.1-100 nm), and has surface effect, small-size effect and macroscopic quantum tunneling effect. When a macroscopic object is subdivided into ultrafine particles (nanoscale), it will exhibit many unusual characteristics, namely its optical, thermal, electrical, magnetic, mechanical and chemical properties will appear to be significantly different when compared to large particulate matter.
Nickel oxide (NiO) is a green to black green solid powdery substance and is widely used in the fields of catalysis, ceramics, sensors, batteries, and the like. It is noted that nickel oxide is a typical P-type semiconductor material with a forbidden band width of 3.6-4.0eV, and due to this characteristic, nickel oxide is increasingly used in the photovoltaic field.
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, larger particle size and the like. The liquid phase method can be classified into sol-gel method, precipitation method, solvothermal method, etc. The conventional precipitation method has simple preparation process and is a method for preparing nickel oxide by more application at present, but generally needs to involve a heating and drying step in the precipitation process, the nano particles are mutually close under the action of interfacial tension, the particles are compact due to surface hydroxyl groups and crystal bridges formed by dissolution and precipitation, and the crystal bridges are mutually combined to form larger blocky agglomerates along with the extension of the drying time. Therefore, the nickel oxide particles prepared by the conventional precipitation method have larger particle size and are easy to agglomerate, and are not beneficial to being dispersed in a medium during application. Therefore, the development of a novel preparation method of superfine nickel oxide has very important significance for expanding the application range of nickel oxide.
Disclosure of Invention
Aiming at the problems that the nickel oxide prepared by a precipitation method in the prior art has larger particle size, is easy to agglomerate and is unfavorable to disperse in a medium, the invention provides a preparation method of superfine nickel oxide nano particles. The invention prepares nickel oxide by precipitation method in ethanol and pyridine type ionic liquid to obtain superfine nano nickel oxide particles, and the particle size distribution is centralized, thus having very important significance for expanding the application field of 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 a 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 morphology and the particle size of the prepared nickel oxide nanoparticles are effectively regulated and controlled, the particle size of the prepared nickel oxide nanoparticles is concentrated at 5nm-15nm, the dispersibility of the prepared nickel oxide nanoparticles in various solvents is improved, and the prepared nickel oxide nanoparticles can be rapidly and uniformly dispersed in subsequent application, so that the application field of the nano nickel oxide particles is favorably enlarged, and the application prospect is higher.
Preferably, the pyridine type ionic liquid is at least one of 1-amino ethyl-pyridine bromide, 1-amino ethyl-2-ethyl pyridine bromide or 1-amino ethyl-3-ethyl pyridine bromide.
The ethanol aqueous solution in the reaction solvent can reduce the occurrence of agglomeration problem when nickel oxide particles are dried, and meanwhile, the preferable pyridine type ionic liquid can be anchored on the surfaces of the nickel oxide particles to reduce the hydroxyl content on the surfaces of the nickel oxide particles, so that the problem of nickel oxide particle agglomeration caused by hydroxyl dehydration condensation is effectively reduced, and the preferable pyridine type ionic liquid covers the surfaces of the nickel oxide particles to increase the steric hindrance between the nickel oxide particles, so that the agglomeration of the nickel oxide particles is further effectively prevented.
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 ethanol water solution to obtain nickel salt mixed solution;
step b, adding pyridine type ionic liquid into the nickel salt mixed solution, and uniformly mixing to obtain nickel salt reaction solution;
and c, adding a precipitator into the nickel salt reaction liquid, reacting, centrifuging, washing, drying and roasting to obtain the superfine nickel oxide nano particles.
Preferably, in the step a, the volume percentage of the absolute ethyl alcohol in the ethyl alcohol 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 to 1.5mol/L.
Illustratively, 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 the 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 from 1:1 to 2:1.
Preferably, in the step c, the roasting temperature is 270-300 ℃ and the roasting time is 2-5 h.
Illustratively, in step c, the drying is performed by a heat drying method or a vacuum drying method.
The invention also provides ultrafine nickel oxide nanoparticles, which are prepared by the method for preparing ultrafine 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, the preparation method is simple, the raw materials are easy to obtain, the preparation method is suitable for industrial production and application, the application range of nano nickel oxide particles is enlarged, and the preparation method 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 chart of nickel oxide nanoparticles prepared in example 1 of the invention;
FIG. 3 is a comparative graph of the resting for 24h of the nickel oxide nanodispersion of example 1 of the present invention, wherein the left graph is 0h and the right graph is 24h;
FIG. 4 is a graph showing the particle size distribution of nano nickel oxide in the nano nickel oxide dispersion liquid according to example 1 of the present invention;
FIG. 5 is a comparative graph of the resting for 24 hours of the nickel oxide nanodispersion of example 2 of the present invention, wherein the left graph is 0h and the right graph is 24h;
FIG. 6 is a graph showing the particle size distribution of nano nickel oxide in the nano nickel oxide dispersion liquid according to example 2 of the present invention;
FIG. 7 is a comparative graph of the resting for 24 hours of the nickel oxide nanodispersion of example 3 of the present invention, wherein the left graph is 0h and the right graph is 24h;
FIG. 8 is a graph showing the particle size distribution of nano nickel oxide in the nano nickel oxide dispersion liquid according to example 3 of the present invention;
FIG. 9 is a comparative graph of the comparative example 1 in which the nickel oxide nanodispersion was left standing still for 24 hours, wherein the left graph is 0h and the right graph is standing for 24 hours;
FIG. 10 is a graph showing the particle size distribution of nano nickel oxide in the nano nickel oxide dispersion liquid according to comparative example 1 of the present invention;
FIG. 11 is a comparative graph of the comparative example 2 in which the nickel oxide nanodispersion was left standing still for 24 hours, wherein the left graph is 0h and the right graph is standing for 24 hours;
FIG. 12 is a graph showing the particle size distribution of nano nickel oxide in the nano nickel oxide dispersion liquid according to comparative example 2 of the present invention;
FIG. 13 is a comparative graph of comparative example 3 in which the nickel oxide nanodispersion was left standing still for 24 hours, wherein the left graph is 0h and the right graph is standing for 24h;
FIG. 14 is a graph showing the particle size distribution of nano nickel oxide in the nano nickel oxide dispersion liquid according to comparative example 3 of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
In order to better illustrate the present invention, the following examples are provided for further illustration.
Example 1
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 in a volume ratio of 1:3 to obtain a nickel salt mixed solution with a concentration of 0.75 mol/L;
step two, adding 1-amino ethyl-pyridine bromide salt into 50mL of the nickel salt mixed solution, wherein the addition amount of the 1-amino ethyl-pyridine bromide salt is 0.03 weight percent of nickel nitrate, so as to obtain nickel salt reaction solution;
step three, 7.5mL of 10mol/L sodium hydroxide solution is rapidly added into the nickel salt reaction solution, and stirring is carried out for 30min at room temperature and 800rpm, so as to obtain nickel hydroxide suspension;
and fourthly, centrifuging the nickel hydroxide suspension for 5min at 6800r/min, washing the obtained solid with a mixed solution of absolute ethyl alcohol and deionized water in a volume ratio of 1:3 for 3 times, drying for 12h at 80 ℃, and roasting for 2h at 270 ℃ to obtain black nickel oxide powder.
The XRD pattern of the nano nickel oxide nanoparticle of this example is shown in fig. 1, and it can be seen from the figure that the three diffraction angles of the nano nickel oxide particle prepared in this example are 37.24 °, 43.27 ° and 62.87 ° consistent with standard cards #47-1049, which indicates that the product has no impurity phase. The three diffraction peaks correspond to the three crystal planes (111), (200) and (220), and the nickel oxide prepared is proved to be in a cubic phase structure.
FIG. 2 is a FT-IR chart of nickel oxide nanoparticles prepared in this example, from which it can be seen that-NH is present in the spectrogram 2 And c=n, indicating that the pyridine-type ionic liquid was successfully adsorbed on the nickel oxide surface.
Fig. 3 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 from the graph that the nano nickel oxide dispersion still has no agglomeration and precipitation phenomenon after standing for 24 hours, which indicates that the nano nickel oxide prepared in this example has good dispersion stability.
FIG. 4 is a graph showing the particle size distribution 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 nano nickel oxide dispersion prepared in this example is concentrated, mainly at about 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, nickel nitrate is dissolved in a mixed solution of absolute ethyl alcohol and deionized water in a volume ratio of 1:1 to obtain a nickel salt mixed solution with a concentration of 0.6 mol/L;
step two, adding 1-amino ethyl-2-ethyl pyridine bromide salt into 50mL of the nickel salt mixed solution, wherein the addition amount of the 1-amino ethyl-2-ethyl pyridine bromide salt is 0.06wt% of nickel nitrate, and obtaining nickel salt reaction solution;
step three, adding 3mL of 10mol/L sodium hydroxide solution into the nickel salt reaction solution rapidly, and stirring at room temperature for 30min at 800rpm to obtain nickel hydroxide suspension;
and fourthly, centrifuging the nickel hydroxide suspension for 5min at 6800r/min, washing the obtained solid with a mixed solution of absolute ethyl alcohol and deionized water in a volume ratio of 1:1 for 3 times, drying for 12h at 80 ℃, and roasting for 2.5h at 300 ℃ to obtain black nickel oxide powder.
Fig. 5 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 from the graph that the nano nickel oxide dispersion still has no agglomeration and precipitation phenomenon after standing for 24 hours, which indicates that the nano nickel oxide prepared in this example has good dispersion stability.
FIG. 6 is a graph showing the particle size distribution 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 nano nickel oxide dispersion prepared in this example is concentrated, mainly at about 10 nm.
Example 3
The embodiment of the invention provides a preparation method of superfine nano nickel oxide, which comprises the following steps:
step one, dissolving nickel chloride in a mixed solution of absolute ethyl alcohol and deionized water in a volume ratio of 1:2 to obtain a nickel salt mixed solution with a concentration of 1.25 mol/L;
step two, adding 1-amino ethyl-3-ethyl pyridine bromide salt into 50mL of the nickel salt mixed solution, wherein the addition amount of the 1-amino ethyl-3-ethyl pyridine bromide salt is 0.01 weight percent of nickel chloride, and obtaining nickel salt reaction solution;
step three, 10mL of 10mol/L potassium hydroxide solution is rapidly added into the nickel salt reaction solution, and stirring is carried out for 30min at room temperature and 800rpm, so as to obtain nickel hydroxide suspension;
and fourthly, centrifuging the nickel hydroxide suspension for 5min at 6800r/min, washing the obtained solid with a mixed solution of absolute ethyl alcohol and deionized water in a volume ratio of 1:2 for 3 times, drying for 12h at 80 ℃, and roasting for 5h at 280 ℃ to obtain black nickel oxide powder.
Fig. 7 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 from the graph that the nano nickel oxide dispersion still has no agglomeration and precipitation phenomenon after standing for 24 hours, which indicates that the nano nickel oxide prepared in this example has good dispersion stability.
FIG. 8 is a graph showing the particle size distribution 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 relatively concentrated, mainly at about 10 nm.
Comparative example 1
The comparative example provides a preparation method of superfine nano nickel oxide, which comprises the following steps:
step one, nickel nitrate is dissolved in deionized water to obtain 0.75mol/L nickel salt solution;
step two, 7.5mL of 10mol/L sodium hydroxide solution is rapidly added into the 50mL of nickel salt solution, and stirring is carried out for 30min at room temperature and 800rpm, thus obtaining nickel hydroxide suspension;
and thirdly, centrifuging the nickel hydroxide suspension for 5min at 6800r/min, washing the obtained solid with deionized water for 3 times, drying for 12h at 80 ℃, and roasting for 2h at 270 ℃ to obtain black nickel oxide powder.
FIG. 9 is a graph showing the effect of the nickel oxide dispersion (2 mg of nickel oxide nanoparticles dispersed in 10mL of water) prepared after standing for 24 hours, and it can be seen from the graph that the nickel oxide dispersion cannot be kept stable for both of 0h and 24 h.
Fig. 10 is a graph showing a particle size distribution of nano nickel oxide in a nickel oxide dispersion (2 mg nickel oxide nanoparticles dispersed in 10mL 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 sedimentation rate of particles is high.
Comparative example 2
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 in a volume ratio of 1:3 to obtain a nickel salt mixed solution with a concentration of 0.75 mol/L;
step two, 7.5mL of 10mol/L sodium hydroxide solution is rapidly added into the 50mL nickel salt mixed solution, and stirring is carried out for 30min at room temperature at the speed of 800rpm, thus obtaining nickel hydroxide suspension;
centrifuging the nickel hydroxide suspension for 5min at 6800r/min, washing the obtained solid with a mixed solution of absolute ethyl alcohol and deionized water in a volume ratio of 1:3 for 3 times, drying at 80 ℃ for 12h, and roasting at 270 ℃ for 2h to obtain black nickel oxide powder.
FIG. 11 is a graph showing the effect of the nickel oxide dispersion (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 nickel oxide dispersion after standing for 24 hours cannot be kept stable.
Fig. 12 is a graph showing a particle size distribution of nano nickel oxide in a nickel oxide dispersion (2 mg nickel oxide nanoparticles dispersed in 10mL 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 sedimentation rate of particles is high.
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 in a volume ratio of 1:3 to obtain a nickel salt mixed solution with a concentration of 0.75 mol/L;
step two, adding methylamine formate ionic liquid into 50mL of the nickel salt mixed solution, wherein the addition amount of the methylamine formate ionic liquid is 0.03 weight percent of nickel nitrate, so as to obtain nickel salt reaction liquid;
step three, 7.5mL of 10mol/L sodium hydroxide solution is rapidly added into the nickel salt reaction solution, and stirring is carried out for 30min at room temperature and 800rpm, so as to obtain nickel hydroxide suspension;
and fourthly, centrifuging the nickel hydroxide suspension for 5min at 6800r/min, washing the obtained solid with a mixed solution of absolute ethyl alcohol and deionized water in a volume ratio of 1:3 for 3 times, drying for 12h at 80 ℃, and roasting for 2h at 270 ℃ to obtain black nickel oxide powder.
FIG. 13 is a graph showing the effect of the nickel oxide dispersion (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 nickel oxide dispersion after standing for 24 hours cannot be kept stable.
Fig. 14 is a graph showing a particle size distribution of nano nickel oxide in a nickel oxide dispersion (2 mg nickel oxide nanoparticles dispersed in 10mL 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 sedimentation rate of particles is high.
Application example
The nano nickel oxide dispersion prepared in example 1 is applied to the preparation of perovskite solar cells, and the steps are as follows:
ITO glass substrate (2X 2 cm) 2 ) Respectively ultrasonically cleaning the glass in deionized water, acetone and isopropanol for 30min, and then treating the glass in an ultraviolet cleaning machine for 20min to obtain the pretreated ITO glass.
Dispersing the nickel oxide prepared in the example 1 in water to obtain a nickel oxide dispersion liquid with the concentration of 20 mg/mL; and spin-coating the nickel oxide dispersion liquid on the surface of the pretreated ITO glass, wherein the spin-coating amount is 80 mu L, and annealing is carried out at 120 ℃ for 20min to obtain the hole transport layer.
Will 509.4mg PbI 2 、71.6mg PbBr 2 179.7mg FAI,20.2mg MABr adding into a reagent bottle, adding 1mL of mixed solvent (DMF: DMSO=4:1, v/v), and stirring for 1h to obtain a precursor solution; spin-coating the precursor solution onto the surface of the hole transport layer at a speed of 3000r/min,and (3) spin coating for 35s, rapidly dripping 200 mu L of chlorobenzene in the 10 th s of spin coating, and rapidly transferring the sample to a heating plate at 100 ℃ for annealing treatment for 30min to form the perovskite film.
Adding 20mg of PCBM into a reagent bottle, adding 1mL of chlorobenzene, and stirring at 60 ℃ for 2 hours to obtain PCBM solution; and (3) taking 50 mu L of PCBM solution, spin-coating the solution on the surface of the perovskite film at the speed of 2000r/min, and spin-coating the solution for 30s to obtain an electron transport layer.
2.5mg of BCP was dissolved in 5mL of isopropyl alcohol, 80. Mu.L of the solution was spin-coated on the surface of the electron transport layer, and spin-coated at 4000r/min for 30s to obtain a BCP barrier layer.
And evaporating an Au electrode with the thickness of 80nm on the surface of the BCP barrier layer through a vacuum thermal evaporation device to obtain the perovskite solar cell.
Perovskite solar cells were subjected to I-V testing with a maximum efficiency of 17.5%.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, or alternatives falling within the spirit and principles of the invention.
Claims (5)
1. A method for preparing ultrafine nickel oxide nanoparticles, comprising the steps of:
step a, dissolving soluble nickel salt in ethanol water solution to obtain nickel salt mixed solution;
step b, adding pyridine type ionic liquid into the nickel salt mixed solution, and uniformly mixing to obtain nickel salt reaction solution;
step c, adding a precipitator into the nickel salt reaction liquid, reacting, centrifuging, washing, drying and roasting to obtain superfine nickel oxide nano particles;
the pyridine type ionic liquid is at least one of 1-amino ethyl-pyridine bromide, 1-amino ethyl-2-ethyl pyridine bromide or 1-amino ethyl-3-ethyl pyridine bromide; 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.
2. The method for preparing ultrafine nickel oxide nanoparticles as recited in claim 1, wherein in step a, the volume percentage of absolute ethanol in the aqueous ethanol solution is 25% -50%.
3. The method for preparing ultrafine nickel oxide nanoparticles as recited in claim 1, wherein in the step a, the concentration of the nickel salt in the nickel salt mixed solution is 0.5mol/L to 1.5mol/L.
4. The method for preparing ultrafine nickel oxide nanoparticles as recited in claim 1, wherein in step c, the precipitant is at least one of ammonia water, urea solution, sodium hydroxide solution, potassium hydroxide solution, or ammonium bicarbonate solution.
5. The method for preparing ultrafine nickel oxide nanoparticles as recited in claim 1 or 4, wherein in step c, the molar ratio of the precipitant to the soluble nickel salt is 1:1 to 2:1; and/or
In the step c, the roasting temperature is 270-300 ℃, and the roasting time is 2-5 h.
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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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| 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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