78 results about "Trioctylphosphine" patented technology

Highly monodisperse nanocrystals (including CdSe, ZnSe, PbSe, Cu_2-xSe, MnSe, Zn_1-xCd_xSe, CuInSe₂, CuInSnSe₂, CdTe, ZnTe, PbTe, etc) have been synthesized by using different “green” starting materials to prepare chalcogenide (Se and Te) precursors successfully. Air-sensitive compounds (alkylphosphine, such as trioctylphosphine (TOP) and tributylphosphine (TBP)) have been eliminated to use in the entire synthetic process. As surface coating agents, amphiphilic oligomer (polymaleic acid aliphatic alcohol ester) with different alkyl chain length has been utilized to form oligomer-coated water-soluble nanocrystals.

The invention relates to a method for preparing quaternary amine dual-functional ionic liquid. The quaternary amine dual-functional ionic liquid is prepared by sequentially adopting an anion exchange reaction, a hydrolysis reaction and an acid-alkali neutralizing reaction; a synthetic route is simple; the reaction can be completed at the normal temperature and under the normal pressure with moderate reaction conditions; an apparatus is simple; in the process of preparing the quaternary amine dual-functional ionic liquid by quaternary ammonium hydroxide and acid through the acid-alkali neutralizing reaction, the reaction is sufficient; through ICP-MS and ionic chromatographic detection, the content of sodion and chloridion in the methyl trioctylphosphine ammonium nitric acid ionic liquid prepared by the acid-alkali neutralizing reaction is obviously lower than that of the methyl trioctylphosphine ammonium nitric acid ionic liquid prepared by the anion exchange reaction. In the invention, superficial characteristics on the decomposition temperature, the density, the moisture content of the prepared dual-functional ionic liquid and the intersolubility of normal organic solvents are carried out.

The invention provides a method for synthesizing ZnxCd1-xSe (x is more than or equal to 0 and less than or equal to 1) and ZnxCd1-xSe/ZnSe, ZnxCd1-xSe/ZnS and ZnxCd1-xSe core/shell structured semiconductor nanocrystals thereof by using long-chain fatty acid salts of cadmium and zinc as precursors of cadmium and zinc, which is the most economical and environment-friendly method for synthesizing high-quality ZnxCd1-xSe and related core/shell structured semiconductor nanocrystals thereof currently. The method avoids using tributylphosphine (TBP) or trioctylphosphine (TOP) dissolved elementary selenium as the precursor of selenium currently in the world, but adopts octadecylene (ODE) dissolved elementary selenium as the precursor of selenium; and the obtained nanocrystals have the quality equal to that of nanocrystals which are synthesized when the TBP or TOP dissolved selenium powder is used as the precursor of selenium. The method is called a phosphine-free method, has the advantages of simple synthesizing process, good repeatability, safety, environmental protection, no need of glove box, and cost conservation of over 60 percent. The synthesized ZnxCd1-xSe and related core/shell structured nanocrystals have a fluorescence range of between 400 and 650nm, and have the advantages of uniform particle size distribution, high efficiency of fluorescent quantum yield (40 to 70 percent) and narrow full width at half maximum. The method is also suitable for synthesizing the ZnxCd1-xS, HgxCd1-xSe, ZnxCd1-xTe nanocrystals and related core/shell structures thereof. More importantly, the method can synthesize high-quality nanocrsytals on a large scale, and has enormous application value both in laboratory synthesis and industrial synthesis.

The invention belongs to the method for compounding cadmium selenide and quanta of cadmium telluride, which is: use cadmium oxide containing 2~18 carbon atom as cadmium source, selenium powder as selenium source and tellurium powder as tellurium source, and the mol ratio of cadmiumsource and selenium source or tellurium source is 5:1-1:5, dissolve the selenium and tellurium powder with tricapryl phosphine, make oleic acid, and tricapryl phosphine oxide as enveloping agent and the mol ratio of cadmium source and enveloping agent is 1:2-1:6, use benzene, toluene, cyclohexane, normal hexane and normal heptane as solvent, under the condition that the density of cadmium source is 0.001-0.015M, the temperature in autoclave is 140-180deg.C, heat them for 0.8-16 hours and obtain cadmium selenide and quanta of cadmium telluride with different sizes by changing the reaction time. The cadmium selenide and quanta of cadmium telluride has narrower size distribution which is shown as narrower shooting of fluorescence whose half-peak width of quanta of cadmium selenide is 22-33nm and that of quanta of cadmium telluride is 29-35nm.

The invention belongs to a method for synthesizing nanometer materials, in particular to a method for synthesizing bar-shaped ZnSe fluorescence nanocrystalline. The method comprises the following steps: with the protection of inert gas, heating and stirring a simple substance Se or dissolving the simple substance Se in trioctylphosphine phosphine in an ultraphonic manner to obtain Se precursor; dissolving zinc source body in octadecylene and adding activating agent long-chain alkylamine with the protection of inert gas and carrying out activation on the mixture; introducing the long-chain alkyl sulfhydryl to carry out 'template' processing on activated Zn precursor; then with the protection of inert gas, raising temperature to reaction temperature (300-350 DEG C); fast adding Se precursor into the Zn precursor and carrying out reaction for a certain period of time, then obtaining original solution crude product of ZnSe nanocrystalline; adding mixed solvent composed of high-polarity organic solvent and low-polarity organic solvent and washing and centrifuging the mixture; finally using the low-polarity organic solvent to obtain the final product ZnSe nano rod transparent solution. The method has the advantages of simple reaction system, easily available raw materials, small environmental pollution, good degree of crystallization and high fluorescence quantum yield.

The invention relates to a solution phase method for synthesizing a tin selenide monocrystal nanowire, and belongs to the technical field of inorganic compound semiconductor nano material. Bis[bis(trimethyl silicon alkyl) amino] tin (II) and selenizing organic phosphine are used as raw materials to rapidly synthesize the tin selenide monocrystal nanowire through assistance of a catalyst at 250-310 DEG C in 1-2 min, in oil amine or a mixed solvent of oil amine and trioctylphosphine phosphorus oxide. The tin selenide monocrystal nanowire synthesized by the invention has advantages of small diameter (average diameter of 21 nm), adjustable average length from hundreds of nanometers to tens of microns, uniform appearance, good crystallinity and good colloidal dispersion, etc. At the same time, the invention has simple process, rapid synthesis (only 1-2 min), no intermediate product, convenient operation and easy popularization, and is suitable for industrial production. The tin selenide monocrystal nanowire prepared by the method provided by the invention has good optical properties, and can be used in the manufacture of optoelectronic devices or solar cell materials.

The invention discloses a prepartion method of CdSe and CdSe-ZnSe nuclear shell quantum dots, first, adding Cd source into organic coating agent and so-solvent, heating to dissolve the Cd source, then cooling to obtain Cd precursor solution; second, adding Se powder into trioctylphosphine and the so-solvent, ultrasonic dispersion at room temperature to dissolve the Se powder to get Se precursor solution; third, mixing the Cd precursor solution with the Se precursor solution, sealing the mixed solution and heating to make it react at certain temperature, the cooling to get CdSe quantum dots original solution; fourth, adding Zn source into the organic coating agent and so-solvent, heating to 100-140 DEG for dissolving the Zn source, cooling to get Zn precursor solution; fifth, mixing the Zn precursor solution, Se precursor solution and CdSe precursor quantum dots original solution, sealing the mixed solution and heating to make it react at certain temperature, then cooling to get the CdSe-ZnSe nuclear shell quantum dots.

The invention discloses a prepartion method of ternary system quantum dots containing Cd[x]Zn[1-x]Se, first, adding Cd source into organic coating agent and so-solvent, heating to dissolve the Cd source into the organic coating agent and so-solvent, and preserving heat to form transparent Cd precursor solution; second, adding Zn source into the organic coating agent and so-solvent, heating to dissolve the Zn source into the organic coating agent and so-solvent, and preserving heat to form transparent Zn precursor solution; third, adding Se powder into trioctylphosphine, ultrasonic dispersion at room temperature to dissolve the Se powder into the trioctylphosphine, and then diluting by the so-solvent to get Se precursor solution, then sealing and storing the Se precursor solution; fourth, mixing the Cd precursor solution, Zn precursor solution and Se precursor solution and the organic coating agent in properticn, using inert gas to remove air, sealing and reacting under protection of inert gas, cooling to room temperature to obtain the ternary system quantum dots containing Cd[x]Zn[1-x]Se.

The invention discloses a low-temperature liquid phase synthesizing method of monodisperse square crystalline phase ferrous selenide square nanometer sheet. The method comprises the following steps of: heating oil amine solution of anhydrous FeC12 to 100-140 DEG C under the protection of high-purity argon until the solid is completely dissolved; adding oleic acid and the prepared trioctylphosphine phosphor of selenium to react for 5-45min at 280-330 DEG C to prepare the monodisperse square crystalline phase ferrous selenide nanometer sheet, wherein the volume ratio of oil amine solution of anhydrous FeC12 to oleic acid is 30:1-3, and the molar ratio of iron ion to selenium is 1:1. The method is a liquid phase synthesizing method of ferrous selenide and can obtain the product directly in the solution at low temperature without calcinations in comparison with the solid phase method. Compared with other liquid phase methods, the method ensures that the obtained product has better regular two-dimensional nanometer structure, the granule has controllable and even size as well as good dispersity and the material is non-toxic FeC12.

The invention discloses a preparation method of a color-adjustable small-size Mn: CsPbCl3 nanocrystal and belongs to the technical field of semiconductor nanomaterial preparation. The preparation method comprises weighing lead chloride, oleic acid, oleylamine and octadecene, putting the materials into a three-necked flask, carrying out vacuum-pumping at 120 DEG C, adding trioetylphosphine into thematerials in the nitrogen gas protective atmosphere at 150 DEG C to obtain a mixed solution, cooling the mixed solution to the room temperature, pouring a cesium oleate solution into the mixed solution for a reaction at the room temperature for 1h to obtain a CsPbCl3 nanocrystal seed, preparing lead bismuth chloride perovskite with different sizes from the CsPbCl3 nanocrystal seed, carrying out purification, adding a manganese salt into the perovskite, and carrying out grinding to obtain Mn: CsPbCl3 nanocrystals in different colors. The preparation method can adjust the amaranth of the Mn: CsPbCl3 nanocrystal to red color. The color-adjustable small-size Mn: CsPbCl3 nanocrystal has the controllable size and high fluorescence efficiency. The preparation method has simple processes, utilizes easily available raw materials, realizes large-scale synthesis and has a wide product application prospect.

The invention especially relates to a method for preparing nano-crystals containing tellurium, selenium or sulfur, wherein the method uses stable phosphine-containing organic compounds (such as dioctylphosphine oxide and the like) having similar structures as a novel solvent of tellurium powder, selenium powder or sulfur powder and uses a novel tellurium, selenium or sulfur solution as a precursor to prepare a plurality of nano-crystals containing tellurium, selenium or sulfur. The method avoids high cost and high risk caused by a case that tributylphosphine (TBP) or trioctylphosphine (TOP) is commonly and internationally used at present to dissolve tellurium, selenium or sulfur in order to generate the tellurium, selenium or sulfur precursor. The synthetic method has the advantages of safe operation, easy operation, and good repeatability, and medicines used in the method are routine and stable and have low toxicities. The nano-crystals containing tellurium, selenium or sulfur reaches even exceeds nano-crystals containing tellurium, selenium or sulfur synthesized through using flammable and explosive compounds comprising TOP/TBP and the like in quality. The method has very high application values in the laboratory field and the industrial production field.

The invention discloses a preparation method of luminescence tin halide perovskite colloid nano-crystals. The tin halide perovskite colloid nano-crystals are prepared through injecting a cesium source-containing precursor solvent to an organic ligand-containing tin halide precursor long-chain alkane solvent in a hot manner and carrying out a reaction. The tin halide perovskite colloid nano-crystals with different luminescence properties and different morphologies can be obtained through controlling the reaction time, the temperature and the concentrations and the proportions of tin and a halogen precursor. The luminescence tin halide perovskite colloid nano-crystals have the advantages of controllable dimensions, morphology and luminescence property, and no use of toxic heavy metal elements, such as lead, cadmium and mercury, or severely toxic organic phosphorus, such as tri-n-octylphosphine and tri-n-butylphosphine, are inorganic nano-crystals with good luminescence properties, and have wide application prospect in the fields of luminescence devices, flat panel display, solar batteries and field effect transistors.

The invention provides a preparation method of a silver sulfide-zinc sulfide semiconductor nanometer heterojunction. The preparation method comprises a step (A) of enabling reaction precursor silver dibutyl dithiocarbamate to undergo pyrolysis in a mixed solvent to obtain silver sulfide particles; and a step (B) of enabling the silver sulfide obtained in the step (A) to serve as a catalyst, enabling an intermediate product formed by pyrolysis of zinc dibutyl dithiocarbamate to be dissolved in the mixed solvent containing the silver sulfide particles, separating out zinc sulfide nanorods from the silver sulfide particles under the effect of trioctylphosphine and n-octadecyl mercaptan, and forming the silver sulfide-zinc sulfide semiconductor nanometer heterojunction. The preparation method of the silver sulfide-zinc sulfide semiconductor nanometer heterojunction is simple and convenient, high in rate of production and suitable for industrial production. The shape and the structure of the silver sulfide-zinc sulfide semiconductor nanometer heterojunction can be controlled under normal pressure, and the rate of production can be over 80%.

A method for preparing and separating monodisperse amorphous nickel nanoparticles comprises the following steps: taking acetylacetone nickel as a raw material; taking whiteruss as a reaction medium; taking trioctyl phosphine and oleylamine as stabilizing agents (or: protective solutes, surface modifying agents); taking an organic ferric compound as a catalyzer; taking polylol as a morphological modifying agent; mixing the above substances in a kettle-type reactor according to a certain ratio; heating the substances with hydrogen to the reaction temperature (150 to 350 DEG C); reacting for 3 hours; obtaining amorphous nickel nanoparticles; and adopting an external applied magnetic field to assist the solvent fractionating method, so as to separate the nickel nanoparticles from the reaction system. The powdery monodisperse amorphous nickel nanoparticles can once again disperse into organic solvents such as chloroform, sherwood oil, etc. without sedimentation.

The invention discloses a preparation method of manganese-doped all-inorganic lead chloride perovskite nanosheets. The method comprises the following steps: adding cesium carbonate into a mixed solution of 1-octadecene and oleic acid to prepare a cesium oleate precursor solution; then, adding metal chlorides PbCl2 and MnCl2, oleic acid, oleylamine and trioctylphosphine into a 1-octadecene solution, heating up to 100-120 DEG C under the vacuum condition to obtain a mixed solution; finally, injecting the mixed solution into the cesium oleate precursor solution, which is heated up to 100-120 DEGC, in a vacuum or an inert atmosphere, continuously heating up to 180-240 DEG C, carrying out heat preservation for 10-30 minutes, cooling and then centrifugally cleaning to obtain the manganese-dopedall-inorganic lead chloride perovskite nanosheets. The synthesis method provided by the invention is simple and convenient to operate and high in repeatability; the synthesized manganese-doped nanosheet fluorescent powder is not only uniform in morphology and size, but is also high in quantum efficiency and good in heat stability.

The invention relates to the technical field of CsPbCl3 nanocrystal material preparation and in particular to a method for increasing the manganese doping concentration and the light emission efficiency of a manganese-doped CsPbCl3 nanocrystal. The method comprises the following steps: preparing a caesium precursor solution; mixing octadecene, oleic acid, oleylamine, tri-n-octylphosphine, lead chloride, lead chloride, manganese chloride and nickel chloride; and forming a Ni-Mn double-doped CsPbCl3 nanocrystal, so as to obtain a Ni-Mn double-doped CsPbCl3 nanocrystal solution. By adopting the method, by adding NiCl2, the crystallinity and the surface defect state of a Mn-doped CsPbCl3 nanocrystal can be improved, the doping concentration of Mn in the manganese-doped CsPbCl3 nanocrystal canbe increased, and the light emission efficiency of the manganese-doped CsPbCl3 nanocrystal can be improved.

A preparation method of a CIST nano wire belongs to the technical field of new-generation thin-film solar cell materials. A toluene solution of Bi nanoparticles and a precursor solution of Se and Te are prepared separately. Then under the protection of nitrogen, trioctylphosphine is heated and added into the toluene solution of the Bi nanoparticles, and then the precursor solution containing indium acetate, copper acetate and Se is added into the mixture. After reactions, the precursor solution containing indium acetate, copper acetate and Se is added drop by drop. After reactions are completed, the mixture is cooled and toluene is added. Then the mixture is subjected to centrifugation. The solid phase is taken, is washed with toluene, and is subjected to centrifugation and vacuum drying. Then the CIST nano wire is obtained. The method uses the metal Bi nanoparticles as a catalyst. The toluene solution of the Bi nanoparticles is used, so that the concentration of the Bi nanoparticles can be effectively controlled, and the liquid form facilitates taking the catalyst. The method is simple in technique, can effectively control the stoichiometric ratio of multi-component materials, and obtains a large batch of high-purity CIST nano wires.

A method for preparing and separating monodisperse superparamagnetic iron nanoparticles that can be completely dissolved in polar and non-polar organic solvents comprises the following steps: taking iron acetylacetonate as a raw material; taking whiteruss as a reaction medium; taking trioctyl phosphine and oleylamine as stabilizing agents (or: protective solutes, surface modifying agents); taking an organic ferric compound as a catalyzer; taking polylol as a morphological modifying agent; mixing the above substances in a kettle-type reactor according to a certain ratio; heating the substances with hydrogen to the reaction temperature (150 to 350 DEG C); reacting for 3 hours; obtaining iron nanoparticles of good crystallinity; and adopting an external applied magnetic field to assist the solvent fractionating method, so as to separate the iron nanoparticles from the reaction system. The powdery iron nanoparticles can once again disperse into organic solvents such as chloroform, sherwood oil, etc. without sedimentation.

The invention provides a catalyst with ultra-low platinum content for a fuel cell and a preparation method thereof. After heat treatment of a metal source and oleylamine and trioctylphosphine, a noblemetal salt is added dropwise and dried to form spherical nanoparticles, The nano-particles containing organic phase are loaded on the surface of graphite electrode and the organic phase is removed simultaneously by vacuum pre-sintering reduction. During the electrochemical treatment, copper is deposited on the surface of graphite electrode to form a monoatomic layer of copper. At last, platinum is replaced by potassium chloroplatinate to form a multilayered core-shell structure of transition metal-precious metal-platinum and finally the required catalyst is prepared by carbon loading. A monoatomic layer formed by underpotential deposition of copper is replaced by platinum, The thickness of the platinum layer can be controlled effectively, and the catalytic active sites on the surface of the platinum layer are not affected, so that the catalytic performance is guaranteed, the manufacturing cost of the catalyst is reduced, and the defects that the thickness of the platinum layer and thereduction of the surface active sites are difficult to be controlled by the catalyst with low platinum loading capacity are overcome.

The invention discloses a method for synthesizing CsSnX3 perovskite quantum dots by microwave-assisted heating, and belongs to the field of semiconductor and nanotechnology. The method comprises the steps: adding cesium carbonate (Cs2CO3), oleic acid (OA) and oleylamine (OAm) according to the molar ratio of 1 to 0.375 to 0.375 to a mixed solvent mixed by octadecene (ODE) and a polar solvent with a volume ratio of (1:3) to (1:5), then placing into a microwave heating apparatus, stirring and vacuumizing, raising the temperature to be 60 to 100 DEG C, preserving heat to be dissolved, obtaining a cesium precursor solution with a molar concentration of 0.5 to 1.5M; introducing inert gas, raising the temperature to be 150 to 190 DEG C, injecting quickly a halide tin (SnX2) trioctylphosphine (TOP) solution, reacting for 1 to 5min, adding methyl acetate or tert-butanol after cooling, centrifuging, washing with n-hexane for 3 to 5 times, and obtaining CsSnX3 quantum dot powder after drying. According to the method for synthesizing the CsSnX3 perovskite quantum dots by microwave-assisted heating, the temperature distribution of the reaction temperature field is uniform and precisely controllable, the heating and cooling speed is fast, the preparation period is short and the yield is high; the quantum point has high crystallinity, less surface defects, uniform size distribution, high fluorescence quantum yield and high safety.

The invention relates to a preparing method of an ultra small near infrared copper indium selenium quantum dot. The method includes firstly preparing nanometer particle nucleuses having a uniform size. A synthetic process includes forming an organic metal compound from copper and indium chlorides and trioctylphosphine/dodecyl amine, stirring at 50-60 DEG C to obtain a colorless uniform mixed solution, and reacting at 200 DEG C so that the organic metal monomer quickly reacts to produce nanometer particles, wherein the color of the reactants changes gradually, lauryl mercaptan in the reaction solution can stabilize the produced nanometer particles, the low reaction temperature improves controllability of a nucleation reaction, and optical stability of the nanometer particles is improved. The method is simple and controllable. The size of the ultra small near infrared copper indium selenium quantum dot is about 2 nm. Water-soluble nanometer particles prepared after functionalization with a polydentate polymer ligand are high in stability and high in fluorescence quantum efficiency. The luminescence spectrum of the quantum dot covers the near infrared zone from 650 nm to 800 nm. The quantum dot can be used for a plurality of kinds of bioluminescence labeling.

The invention discloses a catalyst for generating hydrogen by hydroboron hydrolysis and a preparation method of the catalyst, and relates to a catalyst. The catalyst comprises an active component and a carrier, wherein the active component is cobalt monoxide nanocrystal; the carrier is metal oxide powder and carbon material powder; and the mass percent of the active component in the catalyst is 10%-100%. The preparation method comprises the steps of decomposing a metal precursor of cobalt in alkylamine containing trioctylphosphine phosphorous and ether taking alkylamine as a surfactant, conducting a reaction at 210-260 DEG C, cooling, separating, obtaining the active component with a particular pattern, mixing the active component with the carrier, and obtaining the catalyst. The catalyst can act as a substitute of the currently used noble metal catalyst, and has wide application prospects in the fields of fuel cells and the like. As the cobalt monoxide nanocrystal is taken as the active component, the catalyst has high activity for a hydrogen generation reaction by the hydroboron hydrolysis, is high in hydrogen generation speed, simple in preparation process, and low in cost.

The invention provides a vinasse extract and a preparation method and application thereof. The extraction method comprises the following steps that in a protective atmosphere, trioctylphosphine-modified CdSe/ZnS quantum dots, glyoxal dimethacrylate, 4-vinyl pyridine and gallic acid are subjected to reaction in xylene when initiated by azodiisobutyronitrile, after purification and drying are conducted, filler for extracting an antioxidant component of vinasse is obtained, and a solid-phase extraction cartridge is prepared; the vinasse is added into ethyl alcohol-water mixed liquid for heating and stirring, and extraction liquid is collected; the homemade solid-phase extraction cartridge is used for extracting the vinasse component, and after drying is conducted, the vinasse extract is obtained. The vinasse extract obtained through the method contains a phenolic acid substance, and can be used as a food additive for inhibiting carboxy methyl lysine in a food processing process, novel application of the white liquor vinasse is extended, and a novel path is provided for resource utilization of the vinasse. The method for preparing the vinasse extract is simple and convenient in extraction process and low in cost, industrialized application is easy, and the vinasse can be subjected to mass treatment.

The invention relates to a preparation method of a grafted quaternary phosphonate ionic liquid. The preparation method comprises the following steps of: using 3-(chloropropyl)triethoxysilane and trioctylphosphine to react and generate a chlorinated quaternary phosphonate ionic liquid intermediate, then using the chlorinated ionic liquid intermediate and sodium fluoroborate to synthesize a tetrafluoroborate quaternary phosphonate ionic liquid intermediate, and finally using the tetrafluoroborate ionic liquid intermediate and silica to react and generate the grafted quaternary phosphonate ionic liquid. The grafted quaternary phosphonate ionic liquid provided by the preparation method of the grafted quaternary phosphonate ionic liquid can be used as the CO2 adsorbent alone and can also be used along with other adsorption materials; and compared with the silica gel supported 1-butyl-3-methylimidazolium tetrafluoroborate ionic liquid which is synthesized by the traditional immersion method and the silica gel supported 1-butyl-3-methylimidazolium tetrafluoroborate ionic liquid which is synthesized by the sol-gel method, the grafted quaternary phosphonate ionic liquid has larger cumulative specific surface area and better CO2 adsorption property.