CN106241855A - A kind of preparation method of cuprous sulfide nanometer rose flower - Google Patents

A kind of preparation method of cuprous sulfide nanometer rose flower Download PDF

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CN106241855A
CN106241855A CN201610630960.5A CN201610630960A CN106241855A CN 106241855 A CN106241855 A CN 106241855A CN 201610630960 A CN201610630960 A CN 201610630960A CN 106241855 A CN106241855 A CN 106241855A
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preparation
solution
copper rod
flower
distilled water
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陈年宝
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Fuhua Novel Material Co Ltd Of Section In Hefei
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Fuhua Novel Material Co Ltd Of Section In Hefei
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G3/00—Compounds of copper
    • C01G3/12—Sulfides
    • 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
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/30—Particle morphology extending in three dimensions
    • C01P2004/45—Aggregated particles or particles with an intergrown morphology

Abstract

The invention provides the preparation method of a kind of cuprous sulfide nanometer rose flower, comprise the following steps: the cleaning treatment of (1) copper rod: copper rod acetone, ethanol, the dilute hydrochloric acid of 2mol/L, distilled water are cleaned under Ultrasonic Conditions；(2) cuprous sulfide nanometer rose flower preparation: under room temperature, being dissolved in respectively in distilled water in monovalence silver salt, sulfur source, stirring makes it dissolve；Cleaned described copper rod is put in the test tube of 5mL, instill monovalence silver salt solution with glue head dropper, then instill sulfur source solution, rock test tube and make two solution uniformly mix, test tube is airtight, react 10min ~ 12h under room temperature；After reaction terminates, there is the copper rod of atrament with distilled water flushing growth, naturally dry,.Preparation method of the present invention, repeatability is high, easy and simple to handle, synthesizes low cost, is suitable for preparation of industrialization；Prepared nanometer rose flower specific surface area is big, can be fully contacted with determinand as sensor material.

Description

A kind of preparation method of cuprous sulfide nanometer rose flower
Technical field
The present invention relates to the preparation method of a kind of cuprous sulfide nanometer rose flower.
Background technology
Cholesterol has physiological function widely in vivo, and its concentration is a key index in numerous disease, as dynamic Arteries and veins hardening, phlebothrombosis and cholelithiasis.Therefore find a kind of quickly, the method for Accurate Determining cholesterol be significantly, And we are attempting to a kind of Cholesterol Biosensor reliably of exploitation, owing to it is simple to operate, have Gao Xuan Selecting property and low cost and other advantages, the Cholesterol Biosensor measuring electric current is extensively paid close attention to by people.Wherein, biology is studied emphatically Enzyme sensor, has high sensitivity and good selectivity, but in use the activity of enzyme can reduce, owing to it is intrinsic Unstability and the activity of enzyme be easily subject to pH value, temperature and the impact of poisonous chemical substance, in fixation procedure, enzyme holds Changeableness.Additionally, the repeatability of biological enzyme sensor is not fine, need to improve further.In order to overcome cholesterol enzyme to sense The shortcoming of device, it is necessary to design and manufacture the cholesterol sensor of non-enzymatic, it has the most attractive several advantage, as manufactured Simply, low cost, stable, favorable reproducibility, do not disturbed by the limit of oxygen.
In recent years, along with the development of nano material and it is widely used in different field, partly leading of nanoscale Body is studied widely.As a kind of important p-type semiconductor, Cu2The band gap of S is 1.2 eV, is widely used in raw Thing sensor, solaode, cold cathode emitters, photovoltaic application.It is known that the form of material is to its performance impact very Greatly, so needing to control to synthesize Cu by various methods2The size of S, shape.At present, Cu2S nano material is typically by making The method assisted with gas-solid reaction or surfactant makes.
The Chinese patent of Publication No. CN102807248B discloses the preparation method of a kind of nano-array cuprous sulfide, bag Include following steps: under conditions of room temperature, stirring, mixed homogeneously with ethylenediamine solution by deionized water, then immerse copper rod, ultrasonic Thiourea solution and polyvinylpyrrolidone (PVP), airtight placement 6 ~ 24 hours is added after 20 minutes；Cleaning, drying at room temperature is i.e. Can.The Chinese patent of Publication No. CN101544395A discloses a kind of alcohol heat and sends the preparation of cuprous sulfide nano material processed Methods etc., the power consumption of these methods is high, reaction complexity, and have also uses poisonous reagent, and this kind of technique does not adapt to the modern times and receives The development of rice material.
Therefore, preparation one nanocrystal the most effective, eco-friendly forms combination electrode and realizes non-enzymatic monitoring gallbladder The method of sterin, significant, currently used Cu2S nanometer sheet is carried out the technology of cholesterol detection and is rarely had report.
Summary of the invention
For defect of the prior art, it is an object of the invention to provide the preparation side of a kind of cuprous sulfide nanometer rose flower Method, described preparation method is simple to operate, with low cost, has preferable using value.
The present invention solves technical problem and adopts the following technical scheme that
The present invention relates to the preparation method of a kind of cuprous sulfide nanometer rose flower, comprise the following steps:
(1) cleaning treatment of copper rod: copper rod is used respectively acetone, ethanol, the dilute hydrochloric acid of 2mol/L, distilled water in Ultrasonic Conditions Lower cleaning；
(2) preparation of cuprous sulfide nanometer rose flower: at room temperature, being dissolved in distilled water by monovalence silver salt, stirring makes described Monovalence silver salt fully dissolves, standby；At room temperature, being dissolved in distilled water in sulfur source, stirring makes described monovalence silver salt the most molten Solve, standby；Cleaned described copper rod is put in the test tube of 5mL, instill monovalence silver salt solution with glue head dropper, then instill system The sulfur source solution got ready, rocks test tube and makes two solution uniformly mix and two kinds of liquor capacities are than for 1:1, by airtight for small test tube, React certain time under room temperature；After reaction terminates, there is the copper rod of atrament with distilled water flushing growth, naturally dry, to obtain final product Described nanocrystal.
Preferably, in described step (1), the size of copper rod is cross-sectional area 2.5 mm2, length 4 cm.
Preferably, described monovalence silver salt is AgNO3, described sulfur source solution is sodium sulfide solution.
Preferably, the AgNO of preparation in described step (2)3The concentration of solution is 0.001 mol/L ~ 0.1mol/L, described The concentration of sodium sulfide solution is 0.01 mol/L ~ 0.1mol/L.
Preferably, the AgNO of preparation in described step (2)3The concentration of solution is 0.05mol/L, described sodium sulfide solution Concentration is 0.1mol/L.
Preferably, the AgNO of dropping in described step (2)3Solution with the ratio of the amount of the material of solute in sodium sulfide solution is 1:10~5:1。
Preferably, the AgNO of dropping in described step (2)3Solution with the ratio of the amount of the material of solute in sodium sulfide solution is 1:2~1:10。
Preferably, AgNO in described step (2)3Solution, sodium sulfide are 10min ~ 12h with the response time of copper rod.
Preferably, AgNO in described step (2)3Solution, sodium sulfide are 6h with the response time of copper rod.
Compared with prior art, the present invention has a following beneficial effect:
(1) preparation method of the present invention is carried out at normal temperatures, consumes energy low, and environmentally safe meets the 12 of Green Chemistry Big principle.
(2) copper rod used in the present invention, due to the electric conductivity that it is good, and low cost, be suitable to industrial applications.
(3) preparation method of the present invention, repeatability is high, and material high detection performance is easy and simple to handle, consumes energy low, synthesis Low cost, is suitable for industrial extensive preparation；Prepared cuprous sulfide nanometer rose flower has bigger specific surface area, Can be fully contacted with determinand as sensor material, make electrocatalytic reaction the most efficient.
Accompanying drawing explanation
By the detailed description non-limiting example made with reference to the following drawings of reading, the further feature of the present invention, Purpose and advantage will become more apparent upon:
Fig. 1 is powder x-ray diffraction (XRD) figure of the cuprous sulfide nanometer rose flower of embodiment 1 preparation；
Fig. 2 is the electron scanning micrograph of the low enlargement ratio of the cuprous sulfide nanometer rose flower of embodiment 1 preparation (SEM)；
Fig. 3 is the electron scanning micrograph of the high magnification of the cuprous sulfide nanometer rose flower of embodiment 1 preparation (SEM)；
Fig. 4 is that the cuprous sulfide nanometer rose of embodiment 1 preparation spends the cyclic voltammogram that cholesterol carries out Electrochemical Detection (CV)；
Wherein, curve 1 is the cyclic voltammetry curve not adding cholesterol in 7.0 acetate buffer solutions for pH,
Curve 2 is the cyclic voltammetry curve adding 0.5mM cholesterol in 7.0 acetate buffer solutions for pH,
Curve 3 is the cyclic voltammetry curve having added 1mM cholesterol in 7.0 acetate buffer solutions for pH；
Fig. 5 is copper rod and naked copper carries out the time current curve of Electrochemical Detection (i-t) to cholesterol.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is expanded on further.These embodiments are merely to illustrate the present invention and need not In limiting the scope of the present invention.The experimental technique of unreceipted actual conditions in the following example, generally according to normal condition, such as Sambrook equimolecular is cloned: laboratory manual (New York:Cold Spring Harbor Laboratory Press, 1989) condition described in, or according to the condition proposed by manufacturer.
Embodiment 1:
The present embodiment relates to the preparation method of a kind of cuprous sulfide nanometer rose flower, comprises the following steps:
(1) cleaning treatment of copper rod: copper rod is used respectively acetone, ethanol, the dilute hydrochloric acid of 2mol/L, distilled water in Ultrasonic Conditions Lower cleaning；
(2) preparation of cuprous sulfide nanometer rose flower: at room temperature, 0.85g silver nitrate is dissolved in 100mL distilled water, stirs Mix and make it fully dissolve, be configured to the silver nitrate solution of 0.05mol/L, standby；0.78g sodium sulfide is dissolved in the steaming of 100ml Distilled water is made into the sodium sulfide solution of 0.1mol/L, standby；It is 2.5 mm2 by cleaned cross-sectional area, a length of 4cm's Copper rod is put in the test tube of 5mL, and the 0.05mol/L silver nitrate solution glue head dropper taking 0.5ml instills in test tube, then instills The 0.1mol/L sodium sulfide solution of 0.5ml, rocks test tube and makes two solution uniformly mix, and small test tube is airtight, reacts 6 at normal temperatures Hour；After reaction terminates, there is the copper rod of atrament with distilled water flushing growth, naturally dry, obtain target product.
The target product that the present embodiment obtains is cuprous sulfide nanometer, as shown in Figure 1；And the pattern of gained cuprous sulfide by Nanometer sheet is self-assembled into rose-shaped being grown on copper rod, as shown in Figures 2 and 3.And cuprous sulfide nanometer is prepared by the present invention Flos Rosae Rugosae carries out the detection of electrochemical sensing character, and cholesterol detection content in pH is 7.0 acetate buffer solutions, such as Fig. 4 and Fig. 5 Shown in, its result shows that this electrode really has good electrochemical catalysis effect to cholesterol, and can be directly used as fuel Battery.
Embodiment 2:
The present embodiment relates to the preparation method of a kind of cuprous sulfide nanometer rose flower, comprises the following steps:
(1) cleaning treatment of copper rod: copper rod is used respectively acetone, ethanol, the dilute hydrochloric acid of 2mol/L, distilled water in Ultrasonic Conditions Lower cleaning；
(2) preparation of cuprous sulfide nanometer rose flower: at room temperature, 0.85g silver nitrate is dissolved in 100mL distilled water, stirs Mix and make it fully dissolve, be configured to the silver nitrate solution of 0.05mol/L, standby；0.78g sodium sulfide is dissolved in the steaming of 100ml Distilled water is made into the sodium sulfide solution of 0.1mol/L, standby；It is 2.5 mm2 by cleaned cross-sectional area, a length of 4cm's Copper rod is put in the test tube of 5mL, and the 0.05mol/L silver nitrate solution glue head dropper taking 0.5ml instills in test tube, then instills The 0.1mol/L sodium sulfide solution of 0.5ml, rocks test tube and makes two solution uniformly mix, and small test tube is airtight, reacts at normal temperatures 10min；After reaction terminates, there is the copper rod of atrament with distilled water flushing growth, naturally dry, obtain target product.
The present embodiment is short due to the response time, and gained target product only has sparse nanometer sheet, does not generate rose-shaped Cuprous sulfide.
Embodiment 3:
The present embodiment relates to the preparation method of a kind of cuprous sulfide nanometer rose flower, comprises the following steps:
(1) cleaning treatment of copper rod: copper rod is used respectively acetone, ethanol, the dilute hydrochloric acid of 2mol/L, distilled water in Ultrasonic Conditions Lower cleaning；
(2) preparation of cuprous sulfide nanometer rose flower: at room temperature, 0.85g silver nitrate is dissolved in 100mL distilled water, stirs Mix and make it fully dissolve, be configured to the silver nitrate solution of 0.05mol/L, standby；0.78g sodium sulfide is dissolved in the steaming of 100ml Distilled water is made into the sodium sulfide solution of 0.1mol/L, standby；It is 2.5 mm2 by cleaned cross-sectional area, a length of 4cm's Copper rod is put in the test tube of 5mL, and the 0.05mol/L silver nitrate solution glue head dropper taking 0.5ml instills in test tube, then instills The 0.1mol/L sodium sulfide solution of 0.5ml, rocks test tube and makes two solution uniformly mix, and small test tube is airtight, reacts at normal temperatures 12h；After reaction terminates, there is the copper rod of atrament with distilled water flushing growth, naturally dry, obtain target product.
The present embodiment is long due to the response time, and the nanometer sheet of prepared target product is thicker and flocks together.
Embodiment 4:
The present embodiment relates to the preparation method of a kind of cuprous sulfide nanometer rose flower, comprises the following steps:
(1) cleaning treatment of copper rod: copper rod is used respectively acetone, ethanol, the dilute hydrochloric acid of 2mol/L, distilled water in Ultrasonic Conditions Lower cleaning；
(2) preparation of cuprous sulfide nanometer rose flower: at room temperature, 0.17g silver nitrate is dissolved in 100mL distilled water, stirs Mix and make it fully dissolve, be configured to the silver nitrate solution of 0.01mol/L, standby；0.78g sodium sulfide is dissolved in the steaming of 100ml Distilled water is made into the sodium sulfide solution of 0.1mol/L, standby；It is 2.5 mm by cleaned cross-sectional area2, a length of 4cm's Copper rod is put in the test tube of 5mL, and the 0.01mol/L silver nitrate solution glue head dropper taking 0.5ml instills in test tube, then instills The 0.1mol/L sodium sulfide solution of 0.5ml, rocks test tube and makes two solution uniformly mix, and small test tube is airtight, reacts at normal temperatures 6h；After reaction terminates, there is the copper rod of atrament with distilled water flushing growth, naturally dry, obtain target product.
The pattern of the cuprous sulfide nanometer rose flower that the present embodiment prepares is similar to embodiment 1.
Embodiment 5:
The present embodiment relates to the preparation method of a kind of cuprous sulfide nanometer rose flower, comprises the following steps:
(1) cleaning treatment of copper rod: copper rod is used respectively acetone, ethanol, the dilute hydrochloric acid of 2mol/L, distilled water in Ultrasonic Conditions Lower cleaning；
(2) preparation of cuprous sulfide nanometer rose flower: at room temperature, 0.017g silver nitrate is dissolved in 100mL distilled water, stirs Mix and make it fully dissolve, be configured to the silver nitrate solution of 0.001mol/L, standby；0.78g sodium sulfide is dissolved in the steaming of 100ml Distilled water is made into the sodium sulfide solution of 0.1mol/L, standby；It is 2.5 mm by cleaned cross-sectional area2, a length of 4cm's Copper rod is put in the test tube of 5mL, and the 0.001mol/L silver nitrate solution glue head dropper taking 0.5ml instills in test tube, then instills The 0.1mol/L sodium sulfide solution of 0.5ml, rocks test tube and makes two solution uniformly mix, and small test tube is airtight, reacts at normal temperatures 6h；After reaction terminates, there is the copper rod of atrament with distilled water flushing growth, naturally dry, obtain target product.
The target product that the present embodiment prepares only has some irregular nanometer sheet to be grown in substrate, is formed without Flos Rosae Rugosae Flower-shaped.
Embodiment 6:
The present embodiment relates to the preparation method of a kind of cuprous sulfide nanometer rose flower, comprises the following steps:
(1) cleaning treatment of copper rod: copper rod is used respectively acetone, ethanol, the dilute hydrochloric acid of 2mol/L, distilled water in Ultrasonic Conditions Lower cleaning；
(2) preparation of cuprous sulfide nanometer rose flower: at room temperature, 1.7g silver nitrate is dissolved in 100mL distilled water, stirring Make it fully dissolve, be configured to the silver nitrate solution of 0.1mol/L, standby；0.78g sodium sulfide is dissolved in the distilled water of 100ml In be made into the sodium sulfide solution of 0.1mol/L, standby；It is 2.5 mm by cleaned cross-sectional area2, the copper rod of a length of 4cm Putting in the test tube of 5mL, the 0.1mol/L silver nitrate solution glue head dropper taking 0.5ml instills in test tube, then instills 0.5ml's 0.1mol/L sodium sulfide solution, rocks test tube and makes two solution uniformly mix, and small test tube is airtight, reacts 6h at normal temperatures；Reaction After end, there is the copper rod of atrament with distilled water flushing growth, naturally dry, obtain target product.
The nanometer sheet of the target product that the present embodiment prepares can become thicker, and is packed together.
Embodiment 7:
The present embodiment relates to the preparation method of a kind of cuprous sulfide nanometer rose flower, comprises the following steps:
(1) cleaning treatment of copper rod: copper rod is used respectively acetone, ethanol, the dilute hydrochloric acid of 2mol/L, distilled water in Ultrasonic Conditions Lower cleaning；
(2) preparation of cuprous sulfide nanometer rose flower: at room temperature, 0.85g silver nitrate is dissolved in 100mL distilled water, stirs Mix and make it fully dissolve, be configured to the silver nitrate solution of 0.05mol/L, standby；0.078g sodium sulfide is dissolved in the steaming of 100ml Distilled water is made into the sodium sulfide solution of 0.01mol/L, standby；It is 2.5 mm by cleaned cross-sectional area2, a length of 4cm's Copper rod is put in the test tube of 5mL, and the 0.05mol/L silver nitrate solution glue head dropper taking 0.5ml instills in test tube, then instills The 0.01mol/L sodium sulfide solution of 0.5ml, rocks test tube and makes two solution uniformly mix, and small test tube is airtight, reacts at normal temperatures 6h；After reaction terminates, there is the copper rod of atrament with distilled water flushing growth, naturally dry, obtain target product.
The nanometer sheet of target product that the present embodiment prepares can be the shortest, be rolled into one little flower-shaped.
Embodiment 8:
The present embodiment relates to the preparation method of a kind of cuprous sulfide nanometer rose flower, comprises the following steps:
(1) cleaning treatment of copper rod: copper rod is used respectively acetone, ethanol, the dilute hydrochloric acid of 2mol/L, distilled water in Ultrasonic Conditions Lower cleaning；
(2) preparation of cuprous sulfide nanometer rose flower: at room temperature, 0.85g silver nitrate is dissolved in 100mL distilled water, stirs Mix and make it fully dissolve, be configured to the silver nitrate solution of 0.05mol/L, standby；1.56g sodium sulfide is dissolved in the steaming of 100ml Distilled water is made into the sodium sulfide solution of 0.2mol/L, standby；It is 2.5 mm by cleaned cross-sectional area2, a length of 4cm's Copper rod is put in the test tube of 5mL, and the 0.05mol/L silver nitrate solution glue head dropper taking 0.5ml instills in test tube, then instills The 0.2mol/L sodium sulfide solution of 0.5ml, rocks test tube and makes two solution uniformly mix, and small test tube is airtight, reacts at normal temperatures 6h；After reaction terminates, there is the copper rod of atrament with distilled water flushing growth, naturally dry, obtain target product.
The nanometer sheet of target product that the present embodiment prepares can be the shortest, be rolled into one little flower-shaped.
By above-described embodiment it can be seen that when the concentration of silver nitrate solution is too low or when the response time is too short, institute The nanometer product obtained only has some irregular nanometer sheet to be grown in substrate, is formed without rose-shaped, works as silver nitrate concentration Excessive or time the response time is long, the nanometer wafer of generation is thickening, and is packed together.Only when silver nitrate solution and sulfuration In sodium solution, the ratio of the amount of the material of solute is 1:2 ~ 1:10, and during normal-temperature reaction 6h, the nanocrystalline sector-meeting obtained generates uniform Rose-shaped.Using preparation method of the present invention, technique is simple, synthesizes low cost, and reaction condition is gentle, gained dendrite ratio More uniform, it is suitable for industrialized production.
Above the specific embodiment of the present invention is described.It is to be appreciated that the invention is not limited in above-mentioned Particular implementation, those skilled in the art can make various deformation or amendment within the scope of the claims, this not shadow Ring the flesh and blood of the present invention.

Claims (9)

1. the preparation method of a cuprous sulfide nanometer rose flower, it is characterised in that: comprise the following steps:
(1) cleaning treatment of copper rod: copper rod is used respectively acetone, ethanol, the dilute hydrochloric acid of 2mol/L, distilled water in Ultrasonic Conditions Lower cleaning；
(2) preparation of cuprous sulfide nanometer rose flower: at room temperature, being dissolved in distilled water by monovalence silver salt, stirring makes described Monovalence silver salt fully dissolves, standby；At room temperature, being dissolved in distilled water in sulfur source, stirring makes described monovalence silver salt the most molten Solve, standby；Cleaned described copper rod is put in the test tube of 5mL, instill monovalence silver salt solution with glue head dropper, then instill system The sulfur source solution got ready, rocks test tube and makes two solution uniformly mix and two kinds of liquor capacities are than for 1:1, by airtight for small test tube, React 5 ~ 8 hours under room temperature；After reaction terminates, there is the copper rod of atrament with distilled water flushing growth, naturally dry, obtain institute State nanocrystal.
The preparation method of cuprous sulfide nanometer rose the most according to claim 1 flower, it is characterised in that: described step (1) The size of middle copper rod is cross-sectional area 2.5 mm2, length 4 cm.
The preparation method of cuprous sulfide nanometer rose the most according to claim 1 flower, it is characterised in that: described monovalence silver salt For AgNO3, described sulfur source solution is sodium sulfide solution.
The preparation method of cuprous sulfide nanometer rose the most according to claim 1 flower, it is characterised in that: described step (2) The AgNO of middle preparation3The concentration of solution is 0.001 mol/L ~ 0.1mol/L, and the concentration of described sodium sulfide solution is 0.01 mol/ L~0.1mol/L。
The preparation method of cuprous sulfide nanometer rose the most according to claim 4 flower, it is characterised in that: described step (2) The AgNO of middle preparation3The concentration of solution is 0.05mol/L, and the concentration of described sodium sulfide solution is 0.1mol/L.
The preparation method of cuprous sulfide nanometer rose the most according to claim 1 flower, it is characterised in that: described step (2) The AgNO of middle dropping3Solution is 1:10 ~ 5:1 with the ratio of the amount of the material of solute in sodium sulfide solution.
The preparation method of cuprous sulfide nanometer rose the most according to claim 6 flower, it is characterised in that: described step (2) The AgNO of middle dropping3Solution is 1:2 ~ 1:10 with the ratio of the amount of the material of solute in sodium sulfide solution.
The preparation method of cuprous sulfide nanometer rose the most according to claim 1 flower, it is characterised in that: described step (2) Middle AgNO3Solution, sodium sulfide are 10min ~ 12h with the response time of copper rod.
The preparation method of cuprous sulfide nanometer rose the most according to claim 8 flower, it is characterised in that: described step (2) Middle AgNO3Solution, sodium sulfide are 6h with the response time of copper rod.
CN201610630960.5A 2016-08-04 2016-08-04 A kind of preparation method of cuprous sulfide nanometer rose flower Pending CN106241855A (en)

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CN108682857B (en) * 2018-06-14 2020-11-06 商丘师范学院 Preparation method of porous flower flake lithium battery positive electrode material
CN111320200A (en) * 2020-03-21 2020-06-23 上海健康医学院 Cuprous sulfide nano material for electrochemical sensor and preparation method thereof
CN111320200B (en) * 2020-03-21 2023-03-28 上海健康医学院 Cuprous sulfide nano material for electrochemical sensor and preparation method thereof
CN112279293A (en) * 2020-11-02 2021-01-29 贵州理工学院 Preparation method of copper sulfide nano material
CN112279293B (en) * 2020-11-02 2023-08-25 贵州理工学院 Preparation method of copper sulfide nano material

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