CN105923647A - Preparation method of cuprous oxide nano crystal assembly - Google Patents
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- CN105923647A CN105923647A CN201610230153.4A CN201610230153A CN105923647A CN 105923647 A CN105923647 A CN 105923647A CN 201610230153 A CN201610230153 A CN 201610230153A CN 105923647 A CN105923647 A CN 105923647A
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Abstract
The invention belongs to the technical field of metal oxide preparation, and relates to a preparation method of a cuprous oxide nano crystal assembly. By adopting a low temperature liquid phase synthesis technology and using ascorbic acid to reduce a cuprous oxide precursor, cuprous oxide nano crystal assemblies with two different sizes can be prepared. The cuprous oxide nano crystal assemblies can be used to detect ascorbic acid, dopamine, and uric acid. Cuprous oxide nano crystals with a small size can carry out self-assembly to obtain an assembly modified electrode, which has a better selectivity and higher sensitivity on detecting dopamine. Two nano crystal assemblies have an adsorption effect on Congo red; and the smaller cuprous oxide nano crystal assembly has a better adsorption performance. Moreover, the preparation technology is simple, the principle is reliable, the preparation cost is low, the product purity is high, the electromagnetic properties are good, the application range is wide, and the nano crystal assembly is environment-friendly.
Description
Technical field:
The invention belongs to transition metal oxide preparing technical field, relate to a kind of utilization under the conditions of design temperature
One-step synthesis process prepares the method for weak magnetic oxygenated cuprous nanometer crystal assembly.
Background technology:
Red copper oxide is a kind of important in fields such as agricultural, coating, glass, plastics, pottery and Industrial Catalysis
Inorganic Chemicals, be widely used.Such as, the antibacterial in agricultural and the additive in feedstuff, coating work
The coloring agent etc. in anti-fouling agent, glass industry and ceramic industry in industry.Red copper oxide belongs to p-type semiconductor
Material, the band-gap energy low due to it and the high absorption coefficient of light, and its cheap price and hypotoxicity,
Through being used as gas sensor, high efficiency photocatalyst, eelctro-catalyst and heterogeneous catalyst；Along with synthetic technology
Developing rapidly, the preparation of cuprous nano material has been achieved with rapid progress, many method such as solvent thermal/water
The methods such as thermal synthesis and low temperature liquid phase synthesis have had been reported for multiple cuprous nano material, including multiaspect
The synthesis of body, thin film, nanocages, hollow ball, loose structure etc..Currently, inorganic nano-crystal cluster/assembling
The primary reconstruction preparation of body focuses primarily upon magnetic Nano material, and reaction condition is the harshest, such as synthesis temperature
Spend higher, the response time is longer.The most under cryogenic, weak magnetic or non-is realized based on water solution system
The preparation of the nanocrystalline cluster/assembly of magnetic inorganic still faces significant challenge.Therefore, research cuprous nano
The preparing technique process of brilliant assembly has broad application prospects and huge economic benefit.
Summary of the invention:
It is an object of the invention to the shortcoming overcoming existing synthetic technology to exist, propose one and utilize Low Temperature Liquid to be harmonious
Becoming technical matters, built by synthesis system, the cuprous nano preparing a kind of submicron or micron-scale is brilliant
Assembly.
To achieve these goals, the present invention passes through low temperature liquid phase synthetic technology scheme, with ascorbic acid oxygen reduction
Change the principle of cuprous presoma, prepare two kinds of various sizes of cuprous nano crystalline substance assemblies；Its concrete technology
Process comprises the following steps:
Copper sulfate and the ammonium bicarbonate aqueous solution that 30ml concentration is 6mmol that 120ml concentration is 3mmol are existed
There-necked flask is heated with stirring to after mix homogeneously 45-50 DEG C keep 20 minutes, adds 45mmol Vitamin C
Aqueous acid reduces, and reduction reaction collects precipitate after 60 minutes；Again with deionized water precipitate carried out from
Temperature control 50-60 DEG C drying after heart washing, collects the named CNA-1 of precipitate；Again by the sulfur in above-mentioned steps
Acid copper changes the Schweinfurt green that concentration is 3mmol into, and concentration is the ammonium hydrogen carbonate of 12mmol and concentration is 45mmol
Aqueous ascorbic acid, in there-necked flask, after mix homogeneously, the agitating heating time is 90 minutes, use phase
The named CNA-2 of precipitate that same preparation flow obtains；CNA-1 and CNA-2 is respectively two kinds of Red copper oxides
Nanometer crystal assembly sample, its sample purity is more than 98%；By mol ratio and the reaction of regulation and control pre-reaction material
Temperature, prepares various sizes of cuprous nano crystalline substance assembly, and its crystal size is that the crystal grain of 10nm passes through
Being self-assembly of the cuprous nano crystalline substance assembly of 0.6 μm in order, the Red copper oxide of 1.8 μ m in size is received
The brilliant assembly of rice is made up of the Red copper oxide crystal grain that crystal size is 32nm；Two kinds of cuprous nano crystalline substances assemble
Body all has weak ferromagnetism, and the saturation magnetization of itself CNA-1 and CNA-2 is respectively 3.2emu/g and 9.2
emu/g；Cuprous nano crystalline substance assembly has electrocatalysis characteristic to DA, UA and AA, to organic molecule
Having absorption property, have catalytic performance to oxygen reduction reaction, the cuprous nano crystalline substance of relative small size assembles
The electro-catalysis selectivity of body, absorbability and electro-catalysis ability are the most excellent；Cuprous nano crystalline substance assembly is used
Nano material in Multifunction Sensor.
Red copper oxide colloid nanocrystalline assembly prepared by the present invention be formed by cuprous nano crystalline substance
Between the ordered fabrication that driven of noncovalent interaction (including Van der Waals force, magnetic interaction etc.) form；
The smooth surface of two kinds of various sizes of Red copper oxide colloid nanocrystalline assemblies；CNA-1 sample is irregular
Micro-meter scale flowers shape structure, a size of 1.8 ± 0.3 μm, the cuprous nano crystalline substance of large-size pass through
Intert and assemble and formed；CNA-2 sample is rule and the spherical structure of narrower particle size distribution, the granule of CNA-2
Size is less, is 0.6 ± 0.2 μm, CNA-2 sample rough and have a lot of little granule protruding, by
The cuprous nano crystalline substance of reduced size is formed by self assembly the most in order；Red copper oxide product is nanocrystalline
Assembly structure.
Compared with prior art, its preparation technology is simple for the present invention, and principle is reliable, and preparation cost is low, and product is pure
Degree height, electromagnetic property is good, is widely used, and uses environmental friendliness.
Accompanying drawing illustrates:
Fig. 1 is the X-ray diffractogram of (a) CNA-1 and (b) CNA-2 prepared by the present invention.
Fig. 2 is (a, c) CNA-1 and (b, d) scanning electron microscope diagram of CNA-2 prepared by the present invention.
Fig. 3 is the nitrogen adsorption/desorption curve of (A) CNA-1 and (B) CNA-2 prepared by the present invention, (C)
The BJH pore size distribution curve of CNA-1 and (D) CNA-2.
Fig. 4 is the magnetic hysteresis curve (A) of (a) CNA-1 and (b) CNA-2 prepared by the present invention, and (B) is
The partial enlarged drawing of figure (A).
Fig. 5 is that (a) CNA-1/GCE and (b) CNA-2/GCE prepared by the present invention is containing AA, DA respectively
With the cyclic voltammetry curve in UA electrolyte.
Fig. 6 is that (a) CNA-1/GCE and (b) CNA-2/GCE prepared by the present invention contains AA (1 at the same time
Mmol/L), the differential pulse voltammetry curve in DA (0.8mmol/L) and UA (1mmol/L) electrolyte.
Fig. 7 is that (A) CNA-1/GCE of preparing of the present invention and (B) CNA-2/GCE is at AA (1mmol/L)
Constant with UA (1mmol/L) concentration, during change DA concentration (mmol/L) differential pulse voltammetry curve: (a)
0.1；(b)0.2；(c)0.3；(d)0.4；(e)0.5；(f)0.6；(g)0.7；(h)0.8.
Fig. 8 is product of the present invention (A) CNA-1 and (B) CNA-2 UV, visible light to Congo red at dark
Absorption spectrum spectrogram: (a) 0min, (b) 10min, (c) 20min, (d) 30min, (e) 40min,
(f) 50min, (g) 60min, (h) 70min, (i) 80min, (g) 90min, (k) 120min,
(l) 140min, (m) 160min, (n) 180min.
CNA-1 (a) and CNA-2 (b) at dark is bent to the rate of adsorption of Congo red for Fig. 9 product of the present invention
Line.
Figure 10 be (a) CNA-1/GCE of preparing of the present invention and (b) CNA-2/GCE (a, b) oxygen saturated or
(A) cyclic voltammetry curve recorded in c 0.1mol/L KOH solution that () nitrogen is saturated and (B) are linear
Scanning volt-ampere curve.
Detailed description of the invention:
Below by embodiment and combine accompanying drawing and be described further.
Embodiment:
(1) prepared by cuprous nano crystalline substance assembly:
CuSO by 120mL 3mmol4·5H2O solution and 30mL 6mmol NH4HCO3Solution mix homogeneously
After transfer to 50 DEG C of agitating heating 20min of temperature control in the there-necked flask of 200mL, add 15mL 0.9mmol
Ascorbic acid solution, keep stirring under identical heating-up temperature 1h；Then there-necked flask removal is cooled to room
Temperature, collects brick-red precipitate, and with deionized water centrifuge washing and dry, the precipitate sample of collection is named
CNA-1；The synthetic method of CNA-2 is similar with CNA-1, is a difference in that and changes raw material into 3mmol
Cu(CH3COO)2·5H2The NH of O, 12mmol4HCO3And the ascorbic acid of 4.5mmol, change heat time heating time
For 1.5h.
Fig. 1 is the X-ray energy spectrogram of two kinds of products of CNA-1 and CNA-2, and by Tu Ke get, all of product are spread out
Penetrate the standard diffraction peak all with Red copper oxide (JCPDS, No.05-0667), the peak to match, i.e. 29.60 °,
36.52 °, 42.44 °, cuprous with pure zirconia respectively (110) of the diffraction maximum that occurs of 61.54 ° and 73.69 °,
(111), (200), (220) corresponding with (311) face, show that obtained precipitate sample is oxidation Asia
Copper, and there is no any impurity；Diffraction maximum in analysis chart 1 can obtain, the strongest diffraction maximum ((111) of CNA-2
Face) wider, and the diffraction maximum in CNA-1 (111) face point and narrow, crystallization chi nanocrystalline in CNA-1 is described
Very little bigger；According to thanking to Le formula, half-peak breadth based on (111) crystallographic plane diffraction peak can be calculated in CNA-1
Nanocrystalline crystalline size is 32nm, and crystalline size nanocrystalline in CNA-2 is 10nm；
Fig. 2 is the scanning electron microscope diagram of Red copper oxide, Fig. 2 a, CNA-1 sample be irregular
Micro-meter scale flowers shape structure, size is about 1.8 ± 0.3 μm；Fig. 2 c by amplification is visible, flowers
The Red copper oxide sample of shape micron-scale by the cuprous nano crystalline substance of reduced size by intert assemble and
Formed；CNA-2 sample is then more regular and the spherical structure (Fig. 2 b) of narrower particle size distribution, statistics
Analyze and find that the particle size of CNA-2 is less, be 0.6 ± 0.2 μm；Can clearly see from Fig. 2 d amplified
The surface observing CNA-2 sample is not the most the most smooth and has a lot of little granule protruding, shows CNA-2
It is to be formed by self assembly the most in order by the cuprous nano crystalline substance of reduced size；By prepared sample
Scanning electron microscope diagram is it can be seen that gained Red copper oxide product is nanometer crystal assembly structure；
Fig. 3 is nitrogen adsorption/desorption curve and the BJH pore size distribution curve of CNA-1 and CNA-2；Such as figure
Shown in 3, the absorption/desorption curve of CNA-1 and CNA-2 is IV type, and has time stagnant circle of H1 type；
The average pore size of CNA-1 and CNA-2 is respectively 23.4nm and 13.2nm, shows to be synthesized by this system
Red copper oxide is meso-hole structure, and this result is that the structure of cuprous nano crystalline substance assembly determines and provides support；
Experiment records the specific surface area of CNA-1 and CNA-2 and pore volume is respectively 3.0m2/ g and 0.018cm3/g
And 20.0m2/ g and 0.066cm3/ g, this with sem observation to conclusion match；
(2) magnetic performance of cuprous nano crystalline substance assembly measures:
Fig. 4 is the room temperature hysteresis curve of CNA-1 and CNA-2, by vibrating specimen magnetometer in magnetic field intensity is
1.4×104Gained is measured under Oe；Fig. 4 A is that CNA-1 and CNA-2 sample is in the range of whole magnetic field intensity
Magnetic property curve；CNA-1 sample shows the hysteresis curve typically with saturation magnetization, and
Although the hysteresis curve of CNA-2 sample less meets with conventional shape, however still show compared with fractional value saturated
The intensity of magnetization；From hysteresis curve partial enlarged view (Fig. 4 B), the magnetization of CNA-1 and CNA-2 is bent
Line all demonstrates a relatively small B-H loop, and this shows that CNA-1 and CNA-2 sample is weak ferromagnetism；
(3) preparation of modified electrode:
It is the suspension of 1.5mg/mL with secondary water and cuprous nano crystalline substance assembly configuration concentration, uniformly divides
Take 10 μ L after Saning to be added drop-wise on glass-carbon electrode, under room temperature be dried, be respectively designated as CNA-1/GCE and
CNA-2/GCE；
(4) electrocatalysis characteristic of Red copper oxide modified electrode measures:
Fig. 5 utilizes two kinds of Red copper oxide assembly modified electrode Ascorbic Acids of cyclic voltammetric technique study
(AA), dopamine (DA) and the electro catalytic activity of uric acid (UA)；The oxidation peak of DA and UA is obvious,
And the oxidation peak of AA is wider and catalytic current is relatively low；Comparison diagram 5a and b, AA containing same concentrations,
In the solution of DA or UA, the peak point current of CNA-2/GCE is significantly greater than CNA-1/GCE, shows CNA-2/GCE
There is more preferable electro catalytic activity；
Fig. 6 represents in the case of ascorbic acid, dopamine and three kinds of biomolecule of uric acid coexist, CNA-2/GCE
DA and UA can be detected simultaneously, and CNA-1/GCE has been merely able to the detection to DA, this and the survey of Fig. 5
Test result is consistent；
Fig. 7 is CNA-1/GCE (A) and CNA-2/GCE (B) is at AA (1mmol/L) and UA (1mmol/L)
Concentration is constant, changes DPV curve obtained during DA concentration；Illustration from Fig. 7, Red copper oxide
The catalysis peak point current of assembly modified electrode is along with the most linear increase of the increase of DA concentration, CNA-1/GCE
It is respectively r=0.9935 and r=0.9827 with the linearly dependent coefficient of CNA-2/GCE；The existence of AA and UA is not
The detection of DA can be affected, although the detection of AA, UA can be affected by DA；Comparison diagram 7A and B is visible, CNA-2/GCE
In three kinds of mixed liquors, the detection to DA has more preferable selectivity and higher sensitivity than CNA-1/GCE；
(5) absorption property of Red copper oxide modified electrode measures:
Transition metal oxide can remove debirs by absorption or catalytic property subsequently from aqueous solution.This
Embodiment with Congo red as adsorbate, the absorption property of prepared cuprous nano crystalline substance assembly；Experiment knot
Fruit shows, cuprous nano crystalline substance assembly is in dark condition, natural optical condition and xenon lamp (300W) condition
Under identical to the absorption result of Congo red, show that Congo red is mainly adsorbed onto Red copper oxide by adsorption and receives
On the brilliant assembly of rice；Fig. 8 shows that CNA-1 and CNA-2 all has obvious adsorption to Congo red；Fig. 9
It is shown that adsorption efficiency that the Adsorption experimental results according to Fig. 8 the described change curve with adsorption time；
CNA-2 has more preferable absorbability than CNA-1, and when adsorption time is 2h, CNA-1 adsorbance base
Originally maximum (1.22mg/10mg, Congo red/Red copper oxide) is reached；And CNA-2 is in the 3h of experiment
Saturated still without reaching to adsorb, and its absorbability is more weak；By CNA-2 has less cuprous nano
The loose structure that brilliant and specific group assembling structure is formed is caused；
(6) the hydrogen reduction performance measurement of Red copper oxide modified electrode:
The reaction mechanism of cuprous oxide catalysis oxygen reduction is: in controlled potential range, along with single order oxygen
The existence of dividing potential drop, it should have a speed limit electron transfer adsorption of oxygen to form the superoxides (public affairs of Red copper oxide
Formula 8-1) process, relate to the concurrent reaction (formula 8-2) of a water simultaneously；(figure in the saturated electrolyte of nitrogen
10A), the cyclic voltammetry curve of modified electrode does not has characteristic peak substantially, and in the saturated electrolyte of oxygen
-0.46V has significant negative electrode peak to occur, Figure 10 B linear sweep voltammetry curve also leads to the same conclusion,
Show that cuprous nano crystalline substance assembly has potential catalysis activity to oxygen reduction；
Cu2O-O2+e-→Cu2O-O2 - (1)
Cu2O-O2+H2O+e-→Cu2O-HO2+OH- (2)。
Claims (2)
1. the preparation method of a cuprous nano crystalline substance assembly, it is characterised in that: pass through
Low temperature liquid phase synthetic technology scheme, with the principle of the cuprous presoma of ascorbic acid reduction-oxidation, system
Standby two kinds of various sizes of cuprous nano crystalline substance assemblies, its specific embodiment includes following
Step:
It is the bicarbonate of 6mmol by copper sulfate and 30ml concentration that 120ml concentration is 3mmol
Aqueous ammonium is heated with stirring to 45-50 DEG C in there-necked flask and keeps 20 minutes after mix homogeneously,
Adding the reduction of 45mmol aqueous ascorbic acid, reduction reaction collects precipitate after 60 minutes；
Temperature control 50-60 DEG C drying after precipitate being centrifuged washing with deionized water again, it is heavy to collect
The named CNA-1 of shallow lake thing；It is 3mmol Schweinfurt green that copper sulfate in above-mentioned steps changes into concentration again,
Ammonium bicarbonate concentration is 12mmol and aqueous ascorbic acid concentration is 45mmol, three mouthfuls of burnings
In Ping, after mix homogeneously, the agitating heating time is 90 minutes, uses identical preparation flow to obtain
The named CNA-2 of precipitate.
2. according to the preparation method of cuprous nano crystalline substance assembly described in claim 1, its
It is characterised by: the cuprous nano crystalline substance assembly of preparation includes two kinds of physical dimensions, orders respectively
Entitled CNA-1 and CNA-2, wherein, CNA-1 is irregular micro-meter scale flowers shape structure,
A size of 1.8 ± 0.3 μm, are passed through by the cuprous nano crystal grain that crystal size is 32nm
Intert to assemble and formed；CNA-2 is rule and the spherical structure of narrower particle size distribution, a size of
0.6 ± 0.2 μm, by the cuprous nano crystal grain that crystal size is 10nm by the most in order
Being self-assembly of, CNA-2 is rough and has granule protruding；CNA-1 and CNA-2 is saturated
The intensity of magnetization is respectively 3.2emu/g and 9.2emu/g, and purity is more than 98%, it is possible to antagonism
Bad hematic acid, dopamine and uric acid electro-catalysis, adsorb organic molecule, and catalytic oxidation-reduction reacts；Its
Physical dimension is inversely proportional to electro-catalysis selectivity, absorbability and electro-catalysis ability；For many merits
The nano material of energy sensor.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106902361A (en) * | 2017-03-20 | 2017-06-30 | 厦门大学 | Magnetic resonance contrast agent and preparation based on blending ingredients magnetic nanoparticle assembly |
| CN111200134A (en) * | 2020-02-18 | 2020-05-26 | 金陵科技学院 | Cuprous oxide film and application thereof in fuel cell |
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| CN111200134A (en) * | 2020-02-18 | 2020-05-26 | 金陵科技学院 | Cuprous oxide film and application thereof in fuel cell |
| CN111200134B (en) * | 2020-02-18 | 2022-05-20 | 金陵科技学院 | Cuprous oxide film and application thereof in fuel cell |
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