CN102653412B - Cuprous oxide fifty-surface crystallite as well as preparation method and application thereof - Google Patents
Cuprous oxide fifty-surface crystallite as well as preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a cuprous oxide fifty-surface crystallite as well as a preparation method and application thereof. According to the preparation method, copper acetate monohydrate is used as a copper source, water, strong base and glucose are respectively used as a solvent, a precipitator and a reducing agent, the reaction temperature is 50-80 DEGC, and the cuprous oxide fifty-surface crystallite is obtained through an oxidation-reduction reaction. The cuprous oxide fifty-surface crystallite prepared according to the invention is formed by closing 24 high-index crystal faces ({211} crystal face or {311} crystal face), 12 {110} crystal faces, 8 {111} crystal faces and 6 {100} crystal faces, and comprises 120 ridges and 72 vertexes. The method has the advantages of gentle reaction condition, simple equipment, convenient operation, low cost, high yield, environment protection, suitability for large-scale industrial production and the like. The crystallite has excellent visible light catalytic activity, and has wide application prospect in aspects of solar batteries, hydrogen production, lithium ion batteries, biosensors and the like.
Description
Technical field
The invention belongs to solution chemistry preparation method category, relate to a kind of Red copper oxide five decahedron crystallites and preparation method thereof and application.
Background technology
In recent years, the research of nano material and technology of preparing thereof have caused the generally attention of countries in the world.The isoparametric effectively and accurately regulation and control of composition, size, shape and exposure crystal face to nano material can improve the performances such as it is optical, electrical, magnetic.Synthetic have the micro-nano functional materials that exposes at high proportion high miller index surface and become just gradually one of study hotspot of micro Nano material technology of preparing.High miller index surface contains highdensity atomic steps and dangling bonds conventionally, has open surface tissue, compared with low index crystal face, has more excellent reactive behavior, particularly catalytic reaction activity.Therefore the catalystic material that preparation has a high miller index surface is the effective way that significantly improves catalyst performance.Recently, the grandson of Xiamen University generation has just waited people to adopt a kind of new electrochemical process to prepare first by { 730}, { 520}, { 210}, { the tetrahexahedron Pt nanocrystal grain catalyzer that the high miller index surface such as 310} surrounds, activity and the stability of platinum nano catalyst are significantly improved, be significant and using value (N.Tian in fields such as the energy, catalysis, material, chemical industry, et al.Science 2007,316,732).
Red copper oxide is a kind of typical P-type semiconductor material, has unique optics, electricity and PhotoelectrochemicalProperties Properties, has very large potential using value at aspects such as sun power conversion, environmental catalysis, sensor, lithium ion battery and dielectric devices.Improve by controlling the pattern of Red copper oxide the focus that its performance is all the research of Red copper oxide micro Nano material all the time, and existing a large amount of report.Up to now, the difform Red copper oxide micro-nano granules such as spherical, cubes, octahedron, rhombic dodecahedron has all been designed to be synthesized.But these polyhedrons are mainly by low index face { 100}, { 110} and { 111} sealing forms, and reactive behavior needs further to be improved.This is because with respect to low index crystal face, the surface of high miller index surface can be higher, in crystal growing process along the growth velocity of high miller index surface direction far faster than low index crystal face, cause high miller index surface to be tending towards disappearing, finally can only obtain the crystal that low index crystal face surrounds.In addition, in order to control size and the pattern of Red copper oxide, in synthetic process, conventionally add some special organic additive to make some crystal face of crystal growing process produce preferred orientation.But plane of crystal is adsorbed by these organic additives, the follow-up study of its various performances and application are more widely greatly limited.
Summary of the invention
The object of this invention is to provide a kind of Red copper oxide five decahedron crystallites and preparation method thereof and application.
Red copper oxide five decahedron crystallites provided by the invention, by 24 high miller index surfaces, 12, { { { sealing of 100} crystal face forms, and has 120 ribs and 72 summits for 111} crystal face and 6 for 110} crystal face, 8; Described high miller index surface is { 211} crystal face or { 311} crystal face.
In above-mentioned Red copper oxide five decahedron crystallites, the median size of described Red copper oxide five decahedron crystallites is 1-5 micron, specifically can be 1.8-4.2 micron, 1.8-3.7 micron, 1.8-3.6 micron, 1.8-2.3 micron, 2.3-4.2 micron, 2.3-3.7 micron, 2.3-3.6 micron, 3.6-4.2 micron or 3.7-4.2 micron, preferably 1.5-2.5 micron.When selecting aqueous sodium hydroxide solution as precipitation agent in following method, the high miller index surface in gained Red copper oxide five decahedron crystallites is { 211} crystal face; When selecting potassium hydroxide aqueous solution as precipitation agent in following method, the high miller index surface in gained Red copper oxide five decahedron crystallites is { 311} crystal face.
The method of the described Red copper oxide five decahedron crystallites of preparation provided by the invention, comprise the steps: using a hydration neutralized verdigris as copper source compound, precipitation agent and reductive agent are mixed and reacted with the described copper source compound aqueous solution, react after complete separation washing is dried and obtain described Red copper oxide five decahedron crystallites; Wherein, described precipitation agent is aqueous sodium hydroxide solution or potassium hydroxide aqueous solution, and described reductive agent is D/W.
In the described reactions steps of aforesaid method, temperature is 50-80 DEG C, preferably 60-70 DEG C, and the time is 4-30 minute, preferably 10-17 minute; In described separating step, various conventional separation methods are all applicable to the method, as can be natural subsidence separation or centrifugation; In described step with centrifugal separation, rotating speed is 1000-5000 rev/min, preferably 2000-3000 rev/min, and radius is 7-10cm, preferably 9-10cm, the time is 2-10 minute, preferably 3-5 minute; In described water-washing step, number of times is 3-7 time; In described baking step, temperature is 25-80 DEG C, preferably 50-60 DEG C, and vacuum tightness is 10-200Pa, preferably 50-100Pa.The concentration of the described copper source compound aqueous solution is 0.1-0.4mol/L, preferably 0.2-0.3mol/L; The concentration of described aqueous sodium hydroxide solution and potassium hydroxide aqueous solution is 2-12mol/L, preferably 6-10mol/L; The concentration of described D/W is 0.5-1mol/L, specifically can be 0.65-0.8mol/L, 0.65-0.75mol/L or 0.75-0.8mol/L, preferably 0.6-0.8mol/L; The consumption of the aqueous solution, precipitation agent and the reductive agent of described copper source compound is respectively 2-15ml: 1-6ml: 0.2-1.5ml, specifically can be 5-10ml: 2-5ml: 0.5-2ml, preferably 5-10ml: 2-5ml: 0.5-1ml.
The above-mentioned method of preparing Red copper oxide five decahedron crystallites, specifically can comprise the steps:
1) the described copper source compound aqueous solution is warming up to after 50-80 DEG C, adds described precipitation agent to react, react the complete suspension liquid that obtains;
2) to described step 1) add described reductive agent to react in gained suspension liquid, react complete and be precipitated, gained precipitation is carried out after described separation, washing and oven dry, obtain described Red copper oxide five decahedron crystallites.
Described step 1) in reactions steps, temperature is 50-80 DEG C, preferably 60-70 DEG C, the time is 2-10 minute, specifically can be 5-10 minute, preferably 5-7 minute; Described step 2) in reactions steps, temperature is 50-80 DEG C, preferably 60-70 DEG C, the time is 2-20 minute, specifically can be 5-20 minute or 10-20 minute, preferably 5-10 minute.
In addition, above-mentioned Red copper oxide five decahedron crystallites provided by the invention, in the application of preparing in visible light photocatalysis device, also belong to protection scope of the present invention.
The present invention is at low temperatures by regulating the consumption of highly basic and glucose to regulate and control the pattern of Red copper oxide, and final acquisition contained the Red copper oxide five decahedron crystallites that expose at high proportion high miller index surface ({ 211} crystal face or { 311} crystal face).The method has broken through the technical limitation that Red copper oxide high miller index surface in prior art ({ 211} crystal face or { 311} crystal face) is difficult to preferred orientation, and tool has the following advantages:
1) do not need to be additionally added with organic additive and organic solvent and control the pattern of Red copper oxide, cost is low, aftertreatment is simple and have advantages of environmental protection.
2) median size of the Red copper oxide five decahedron crystallites of preparing by the method is 1-5 micron, and corner angle are clear, regular shape, size homogeneous, good dispersity; Red copper oxide five decahedron crystallites contain 50 crystal faces, 120 ribs and 72 summits, and wherein 50 crystal faces comprise 24 high miller index surfaces ({ 211} crystal face or { 311} crystal face), 12 { 110} crystal face, 8 { 111} crystal face and 6 { 100} crystal faces.
3) starting material are cheap and easy to get, reaction yield is high, production unit is simple, easy to operate, be easy to realize large-scale industrial production.
4) the step solution chemical method adopting, temperature of reaction is low and gentle, and minimum response temperature is only 50 DEG C, greatly cost-saving.
The method of preparing Red copper oxide five decahedron crystallites provided by the invention, using a hydration neutralized verdigris as copper source, make respectively water, highly basic (sodium hydroxide or potassium hydroxide) and glucose as solvent, precipitation agent and reductive agent, in the time that temperature of reaction is 50-80 DEG C, obtain Red copper oxide five decahedron crystallites by redox reaction.The method has reaction conditions gentleness, equipment is simple, easy to operate, cost is low, productive rate is high, environmentally friendly and be suitable for the advantages such as large-scale industrial production.This crystallite has excellent visible light catalysis activity, has broad application prospects at aspects such as solar cell, hydrogen manufacturing, lithium ion battery and biosensors.
Brief description of the drawings
Fig. 1 is the electron scanning micrograph of the Red copper oxide five decahedron crystallites prepared according to the method for the embodiment of the present invention 1.
Fig. 2 is single Red copper oxide five electron scanning micrographs of decahedron crystallite and the structural representation of theoretical modeling (illustration) of preparing according to the method for the embodiment of the present invention 1.
Fig. 3 is the x-ray diffraction pattern of the Red copper oxide five decahedron crystallites prepared according to the method for the embodiment of the present invention 1.
Fig. 4 is the electron scanning micrograph of the Red copper oxide five decahedron crystallites prepared according to the method for the embodiment of the present invention 2.
Fig. 5 is the electron scanning micrograph of the Red copper oxide five decahedron crystallites prepared according to the method for the embodiment of the present invention 3.
Fig. 6 is the electron scanning micrograph of the Red copper oxide five decahedron crystallites prepared according to the method for the embodiment of the present invention 4.
Fig. 7 is single Red copper oxide five electron scanning micrographs of decahedron crystallite and the structural representation of theoretical modeling (illustration) of preparing according to the method for the embodiment of the present invention 5.
Fig. 8 is the electron scanning micrograph of the Red copper oxide five decahedron crystallites prepared according to the method for the embodiment of the present invention 5.
Fig. 9 is the electron scanning micrograph of the Red copper oxide cubes crystallite prepared according to the method for reference examples 1.
Figure 10 is the electron scanning micrograph of the octahedra crystallite of the Red copper oxide prepared according to the method for reference examples 2.
Figure 11 is the graphic representation of Red copper oxide crystallite catalyzed degradation tropeolin-D under radiation of visible light.
Embodiment
Below in conjunction with specific embodiment, the present invention is further elaborated, but the present invention is not limited to following examples.Described method is ordinary method if no special instructions.Described material all can obtain from open commercial sources if no special instructions.
Embodiment 1
1) copper source compound one hydration neutralized verdigris is dissolved in 5ml deionized water, the aqueous solution of the transparent hydration neutralized verdigris that formation concentration is 0.2mol/L, then be warmed up to 70 DEG C, add the precipitation agent aqueous sodium hydroxide solution 2ml of 6mol/L to react 5 minutes, obtain suspension liquid;
2) to step 1) add again in gained suspension liquid the reductive agent D/W 1ml of 0.75mol/L in 70 DEG C of reactions 5 minutes, react complete being precipitated, the throw out of generation natural subsidence from solution is separated, wash with water after 7 times, in the vacuum drying oven that 60 DEG C, vacuum tightness are 100Pa, dry, finally obtain that corner angle are clear, the Red copper oxide five decahedron crystallites of regular shape, size homogeneous, good dispersity.
The stereoscan photograph of this product as shown in Figure 1, compare with five decahedron structural representations of corresponding theoretical modeling (seeing Fig. 2), can determine that it is Red copper oxide five decahedron crystallites that this embodiment prepares products therefrom, and be that { { { { sealing of 100} crystal face forms for 111} crystal face and 6 for 110} crystal face, 8 for 211} high miller index surface, 12 by 24.The x-ray diffraction pattern figure of these Red copper oxide five decahedron crystallites shows that prepared Red copper oxide five decahedron crystallites are simple cubic crystal formation (seeing Fig. 3), and median size is 2.3 microns.
Embodiment 2
1) copper source compound one hydration neutralized verdigris is dissolved in 5ml deionized water, the aqueous solution of the transparent hydration neutralized verdigris that formation concentration is 0.2mol/L, then be warmed up to 50 DEG C, add the precipitation agent aqueous sodium hydroxide solution 2ml of 6mol/L to react 5 minutes, obtain suspension liquid;
2) to step 1) add again in gained suspension liquid the reductive agent D/W 1ml of 0.65mol/L in 50 DEG C of reactions 20 minutes, react complete being precipitated, the throw out of generation natural subsidence from solution is separated, wash with water after 7 times, in the vacuum drying oven that 60 DEG C, vacuum tightness are 100Pa, dry, finally obtain that corner angle are clear, the Red copper oxide five decahedron crystallites of regular shape, size homogeneous, good dispersity.
Compared with embodiment 1, the Red copper oxide five decahedron crystallites that the present embodiment obtains, size distribution is very inhomogeneous, and as shown in Figure 4, median size is 4.2 microns.
Embodiment 3
1) copper source compound one hydration neutralized verdigris is dissolved in 5ml deionized water, the solution of the transparent hydration neutralized verdigris that formation concentration is 0.3mol/L, then be warmed up to 70 DEG C, add the precipitation agent aqueous sodium hydroxide solution 2ml of 10mol/L to react 5 minutes, obtain suspension liquid;
2) to step 1) add again in gained suspension liquid the reductive agent glucose solution 1ml of 0.8mol/L in 70 DEG C of reactions 5 minutes, react complete being precipitated, the throw out of generation natural subsidence from solution is separated, wash with water after 3 times, in the vacuum drying oven that 60 DEG C, vacuum tightness are 100Pa, dry, finally obtain Red copper oxide five decahedron crystallites.
Compared with embodiment 1, the Red copper oxide five decahedron crystallites that the present embodiment obtains 211} high miller index surface obviously increases, and other expose crystal faces obviously dwindle (seeing Fig. 5), median size is 3.6 microns.
Embodiment 4
1) copper source compound one hydration neutralized verdigris is dissolved in 10ml deionized water, the solution of the transparent hydration neutralized verdigris that formation concentration is 0.3mol/L, then be warmed up to 70 DEG C, add the precipitation agent aqueous sodium hydroxide solution 5ml of 6mol/L to react 10 minutes, obtain suspension liquid;
2) to step 1) add again in gained suspension liquid the reductive agent D/W 2ml of 0.75mol/L in 70 DEG C of reactions 10 minutes, react complete being precipitated, the throw out of generation natural subsidence from solution is separated, wash with water after 5 times, in the vacuum drying oven that 60 DEG C, vacuum tightness are 100Pa, dry, finally obtain Red copper oxide five decahedron crystallites.
Compared with embodiment 1, the Red copper oxide five decahedron crystallites that the present embodiment obtains 211} high miller index surface slightly increases, and other expose crystal faces slightly dwindle (seeing Fig. 6), median size is 3.7 microns.
Embodiment 5
1) copper source compound one hydration neutralized verdigris is dissolved in 5ml deionized water, the solution of the transparent hydration neutralized verdigris that formation concentration is 0.2mol/L, then be warmed up to 70 DEG C, add the precipitation agent potassium hydroxide aqueous solution 2ml of 6mol/L to react 5 minutes, obtain suspension liquid;
2) to step 1) add again in gained suspension liquid the reductive agent D/W 1ml of 0.75mol/L in 70 DEG C of reactions 5 minutes, react complete being precipitated, rotating speed centrifugation 5 minutes (angle rotor radius is as 9cm) by the throw out generating taking 2000 revs/min, wash with water after 5 times, in the vacuum drying oven that 60 DEG C, vacuum tightness are 100Pa, dry, finally obtain Red copper oxide five decahedron crystallites.
Five decahedron structural representations of its corresponding theoretical modeling of Red copper oxide five decahedron crystallite that the present embodiment obtains are compared (seeing Fig. 7), can determine that { { { { sealing of 100} crystal face forms for 111} crystal face and 6 for 110} crystal face, 8 for 311} high miller index surface, 12 by 24.Compared with embodiment 1, gained crystallite particle diameter slightly diminish (seeing Fig. 8), 110} crystal face obviously increase and 111} crystal face slightly dwindles, and high miller index surface become trapezoidal 311} crystal face and non-rectangle { 211} crystal face, median size is 1.8 microns.
Reference examples 1
1) a hydration neutralized verdigris is dissolved in 5ml deionized water, the clear solution that formation concentration is 0.2mol/L, is then warmed up to 70 DEG C, adds the aqueous sodium hydroxide solution 2ml of 1.5mol/L to react 5 minutes, obtains suspension liquid;
2) to step 1) add again in gained suspension liquid the reductive agent D/W 1ml of 0.5mol/L in 70 DEG C of reactions 10 minutes, react complete being precipitated, rotating speed centrifugation 5 minutes (angle rotor radius is as 9cm) by the throw out generating taking 2000 revs/min, wash with water after 7 times, in the vacuum drying oven that 60 DEG C, vacuum tightness are 100Pa, dry, finally obtain by 6 { Red copper oxide cubes crystallites that 100} crystal face surrounds, median size is 1.2 microns, and its stereoscan photograph figure as shown in Figure 9.
Reference examples 2
1) a hydration neutralized verdigris is dissolved in 5ml deionized water, the clear solution that formation concentration is 0.2mol/L, is then warmed up to 70 DEG C, adds the aqueous sodium hydroxide solution 3.5ml of 6mol/L to react 5 minutes, obtains suspension liquid;
2) to step 1) add again in gained suspension liquid the reductive agent D/W 1ml of 0.75mol/L in 70 DEG C of reactions 5 minutes, react complete being precipitated, the throw out of generation natural subsidence from solution is separated, wash with water after 7 times, in the vacuum drying oven that 60 DEG C, vacuum tightness are 100Pa, dry, finally obtain by 8 the octahedra crystallite of Red copper oxide that 111} crystal face surrounds, median size is 3.5 microns, its stereoscan photograph figure is as shown in figure 10.
The Visible Light Induced Photocatalytic reaction test of tropeolin-D:
Used photocatalysis experimental installation is XPA-7 photochemical reaction instrument, and visible-light photocatalyst is selected the Red copper oxide crystallite of embodiment 4,5 and reference examples 1 and 2 gained.Light source is for being equipped with the 500W xenon source of spectral filter (λ > 400nm), and reactor is the 50mL tool plug quartz test tube that is placed in water-bath, and the distance of light source and test tube sidewall is 4cm.It is 1200 revs/min that whole experimental stage keeps magneton rotating speed in test tube, and bath temperature is 20 ± 2 DEG C.
Concrete steps are as follows: in 4 test tubes, add respectively the methyl orange aqueous solution 25ml of 15mg/L, then add respectively above-mentioned cuprous oxide powder 25mg, lucifuge stirs after 1h, open light source and carry out the Visible Light Induced Photocatalytic reaction of tropeolin-D.Every 1h sampling 0.5ml, with the rotating speed centrifugations of 5000 revs/min 5 minutes, removes the rear maximum absorption peak A that measures solution with UV 3900 type ultraviolet spectrophotometers of precipitation.The maximum absorption peak A of the methyl orange aqueous solution of A and 15mg/L
0ratio A/A
0with the photodegradation rate C/C of tropeolin-D
0value equates.Use C/C
0to time t, mapping can be described the Visible Light Induced Photocatalytic effect (see Figure 11) of Red copper oxide to tropeolin-D.As seen from the figure, the embodiment of the present invention 4 and 5 is prepared gained Red copper oxide five decahedron crystallites and is shown than reference examples 1 gained cubes and the better visible light photocatalytic degradation tropeolin-D of the octahedra crystallite of reference examples 2 gained effect owing to having high miller index surface and many rib and angle.Prepare gained Red copper oxide five decahedron crystallites for embodiment of the present invention 1-3, the Visible Light Induced Photocatalytic reaction test result thing substantive difference therewith of its tropeolin-D, no longer endures and states herein.
Claims (7)
1. prepare the method for Red copper oxide five decahedron crystallites for one kind, comprise the steps: using a hydration neutralized verdigris as copper source compound, precipitation agent and reductive agent are mixed and reacted with the aqueous solution of described copper source compound, react after complete separation washing is dried and obtain described Red copper oxide five decahedron crystallites; Wherein, described precipitation agent is aqueous sodium hydroxide solution or potassium hydroxide aqueous solution, and described reductive agent is D/W;
Described Red copper oxide five decahedron crystallites, by 24 high miller index surfaces, 12, { { { sealing of 100} crystal face forms, and has 120 ribs and 72 summits for 111} crystal face and 6 for 110} crystal face, 8; Described high miller index surface is { 311} crystal face;
Concrete steps are as follows:
1) aqueous solution of described copper source compound is warming up to after 50-80 DEG C, adds described precipitation agent to react, react the complete suspension liquid that obtains;
2) to described step 1) add described reductive agent to react in gained suspension liquid, react complete and be precipitated, gained precipitation is carried out after described separation, washing and oven dry, obtain described Red copper oxide five decahedron crystallites;
Described step 1) in reactions steps, temperature is 50-80 DEG C, the time is 2-10 minute;
Described step 2) in reactions steps, temperature is 50-80 DEG C, the time is 2-20 minute;
The concentration of the aqueous solution of described copper source compound is 0.2-0.3mol/L; The concentration of described aqueous sodium hydroxide solution and potassium hydroxide aqueous solution is 6-10mol/L; The concentration of described D/W is 0.6-0.8mol/L; The amount ratio of the aqueous solution, precipitation agent and the reductive agent of described copper source compound is 5-10mL:2-5mL:0.5-1mL.
2. method according to claim 1, is characterized in that:
In described separating step, separation method is that natural subsidence separates or centrifugation;
In described water-washing step, number of times is 3-7 time;
In described baking step, temperature is 25-80 DEG C, and vacuum tightness is 10-200Pa.
3. method according to claim 2, is characterized in that: in described step with centrifugal separation, rotating speed is 1000-5000 rev/min, and radius is 7-10cm, and the time is 2-10 minute.
4. method according to claim 3, is characterized in that: in described step with centrifugal separation, rotating speed is 2000-3000 rev/min, and radius is 9-10cm, and the time is 3-5 minute.
5. method according to claim 1, is characterized in that: described step 1) in reactions steps, temperature is 60-70 DEG C, the time is 5-7 minute;
Described step 2) in reactions steps, temperature is 60-70 DEG C, the time is 5-10 minute.
6. method according to claim 1, is characterized in that: the median size of described Red copper oxide five decahedron crystallites is 1-5 micron.
7. method according to claim 6, is characterized in that: the median size of described Red copper oxide five decahedron crystallites is 1.5-2.5 micron.
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| CN110156064A (en) * | 2019-04-30 | 2019-08-23 | 南开大学 | A kind of low indices of crystallographic plane Cu2The preparation method of O Polyhedral Particles |
| CN110510656B (en) * | 2019-08-29 | 2020-06-23 | 东莞东阳光科研发有限公司 | Cu2O-nano microcrystal and preparation method and application thereof |
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| CN111534833B (en) * | 2020-04-08 | 2021-08-17 | 北京化工大学 | Copper nano electrode with high-index crystal face and preparation method and application thereof |
| CN114762826A (en) * | 2021-07-21 | 2022-07-19 | 天津科技大学 | High index crystal plane Cu2Preparation method and application of O photocatalyst |
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