CN108502925A - A kind of preparation method and applications of { 110 } high energy crystal face exposure BiOCl materials - Google Patents
A kind of preparation method and applications of { 110 } high energy crystal face exposure BiOCl materials Download PDFInfo
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- CN108502925A CN108502925A CN201810323243.7A CN201810323243A CN108502925A CN 108502925 A CN108502925 A CN 108502925A CN 201810323243 A CN201810323243 A CN 201810323243A CN 108502925 A CN108502925 A CN 108502925A
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- C01G29/00—Compounds of bismuth
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/24—Electrodes for alkaline accumulators
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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Abstract
The present invention relates to the preparation method and applications that a kind of { 110 } high energy crystal face exposes BiOCl materials.Bismuth source, chlorine source and saccharide compound are mixed in a certain ratio uniformly by the present invention, by the mechanical force synchronous effect of high-energy ball milling in chemical reaction, are then heat-treated at 200~600 DEG C, and BiOCl materials are prepared using washing impurity-removing, separation of solid and liquid, drying.Prepared BiOCl materials are made of the nanometer sheet of 2~20nm of thickness, 100~1000nm of the length of side, and { 110 } crystal face degree of exposure is 50~100%.The present invention has that preparation process is simple, advantages such as at low cost, environmental-friendly of easily realizing industrialized production, manufacturing process.Prepared { 110 } high energy crystal face exposure BiOCl materials have extensive use in ultracapacitor, alkaline secondary cell, lithium ion battery, photochemical catalyst, pearlescent pigment, medicine and other fields.
Description
Technical field
The present invention relates to the preparation method and applications that a kind of { 110 } high energy crystal face exposes BiOCl materials, belong to novel work(
It can Material Field.
Background technology
Bismuth oxychloride is a kind of important functional material, due to its unique microstructure and physicochemical properties, and
It is nontoxic, inexpensive, in electrode active material, catalyst, pigment, cosmetics, gas sensor, electronic material, medical material etc.
Field has potential extensive use.BiOCl crystal is by double Cl-Sheath and [Bi2O2]2+Layer is alternately arranged structure along (001) direction
At anisotropic layer structure, this layer structure is conducive to the transmission of electronics.Due to the low energy that { 001 } crystal face is BiOCl
Crystal face at present exposes particular crystal plane the research of BiOCl materials based on the exposure of { 001 } crystal face.However, { 001 } crystal face is sudden and violent
The surface for revealing BiOCl materials is oxygen atomic layer, it is possible to provide the reactivity site of electron exchange is less.If can prepare
{ 010 }, the BiOCl materials of the high energy crystal face such as { 110 } exposure, it is likely that more active sites are provided, so as to improve BiOCl
The reactivity of material.
The method of high energy crystal face exposure BiOCl materials is prepared at present with coprecipitation, based on hydro-thermal method and solvent-thermal method.
[the J.American Chemical Sosiety 134 (2012) such as Jiang:4473-4476] it is found that at first in hydrothermal system
In by adjust solution ph can control BiOCl crystal from { 001 } crystal face exposure be changed into { 010 } high energy crystal face exposure.
[the ACS Sustainable Chemistry＆Engineering 5 (2017) such as Zhang:4619-4629] by by bismuth nitrate
Ordinary-temp hydrolysis reaction is carried out under ammonium hydroxide/alcohol solvent system prepare the BiOCl materials that { 010 } crystal face exposes with sodium chloride,
The material has stronger dyestuff absorbability and higher charge carrier transport efficiency, thus with more preferably photocatalytic
Energy.[the J.Alloys and Compounds 549 (2013) such as Cui:70-76] by the way that bismuth nitrate, potassium chloride and urea are dissolved in
In ethylene glycol solution, the BiOCl materials that hydro-thermal reaction prepares the exposure of { 110 } crystal face are carried out at 90 DEG C, the material is ultraviolet
It can effective decomposition of methyl orange under light or radiation of visible light.Wangdan [the synthesis and its photocatalysis of the controllable BiOCl nano materials of crystal face
Performance study (D), Anhui Normal University, 2015] use glucose as structure directing agent, by Bi2O3Nanometer rods and hydrochloric acid exist
Hydro-thermal reaction prepares the one-dimensional BiOCl materials of { 110 } crystal face exposure at 160 DEG C, and has studied it under ultraviolet light to Luo Dan
The photocatalysis performance of bright B.[Harbin Teachers' Univ.'s nature journal 31 (2015) such as Bian Yuzhuo:119-122] by bismuth nitrate and chlorine
Change potassium and carry out solvent thermal reaction in glycerin solution, be prepared for the BiOCl microballoons of { 110 } crystal face exposure, compares coprecipitation
The BiOCl materials of preparation have higher photocatalytic activity.
However, these synthetic methods or needing to control pH value of reaction system, or need to carry out at high temperature under high pressure anti-
It answers, there is complex steps, manufacturing cost is high, is not suitable for the problems such as industrialized production.Therefore, it is raw to be easy to batch for exploitation one kind
It produces and the method that can obtain the BiOCl materials that there is high energy crystal face to expose is most important.
Invention content
The purpose of the present invention is to provide the preparation method and applications that a kind of { 110 } high energy crystal face exposes BiOCl materials.
The present invention has that preparation process is simple, advantages such as at low cost, environmental-friendly of easily realizing industrialized production, manufacturing process；Gained
The features such as BiOCl materials have crystalline phase pure, and { 110 } high energy crystal face degree of exposure is high.
The invention is realized by the following technical scheme：
A kind of preparation method of { 110 } high energy crystal face exposure BiOCl materials, includes the following steps：
(1) bismuth source, chlorine source and saccharide compound are pressed 1:(0~2):The molar ratio (the ratio between amount of substance) of (0.01~1)
It is uniformly mixed, obtains raw mixture；
(2) raw mixture obtained by step (1) is pressed 1 with abrading-ball:The mass ratio of (0.5~100) is put into ball mill,
0.2~20h of ball milling under protective atmosphere；
(3) ball-milled mixtures that step (2) obtains are placed in high temperature furnace 0.5~10h of heat treatment at 200~600 DEG C,
Mixture after heat treatment is passed through into washing impurity-removing, is then separated by solid-liquid separation, dried and expose to get { 110 } high energy crystal face
BiOCl materials.
Further, the bismuth source be bismuth metal, bismuth oxide, bismuth hydroxide, waltherite, basic bismuth carbonate, bismuth nitrate,
One or both of novismuth, bismuth sulfate, sulfuric acid oxygen bismuth, bismuth chloride, sodium bismuthate, bismuthic acid lithium, bismuthic acid potassium, bismuthic acid magnesium with
On.
Further, the chlorine source be chloride ion-containing compound, preferably hydrochloric acid, sodium chloride, potassium chloride, ammonium chloride,
One or more of zinc chloride, iron chloride, copper chloride, aluminium chloride, calcium chloride, magnesium chloride.
Further, the saccharide compound is monosaccharide and disaccharide (or disaccharides), polysaccharide, glycan or glycoconjugate, preferably Portugal
One or more of grape sugar, fructose, lactose, sucrose, maltose.
Further, the protective atmosphere is one or more of nitrogen, argon gas, carbon dioxide, air.
Further, the rotating speed of ball mill is 30~3000rpm.
Further, the ball mill is selected from various types in the market；The abrading-ball be agate ball, corundum ball,
One or more of zirconia ball, porcelain ball, stainless steel ball.
Above-mentioned obtained { 110 } the high energy crystal face exposure BiOCl materials of preparation method are in ultracapacitor, alkali secondary electricity
Application in pond, lithium ion battery, photochemical catalyst, pearlescent pigment or medicine and other fields.
The beneficial effects of the present invention are：
(1) the method for the present invention preparation process is simple, process conditions are relatively mild, is easy to industrialized production, production process environment
Close friend does not generate poisonous and harmful by-product.
(2) prepared by the present invention BiOCl material crystalline phases are pure, { 110 } high energy crystal face degree of exposure is high, the microcosmic shape of product
Looks are easily controllable, and are widely used.
Description of the drawings
Fig. 1 is the X-ray powder diffraction test chart of the BiOCl materials prepared by embodiment 1.
Fig. 2,3 for the BiOCl materials prepared by embodiment 1 transmission electron microscope figure.
Fig. 4 is the scanning electron microscope diagram of the BiOCl materials prepared by embodiment 2.
Constant current charge-discharge test chart of the battery that Fig. 5 is assembled by embodiment 3 under different current densities.
Specific implementation mode
The technical solution further illustrated the present invention below with specific embodiment, but the invention is not limited in embodiments.
Embodiment 1
1, raw material 10mmol bismuth nitrates, 10mmol potassium chloride and 2mmol glucose are uniformly mixed, by raw mixture and
Corundum abrading-ball presses 1:50 mass ratio is added in ball mill, and ball milling 5h obtains presoma under the conditions of rotating speed is 1500rpm, then will
Presoma is placed in Muffle furnace, sets heating rate as 5 DEG C/min, and constant temperature 4h postcoolings take out sample to room temperature at 450 DEG C,
It is separated by solid-liquid separation again by sample deionized water and absolute ethyl alcohol washing impurity-removing, using filtering, finally consolidating filtering gained
Body product is dried in vacuo 12h at 100 DEG C and prepares BiOCl materials.
2, X-ray diffraction test is carried out to the BiOCl materials prepared by embodiment 1, as shown in Figure 1, gained BiOCl productions
Product crystalline phase is pure, and without other impurity peaks, better crystallinity degree, and the corresponding diffraction maximum of (110) crystal face is apparently higher than standard card.It is right
BiOCl materials prepared by embodiment 1 carry out transmissioning electric mirror test, and as shown in Figure 2,3, can measure interplanar distance by Fig. 2 is
0.7228nm is matched, it was demonstrated that sample exposes { 110 } high energy crystal face with (001) interplanar distance in PDF cards.It can be with from Fig. 3
See, sample is made of the nanometer sheet that the length of side is 70~160nm, thickness is 13~20nm, and { 010 } crystal face degree of exposure is about
73%.
Embodiment 2
1, raw material 10mmol bismuth sulfates, 10mmol ammonium chlorides and 1mmol sucrose are uniformly mixed, by raw mixture and oxygen
Change zirconium abrading-ball and presses 1:80 mass ratio is added in ball mill, and ball milling 8h obtains presoma under the conditions of rotating speed is 1000rpm, then will
Presoma is placed in Muffle furnace, sets heating rate as 4 DEG C/min, and constant temperature 4h postcoolings take out sample to room temperature at 500 DEG C,
It is separated by solid-liquid separation again by sample deionized water and absolute ethyl alcohol washing impurity-removing, using filtering, finally consolidating filtering gained
Body product dry 12h at 110 DEG C prepares BiOCl materials.
2, testing electronic microscope is scanned to the BiOCl materials prepared by embodiment 2, as shown in figure 4, sample be by
The nanometer sheet or nano particle that size is 50~200nm are constituted.
Embodiment 3
By prepared by embodiment 1 BiOCl materials and the nickel hydroxide anode material bought be fabricated to electrode slice, adopt
It is that electrolyte is assembled into alkaline secondary cell with 6mol/L KOH solutions, using the CHI660A electrifications of Shanghai Chen Hua company production
Work station is learned, constant current charge-discharge test is carried out at room temperature to the battery constructed, as shown in figure 5, the sample is in 1A/g electric currents
The specific capacity for having 213mAh/g under density still has the specific capacity of 190mAh/g at 5A/g, illustrates good high rate performance.
Claims (10)
1. a kind of preparation method of { 110 } high energy crystal face exposure BiOCl materials, which is characterized in that the BiOCl materials are by thickness
The nanometer sheet composition of 2~20nm, 100~1000nm of the length of side are spent, { 110 } crystal face degree of exposure is 50~100%；Preparation method
Include the following steps：
(1) bismuth source, chlorine source and saccharide compound are pressed 1:(0~2):The molar ratio of (0.01~1) is uniformly mixed, and it is mixed to obtain raw material
Close object；
(2) raw mixture obtained by step (1) is pressed 1 with abrading-ball:The mass ratio of (0.5~100) is put into ball mill, is being protected
0.2~20h of ball milling under atmosphere；
(3) ball-milled mixtures that step (2) obtains are placed in high temperature furnace 0.5~10h of heat treatment at 200~600 DEG C, it will be hot
Treated, and mixture passes through washing impurity-removing, is then separated by solid-liquid separation, dries the BiOCl exposed to get { 110 } high energy crystal face
Material.
2. the preparation method of { 110 } high energy crystal face exposure BiOCl materials according to claim 1, which is characterized in that described
Bismuth source be bismuth metal, bismuth oxide, bismuth hydroxide, waltherite, basic bismuth carbonate, bismuth nitrate, novismuth, bismuth sulfate, sulfuric acid
One or more of oxygen bismuth, bismuth chloride, sodium bismuthate, bismuthic acid lithium, bismuthic acid potassium, bismuthic acid magnesium.
3. the preparation method of { 110 } high energy crystal face exposure BiOCl materials according to claim 1, which is characterized in that described
Chlorine source be chloride ion-containing compound.
4. the preparation method of { 110 } high energy crystal face exposure BiOCl materials according to claim 1, which is characterized in that described
Chlorine source be hydrochloric acid, sodium chloride, potassium chloride, ammonium chloride, zinc chloride, iron chloride, copper chloride, aluminium chloride, calcium chloride, in magnesium chloride
One or more.
5. the preparation method of { 110 } high energy crystal face exposure BiOCl materials according to claim 1, which is characterized in that described
Saccharide compound be monosaccharide and disaccharide, polysaccharide, glycan or glycoconjugate.
6. the preparation method of { 110 } high energy crystal face exposure BiOCl materials according to claim 1, which is characterized in that described
Saccharide compound be glucose, fructose, lactose, sucrose, one or more of maltose.
7. the preparation method of { 110 } high energy crystal face exposure BiOCl materials according to claim 1, which is characterized in that described
Protective atmosphere be nitrogen, argon gas, carbon dioxide, one or more of air.
8. the preparation method of { 110 } high energy crystal face exposure BiOCl materials according to claim 1, which is characterized in that ball milling
The rotating speed of machine is 30~3000rpm.
9. the preparation method of { 110 } high energy crystal face exposure BiOCl materials according to claim 1, which is characterized in that described
Ball mill be selected from various types in the market；The abrading-ball is agate ball, corundum ball, zirconia ball, porcelain ball, stainless steel ball
One or more of.
10. { 110 } high energy crystal face that claim 1 to 9 any one of them preparation method obtains exposes BiOCl materials super
Application in capacitor, alkaline secondary cell, lithium ion battery, photochemical catalyst, pearlescent pigment or field of medicaments.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106984339A (en) * | 2017-04-27 | 2017-07-28 | 武汉纺织大学 | A kind of preparation method of BiOCl photocatalytic material and obtained catalysis material and application |
| CN107162051A (en) * | 2017-04-27 | 2017-09-15 | 武汉纺织大学 | The preparation method of flower-shaped BiOCl photochemical catalysts and obtained BiOCl photochemical catalysts and application |
| CN107262120A (en) * | 2017-07-11 | 2017-10-20 | 四川理工学院 | The preparation method that a kind of BiOCl surface photovoltages signal is significantly increased |
-
2018
- 2018-04-11 CN CN201810323243.7A patent/CN108502925A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106984339A (en) * | 2017-04-27 | 2017-07-28 | 武汉纺织大学 | A kind of preparation method of BiOCl photocatalytic material and obtained catalysis material and application |
| CN107162051A (en) * | 2017-04-27 | 2017-09-15 | 武汉纺织大学 | The preparation method of flower-shaped BiOCl photochemical catalysts and obtained BiOCl photochemical catalysts and application |
| CN107262120A (en) * | 2017-07-11 | 2017-10-20 | 四川理工学院 | The preparation method that a kind of BiOCl surface photovoltages signal is significantly increased |
Non-Patent Citations (2)
| Title |
|---|
| JING XIE,ET.AL: "Room-temperature Solid-state synthesis of BiOCl hierarchical microspheres with nanoplates", 《CATALYSIS COMMUNICATIONS》 * |
| 王丹: "晶面可控的BiOCl纳米材料的合成及其光催化性能研究", 《中国优秀硕士学位论文全文数据库(电子期刊)，工程科技Ⅰ辑》 * |
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