CN105733003A - Anionic polymer and bismuth oxychloride or bismuth oxybromide composite thin film and preparation method thereof - Google Patents
Anionic polymer and bismuth oxychloride or bismuth oxybromide composite thin film and preparation method thereof Download PDFInfo
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- CN105733003A CN105733003A CN201610214689.7A CN201610214689A CN105733003A CN 105733003 A CN105733003 A CN 105733003A CN 201610214689 A CN201610214689 A CN 201610214689A CN 105733003 A CN105733003 A CN 105733003A
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- C08J2325/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Derivatives of such polymers
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- C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
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Abstract
The invention discloses an anionic polymer and bismuth oxychloride or bismuth oxybromide composite thin film and a preparation method thereof.The method comprises the step that anionic polymers and bismuth oxychloride or bismuth oxybromide positive charge nanosheets prepared in an aqueous solution are assembled layer by layer, and the anionic polymer and bismuth oxychloride or bismuth oxybromide composite thin film which has an ordered structure is formed.According to the composite functional material, the layer structure of bismuth oxychloride or bismuth oxybromide, the confinement effect of a two-dimensional space, interaction of a subject and an object and a specific effect of the anionic polymers in the solution are fully utilized, the anionic polymers are uniformly dispersed among bismuth oxychloride or bismuth oxybromide layers, photoelectric function optimization and regulation of bismuth oxychloride or bismuth oxybromide are achieved, and a road is paved for further functionalization and device manufacturing of a molecular self-assembly system and the bismuth oxychloride or bismuth oxybromide material.
Description
Technical field
The invention belongs to composite organic-inorganic material preparing technical field, particularly to the laminated film and preparation method thereof of a kind of anionic polymer and chlorine oxygen bismuth or bromine oxygen bismuth.
Background technology
Chlorine oxygen bismuth is a kind of rapid lamellar compound of development in recent years, is a kind of inorganic semiconductor material with wide range of application.It has the layer structure similar with Graphene, by the BiO of positively charged+Layer and electronegative Cl-Layer stack is built and is formed, middle Cl-Laminate can by other ionic replacement, for instance Br-, molecular formula can be expressed as BiOCl.
As a kind of 4-5-6 race ternary semiconductor, BiOCl belongs to tetragonal crystal system, and it is the structure of a kind of opening, [Cl-Bi-O-Bi-Cl] repetitive pile up and form, and interlayer is combined by non-covalent bond (such as Van der Waals force).In each [Cl-Bi-O-Bi-Cl] layer, around a bismuth atom, there are 4 oxygen atoms and 4 chlorine atoms.Owing to the key in layer is very firm, the key of interlayer is very weak, and BiOCl is a kind of anisotropic structure, has the electricity of excellence, optics and chemical property.Its peculiar property determines and is with a wide range of applications, and in photocatalytic water and degradation of dye, performance is very superior.
The kind of anionic polymer is more, mainly has: kayexalate (PSS), sodium polyacrylate (PAAS) etc. and derivant thereof.This base polymer presents electronegativity in the solution, in layer assembly process, is a desirable negative electricity layer material of class.
LBL self-assembly is the method utilizing successively alternating deposit, by the intermolecular weak interaction of each layer (such as electrostatic attraction, hydrogen bond, coordinate bond etc.), layer and layer is made spontaneously to form and be formed structural integrity, stable performance, have the molecule aggregate of certain specific function or the process of supramolecular structure.Past, preparing thin film with layer-by-layer had very big breakthrough, especially hydrotalcite material these years.Chlorine oxygen bismuth is a kind of rapid lamellar compound of development in recent years, has developed a lot of composites, but application LBL self-assembly is prepared chlorine oxygen bismuth composite and rarely had report based on chlorine oxygen bismuth.Chlorine oxygen bismuth is stratified material, by the BiO of positively charged+Layer and electronegative Cl-Layer stack is built and is formed, and based on this special structure, the invention achieves the LBL self-assembly of chlorine oxygen bismuth and anionic polymer.
Summary of the invention
It is an object of the invention to provide a kind of anionic polymer laminated film with chlorine oxygen bismuth or bromine oxygen bismuth and preparation method thereof.Its preparation process is simple, and film photoelectric performance and thickness can at Nano grade controllable precise.
The technical scheme is that the chlorine oxygen bismuth prepared with aqueous solution by anionic polymer or bromine oxygen bismuth positive charge nanometer sheet are through layer assembly method, form structurally ordered anionic polymer and chlorine oxygen bismuth or bromine oxygen bismuth composite film material.This composite functional material takes full advantage of the layer structure of chlorine oxygen bismuth or bromine oxygen bismuth and the confinement effect of two-dimensional space and host-guest interaction, and the specific function that anionic polymer is in the solution, make anionic polymer dispersed at chlorine oxygen bismuth or bromine oxygen bismuth interlayer, achieving photoelectric functional optimization and the regulation and control of chlorine oxygen bismuth and bromine oxygen bismuth, further functionalization and device for molecular self-assembly and chlorine oxygen bismuth or bromine oxygen bismuth material have paved road.
The laminated film of anionic polymer of the present invention and chlorine oxygen bismuth or bromine oxygen bismuth is photoelectric function thin films, it is alternately assembled layer by layer at three dimensions by the positive charge nanometer sheet of organic component anionic polymer and inorganic component chlorine oxygen bismuth or bromine oxygen bismuth and is formed, there is obvious layer structure feature, film thickness uniformly can be regulated and controled between 8-600 nanometer by changing the assembling number of plies and anionic polymer concentration.
Anionic polymer of the present invention is as follows with the preparation method of chlorine oxygen bismuth or the laminated film of bromine oxygen bismuth:
1) chlorine oxygen bismuth or bromine oxygen bismuth are dispersed in water, dispersion concentration is 0.5-5g/L, 3000-5000 rev/min is stirred 3-5 hour, it is subsequently adding the silver acetate solutions that concentration is 0.01-0.05mol/L, the mol ratio of silver and bismuth element is 1:1-2:1, continuing sucking filtration after stirring 12-15 hour, the filtrate obtained is the positive charge nanometer sheet colloid solution of the chlorine oxygen bismuth of clear or bromine oxygen bismuth, is designated as solution A；
2) prepare the anionic polymer solution of 1-5g/L, be designated as solution B；
3) take out after substrate electronegative after hydrophilicity-imparting treatment being soaked 10-20 minute in solution A, after fully cleaning with deionized water, place in solution B, take out after soaking 10-20 minute, fully clean with deionized water, the laminated film of the anionic polymer once circulated and chlorine oxygen bismuth or bromine oxygen bismuth；
4) step 3 is repeated), in solution A and solution B, alternate immersion operates 1-100 time, obtains the laminated film of multilamellar anionic polymer and chlorine oxygen bismuth or bromine oxygen bismuth.
The mol ratio of the bismuth in described chlorine oxygen bismuth or the laminate of bromine oxygen bismuth and oxygen is 1:1-1:1.2.
Described anionic polymer is selected from kayexalate and derivant, sodium polyacrylate and derivant, polymethylacrylic acid and derivant thereof.
Described substrate is piezoid, silicon chip or ITO sheet.
The method of described hydrophilicity-imparting treatment is: by concentrated sulphuric acid that substrate volume ratio is 9:1-1:1 and hydrogen peroxide mixed liquid dipping 30-60 minute, then fully clean with deionized water.
The invention has the beneficial effects as follows: based on electrostatic force, namely positive and negative charge attracts, the present invention breaches the limitation in the past preparing chlorine oxygen bismuth and bromine oxygen bismuth composite process, creativeness achieves the LBL self-assembly of anionic polymer and inorganic chlorine oxygen bismuth and bromine oxygen bismuth nanometer sheet, achieve the optimization to chlorine oxygen bismuth and bromine oxygen bismuth photoelectric functional, the breakthrough of regulation and control and chlorine oxygen bismuth and bromine oxygen bismuth composite material and preparation method thereof, assembling category and the range of application of inorganic supramolecular materials are expanded, and the preparation method and application scope for chlorine oxygen bismuth and bromine oxygen bismuth composite provides basic research.
Accompanying drawing explanation
Fig. 1 is the uv absorption spectra of the kayexalate that the assembling number of plies is 5 to 15 layers that obtains of embodiment 1 and chlorine oxygen bismuth laminated film, for carrying out a ultraviolet spectra test every 5 layers in figure.Illustration is that 193 and 224 nanometers absorbances are with assembling the situation of change that the number of plies increases.
Fig. 2 is the uv absorption spectra of the sodium polyacrylate that the assembling number of plies is 5 to 15 layers that obtains of embodiment 2 and chlorine oxygen bismuth laminated film, for carrying out a ultraviolet spectra test every 5 layers in figure.Illustration is that 215 and 261 nanometers absorbances are with assembling the situation of change that the number of plies increases.
Fig. 3 is the uv absorption spectra of the kayexalate that the assembling number of plies is 5 to 15 layers that obtains of embodiment 3 and chlorine oxygen bismuth laminated film, for carrying out a ultraviolet spectra test every 5 layers in figure.Illustration is that 193 and 225 nanometers absorbances are with assembling the situation of change that the number of plies increases.
Fig. 4 is the uv absorption spectra of the kayexalate that the assembling number of plies is 5 to 15 layers that obtains of embodiment 4 and bromine oxygen bismuth laminated film, for carrying out a ultraviolet spectra test every 5 layers in figure.Illustration is that 193 and 225 nanometers absorbances are with assembling the situation of change that the number of plies increases.
Fig. 5 is that the kayexalate that embodiment 1 obtains assembles the little angle XRD figure when number of plies is 40 layers with chlorine oxygen bismuth laminated film.
Detailed description of the invention
[embodiment 1]
1. hydro-thermal method prepares chlorine oxygen bismuth precursor:
A. by the solid Bi (NO of 0.01mol3)2·5H2O is dissolved in the salpeter solution of 20mL0.9M；
B. 0.015mol halogenated phosphates CPC is dissolved in 60mL deionized water, stirring；
C. it is slowly added in b by solution in a solution, continues stirring 1 hour, then mixed solution is proceeded in the water heating kettle of polytetrafluoroethylsubstrate substrate, 160 DEG C are reacted 16 hours, priority ethanol and deionization hot water centrifuge washing are repeatedly clarified to supernatant, and 60 DEG C dry 10 hours, obtain chlorine oxygen bismuth precursor；
2. take in the above-mentioned chlorine oxygen bismuth precursor addition 200mL water of 0.15g and disperse, mixing speed is 3000 revs/min, mixing time is 3 hours, it is subsequently adding the silver acetate solutions that 50mL concentration is 0.01mol/L and continues stirring, sucking filtration after reacting 12 hours, obtaining filtrate is clear chlorine oxygen bismuth positive charge nanometer sheet colloid solution, is designated as solution A；
3. prepare the kayexalate solution of 1g/L, be designated as solution B；
4. by the dense H of piezoid volume ratio 7:32SO4With hydrogen peroxide mixed liquid dipping 30 minutes, after deionized water fully cleans, put in solution A and soak 10 minutes；Take out, after fully cleaning with deionized water, then place in solution B, soak 10 minutes and fully clean with deionized water, the kayexalate once circulated and chlorine oxygen bismuth laminated film；
5. repeat alternate immersion operation 4 times, 9 times, 14 times, 49 times in solution A and solution B in step 4, respectively obtain kayexalate and the chlorine oxygen bismuth laminated film of 5 layers, 10 layers, 15 layers, 50 layers.
Characterize assembling the thin film that the number of plies is 15 layers: as shown in Figure 1, kayexalate and chlorine oxygen bismuth laminated film are along with the increase assembling the number of plies, the maximum absorption band of its ultra-violet absorption spectrum presents continuous growth trend, and absorbance and the assembling number of plies are close to linear relationship, it was shown that the kayexalate assembled is fixed value every time.
[embodiment 2]
The kayexalate solution of the 1g/L in embodiment 1 replaces with the sodium polyacrylate solution of 1g/L, and all the other conditions, with embodiment 1, obtain sodium polyacrylate and the chlorine oxygen bismuth laminated film of 5 layers, 10 layers, 15 layers.
Gained assembles the polyacrylic acid that the number of plies is 15 layers characterize with chlorine oxygen bismuth laminated film: characterized from the ultra-violet absorption spectrum of Fig. 2, along with the increase assembling the number of plies, the maximum absorption band of its ultra-violet absorption spectrum presents continuous growth trend, and absorbance and the assembling number of plies are close to linear relationship, it was shown that the polyacrylic acid assembled is fixed value every time.
[embodiment 3]
1. nucleation/crystallization isolation method prepares chlorine oxygen bismuth precursor:
A. by the solid Bi (NO of 0.02mol3)2·5H2O is dissolved in the salpeter solution of 50mL0.9M；
B. 0.03mol halogenated phosphates CPC is dissolved in 100mL deionized water, stirring；
C. by step a, the solution of b preparation rapidly joins colloid mill, rotating speed 4000 revs/min, react 1 minute, proceeding in the water heating kettle of polytetrafluoroethylsubstrate substrate, 160 DEG C are reacted 16 hours, successively use ethanol and deionization hot water centrifuge washing repeatedly to supernatant clarification, 60 DEG C dry 10 hours, obtain chlorine oxygen bismuth precursor；
2. take in the above-mentioned chlorine oxygen bismuth precursor addition 200mL water of 0.15g and disperse, mixing speed is 5000 revs/min, mixing time is 3 hours, it is subsequently adding the silver acetate solutions that 60mL concentration is 0.01mol/L and continues stirring, filtered off with suction after reacting 12 hours, collecting filter cake, obtaining filtrate is clear chlorine oxygen bismuth positive charge nanometer sheet colloid solution, is designated as solution A；
3. prepare the kayexalate solution of 1g/L, be designated as solution B；
4. by the dense H of piezoid volume ratio 7:32SO4With hydrogen peroxide mixed liquid dipping 30 minutes, after deionized water fully cleans, put in solution A and soak 10 minutes；Take out, after fully cleaning with deionized water, then place in solution B, soak 10 minutes and fully clean with deionized water, the kayexalate once circulated and chlorine oxygen bismuth laminated film；
5. repeat alternate immersion operation 4 times, 9 times, 14 times in solution A and solution B in step 4, respectively obtain kayexalate and the chlorine oxygen bismuth laminated film of 5 layers, 10 layers, 15 layers.
Gained assembles the kayexalate that the number of plies is 15 layers characterize with chlorine oxygen bismuth laminated film: characterized from the ultra-violet absorption spectrum of Fig. 3, along with the increase assembling the number of plies, the maximum absorption band of its ultra-violet absorption spectrum presents continuous growth trend, and absorbance and the assembling number of plies are close to linear relationship, it was shown that the kayexalate assembled is fixed value every time.
[embodiment 4]
Halogenated phosphates CPC in embodiment 3 is replaced with bromide sixteen alkyls pyridine CPB, and all the other conditions, with embodiment 3, respectively obtain kayexalate and the bromine oxygen bismuth laminated film of 5 layers, 10 layers, 15 layers.
Gained assembles the kayexalate that the number of plies is 15 layers characterize with bromine oxygen bismuth laminated film: characterized from the ultra-violet absorption spectrum of Fig. 4, along with the increase assembling the number of plies, the maximum absorption band of its ultra-violet absorption spectrum presents continuous growth trend, and absorbance and the assembling number of plies are close to linear relationship, it was shown that the kayexalate assembled is fixed value every time.
Claims (6)
1. the laminated film of an anionic polymer and chlorine oxygen bismuth or bromine oxygen bismuth, it is characterized in that, this laminated film is photoelectric function thin films, it is alternately assembled layer by layer at three dimensions by the positive charge nanometer sheet of organic component anionic polymer and inorganic component chlorine oxygen bismuth or bromine oxygen bismuth and is formed, there is obvious layer structure feature, film thickness uniformly can be regulated and controled between 8-600 nanometer by changing the assembling number of plies and anionic polymer concentration.
2. the preparation method of the laminated film of an anionic polymer and chlorine oxygen bismuth or bromine oxygen bismuth, it is characterised in that its concrete operation step is as follows:
1) chlorine oxygen bismuth or bromine oxygen bismuth are dispersed in water, dispersion concentration is 0.5-5g/L, 3000-5000 rev/min is stirred 3-5 hour, it is subsequently adding the silver acetate solutions that concentration is 0.01-0.05mol/L, the mol ratio of silver and bismuth element is 1:1-2:1, continuing sucking filtration after stirring 12-15 hour, the filtrate obtained is the positive charge nanometer sheet colloid solution of the chlorine oxygen bismuth of clear or bromine oxygen bismuth, is designated as solution A；
2) prepare the anionic polymer solution of 1-5g/L, be designated as solution B；
3) take out after substrate electronegative after hydrophilicity-imparting treatment being soaked 10-20 minute in solution A, after fully cleaning with deionized water, place in solution B, take out after soaking 10-20 minute, fully clean with deionized water, the laminated film of the anionic polymer once circulated and chlorine oxygen bismuth or bromine oxygen bismuth；
4) step 3 is repeated), in solution A and solution B, alternate immersion operates 1-100 time, obtains the laminated film of multilamellar anionic polymer and chlorine oxygen bismuth or bromine oxygen bismuth.
3. preparation method according to claim 2, it is characterised in that the mol ratio of the bismuth in described chlorine oxygen bismuth or the laminate of bromine oxygen bismuth and oxygen is 1:1-1:1.2.
4. preparation method according to claim 2, it is characterised in that described anionic polymer is selected from kayexalate and derivant, sodium polyacrylate and derivant, polymethylacrylic acid and derivant thereof.
5. preparation method according to claim 2, it is characterised in that described substrate is piezoid, silicon chip or ITO sheet.
6. preparation method according to claim 2, it is characterised in that the method for described hydrophilicity-imparting treatment is: by concentrated sulphuric acid that substrate volume ratio is 9:1-1:1 and hydrogen peroxide mixed liquid dipping 30-60 minute, then fully clean with deionized water.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106732443A (en) * | 2016-11-28 | 2017-05-31 | 桂林奥尼斯特节能环保科技有限责任公司 | A kind of defluorination absorbing material and preparation method thereof and the method that the exceeded water of fluorine is processed using it |
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| CN101465214A (en) * | 2009-01-09 | 2009-06-24 | 清华大学 | Inorganic/organic compound film photoelectric pole and preparation method thereof |
| CN102089684A (en) * | 2008-05-15 | 2011-06-08 | 巴斯夫公司 | Method of making thin film structure and compositions thereof |
| CN104117391A (en) * | 2014-08-01 | 2014-10-29 | 太原理工大学 | Preparation of photoelectric catalytic membrane for preparing hydrogen by decomposing water |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102089684A (en) * | 2008-05-15 | 2011-06-08 | 巴斯夫公司 | Method of making thin film structure and compositions thereof |
| CN101465214A (en) * | 2009-01-09 | 2009-06-24 | 清华大学 | Inorganic/organic compound film photoelectric pole and preparation method thereof |
| CN104117391A (en) * | 2014-08-01 | 2014-10-29 | 太原理工大学 | Preparation of photoelectric catalytic membrane for preparing hydrogen by decomposing water |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106732443A (en) * | 2016-11-28 | 2017-05-31 | 桂林奥尼斯特节能环保科技有限责任公司 | A kind of defluorination absorbing material and preparation method thereof and the method that the exceeded water of fluorine is processed using it |
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