CN107262124A - A kind of preparation method of the CuI BiOI/Cu thin-film materials with antibacterial functions - Google Patents
A kind of preparation method of the CuI BiOI/Cu thin-film materials with antibacterial functions Download PDFInfo
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- CN107262124A CN107262124A CN201710615688.8A CN201710615688A CN107262124A CN 107262124 A CN107262124 A CN 107262124A CN 201710615688 A CN201710615688 A CN 201710615688A CN 107262124 A CN107262124 A CN 107262124A
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- 239000000463 material Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 20
- 239000010409 thin film Substances 0.000 title claims abstract description 13
- 239000010949 copper Substances 0.000 claims abstract description 67
- 239000010408 film Substances 0.000 claims abstract description 31
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910052802 copper Inorganic materials 0.000 claims abstract description 23
- 239000002131 composite material Substances 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 11
- 239000007864 aqueous solution Substances 0.000 claims abstract description 11
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 11
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 48
- 239000000243 solution Substances 0.000 claims description 48
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 32
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- 239000000843 powder Substances 0.000 claims description 14
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims description 9
- 239000011259 mixed solution Substances 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 7
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 7
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 5
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims description 5
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims description 4
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 2
- 229920002554 vinyl polymer Polymers 0.000 claims description 2
- 241000894006 Bacteria Species 0.000 abstract description 16
- 238000006243 chemical reaction Methods 0.000 abstract description 12
- 239000008236 heating water Substances 0.000 abstract description 6
- 230000001699 photocatalysis Effects 0.000 abstract description 5
- 238000007146 photocatalysis Methods 0.000 abstract description 5
- 239000012528 membrane Substances 0.000 abstract description 4
- 230000003197 catalytic effect Effects 0.000 abstract description 3
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 3
- 238000011109 contamination Methods 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 abstract description 2
- 235000012054 meals Nutrition 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 abstract 1
- 229910052740 iodine Inorganic materials 0.000 abstract 1
- 239000011630 iodine Substances 0.000 abstract 1
- CJJMLLCUQDSZIZ-UHFFFAOYSA-N oxobismuth Chemical compound [Bi]=O CJJMLLCUQDSZIZ-UHFFFAOYSA-N 0.000 abstract 1
- 238000002474 experimental method Methods 0.000 description 18
- 230000005764 inhibitory process Effects 0.000 description 17
- 239000006916 nutrient agar Substances 0.000 description 15
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 239000012895 dilution Substances 0.000 description 5
- 238000010790 dilution Methods 0.000 description 5
- 238000005286 illumination Methods 0.000 description 5
- 235000013372 meat Nutrition 0.000 description 5
- 235000014347 soups Nutrition 0.000 description 5
- 229910052724 xenon Inorganic materials 0.000 description 5
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 4
- 150000004694 iodide salts Chemical class 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 230000000845 anti-microbial effect Effects 0.000 description 3
- 229910021595 Copper(I) iodide Inorganic materials 0.000 description 2
- URVGHPZOLQFKJZ-UHFFFAOYSA-N [Bi]=O.[I] Chemical compound [Bi]=O.[I] URVGHPZOLQFKJZ-UHFFFAOYSA-N 0.000 description 2
- LSXDOTMGLUJQCM-UHFFFAOYSA-M copper(i) iodide Chemical compound I[Cu] LSXDOTMGLUJQCM-UHFFFAOYSA-M 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 230000010718 Oxidation Activity Effects 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- -1 bismuthino Chemical group 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000002779 inactivation Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 239000002887 superconductor Substances 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/06—Halogens; Compounds thereof
- B01J27/08—Halides
- B01J27/122—Halides of copper
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/58—Fabrics or filaments
- B01J35/59—Membranes
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
Abstract
The invention discloses a kind of preparation method of the CuI BiOI/Cu thin-film materials with antibacterial functions, belong to field of material synthesis technology.Iodine oxygen bismuth meal end obtained by being prepared as solvent-thermal method is added in the aqueous solution containing a certain amount of polyethylene glycol, places into pretreated copper sheet, CuI BiOI/Cu composite film materials are obtained by heating water bath certain time.The present invention prepares that method is simple, and equipment and technical process are simple to operation, and the membrane material application prospect of preparation is good, it is adaptable to warms, use in high humidity, the environment of easy breed bacteria；This method has the advantages that using reagent contamination is small, reaction reproducible, preparation condition is gentle.The CuI BiOI/Cu composite film materials of gained show good catalytic activity in photocatalysis antibacterial, and performance is stable, cyclicity is good.
Description
Technical field
The invention belongs to photocatalysis nano material synthesis technical field, and in particular to a kind of CuI- with antibacterial functions
The preparation method of BiOI/Cu thin-film materials.
Background technology
TiO is found from researcher in 19722Since hydrogen and oxygen being split water under ultraviolet light, partly lead
Body photocatalysis greatly causes the strong interest of domestic and international researcher.Under illumination condition, semiconducting external layer electronics is excited,
Conduction band is transitted to from valence band, so as to produce electron-hole pair.Photo-generate electron-hole can directly attack bacteria, in addition electronic energy
Other active species are changed into, for example：•O2 -, the outer membrane of further oxidizing bacteria is removed, meanwhile, other oxidation activity species,
Such as OH, H2O2,•HO2, can also be produced by electronics and hole from water, so as to realize many inactivations to bacterium.But
It is the compound process competitive reaction with antibacterial that light excites rear electron-hole pair, the presence of the reaction has had a strong impact on light reaction
Efficiency.
Visibility region is most concentrated mainly on by force due to being distributed in sunshine spectrum, therefore design has high quantum in visual field
The catalyst of efficiency is to make full use of solar energy, improves the key of anti-microbial property.
Iodine oxygen bismuth is as a kind of bismuthino semi-conducting material, due to the electrical and optical properties of its protrusion, pharmacy, fuel,
Good application prospect is suffered from catalyst and sensor field.Cuprous iodide is a kind of water-insoluble crystal, with α,
Tri- kinds of crystalline phases of β, γ, cuprous iodide is at low temperature（< 350 ℃）It is the p-type semiconductor material of cubic structure for γ crystalline phases, tool
There is 3.1eV direct band gap, because its special electric property, can be used as solar cell material and superconductor.Compared to
Relatively conventional fine catalyst, the CuI-BiOI/Cu composite film materials this time synthesized make in the recovery and circulation of catalyst
There is more prominent performance in terms of.
The content of the invention
It is an object of the invention in view of the shortcomings of the prior art, a kind of CuI-BiOI/Cu with antibacterial functions of offer is thin
The preparation method of membrane material.The CuI-BiOI/Cu composite film materials of gained produced by the present invention are showed in photocatalysis antibacterial
Go out good catalytic activity, and performance is stable, cyclicity is good, it is adaptable to warm, use in high humidity, the environment of easy breed bacteria；
This method has the advantages that to use reproducible, the preparation condition temperature that reagent contamination is small, react.
To achieve the above object, the present invention is adopted the following technical scheme that：
A kind of preparation method of the CuI-BiOI/Cu thin-film materials with antibacterial functions, be will be prepared as solvent-thermal method obtained by
Iodine oxygen bismuth meal end add in the aqueous solution containing a certain amount of polyethylene glycol, place into pretreated copper sheet, by water-bath plus
Hot certain time obtains CuI-BiOI/Cu composite film materials；Concrete operation step is as follows：
（1）Into the mixed solution of ethylene glycol and water, bismuth nitrate solution, liquor kalii iodide and polyvinylpyrrolidone are added, will
After resulting solution is fully stirred evenly, in the reactor for pouring into 100ml polytetrafluoroethyllining linings, it is put into baking oven and is heated；
（2）By step（1）The solution of gained, is collected, cleans, centrifuges, and grinding obtains orange-yellow BiOI repeatedly after drying
Powder；
（3）By step（2）The BiOI powder of gained is added in the aqueous solution of polyethylene glycol；
（4）Copper sheet by pretreatment is put into step（3）In resulting solution, water bath with thermostatic control heating is carried out under stirring；
（5）By step（4）The copper sheet of gained takes out, and is dried to obtain CuI-BiOI/Cu composite film materials.
Step（1）In described ethylene glycol and the mixed solution of water, the volume ratio of ethylene glycol and water is 2:1~9:1.
The step（1）In bismuth nitrate solution and liquor kalii iodide concentration be 0.05 ~ 0.3mol/L, polyvinyl pyrrole
The amount of alkanone is 10 ~ 70mg.
The step（1）The technological parameter of middle heating process is：Heating-up temperature is 80 ~ 180 DEG C；Heat time be 1 ~
6h。
Step（3）Described in polyethylene glycol the aqueous solution concentration be 0.1 ~ 0.4g/mL.
Step（4）Described in water bath with thermostatic control heating technological parameter be：Heating-up temperature be 40 ~ 70 DEG C, the heat time be 6 ~
24h。
Step（4）Described in the preparation method of copper sheet that pre-processes be：By copper sheet sequentially pass through acetone, absolute ethyl alcohol and
After the pretreatment of 0.1M hydrochloric acid solutions, the copper sheet that size is 3.5cm × 3.5cm is obtained.
Step（2）And step（5）In drying temperature be 50 ~ 80 DEG C.
The beneficial effects of the present invention are：
（1）The present invention prepares that method is simple, and equipment and technical process are simple to operation, the membrane material application prospect of preparation
Well, it is adaptable to warm, use in high humidity, the environment of easy breed bacteria；
（2）This method has the advantages that using reagent contamination is small, reaction reproducible, preparation condition is gentle, the CuI- of gained
BiOI/Cu composite film materials show good catalytic activity in photocatalysis antibacterial, and performance is stable, cyclicity is good.
Brief description of the drawings
Fig. 1 is CuI-BiOI/Cu composite film material anti-microbial property kinetic curves；
Fig. 2,3,4,5 are the CuI-BiOI/Cu composite film material inhibition zone design sketch for preparing under different condition；
Fig. 6 is CuI-BiOI/Cu composite film material XRDs.
Embodiment
Below in conjunction with specific embodiment, the present invention will be further described, but the present invention is not limited only to these embodiments.
Embodiment 1
Be 70 DEG C in bath temperature, water bath time be the preparation of CuI-BiOI/Cu composite film materials for preparing under the conditions of 24h and
Anti-microbial property test
It is prepared by CuI-BiOI/Cu composite film materials
Into the mixed solution of 20ml ethylene glycol and water（The volume ratio 7 of ethylene glycol and water:1）, add 20mL bismuth nitrate solution
（Concentration is 0.05mol/L）, 20mL liquor kalii iodide（Concentration is 0.05mol/L）With 50mg polyvinylpyrrolidones, by institute
After solution fully stirs evenly, in the reactor for pouring into 100ml polytetrafluoroethyllining linings, be put into baking oven and heated at 180 DEG C, plus
Hot 3h；By the solution of gained, it is collected, cleans, centrifuges, grinding obtains orange repeatedly after being dried at ambient pressure in 60 DEG C of baking ovens
The BiOI powder of color；Obtained BiOI powder is added in the 50ml aqueous solution containing 10g molecular weight for 2000 polyethylene glycol；
The copper sheet that acetone, absolute ethyl alcohol and the pretreated size of 0.1M hydrochloric acid solutions are 3.5cm × 3.5cm will be sequentially passed through to be put into
State in resulting solution；Heating water bath 24h in 70 DEG C of water-bath, and add magneton and be stirred, stir speed (S.S.) maintains 350r/
min；Reaction takes out the copper sheet of gained after terminating, and is dried to obtain CuI-BiOI/Cu laminated films in 60 DEG C of baking ovens at ambient pressure
Material.
Antibacterial test
The used strain of experiment, at 37 DEG C, in MH（mueller hinton）PBS solution is used immediately after meat soup culture 18h
Dilution, the concentration of the bacterium finally given is 106.5cfu /ml.In whole experiment process, all glassware and PBS
Solution be all by deionized water clean and autoclaving is obtained after 20 minutes under 121 DEG C of high steams.0.5ml strains are taken,
It is dispersed on freshly prepared nutrient agar panel, size is placed in for 1cm × 1cm CuI-BiOI/Cu laminated films
The centre of nutrient agar panel, uses xenon source（Filter off below 400nm wavelength）Simulated solar irradiation, carries out sterilizing reaction.Light
It is 2h according to the time, takes 0.5ml bacterium solutions to be dispersed on nutrient agar every 0.5h, is placed in cultivating in 37 DEG C of constant incubators
24h.The efficiency of antibacterial can be to 99.9% under visible ray.Reacted copper sheet is taken out after cleaning and drying, entered using same procedure
Row repeats to test.The kinetic curve of third-order reaction is shown in Fig. 1.
Embodiment 2
It it is 70 DEG C in bath temperature, water bath time is the inhibition zone of the CuI-BiOI/Cu composite film materials prepared under the conditions of 16h
Experiment
It is prepared by CuI-BiOI/Cu composite film materials
Into the mixed solution of 40ml ethylene glycol and water（The volume ratio 7 of ethylene glycol and water:1）, add 20mL bismuth nitrate solution
（Concentration is 0.2mol/L）, 20mL liquor kalii iodides（Concentration is 0.2mol/L）With 50mg polyvinylpyrrolidones, gained is molten
After liquid is fully stirred evenly, in the reactor for pouring into 100ml polytetrafluoroethyllining linings, it is put into baking oven and is heated at 180 DEG C, heating
3h；By the solution of gained, it is collected, cleans, centrifuges, grinding obtains orange-yellow repeatedly after being dried at ambient pressure in 60 DEG C of baking ovens
BiOI powder；Obtained BiOI powder is added in the 50ml aqueous solution containing 10g molecular weight for 2000 polyethylene glycol；Will
Sequentially pass through acetone, absolute ethyl alcohol and the pretreated size of 0.1M hydrochloric acid solutions be 3.5cm × 3.5cm copper sheet be put into it is above-mentioned
In resulting solution；Heating water bath 16h in 70 DEG C of water-bath, and add magneton and be stirred, stir speed (S.S.) maintains 500r/
min；Reaction takes out the copper sheet of gained after terminating, and is dried to obtain CuI-BiOI/Cu laminated films in 60 DEG C of baking ovens at ambient pressure
Material；
The used strain of experiment, at 37 DEG C, in MH（mueller hinton）PBS solution is used immediately after meat soup culture 18h
Dilution, the concentration of the bacterium finally given is 106.5cfu /ml.In whole experiment process, all glassware and PBS
Solution be all by deionized water clean and autoclaving is obtained after 20 minutes under 121 DEG C of high steams.The 0.5ml concentration is taken to be
106.5Cfu/ml bacterium solutions, are dispersed on freshly prepared nutrient agar panel, after standing five minutes, are 1cm by size
× 1cm CuI-BiOI/Cu laminated films are placed in the centre of nutrient agar panel, use xenon source（Filter off below 400nm ripples
It is long）Simulated solar irradiation, carries out inhibition zone test experiments, light application time is 2h.After illumination, nutrient agar panel is placed in 37 DEG C of perseverances
24h is cultivated in warm incubator.The inhibition zone finally given is shown in Fig. 2（Circle represents its inhibition zone size in Fig. 2）.
Embodiment 3
It it is 55 DEG C in bath temperature, water bath time is the inhibition zone of the CuI-BiOI/Cu composite film materials prepared under the conditions of 24h
Experiment
It is prepared by CuI-BiOI/Cu composite film materials
Into the mixed solution of 40ml ethylene glycol and water（The volume ratio 7 of ethylene glycol and water:1）, add 13.3mL bismuth nitrate it is molten
Liquid（Concentration is 0.3mol/L）, 13.3mL liquor kalii iodides（Concentration is 0.3mol/L）With 50mg polyvinylpyrrolidones, by institute
After solution fully stirs evenly, in the reactor for pouring into 100ml polytetrafluoroethyllining linings, be put into baking oven and heated at 180 DEG C, plus
Hot 3h；By the solution of gained, it is collected, cleans, centrifuges, grinding obtains orange repeatedly after being dried at ambient pressure in 60 DEG C of baking ovens
The BiOI powder of color；Obtained BiOI powder is added in the 50ml aqueous solution containing 10g molecular weight for 2000 polyethylene glycol；
The copper sheet that acetone, absolute ethyl alcohol and the pretreated size of 0.1M hydrochloric acid solutions are 3.5cm × 3.5cm will be sequentially passed through to be put into
State in resulting solution；Heating water bath 24h in 55 DEG C of water-bath, and add magneton and be stirred, stir speed (S.S.) maintains 400r/
min；Reaction takes out the copper sheet of gained after terminating, and is dried to obtain CuI-BiOI/Cu laminated films in 60 DEG C of baking ovens at ambient pressure
Material；
The used strain of experiment, at 37 DEG C, in MH（mueller hinton）PBS solution is used immediately after meat soup culture 18h
Dilution, the concentration of the bacterium finally given is 106.5cfu /ml.In whole experiment process, all glassware and PBS
Solution be all by deionized water clean and autoclaving is obtained after 20 minutes under 121 DEG C of high steams.The 0.5ml concentration is taken to be
106.5Cfu/ml bacterium solutions, are dispersed on freshly prepared nutrient agar panel, after standing five minutes, are 1cm by size
× 1cm CuI-BiOI/Cu laminated films are placed in the centre of nutrient agar panel, use xenon source（Filter off below 400nm ripples
It is long）Simulated solar irradiation, carries out inhibition zone test experiments, light application time is 2h.After illumination, nutrient agar panel is placed in 37 DEG C of perseverances
24h is cultivated in warm incubator.The inhibition zone finally given is shown in Fig. 3（Circle represents its inhibition zone size in Fig. 3）.
Embodiment 4
It it is 40 DEG C in bath temperature, water bath time is the inhibition zone of the CuI-BiOI/Cu composite film materials prepared under the conditions of 12h
Experiment
It is prepared by CuI-BiOI/Cu composite film materials
Into the mixed solution of 40ml ethylene glycol and water（The volume ratio 7 of ethylene glycol and water:1）, add 20mL bismuth nitrate solution
（Concentration is 0.2mol/L）, 20mL liquor kalii iodides（Concentration is 0.2mol/L）With 10mg polyvinylpyrrolidones, gained is molten
After liquid is fully stirred evenly, in the reactor for pouring into 100ml polytetrafluoroethyllining linings, it is put into baking oven and is heated at 80 DEG C, heat 6h；
By the solution of gained, it is collected, cleans, centrifuges, grinding obtains orange-yellow repeatedly after being dried at ambient pressure in 60 DEG C of baking ovens
BiOI powder；Obtained BiOI powder is added in the 50ml aqueous solution containing 10g molecular weight for 2000 polyethylene glycol；Will be according to
Secondary process acetone, absolute ethyl alcohol and the pretreated size of 0.1M hydrochloric acid solutions are put into above-mentioned institute for 3.5cm × 3.5cm copper sheet
Obtain in solution；Heating water bath 12h in 40 DEG C of water-bath, and add magneton and be stirred, stir speed (S.S.) maintains 450r/min；
Reaction takes out the copper sheet of gained after terminating, and is dried to obtain CuI-BiOI/Cu composite film materials in 60 DEG C of baking ovens at ambient pressure；
The used strain of experiment, at 37 DEG C, in MH（mueller hinton）PBS solution is used immediately after meat soup culture 18h
Dilution, the concentration of the bacterium finally given is 106.5cfu /ml.In whole experiment process, all glassware and PBS
Solution be all by deionized water clean and autoclaving is obtained after 20 minutes under 121 DEG C of high steams.The 0.5ml concentration is taken to be
106.5Cfu/ml bacterium solutions, are dispersed on freshly prepared nutrient agar panel, after standing five minutes, are 1cm by size
× 1cm CuI-BiOI/Cu laminated films are placed in the centre of nutrient agar panel, use xenon source（Filter off below 400nm ripples
It is long）Simulated solar irradiation, carries out inhibition zone test experiments, light application time is 2h.After illumination, nutrient agar panel is placed in 37 DEG C of perseverances
24h is cultivated in warm incubator.The inhibition zone finally given is shown in Fig. 4（Circle represents its inhibition zone size in Fig. 4）.
Embodiment 5
It it is 70 DEG C in bath temperature, water bath time is the inhibition zone of the CuI-BiOI/Cu composite film materials prepared under 8 hs
Experiment
It is prepared by CuI-BiOI/Cu composite film materials
Into the mixed solution of 40ml ethylene glycol and water（The volume ratio 7 of ethylene glycol and water:1）, add 20mL bismuth nitrate solution
（Concentration is 0.2mol/L）, 20mL liquor kalii iodides（Concentration is 0.2mol/L）With 70mg polyvinylpyrrolidones, gained is molten
After liquid is fully stirred evenly, in the reactor for pouring into 100ml polytetrafluoroethyllining linings, it is put into baking oven and is heated at 130 DEG C, heating
1h；By the solution of gained, it is collected, cleans, centrifuges, grinding obtains orange-yellow repeatedly after being dried at ambient pressure in 60 DEG C of baking ovens
BiOI powder；Obtained BiOI powder is added in the 50ml aqueous solution containing 10g molecular weight for 2000 polyethylene glycol；Will
Sequentially pass through acetone, absolute ethyl alcohol and the pretreated size of 0.1M hydrochloric acid solutions be 3.5cm × 3.5cm copper sheet be put into it is above-mentioned
In resulting solution；Heating water bath 8h in 70 DEG C of water-bath, and add magneton and be stirred, stir speed (S.S.) maintains 400r/
min；Reaction takes out the copper sheet of gained after terminating, and is dried to obtain CuI-BiOI/Cu laminated films in 60 DEG C of baking ovens at ambient pressure
Material；
The used strain of experiment, at 37 DEG C, in MH（mueller hinton）PBS solution is used immediately after meat soup culture 18h
Dilution, the concentration of the bacterium finally given is 106.5cfu /ml.In whole experiment process, all glassware and PBS
Solution be all by deionized water clean and autoclaving is obtained after 20 minutes under 121 DEG C of high steams.The 0.5ml concentration is taken to be
106.5Cfu/ml bacterium solutions, are dispersed on freshly prepared nutrient agar panel, after standing five minutes, are 1cm by size
× 1cm CuI-BiOI/Cu laminated films are placed in the centre of nutrient agar panel, use xenon source（Filter off below 400nm ripples
It is long）Simulated solar irradiation, carries out inhibition zone test experiments, light application time is 2h.After illumination, nutrient agar panel is placed in 37 DEG C of perseverances
24h is cultivated in warm incubator.The inhibition zone finally given is shown in Fig. 5（Circle represents its inhibition zone size in Fig. 5）
Presently preferred embodiments of the present invention is the foregoing is only, all equivalent changes done according to scope of the present invention patent are with repairing
Decorations, should all belong to the covering scope of the present invention.
Claims (8)
1. a kind of preparation method of the CuI-BiOI/Cu thin-film materials with antibacterial functions, it is characterised in that：Concrete operation step
It is as follows：
（1）Into the mixed solution of ethylene glycol and water, bismuth nitrate solution, liquor kalii iodide and polyvinylpyrrolidone are added, will
After resulting solution is fully stirred evenly, in the reactor for pouring into 100ml polytetrafluoroethyllining linings, it is put into baking oven and is heated；
（2）By step（1）The solution of gained, is collected, cleans, centrifuges, and grinding obtains orange-yellow BiOI repeatedly after drying
Powder；
（3）By step（2）The BiOI powder of gained is added in the aqueous solution of polyethylene glycol；
（4）Copper sheet by pretreatment is put into step（3）In resulting solution, water bath with thermostatic control heating is carried out under stirring；
（5）By step（4）The copper sheet of gained takes out, and is dried to obtain CuI-BiOI/Cu composite film materials.
2. a kind of preparation method of CuI-BiOI/Cu thin-film materials with antibacterial functions according to claim 1, it is special
Levy and be：Step（1）In described ethylene glycol and the mixed solution of water, the volume ratio of ethylene glycol and water is 2:1~9:1.
3. a kind of preparation method of CuI-BiOI/Cu thin-film materials with antibacterial functions according to claim 1, it is special
Levy and be：The step（1）In bismuth nitrate solution and liquor kalii iodide concentration be 0.05 ~ 0.3mol/L, polyvinyl pyrrole
The amount of alkanone is 10 ~ 70mg.
4. a kind of preparation method of CuI-BiOI/Cu thin-film materials with antibacterial functions according to claim 1, it is special
Levy and be：The step（1）The technological parameter of middle heating process is：Heating-up temperature is 80 ~ 180 DEG C；Heat time is 1 ~ 6h.
5. a kind of preparation method of CuI-BiOI/Cu thin-film materials with antibacterial functions according to claim 1, it is special
Levy and be：Step（3）Described in polyethylene glycol the aqueous solution concentration be 0.1 ~ 0.4g/mL.
6. a kind of preparation method of CuI-BiOI/Cu thin-film materials with antibacterial functions according to claim 1, it is special
Levy and be：Step（4）Described in water bath with thermostatic control heating technological parameter be：Heating-up temperature be 40 ~ 70 DEG C, the heat time be 6 ~
24h。
7. a kind of preparation method of CuI-BiOI/Cu thin-film materials with antibacterial functions according to claim 1, it is special
Levy and be：Step（4）Described in the preparation method of copper sheet that pre-processes be：By copper sheet sequentially pass through acetone, absolute ethyl alcohol and
After the pretreatment of 0.1M hydrochloric acid solutions, the copper sheet that size is 3.5cm × 3.5cm is obtained.
8. a kind of preparation method of CuI-BiOI/Cu thin-film materials with antibacterial functions according to claim 1, it is special
Levy and be：Step（2）And step（5）In drying temperature be 50 ~ 80 DEG C.
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| CN110180488A (en) * | 2019-05-07 | 2019-08-30 | 东北大学 | A kind of high adsorption activity BiOI and the preparation method and application thereof |
| CN115368602A (en) * | 2022-08-09 | 2022-11-22 | 山东农业大学 | Preparation method of carbon nitride based green light catalytic preservative film |
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| CN106179425A (en) * | 2016-06-30 | 2016-12-07 | 中国科学院海洋研究所 | A kind of photocatalysis film material and preparation method thereof |
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| CN102296337A (en) * | 2011-06-09 | 2011-12-28 | 浙江东晶光电科技有限公司 | Preparation method of CuI film |
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| CN115368602A (en) * | 2022-08-09 | 2022-11-22 | 山东农业大学 | Preparation method of carbon nitride based green light catalytic preservative film |
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