CN107262124B - A kind of preparation method of the CuI-BiOI/Cu thin-film material with antibacterial functions - Google Patents
A kind of preparation method of the CuI-BiOI/Cu thin-film material with antibacterial functions Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 20
- 239000010409 thin film Substances 0.000 title claims abstract description 14
- 239000010949 copper Substances 0.000 claims abstract description 67
- 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
- 238000006243 chemical reaction Methods 0.000 claims abstract description 21
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 11
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 11
- 239000007864 aqueous solution Substances 0.000 claims abstract description 9
- 239000000243 solution Substances 0.000 claims description 54
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 48
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 35
- 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
- 238000010438 heat treatment Methods 0.000 claims description 14
- 239000000843 powder Substances 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 12
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims description 9
- 239000011259 mixed solution Substances 0.000 claims description 9
- 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 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 7
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 6
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 6
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims description 4
- 229920002554 vinyl polymer Polymers 0.000 claims description 2
- 239000010408 film Substances 0.000 abstract description 30
- 239000002131 composite material Substances 0.000 abstract description 22
- 241000894006 Bacteria Species 0.000 abstract description 21
- 238000000034 method Methods 0.000 abstract description 17
- 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
- URVGHPZOLQFKJZ-UHFFFAOYSA-N [Bi]=O.[I] Chemical compound [Bi]=O.[I] URVGHPZOLQFKJZ-UHFFFAOYSA-N 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 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
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 235000012054 meals Nutrition 0.000 abstract description 2
- 238000002474 experimental method Methods 0.000 description 19
- 239000006916 nutrient agar Substances 0.000 description 15
- 230000005764 inhibitory process Effects 0.000 description 13
- 230000001954 sterilising effect Effects 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 238000010790 dilution Methods 0.000 description 5
- 239000012895 dilution Substances 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
- 238000004659 sterilization and disinfection Methods 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
- 238000000227 grinding Methods 0.000 description 4
- 230000001629 suppression Effects 0.000 description 4
- 230000000845 anti-microbial effect Effects 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 229910021595 Copper(I) iodide Inorganic materials 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
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 230000010718 Oxidation Activity Effects 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
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 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
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001914 filtration 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
- 150000002576 ketones Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 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
- 229920006316 polyvinylpyrrolidine Polymers 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000002887 superconductor Substances 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
Classifications
-
- 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
-
- B01J35/39—
-
- B01J35/59—
Abstract
The preparation method of the invention discloses a kind of CuI-BiOI/Cu thin-film material with antibacterial functions, belongs to field of material synthesis technology.It is added resulting iodine oxygen bismuth meal end is prepared by solvent-thermal method in the aqueous solution containing a certain amount of polyethylene glycol, places into pretreated copper sheet, CuI-BiOI/Cu composite film material is obtained by heating water bath certain time.Prepared by the present invention method is simple, and equipment and technical process are simple to operation, and the membrane material application prospect of preparation is good, suitable for warm, high humidity, Yi Zisheng bacterium environment use；This method has many advantages, such as to use small reagent contamination, the reproducible of reaction, preparation condition mild.Resulting CuI-BiOI/Cu composite film material shows 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 fields, and in particular to a kind of CuI- with antibacterial functions
The preparation method of BiOI/Cu thin-film material.
Background technique
TiO is found from researcher in 19722Since hydrogen and oxygen capable of 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, to generate electron-hole pair.Photo-generate electron-hole can direct attack bacteria, other electronics energy
Other active species are converted to, such as: O2 -, the outer membrane of further oxidizing bacteria is removed, meanwhile, other oxidation activity species,
Such as OH, H2O2,•HO2, can also be generated from water by electrons and holes, to realize the inactivation of various pairs of bacteriums.But
It is the process competitive reaction of the compound and antibacterial of electron-hole pair after light excites, the presence of the reaction has seriously affected light reaction
Efficiency.
It is most concentrated mainly on visibility region by force due to being distributed in sunlight spectrum, 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 semiconductor material, due to its electrical and optical properties outstanding, pharmacy, fuel,
Good application prospect is suffered from catalyst and sensor field.Cuprous iodide is a kind of water-insoluble crystal, have α,
Tri- kinds of crystal phases of β, γ, cuprous iodide at low temperature (< 350 DEG C) be γ crystal phase, be the p-type semiconductor material of cubic structure, tool
There is the direct band gap of 3.1eV, because its special electric property, can be used as solar cell material and superconductor.Compared to
Relatively conventional fine catalyst, this time the CuI-BiOI/Cu composite film material of synthesis makes in the recycling of catalyst and circulation
With etc. have performance more outstanding.
Summary of the invention
It is an object of the invention in view of the shortcomings of the prior art, to provide a kind of CuI-BiOI/Cu with antibacterial functions thin
The preparation method of membrane material.Resulting CuI-BiOI/Cu composite film material produced by the present invention shows in photocatalysis antibacterial
Good catalytic activity out, and performance is stable, cyclicity is good, suitable for warm, high humidity, Yi Zisheng bacterium environment use；
This method has many advantages, such as small using reagent contamination, reaction reproducible, preparation condition temperature.
To achieve the above object, the present invention adopts the following technical scheme:
A kind of preparation method of the CuI-BiOI/Cu thin-film material with antibacterial functions, is that will be prepared by solvent-thermal method
Resulting iodine oxygen bismuth meal end is added in the aqueous solution containing a certain amount of polyethylene glycol, places into pretreated copper sheet, passes through water
Bath heating certain time obtains CuI-BiOI/Cu composite film material；Specific steps are as follows:
(1) into the mixed solution of ethylene glycol and water, bismuth nitrate solution, liquor kalii iodide and polyvinylpyrrolidine is added
Ketone after sufficiently stirring evenly acquired solution, pours into the reaction kettle of 100ml polytetrafluoroethyllining lining, is put into baking oven and is heated；
(2) by step (1) resulting solution, be collected, clean, be centrifuged, it is dry after repeatedly grinding obtain it is orange-yellow
BiOI powder；
(3) the resulting BiOI powder of step (2) is added in the aqueous solution of polyethylene glycol；
(4) it will be put into step (3) acquired solution by pretreated copper sheet, water bath with thermostatic control is carried out under stirring and is added
Heat；
(5) the resulting copper sheet of step (4) is taken out, is dried to obtain CuI-BiOI/Cu composite film material.
In the mixed solution of ethylene glycol described in step (1) and water, the volume ratio of ethylene glycol and water is 2:1 ~ 9:1.
The concentration of bismuth nitrate solution and liquor kalii iodide in the step (1) is 0.05 ~ 0.3mol/L, polyvinyl pyrrole
The amount of alkanone is 10 ~ 70mg.
The technological parameter of heating process in the step (1) are as follows: heating temperature is 80 ~ 180 DEG C；Heating time be 1 ~
6h。
The concentration of the aqueous solution of polyethylene glycol described in step (3) is 0.1 ~ 0.4g/mL.
Water bath with thermostatic control described in step (4) heating technological parameter are as follows: heating temperature be 40 ~ 70 DEG C, heating time be 6 ~
24h。
Pretreated copper sheet described in step (4) the preparation method comprises the following steps: copper sheet is successively passed through acetone, dehydrated alcohol and
After the pretreatment of 0.1M hydrochloric acid solution, the copper sheet that size is 3.5cm × 3.5cm is obtained.
Drying temperature in step (2) and step (5) is 50 ~ 80 DEG C.
The beneficial effects of the present invention are:
(1) prepared by the present invention method is simple, and equipment and technical process are simple to operation, the membrane material application of preparation
Have good prospects, suitable for warm, high humidity, Yi Zisheng bacterium environment use；
(2) this method has many advantages, such as to use small reagent contamination, the reproducible of reaction, preparation condition mild, resulting
CuI-BiOI/Cu composite film material shows good catalytic activity in photocatalysis antibacterial, and performance is stable, cyclicity
It is good.
Detailed description of the invention
Fig. 1 is CuI-BiOI/Cu composite film material anti-microbial property kinetic curve；
Fig. 2,3,4,5 are the CuI-BiOI/Cu composite film material inhibition zone effect picture prepared under different condition；
Fig. 6 is CuI-BiOI/Cu composite film material XRD diagram.
Specific 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 for 24 hours under the conditions of the system of CuI-BiOI/Cu composite film material for preparing
Standby and anti-microbial property test
The preparation of CuI-BiOI/Cu composite film material
To (the volume ratio 7:1 of ethylene glycol and water) in the mixed solution of 20ml ethylene glycol and water, the bismuth nitrate of 20mL is added
The liquor kalii iodide (concentration 0.05mol/L) and 50mg polyvinylpyrrolidone of solution (concentration 0.05mol/L), 20mL,
It after acquired solution is sufficiently stirred evenly, pours into the reaction kettle of 100ml polytetrafluoroethyllining lining, is put into baking oven and adds at 180 DEG C
Heat heats 3h；It by resulting solution, is collected, cleans, is centrifuged, ground repeatedly after drying in 60 DEG C of baking ovens under normal pressure
To orange-yellow BiOI powder；Obtained BiOI powder is added to the 50ml water for the polyethylene glycol for being 2000 containing 10g molecular weight
In solution；The copper that acetone, dehydrated alcohol and the pretreated size of 0.1M hydrochloric acid solution are 3.5cm × 3.5cm will successively be passed through
Piece is put into above-mentioned acquired solution；Heating water bath for 24 hours, and is added magneton and is stirred in 70 DEG C of water-bath, stirring rate dimension
It holds in 350r/min；Resulting copper sheet is taken out after reaction, is dried to obtain CuI-BiOI/Cu in 60 DEG C of baking ovens under normal pressure
Composite film material.
Antibacterial test
The used strain of experiment, at 37 DEG C, in MH(mueller hinton) PBS is used immediately after meat soup culture 18h
Solution dilution, the concentration of finally obtained bacterium are 106.5cfu /ml.In the entire experiment process, all glasswares and
PBS solution is all clean by deionized water and high pressure sterilization obtains after twenty minutes under 121 DEG C of high steams.Take 0.5ml bacterium
Kind, it is dispersed on freshly prepared nutrient agar panel, the CuI-BiOI/Cu laminated film that size is 1cm × 1cm is set
Sterilizing reaction is carried out with xenon source (filtering off 400nm or less wavelength) simulated solar irradiation in the centre of nutrient agar panel.
Light application time is 2h, takes 0.5ml bacterium solution to be dispersed on nutrient agar every 0.5h, is placed in 37 DEG C of constant incubators and trains
It supports for 24 hours.The efficiency of antibacterial can be to 99.9% under visible light.Copper sheet after reaction is taken out after cleaning and drying, using same procedure
It carries out repeating experiment.The kinetic curve of third-order reaction is shown in Fig. 1.
Embodiment 2
It is 70 DEG C in bath temperature, the suppression for the CuI-BiOI/Cu composite film material that water bath time is prepared under the conditions of being 16h
The experiment of bacterium circle
The preparation of CuI-BiOI/Cu composite film material
To (the volume ratio 7:1 of ethylene glycol and water) in the mixed solution of 40ml ethylene glycol and water, the bismuth nitrate of 20mL is added
Solution (concentration 0.2mol/L), 20mL liquor kalii iodide (concentration 0.2mol/L) and 50mg polyvinylpyrrolidone, by institute
After solution sufficiently stirs evenly, pour into the reaction kettle of 100ml polytetrafluoroethyllining lining, be put into baking oven and heated at 180 DEG C, added
Hot 3h；By resulting solution, be collected, clean, be centrifuged, it is dry in 60 DEG C of baking ovens under normal pressure after repeatedly grinding obtain it is orange
The BiOI powder of color；Obtained BiOI powder is added in the 50ml aqueous solution for the polyethylene glycol for being 2000 containing 10g molecular weight；
The copper sheet that acetone, dehydrated alcohol and the pretreated size of 0.1M hydrochloric acid solution are 3.5cm × 3.5cm will successively be passed through to be put into
It states in acquired solution；Heating water bath 16h in 70 DEG C of water-bath, and magneton is added and is stirred, stirring rate maintains 500r/
min；Resulting copper sheet is taken out after reaction, is dried to obtain CuI-BiOI/Cu laminated film in 60 DEG C of baking ovens under normal pressure
Material；
The used strain of experiment, at 37 DEG C, in MH(mueller hinton) PBS is used immediately after meat soup culture 18h
Solution dilution, the concentration of finally obtained bacterium are 106.5cfu /ml.In the entire experiment process, all glasswares and
PBS solution is all clean by deionized water and high pressure sterilization obtains after twenty minutes under 121 DEG C of high steams.Take 0.5ml dense
Degree is 106.5Cfu/ml bacterium solution is dispersed on freshly prepared nutrient agar panel, after standing five minutes, is by size
The CuI-BiOI/Cu laminated film of 1cm × 1cm is placed in the centre of nutrient agar panel, with xenon source (filter off 400nm with
Lower wavelength) simulated solar irradiation, carry out inhibition zone test experiments, light application time 2h.After illumination, nutrient agar panel is placed in 37
It is cultivated for 24 hours in DEG C constant incubator.Finally obtained inhibition zone is shown in Fig. 2 (circle represents its inhibition zone size in Fig. 2).
Embodiment 3
Be 55 DEG C in bath temperature, water bath time be for 24 hours under the conditions of the suppression of CuI-BiOI/Cu composite film material for preparing
The experiment of bacterium circle
The preparation of CuI-BiOI/Cu composite film material
To (the volume ratio 7:1 of ethylene glycol and water) in the mixed solution of 40ml ethylene glycol and water, the nitric acid of 13.3mL is added
Bismuth solution (concentration 0.3mol/L), 13.3mL liquor kalii iodide (concentration 0.3mol/L) and 50mg polyvinylpyrrolidone,
It after acquired solution is sufficiently stirred evenly, pours into the reaction kettle of 100ml polytetrafluoroethyllining lining, is put into baking oven and adds at 180 DEG C
Heat heats 3h；It by resulting solution, is collected, cleans, is centrifuged, ground repeatedly after drying in 60 DEG C of baking ovens under normal pressure
To orange-yellow BiOI powder；Obtained BiOI powder is added to the 50ml water for the polyethylene glycol for being 2000 containing 10g molecular weight
In solution；The copper that acetone, dehydrated alcohol and the pretreated size of 0.1M hydrochloric acid solution are 3.5cm × 3.5cm will successively be passed through
Piece is put into above-mentioned acquired solution；Heating water bath for 24 hours, and is added magneton and is stirred in 55 DEG C of water-bath, stirring rate dimension
It holds in 400r/min；Resulting copper sheet is taken out after reaction, is dried to obtain CuI-BiOI/Cu in 60 DEG C of baking ovens under normal pressure
Composite film material；
The used strain of experiment, at 37 DEG C, in MH(mueller hinton) PBS is used immediately after meat soup culture 18h
Solution dilution, the concentration of finally obtained bacterium are 106.5cfu /ml.In the entire experiment process, all glasswares and
PBS solution is all clean by deionized water and high pressure sterilization obtains after twenty minutes under 121 DEG C of high steams.Take 0.5ml dense
Degree is 106.5Cfu/ml bacterium solution is dispersed on freshly prepared nutrient agar panel, after standing five minutes, is by size
The CuI-BiOI/Cu laminated film of 1cm × 1cm is placed in the centre of nutrient agar panel, with xenon source (filter off 400nm with
Lower wavelength) simulated solar irradiation, carry out inhibition zone test experiments, light application time 2h.After illumination, nutrient agar panel is placed in 37
It is cultivated for 24 hours in DEG C constant incubator.Finally obtained inhibition zone is shown in Fig. 3 (circle represents its inhibition zone size in Fig. 3).
Embodiment 4
It is 40 DEG C in bath temperature, the suppression for the CuI-BiOI/Cu composite film material that water bath time is prepared under the conditions of being 12h
The experiment of bacterium circle
The preparation of CuI-BiOI/Cu composite film material
To (the volume ratio 7:1 of ethylene glycol and water) in the mixed solution of 40ml ethylene glycol and water, the bismuth nitrate of 20mL is added
Solution (concentration 0.2mol/L), 20mL liquor kalii iodide (concentration 0.2mol/L) and 10mg polyvinylpyrrolidone, by institute
After solution sufficiently stirs evenly, pour into the reaction kettle of 100ml polytetrafluoroethyllining lining, be put into baking oven and heated at 80 DEG C, added
Hot 6h；By resulting solution, be collected, clean, be centrifuged, it is dry in 60 DEG C of baking ovens under normal pressure after repeatedly grinding obtain it is orange
The BiOI powder of color；Obtained BiOI powder is added in the 50ml aqueous solution for the polyethylene glycol for being 2000 containing 10g molecular weight；
The copper sheet that acetone, dehydrated alcohol and the pretreated size of 0.1M hydrochloric acid solution are 3.5cm × 3.5cm will successively be passed through to be put into
It states in acquired solution；Heating water bath 12h in 40 DEG C of water-bath, and magneton is added and is stirred, stirring rate maintains 450r/
min；Resulting copper sheet is taken out after reaction, is dried to obtain CuI-BiOI/Cu laminated film in 60 DEG C of baking ovens under normal pressure
Material；
The used strain of experiment, at 37 DEG C, in MH(mueller hinton) PBS is used immediately after meat soup culture 18h
Solution dilution, the concentration of finally obtained bacterium are 106.5cfu /ml.In the entire experiment process, all glasswares and
PBS solution is all clean by deionized water and high pressure sterilization obtains after twenty minutes under 121 DEG C of high steams.Take 0.5ml dense
Degree is 106.5Cfu/ml bacterium solution is dispersed on freshly prepared nutrient agar panel, after standing five minutes, is by size
The CuI-BiOI/Cu laminated film of 1cm × 1cm is placed in the centre of nutrient agar panel, with xenon source (filter off 400nm with
Lower wavelength) simulated solar irradiation, carry out inhibition zone test experiments, light application time 2h.After illumination, nutrient agar panel is placed in 37
It is cultivated for 24 hours in DEG C constant incubator.Finally obtained inhibition zone is shown in Fig. 4 (circle represents its inhibition zone size in Fig. 4).
Embodiment 5
It is 70 DEG C in bath temperature, water bath time is the suppression of the CuI-BiOI/Cu composite film material prepared under 8 h conditions
The experiment of bacterium circle
The preparation of CuI-BiOI/Cu composite film material
To (the volume ratio 7:1 of ethylene glycol and water) in the mixed solution of 40ml ethylene glycol and water, the bismuth nitrate of 20mL is added
Solution (concentration 0.2mol/L), 20mL liquor kalii iodide (concentration 0.2mol/L) and 70mg polyvinylpyrrolidone, by institute
After solution sufficiently stirs evenly, pour into the reaction kettle of 100ml polytetrafluoroethyllining lining, be put into baking oven and heated at 130 DEG C, added
Hot 1h；By resulting solution, be collected, clean, be centrifuged, it is dry in 60 DEG C of baking ovens under normal pressure after repeatedly grinding obtain it is orange
The BiOI powder of color；Obtained BiOI powder is added in the 50ml aqueous solution for the polyethylene glycol for being 2000 containing 10g molecular weight；
The copper sheet that acetone, dehydrated alcohol and the pretreated size of 0.1M hydrochloric acid solution are 3.5cm × 3.5cm will successively be passed through to be put into
It states in acquired solution；Heating water bath 8h in 70 DEG C of water-bath, and magneton is added and is stirred, stirring rate maintains 400r/
min；Resulting copper sheet is taken out after reaction, is dried to obtain CuI-BiOI/Cu laminated film in 60 DEG C of baking ovens under normal pressure
Material；
The used strain of experiment, at 37 DEG C, in MH(mueller hinton) PBS is used immediately after meat soup culture 18h
Solution dilution, the concentration of finally obtained bacterium are 106.5cfu /ml.In the entire experiment process, all glasswares and
PBS solution is all clean by deionized water and high pressure sterilization obtains after twenty minutes under 121 DEG C of high steams.Take 0.5ml dense
Degree is 106.5Cfu/ml bacterium solution is dispersed on freshly prepared nutrient agar panel, after standing five minutes, is by size
The CuI-BiOI/Cu laminated film of 1cm × 1cm is placed in the centre of nutrient agar panel, with xenon source (filter off 400nm with
Lower wavelength) simulated solar irradiation, carry out inhibition zone test experiments, light application time 2h.After illumination, nutrient agar panel is placed in 37
It is cultivated for 24 hours in DEG C constant incubator.Finally obtained inhibition zone is shown in Fig. 5 (circle represents its inhibition zone size in Fig. 5)
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification, is all covered by the present invention.
Claims (8)
1. a kind of preparation method of the CuI-BiOI/Cu thin-film material 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 is added, it will
After acquired solution sufficiently stirs evenly, pours into the reaction kettle of 100ml polytetrafluoroethyllining lining, be put into baking oven and heated；
(2) it by step (1) resulting solution, is collected, cleans, is centrifuged, ground repeatedly after dry and obtain orange-yellow BiOI
Powder；
(3) the resulting BiOI powder of step (2) is added in the aqueous solution of polyethylene glycol；
(4) it will be put into step (3) acquired solution by pretreated copper sheet, water bath with thermostatic control heating is carried out under stirring；
(5) the resulting copper sheet of step (4) is taken out, is dried to obtain CuI-BiOI/Cu thin-film material.
2. a kind of preparation method of CuI-BiOI/Cu thin-film material with antibacterial functions according to claim 1, special
Sign is: in the mixed solution of ethylene glycol described in step (1) and 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 material with antibacterial functions according to claim 1, special
Sign is: the concentration of bismuth nitrate solution and liquor kalii iodide in the step (1) is 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 material with antibacterial functions according to claim 1, special
Sign is: the technological parameter of heating process in the step (1) are as follows: heating temperature is 80 ~ 180 DEG C；Heating time is 1 ~ 6h.
5. a kind of preparation method of CuI-BiOI/Cu thin-film material with antibacterial functions according to claim 1, special
Sign is: the concentration of the aqueous solution of polyethylene glycol described in step (3) is 0.1 ~ 0.4g/mL.
6. a kind of preparation method of CuI-BiOI/Cu thin-film material with antibacterial functions according to claim 1, special
Sign is: water bath with thermostatic control described in step (4) heating technological parameter are as follows: heating temperature be 40 ~ 70 DEG C, heating time be 6 ~
24h。
7. a kind of preparation method of CuI-BiOI/Cu thin-film material with antibacterial functions according to claim 1, special
Sign is: pretreated copper sheet described in step (4) the preparation method comprises the following steps: copper sheet is successively passed through acetone, dehydrated alcohol and
After the pretreatment of 0.1M hydrochloric acid solution, the copper sheet that size is 3.5cm × 3.5cm is obtained.
8. a kind of preparation method of CuI-BiOI/Cu thin-film material with antibacterial functions according to claim 1, special
Sign is: the drying temperature in step (2) and step (5) is 50 ~ 80 DEG C.
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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 |
| CN104393099A (en) * | 2014-10-09 | 2015-03-04 | 浙江大学 | Preparation method of sodium yttrium tetrafluoride bismuth oxyiodide composite solar film |
| CN105709782A (en) * | 2016-03-09 | 2016-06-29 | 安徽工业大学 | Preparing method and application of Ag/AgBr/BiOCl-(001) nanometer composite material |
| 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 |
| CN106964379A (en) * | 2017-03-23 | 2017-07-21 | 福州大学 | Contain ZnI with photocatalysis antibacterial function2The preparation method of I/ZnO composites |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104393099A (en) * | 2014-10-09 | 2015-03-04 | 浙江大学 | Preparation method of sodium yttrium tetrafluoride bismuth oxyiodide composite solar film |
| CN105709782A (en) * | 2016-03-09 | 2016-06-29 | 安徽工业大学 | Preparing method and application of Ag/AgBr/BiOCl-(001) nanometer composite material |
| 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 |
| CN106964379A (en) * | 2017-03-23 | 2017-07-21 | 福州大学 | Contain ZnI with photocatalysis antibacterial function2The preparation method of I/ZnO composites |
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