CN107789673A - A kind of three-dimensional flower-shaped hybrid coating preparation method with photocatalysis performance excited by 660 nano red lights - Google Patents
A kind of three-dimensional flower-shaped hybrid coating preparation method with photocatalysis performance excited by 660 nano red lights Download PDFInfo
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- CN107789673A CN107789673A CN201710858473.9A CN201710858473A CN107789673A CN 107789673 A CN107789673 A CN 107789673A CN 201710858473 A CN201710858473 A CN 201710858473A CN 107789673 A CN107789673 A CN 107789673A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
- A61L31/08—Materials for coatings
- A61L31/082—Inorganic materials
- A61L31/084—Carbon; Graphite
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
- A61L31/02—Inorganic materials
- A61L31/022—Metals or alloys
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
- A61L31/14—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2420/00—Materials or methods for coatings medical devices
- A61L2420/02—Methods for coating medical devices
Abstract
A kind of three-dimensional flower-shaped hybrid coating preparation method with photocatalysis performance excited by 660 nano red lights, specifically comprises the following steps：S1, three-dimensional flower-shaped titanium dioxide nano-rod preparation；The preparation of molybdenum disulfide petal on S2, three-dimensional flower-shaped titanium dioxide nano-rod；S3, graphene oxide spin coating：The step S2 titanium sheet obtained is adsorbed on spin coating instrument, then graphene oxide solution is spun on titanium plate surface, repeats 46 times, that is, obtains the three-dimensional flower-shaped hybrid coating with photocatalysis performance.Its advantage is：In the flower-shaped titanium dioxide nano-rod of titanium plate surface growing three-dimensional, the load area of molybdenum disulfide is increased, there is good light power antibacterial activity, generation active oxygen that both under visible light illumination can be rapidly and efficiently, so as to kill bacterium, while bacterium will not be made to produce drug resistance.
Description
Technical field
It is more particularly to a kind of to be excited by 660 nano red lights the present invention relates to material science and technical field of nano material
Three-dimensional flower-shaped hybrid coating preparation method with photocatalysis performance.
Background technology
Got more and more people's extensive concerning as the bacterium infection caused by medical implant, various antibacterials are largely made
With although the problem of largely solving bacterium infection, it also has potential hidden danger, that is, the life of drug-fast bacteria
Into；Therefore, a kind of product having enhanced antibacterial action how is prepared, while the antimicrobial coating that will not produce drug tolerant bacteria again is urgently to solve at present
Technical problem certainly.
The content of the invention
, specifically will oxidation the invention provides a kind of three-dimensional flower-shaped hybrid coating preparation method with photocatalysis performance
Graphene, molybdenum disulfide and titanium dioxide three organically combine, and pass through three-dimensional flower-shaped titanium dioxide nano-rod, it is possible to increase
The load capacity of molybdenum disulfide and three-dimensional molybdenum disulfide increases molybdenum disulfide specific surface area, improve its photocatalysis efficiency, and finally
One layer of graphene oxide of covering can promote the light power performance of prepared hybrid coating material.
A kind of three-dimensional flower-shaped hybrid coating preparation method with photocatalysis performance excited by 660 nano red lights, specifically
Comprise the following steps：
S1, three-dimensional flower-shaped titanium dioxide nano-rod preparation：First concentrated hydrochloric acid, butyl titanate are mixed, to prepare mixing
Liquid A, then the mixed liquor A of preparation is reacted to entering to be placed with the reactor of titanium sheet, question response take out titanium sheet, standby after terminating；
The preparation of molybdenum disulfide petal on S2, three-dimensional flower-shaped titanium dioxide nano-rod：Sodium molybdate, thioacetamide is taken to be dissolved in
In deionized water, and stir, to obtain mixed liquid B；The step S1 titanium sheet obtained is put into reactor again, while will be mixed
Close liquid B and also arrive in the reactor equipped with titanium sheet and react；
S3, graphene oxide spin coating：The step S2 titanium sheet obtained is adsorbed on spin coating instrument, then graphene oxide is molten
Liquid is spun on titanium plate surface, repeats 4-6 times, that is, obtains the three-dimensional flower-shaped hybrid coating with photocatalysis performance.
Preferably, step S1 comprises the following steps：
S11, deionized water stirring 5min will be added in concentrated hydrochloric acid, after making it well mixed, add butyl titanate and stir
Mix to be prepared into mixed liquor A, wherein, the mixed liquor of every 40ml hydrochloric acid and deionized water adds 0.955ml butyl titanates, and hydrochloric acid
Volume ratio with deionized water is 1:1；
S12, the step S11 mixed liquor As prepared are put into the reactor equipped with titanium sheet, it is anti-under the conditions of 140-160 DEG C
Answer 4-6h；
S13, titanium sheet is taken out after step S12 reactions terminate, and be washed with deionized and dry, be standby.
Further, concentrated hydrochloric acid mass fraction is 36%-38% in step S11, and the concentration of butyl titanate is 98%；
In step S11,10~20min is stirred after adding butyl titanate；Preferably 15min；
In step S12, reaction temperature is 150 DEG C, and the reaction time is 5 hours；
Preferably, in step S2, sodium molybdate, thioacetamide, the volume ratio of deionized water are 1:2:2；And sodium molybdate
Concentration is 0.5mg/ml, and the concentration of thioacetamide is 1mg/ml；
Further, in step S2,30min is stirred；And titanium sheet reacts 23- under the conditions of in reactor 190-210 DEG C
25h；It is preferred that 200 DEG C, reaction time 24h；
Further, in step S2, will be washed successively with deionized water, ethanol in reacted titanium sheet in reactor, then
It is dry, standby.
Preferably, in step S3, graphene oxide solution concentration is 0.5mg/ml, and the amount being added dropwise is 25-35 μ l；It is preferred that
Spin coating number is 5 times, and the amount that graphene oxide solution is added dropwise is 30 μ l.
A kind of three-dimensional flower-shaped hybrid coating preparation method with photocatalysis performance excited by 660 nano red lights, has
Following advantage：
(1) because molybdenum disulfide has good photocatalysis characteristic, activity can be quickly produced under 660nm radiation of visible light
Oxygen, the materials such as DNA, protein and the unrighted acid of bacterium are destroyed by active oxygen, can effectively kill bacterium；Cause
For this present invention by hydro-thermal method in the flower-shaped titanium dioxide nano-rod of titanium plate surface growing three-dimensional, its combination is more firm, and increases
The load area of molybdenum disulfide, that is, add the load capacity of molybdenum disulfide；Molybdenum disulfide forms three-dimensional structure simultaneously, this knot
Structure is advantageous to absorb the photocatalysis performance that photon improves titanium dioxide and molybdenum disulfide；
(2) add graphene oxide can by itself energy fast transfer electronics, specific surface area is big the characteristics of, can be quick
Caused electronics is transferred to surface of graphene oxide after titanium dioxide/molybdenum disulfide is absorbed into photon, effectively improves active oxygen
Generation speed, avoid the internal consumption of electronics, so as to improve the photocatalysis performance of material, improve antibacterial activity；May be used also simultaneously
To improve the propagation of stem cell and differentiation, cytotoxicity is low., can be with and graphene oxide has many oxygen-content active functional groups
Easily combined with other materials, further promote its biocompatibility or connect other antibacterials to be used for antibacterial；
(3) hybrid coating prepared has good light power antibacterial activity, both under visible light illumination can be rapidly and efficiently
Generation active oxygen, so as to kill bacterium, at the same will not make bacterium produce drug resistance.
Brief description of the drawings
Fig. 1 is the SEM figures that titanium dioxide is grown in embodiment 1, embodiment 3, embodiment 4；
Fig. 2 is the figure of regrowth molybdenum disulfide after growth titanium dioxide in embodiment 1, embodiment 4；
Fig. 3 is that the SEM in embodiment 2 in the flower-shaped molybdenum disulfide of titanium plate surface growing three-dimensional schemes；
Fig. 4 be in embodiment 2 after the flower-shaped molybdenum disulfide of titanium plate surface growing three-dimensional the SEM of grafted graphene oxide again
Figure；
Fig. 5 is that sample EDS schemes in embodiment 1；
Fig. 6 is obtained the antimicrobial flat-plate figure of product progress by embodiment 1；
Fig. 7 is obtained the antimicrobial flat-plate figure of product progress by embodiment 2；
Fig. 8 is obtained the antimicrobial flat-plate figure of product progress by embodiment 3；
Fig. 9 is obtained the antimicrobial flat-plate figure of product progress by embodiment 4.
Embodiment
To be best understood from the present invention, the present invention is done further described in detail with reference to the accompanying drawings and examples：
The mass fraction of hydrochloric acid used is 36%-38% in following embodiments；The purity of the butanol of metatitanic acid four is 98%.
Embodiment 1：
(1) by medical titanium sheet respectively with the sand paper that specification is 240#, 400#, 600#, 800#, 1200# in polishing grinding machine
On be polishing to smooth mirror surface, washing is standby；
(2) 20ml concentrated hydrochloric acids and 20ml deionized waters are mixed 5 minutes, then adds the fourth of 0.955ml metatitanic acids four
Ester stirs 15 minutes, obtains mixed liquor A, finally pours into mixed liquor and be placed with the 50ml reactors of titanium sheet, reacted at 150 DEG C
5 hours, question response terminate after take out titanium sheet be washed with deionized dry (the three-dimensional flower-shaped titanium dioxide nano-rod figure of acquisition is such as
Shown in Fig. 1)；
(3) take 20mg sodium molybdates and 40mg thioacetamides to be dissolved in 40ml deionized waters, stir 30 minutes, mixed
Liquid B.Above-mentioned titanium sheet is placed again into reactor, and the mixed liquid B prepared is poured into reactor, reacts 24 at 200 DEG C
Hour, finally washed and dried (SEM for obtaining material schemes as shown in Figure 2) with deionized water and ethanol successively；
(4) 30 μ l 0.5mg/ml graphene oxide solution is added dropwise on spin coating instrument in titanium sheet obtained above absorption,
And graphene oxide is uniformly spin-coated on by titanium plate surface by high speed rotation, it is repeated 5 times.
The experiment effect of embodiment 1 can be seen that Fig. 1：Titanium sheet is received by the flower-shaped titanium dioxide of hydro-thermal reaction growing three-dimensional
Picture after rice rod, titanium dioxide can be grown in titanium plate surface very well, while increase the growth area of molybdenum disulfide；Fig. 2：Water
SEM figures after thermally grown molybdenum disulfide, it is seen that on titanium dioxide nano-rod, stereochemical structure has molybdenum disulfide petal homoepitaxial
Beneficial to its photocatalysis performance of raising；
Embodiment 2：
(1) by medical titanium sheet respectively with the sand paper that specification is 240#, 400#, 600#, 800#, 1200# in polishing grinding machine
On be polishing to smooth mirror surface, washing is standby；
(2) take 20mg sodium molybdates and 40mg thioacetamides to be dissolved in 40ml deionized waters, stir 30 minutes.By above-mentioned titanium
Piece is put into reactor, and the mixed liquor prepared is poured into reactor, is reacted 24 hours at 200 DEG C, is finally spent successively
Ionized water and ethanol washing are dried (as shown in Figure 3 in the SEM figures of the flower-shaped molybdenum disulfide of titanium plate surface growing three-dimensional)；
(3) 30 μ l 0.5mg/ml graphene oxide solution is added dropwise on spin coating instrument in titanium sheet obtained above absorption,
And graphene oxide is uniformly spin-coated on by titanium plate surface by high speed rotation, it is repeated 5 times (in titanium plate surface growing three-dimensional flower-shaped two
The SEM figures of grafted graphene oxide are as shown in Figure 4 again after molybdenum sulfide).
The experiment effect of embodiment 2 can be seen that molybdenum disulfide load area is small, load capacity is low and non-cubic structure.
Embodiment 3：
(1) by medical titanium sheet respectively with the sand paper that specification is 240#, 400#, 600#, 800#, 1200# in polishing grinding machine
On be polishing to smooth mirror surface, washing is standby；
(2) 20ml concentrated hydrochloric acids and 20ml deionized waters are mixed 5 minutes, then adds 1ml butyl titanates and stir
Mix 15 minutes, finally mixed liquor is poured into and is placed with the 50ml reactors of titanium sheet, reacted 5 hours at 150 DEG C, question response terminates
Titanium sheet is taken out afterwards to be washed with deionized dry (the three-dimensional flower-shaped titanium dioxide nano-rod figure of acquisition is as shown in Figure 1)；
(3) 30 μ l 0.5mg/ml graphene oxide solution is added dropwise on spin coating instrument in titanium sheet obtained above absorption,
And graphene oxide is uniformly spin-coated on by titanium plate surface by high speed rotation, it is repeated 5 times.
Embodiment 4：
(1) by medical titanium sheet respectively with the sand paper that specification is 240#, 400#, 600#, 800#, 1200# in polishing grinding machine
On be polishing to smooth mirror surface, washing is standby；
(2) 20ml concentrated hydrochloric acids and 20ml deionized waters are mixed 5 minutes, then adds 1ml butyl titanates and stir
Mix 15 minutes, finally mixed liquor is poured into and is placed with the 50ml reactors of titanium sheet, reacted 5 hours at 150 DEG C, question response terminates
Titanium sheet is taken out afterwards to be washed with deionized dry (the three-dimensional flower-shaped titanium dioxide nano-rod figure of acquisition is as shown in Figure 1)；
(3) take 20mg sodium molybdates and 40mg thioacetamides to be dissolved in 40ml deionized waters, stir 30 minutes.By above-mentioned titanium
Piece is placed again into reactor, and the mixed liquor prepared is poured into reactor, reacts 24 hours at 200 DEG C, successively finally
Washed and dried (the SEM figures for obtaining material are as shown in Figure 2) with deionized water and ethanol；
The product of acquisition is detected, specific detection is as follows：
First, detect whether each element is coated on titanium, and it is in combination；
The product that embodiment 1 obtains is detected by energy disperse spectroscopy, (S overlaps with Mo peak) as shown in Figure 5, explanation
Titanium, molybdenum, sulphur are covered on titanium, while illustrate that hybrid coating is successfully prepared；
2nd, the product for obtaining embodiment 1 to embodiment 4 is divided into four groups, is added respectively together with bacterium solution in 96 orifice plates, warp
After crossing 660 nanometers of radiation of visible light 15min, extraction bacterium solution does flat board coating (the flat board coating result of embodiment 1 to embodiment 4
Successively as shown in Fig. 6 to 9), each bacterium colony represents a bacterium, the fewer representative sample antibacterial ability of bacterial number in flat board coating
Better.It was found from Fig. 6 to Fig. 9, the anti-microbial property of embodiment one is best.
Symbol below Fig. 1 is identical with Fig. 2.
From above-described embodiment and detection：
1) proved by SEM, hydro-thermal method can be with the flower-shaped titanium dioxide nano-rod of growing three-dimensional, while molybdenum disulfide can pass through
Hydrothermal Growth adds the load capacity of molybdenum disulfide, while this stereochemical structure formed can improve on titanium dioxide stud surface
The photocatalysis efficiency of coating；
2) can be proved by flat board coating, this coating can be effective in the short time under 660nm radiation of visible light
Bacterium is killed, and does not have antibacterial ability under dark condition, at the same it is little to impact cell；
3) by flat board coat prove, lack titanium dioxide, three kinds of materials of molybdenum disulfide and graphene oxide it is any
When a kind of, the antibacterial ability of its coating can all decline, and only triplicity can be only achieved good antibacterial effect.
It the above is only the concrete application example of the present invention, protection scope of the present invention be not limited in any way.Except above-mentioned
Outside embodiment, the present invention can also have other embodiment.All technical schemes formed using equivalent substitution or equivalent transformation,
Fall within scope of the present invention.
Claims (8)
1. a kind of three-dimensional flower-shaped hybrid coating preparation method with photocatalysis performance excited by 660 nano red lights, its feature
It is：Specifically comprise the following steps：
S1, three-dimensional flower-shaped titanium dioxide nano-rod preparation：First concentrated hydrochloric acid, butyl titanate are mixed, to prepare mixed liquor A,
The mixed liquor A of preparation is reacted to entering to be placed with the reactor of titanium sheet again, question response takes out titanium sheet, standby after terminating；
The preparation of molybdenum disulfide petal on S2, three-dimensional flower-shaped titanium dioxide nano-rod：Take sodium molybdate, thioacetamide be dissolved in from
In sub- water, and stir, to obtain mixed liquid B；The step S1 titanium sheet obtained is put into reactor again, while by mixed liquor
B, which is also arrived in the reactor equipped with titanium sheet, to react；
S3, graphene oxide spin coating：The step S2 titanium sheet obtained is adsorbed on spin coating instrument, then graphene oxide solution is revolved
Titanium plate surface is applied to, repeats 4-6 times, that is, obtains the three-dimensional flower-shaped hybrid coating with photocatalysis performance.
2. method according to claim 1, it is characterised in that：
Step S1 comprises the following steps：
S11, deionized water stirring 5min will be added in concentrated hydrochloric acid, after making it well mixed, add butyl titanate stirring with
Mixed liquor A is prepared into, wherein, the mixed liquor of every 40ml hydrochloric acid and deionized water adds 0.955ml butyl titanates；
S12, the step S11 mixed liquor As prepared are put into the reactor equipped with titanium sheet, 4- is reacted under the conditions of 140-160 DEG C
6h；
S13, titanium sheet is taken out after step S12 reactions terminate, and be washed with deionized and dry, be standby.
3. method according to claim 2, it is characterised in that：The volume ratio of hydrochloric acid and deionized water is 1:1.
4. method according to claim 1, it is characterised in that：Concentrated hydrochloric acid mass fraction is 36%-38% in step S11, titanium
The concentration of sour four butyl esters is 98%.
5. method according to claim 2, it is characterised in that：10~20min is stirred after adding butyl titanate.
6. method according to claim 1, it is characterised in that：In step S2, sodium molybdate, thioacetamide, deionized water
Volume ratio is 1:2:2；And the concentration of sodium molybdate is 0.5mg/ml, the concentration of thioacetamide is 1mg/ml.
7. method according to claim 1, it is characterised in that：In step S2,30min is stirred；And titanium sheet is in reactor
23-25h is reacted under the conditions of 190-210 DEG C.
8. method according to claim 1, it is characterised in that：In step S3, graphene oxide solution concentration is 0.5mg/ml,
And the amount being added dropwise is 25-35 μ l.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110624532A (en) * | 2019-09-19 | 2019-12-31 | 华南理工大学 | TiO 22-BiVO4-graphene ternary composite photocatalytic material and preparation method thereof |
| CN113058622A (en) * | 2021-03-26 | 2021-07-02 | 安徽大学 | Nickel sulfide/molybdenum disulfide composite nano array for photoelectrocatalysis killing of drug-resistant bacteria and preparation method thereof |
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| CN103521163A (en) * | 2013-10-16 | 2014-01-22 | 江苏大学 | Method for preparing nanometer composite with chrysanthemum structure |
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Application publication date: 20180313 |