CN106917131B - A kind of preparation method of chitosan/molybdenum disulfide photocatalysis antibacterial coating - Google Patents
A kind of preparation method of chitosan/molybdenum disulfide photocatalysis antibacterial coating Download PDFInfo
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- CN106917131B CN106917131B CN201710111951.XA CN201710111951A CN106917131B CN 106917131 B CN106917131 B CN 106917131B CN 201710111951 A CN201710111951 A CN 201710111951A CN 106917131 B CN106917131 B CN 106917131B
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Abstract
The present invention provides a kind of preparation methods of chitosan/molybdenum disulfide photocatalysis antibacterial coating, the method makes titanium alloy surface have loose porous bigger serface structure by alkali heat-treatment, then so that titanium alloy surface is had by electro-deposition and not only possess visible light catalytic antibacterial effect, but also chitosan/molybdenum disulfide visible light catalytic antimicrobial coating with preferable biocompatibility.Preparation method of the present invention is simple, and reaction medium is recyclable, and chitosan and molybdenum disulfide nano composite coating with bioactivity and photocatalysis antibacterial are prepared with electrophoretic deposition；The present invention prepares gained chitosan and molybdenum disulfide nano photocatalysis antibacterial coating, while capable of making chitosan that molybdenum disulfide be helped to improve antibiotic property, improves the bioactivity of molybdenum disulfide.
Description
Technical field
The present invention relates to material science and technical field of nano material, more particularly to a kind of chitosan/molybdenum disulfide light is urged
Change the preparation method of antimicrobial coating.
Background technology
Class grapheme two-dimension material MoS2, have with layer structure as graphite-like, between layers by relatively weak
Van der Waals force maintains, and in machinery, electronics, the fields such as photocatalysis show many excellent properties, and in biomedicine field exhibition
Reveal application potential, however its still have in the influence of environment and biology it is to be developed.Laminar nano MoS2Energy gap exist
1.80eV or so has photocatalytic activity under visible light, simultaneously as the MoS of nanostructure2There are one larger ratio tables
Area can enhance its catalytic activity
Currently, nano molybdenum disulfide preparation method mainly has liquid phase method and solid phase method two major classes：There are product rulers for liquid phase method
It is very little it is not easy to control with pattern, bad dispersibility, easily polymerize, the features such as crystallinity is poor：There are the high products of reaction temperature for solid phase method
Or often contain the sulfurous gas of pollution environment in reactant.Therefore.The research of nano molybdenum disulfide should be concentrated on following two
Aspect：(1) low cost, cleaning nano molybdenum disulfide new preparation process exploitation；(2) application of different-shape nano molybdenum disulfide is opened
Hair research.
Chitosan (chitosan) is also known as chitosan, is chitin (chitin) warp being widely present by nature
Cross what deacetylation obtained, chemical name is Chitosan (1-4) -2- amino-B-D glucose.From 1859, Frenchman
After Rouget obtains chitosan first, the biological functionality and compatibility of this natural polymer, blood compatibility, safety,
The excellent performances such as microbic resolvability are by all trades and professions extensive concern, in medicine, food, chemical industry, cosmetics, water process, metal
The application of the numerous areas such as extraction and recycling, biochemical and biomedical engineering is gradually exploited.Chitosan surfactant category
In sugar surfactants, good surface-active is shown.Such surfactant is nontoxic, nuisanceless, has good pH steady
Qualitative energy, antioxygenic property, therefore it can be applied in cosmetic formulations and food completely, chitosan surfactant is in addition
Pure natural surfactant has the properties such as good surface-active, emulsibility, moisture absorbability and moisture retentivity, solubilising, antibiotic property,
It can be used widely in the multiple fields such as washing, medicine, food, cosmetics, textile printing and dyeing, oil, environmental protection.
Characteristic and the mutual effect for how utilizing molybdenum disulfide and chitosan, improve the antibacterial on medical implant surface
Ability is a direction for being worth research.
Invention content
To solve the above-mentioned problems, the present invention provides a kind of preparations of chitosan/molybdenum disulfide photocatalysis antibacterial coating
Method, the method make titanium alloy surface have loose porous bigger serface structure, then pass through electricity by alkali heat-treatment
Deposition makes titanium alloy surface have and not only possesses visible light catalytic antibacterial effect, but also the chitosan with preferable biocompatibility/
Molybdenum disulfide visible light catalytic antimicrobial coating.
The technical scheme is that：A kind of preparation method of chitosan/molybdenum disulfide photocatalysis antibacterial coating, feature
It is, specifically comprises the following steps：
S1. 100-250mg molybdenum disulfide and 100-200mg chitosans are put into mortar and grind 15-30min, added
In the ionic liquid to mortar of 0.5ml, 60-120min is then ground again；
S2. grinding product is collected, it is 0.5-1%'s to use acetone, n,N-Dimethylformamide (DMF) and mass concentration successively
Grinding product described in acetic acid centrifuge washing, the acetone, n,N-Dimethylformamide (DMF) and mass concentration are 0.5-1%'s
Acetic acid respectively washs grinding product three times, removes grinding product intermediate ion liquid and extra chitosan (CS)；After the completion of washing
Obtained precipitation is distributed in deionized water, centrifuges 20min in 1500-1800rpm speed to remove unstripped molybdenum disulfide
(MoS2), chitosan/molybdenum disulfide nano disperse system is obtained, by the chitosan/molybdenum disulfide nano disperse system (CS-MoS2)
It is diluted to 100ml with deionized water and obtains chitosan/molybdenum disulfide disperse system solution, the chitosan/molybdenum disulfide is disperseed
It is that solution storage is for use at 4 DEG C；
S3. titanium alloy round abrasive sheet is polished step by step, is cleaned by ultrasonic in ethyl alcohol, deionized water successively, cleaned titanium
2-4min is etched with the mixed acid solution of deionized water/nitric/hydrofluoric after piece drying, is cleaned later with deionized water；
S4. titanium alloy disk etched made from step S2 is put into the reaction kettle for filling NaOH solution, then again
Reaction kettle is put into baking oven, reacts 2-3h at 60-80 DEG C, surface, which is made, has the titanium alloy disk of porous coarse structure,
Cleaning titanium alloy disk obtained；
S5. 1-1.5ml acetic acid and 4-5ml second are added in the chitosan/molybdenum disulfide disperse system solution configured to step S2
Alcohol, ultrasonic 1.5-2h, magnetic agitation 22-24h；
S6. the chitosan being stirred using in step S5/molybdenum disulfide disperse system solution is as electrodeposit liquid, by step S4 systems
The titanium alloy disk obtained makees cathode, and platinum plate electrode makees anode, electrode distance 10mm, voltage 40-60V, and sedimentation time is
150-300s；The titanium alloy disk that overlay film is taken out from the electrodeposit liquid sprays the titanium alloy disk table with clear water
Face removes the extra substance of adsorption, places into drying oven, goes moisture removal to get to chitosan/bis- of titanium alloy surface
Molybdenum sulfide photocatalysis antibacterial coating.
The step S1 intermediate ion liquid is 1- butyl -3- methylimidazole hexafluorophosphates.
The volume parts of each component are in the mixed acid solution of deionized water/nitric/hydrofluoric in the step S3：5 parts
Ionized water, 2-4 part nitric acid and 1-3 parts of hydrofluoric acid.
The nitric acid is that analysis is pure；The hydrofluoric acid is that analysis is pure.
Drying oven setting temperature is 150 DEG C in the step S6, baking time 60min.
The present invention technique effect be：
(1) synthesis chitosan/molybdenum disulfide lamellar structure takes short and is not necessarily to expensive equipment；
(2) due to the related photocatalytic activity of molybdenum disulfide, then compared to simple chitosan film, prepared by the present invention
Because the synergistic effect of molybdenum disulfide and chitosan makes it have better visible light catalytic antibiotic property in antimicrobial coating；
(3) described preparation method is simple, and the medium of first step reaction is ionic liquid, recyclable, environmentally protective, electricity
Swimming deposition chitosan is nontoxic as dispersant and surfactant, there is good pH stabilities, chitosan/bis- obtained
Molybdenum sulfide antimicrobial coating has better storage stability, with titanium-based there is good associativity and good biocompatibility,
Possibility is provided for application of the function molybdenum disulfide coating in nanometer medicine.
To sum up, preparation method of the present invention is simple, and reaction medium is recyclable, and being prepared with electrophoretic deposition has bioactivity
With the chitosan and molybdenum disulfide nano composite coating of photocatalysis antibacterial；The present invention prepares gained chitosan and is received with molybdenum disulfide
Rice photocatalysis antibacterial coating, while capable of making chitosan that molybdenum disulfide be helped to improve antibiotic property, the biology for improving molybdenum disulfide is living
Property.
Description of the drawings
Fig. 1 is the SEM of the titanium alloy disk with chitosan/molybdenum disulfide visible light catalytic antimicrobial coating in embodiment 1
Figure.
Fig. 2-1 is that pure titanium disk coats titanium alloy disk in the discontinuous visible light photographs of 10min with composite coating in embodiment 2
Under to the antibacterial effect figures of Escherichia coli.
Fig. 2-2 is that pure titanium disk coats titanium alloy disk in the discontinuous visible light photographs of 10min with composite coating in embodiment 2
Under to the antibacterial effect figure of staphylococcus aureus.
Fig. 3-1 is the SEM figures of pure titanium alloy surface Escherichia coli in embodiment 3.
Fig. 3-2 is the big of the titanium alloy disk surfaces with chitosan/molybdenum disulfide photocatalysis antibacterial coating in embodiment 3
The SEM of enterobacteria schemes.
Fig. 3-3 is the SEM figures of the staphylococcus aureus of pure titanium alloy surface in embodiment 3.
Fig. 3-4 is the gold of the titanium alloy disk surfaces with chitosan/molybdenum disulfide photocatalysis antibacterial coating in embodiment 3
The SEM of staphylococcus aureus schemes.
Specific implementation mode
To be best understood from the present invention, the present invention is done further be described in detail with reference to the accompanying drawings and examples, still
The scope of protection of present invention is not limited to the range of embodiment expression.
Embodiment 1：
250mg molybdenum disulfide is put into mortar with 200mg chitosans and grinds 30min, the 1- butyl -3- methyl miaows of 0.5ml
Azoles hexafluorophosphate (ion assisted milling solution) is added in mortar, and then another straight grinding 120min, collects grinding product,
Use acetone successively, the acetic acid of DMF and 1% carrys out centrifuge washing product with 9000rpm, each washing three times, come remove ionic liquid and
Extra chitosan.Finally, make precipitation dispersion in deionized water, it is unstripped to remove in 1800rpm speed centrifugation 20min
MoS2, the chitosan/molybdenum disulfide nano disperse system obtained at this time is diluted to 100ml with deionized water and obtains the sulphur of chitosan/bis-
Change molybdenum research on nano-disperse systems solution and be stored at 4 DEG C, for use.
Titanium alloy disk (diameter 6mm, thickness 2.5mm) sand paper is polished step by step, until 800#, successively in ethyl alcohol, go from
It is cleaned by ultrasonic in sub- water, it is 5 that cleaned titanium sheet uses volume ratio after the drying:4:1 deionized water/nitric/hydrofluoric nitration mixture
Solution etches 2min, is cleaned with deionized water later, and then etched titanium alloy disk is put into reaction kettle, reaction kettle
In fill the NaOH solution of outfit, reaction kettle is put into baking oven, reacts 2h at 80 DEG C, is made with porous coarse structure
Surface, after the completion cleaning sample.
The addition 1ml acetic acid into the chitosan previously configured/molybdenum disulfide disperse system solution, 5ml ethyl alcohol, ultrasonic 1.5h,
For 24 hours, obtained chitosan/molybdenum disulfide disperse system solution, will be aforementioned obtained with porous as electrodeposit liquid for magnetic agitation
The titanium alloy disk of coarse structure makees cathode, and platinum plate electrode makees anode, electrode distance 10mm, voltage 40V, and sedimentation time is
150s.The print that overlay film is taken out from electrodeposit liquid sprays sample surface with clear water, removes the fifth wheel of adsorption
Matter is put into 150 DEG C of drying oven, keeps this temperature 60min, removes moisture removal, obtains titanium alloy surface chitosan/molybdenum disulfide light and urges
Change antimicrobial coating.
Embodiment 2：
250mg molybdenum disulfide is put into mortar with 100mg chitosans and grinds 15min, the 1- butyl -3- methyl miaows of 0.5ml
Azoles hexafluorophosphate (ion assisted milling solution) is added in mortar, and then another straight grinding 90min, collects grinding product,
Acetone, the acetic acid of DMF and 0.5% is used to carry out centrifuge washing product with 9000rpm successively, it is each to wash three times, to remove ionic liquid
With extra chitosan.Finally, make precipitation dispersion in deionized water, it is unstripped to remove in 1500rpm speed centrifugation 20min
MoS2, the chitosan/molybdenum disulfide nano disperse system obtained at this time is diluted to 100ml with deionized water and obtains chitosan/bis-
Molybdenum sulfide research on nano-disperse systems solution is simultaneously stored at 4 DEG C, for use.
Titanium alloy disk (diameter 6mm, thickness 2.5mm) sand paper is polished step by step, until 800#, successively in ethyl alcohol, go from
It is cleaned by ultrasonic in sub- water, it is 5 that cleaned titanium sheet uses volume ratio after the drying:2:3 deionized water/nitric/hydrofluoric nitration mixture
Solution etches 4min, is cleaned with deionized water later, and then etched titanium alloy disk is put into reaction kettle, reaction kettle
In fill the NaOH solution of outfit, reaction kettle is put into baking oven, reacts 2h at 80 DEG C, is made with porous coarse structure
Surface, after the completion cleaning sample.
1.5ml acetic acid, 5ml ethyl alcohol, ultrasound are added into the chitosan previously configured/molybdenum disulfide disperse system solution
1.5h, magnetic agitation 22h, obtain chitosan/molybdenum disulfide disperse system solution as electrodeposit liquid, will it is aforementioned it is obtained have it is more
The titanium alloy disk of hole coarse structure makees cathode, and platinum plate electrode makees anode, electrode distance 10mm, voltage 20V, sedimentation time
For 150s.The print that overlay film is taken out from electrodeposit liquid sprays sample surface with clear water, removes the fifth wheel of adsorption
Matter is put into 150 DEG C of drying oven, keeps this temperature 60min, removes moisture removal, obtains titanium alloy surface chitosan/molybdenum disulfide light and urges
Change antimicrobial coating.
Embodiment 3：
150mg molybdenum disulfide is put into mortar with 200mg chitosans and grinds 30min, the 1- butyl -3- methyl miaows of 0.5ml
Azoles hexafluorophosphate (ion assisted milling solution) is added in mortar, and then another straight grinding 120min, collects grinding product,
Use acetone successively, the acetic acid of DMF and 1% carrys out centrifuge washing product with 9000rpm, each washing three times, come remove ionic liquid and
Extra chitosan.Finally, make precipitation dispersion in deionized water, it is unstripped to remove in 1800rpm speed centrifugation 20min
MoS2, the chitosan/molybdenum disulfide nano disperse system obtained at this time is diluted to 100ml with deionized water and obtains the sulphur of chitosan/bis-
Change molybdenum research on nano-disperse systems solution and be stored at 4 DEG C, for use.
Titanium alloy disk (diameter 6mm, thickness 2.5mm) sand paper is polished step by step, until 800#, successively in ethyl alcohol, go from
It is cleaned by ultrasonic in sub- water, it is 5 that cleaned titanium sheet uses volume ratio after the drying:3:2 deionized water/nitric/hydrofluoric nitration mixture
Solution etches 6min, is cleaned with deionized water later, and then etched titanium alloy disk is put into reaction kettle, reaction kettle
In fill the NaOH solution of outfit, reaction kettle is put into baking oven, reacts 2h at 80 DEG C, is made with porous coarse structure
Surface, after the completion cleaning sample.
The addition 1ml acetic acid into the chitosan previously configured/molybdenum disulfide disperse system solution, 5ml ethyl alcohol, ultrasonic 1.5h,
For 24 hours, obtained chitosan/molybdenum disulfide disperse system solution, will be aforementioned obtained with porous as electrodeposit liquid for magnetic agitation
The titanium alloy disk of coarse structure makees cathode, and platinum plate electrode makees anode, electrode distance 10mm, voltage 60V, and sedimentation time is
150s.The print that overlay film is taken out from electrodeposit liquid sprays sample surface with clear water, removes the fifth wheel of adsorption
Matter is put into 150 DEG C of drying oven, keeps this temperature 60min, removes moisture removal, obtains titanium alloy surface chitosan/molybdenum disulfide light and urges
Change antimicrobial coating.
Embodiment 4：
150mg molybdenum disulfide is put into mortar with 100mg chitosans and grinds 15min, the 1- butyl -3- methyl miaows of 0.5ml
Azoles hexafluorophosphate (ion assisted milling solution) is added in mortar, and then another straight grinding 60min, collects grinding product,
Acetone, the acetic acid of DMF and 0.5% is used to carry out centrifuge washing product with 8000rpm successively, it is each to wash three times, to remove ionic liquid
With extra chitosan.Finally, make precipitation dispersion in deionized water, it is unstripped to remove in 1500rpm speed centrifugation 20min
MoS2, the chitosan/molybdenum disulfide nano disperse system obtained at this time is diluted to 100ml with deionized water and obtains chitosan/bis-
Molybdenum sulfide research on nano-disperse systems solution is simultaneously stored at 4 DEG C, for use.
Titanium alloy disk (diameter 6mm, thickness 2.5mm) sand paper is polished step by step, until 800#, successively in ethyl alcohol, go from
It is cleaned by ultrasonic in sub- water, it is 5 that cleaned titanium sheet uses volume ratio after the drying:4:1 deionized water/nitric/hydrofluoric nitration mixture
Solution etches 2min, is cleaned with deionized water later, and then etched titanium alloy disk is put into reaction kettle, reaction kettle
In fill the NaOH solution of outfit, reaction kettle is put into baking oven, reacts 3h at 60 DEG C, is made with porous coarse structure
Surface, after the completion cleaning sample.
1ml acetic acid, 4ml ethyl alcohol, ultrasonic 2h, magnetic are added into the chitosan previously configured/molybdenum disulfide disperse system solution
Power stirs for 24 hours, and obtained chitosan/molybdenum disulfide disperse system solution is aforementioned obtained with porous coarse as electrodeposit liquid
The titanium alloy disk of structure makees cathode, and platinum plate electrode makees anode, electrode distance 10mm, voltage 40V, and sedimentation time is
150s.The print that overlay film is taken out from electrodeposit liquid sprays sample surface with clear water, removes the fifth wheel of adsorption
Matter is put into 150 DEG C of drying oven, keeps this temperature 60min, removes moisture removal, obtains titanium alloy surface chitosan/molybdenum disulfide light and urges
Change antimicrobial coating.
By the titanium alloy disk obtained for having chitosan/molybdenum disulfide photocatalysis antibacterial coating in embodiment 1-4, it is put into 96
Certain density Escherichia coli bacteria liquid is added on its surface, it is seen that laser photo-irradiation treatment 5min, 10min add phosphoric acid in orifice plate
Buffer solution is ultrasonically treated, is inoculated into solid agar medium in right amount from being taken in the phosphate buffer containing bacterium solution, observation bacterium colony life
Long situation, while by the bacteria adhension of the titanium alloy disk after culture bacterium, observing bacterium under a scanning electron microscope later
Pattern.
It is tested through analysis, a kind of preparation side of chitosan/molybdenum disulfide visible light catalytic antimicrobial coating of the present invention
Product made from method can be drawn the following conclusions after being detected：1) contact angle test is carried out to titanium alloy disk, often passes through one
The titanium alloy surface contact angle of step processing has significant change；2) the titanium alloy disk surfaces not being modified by surface is golden yellow
Color staphylococcus and Bacillus coli cells film are complete, show bacterial growth and are not suppressed, and have in chitosan/molybdenum disulfide
There is damaged or shrinkage, table in the staphylococcus aureus on nanometer visible light catalytic antimicrobial coating surface and Bacillus coli cells film
Good antibacterial ability is revealed, the antibacterial effect to staphylococcus aureus is better than to the antibacterial effect of Escherichia coli, is added
The titanium surface 3 of only chitosan coat will be substantially better than by entering the photocatalysis antibacterial effect of molybdenum disulfide) it is assisted using ionic liquid
Stripping method with the chitosan-modified molybdenum disulfide lamella good dispersion at functionalization, shows fabulous colloidal stability, shell again
Glycan/molybdenum disulfide electrodepositing is uniformly distributed after titanium alloy surface, and preparation method is simple, using the technology of the present invention system
A kind of standby chitosan/molybdenum disulfide nano visible light catalytic antimicrobial coating, equipment investment is few, and consumption resource is few, and enforcement difficulty is small.
Certainly, the specific application example that the above is only the present invention, is not limited in any way protection scope of the present invention.It removes
Outside above-described embodiment, the present invention can also have other embodiment.All technical sides formed using equivalent substitution or equivalent transformation
Case is all fallen within scope of the present invention.
Claims (4)
1. a kind of preparation method of chitosan/molybdenum disulfide photocatalysis antibacterial coating, which is characterized in that specifically include following step
Suddenly：
S1. 100-250mg molybdenum disulfide and 100-200mg chitosans are put into mortar and grind 15-30min, add 0.5ml
Ionic liquid to mortar in, then grind 60-120min again；
S2. grinding product is collected, uses acetone, n,N-Dimethylformamide (DMF) and the acetic acid that mass concentration is 0.5-1% successively
Grinding product described in centrifuge washing, the acetone, n,N-Dimethylformamide (DMF) and mass concentration are the acetic acid of 0.5-1%
Each washing grinding product three times, removes grinding product intermediate ion liquid and extra chitosan (CS)；It will be obtained after the completion of washing
Precipitation be distributed in deionized water, centrifuging 20min in 1500-1800rpm speed removes unstripped molybdenum disulfide
(MoS2), chitosan/molybdenum disulfide nano disperse system is obtained, by the chitosan/molybdenum disulfide nano disperse system (CS-MoS2)
It is diluted to 100ml with deionized water and obtains chitosan/molybdenum disulfide disperse system solution, the chitosan/molybdenum disulfide is disperseed
It is that solution storage is for use at 4 DEG C；
S3. titanium alloy round abrasive sheet is polished step by step, is cleaned by ultrasonic in ethyl alcohol, deionized water successively, cleaned titanium sheet is dry
2-4min is etched with the mixed acid solution of deionized water/nitric/hydrofluoric after dry, is cleaned later with deionized water；
S4. titanium alloy disk etched made from step S2 is put into the reaction kettle for filling NaOH solution, it then again will be anti-
It answers kettle to be put into baking oven, reacts 2-3h at 60-80 DEG C, surface, which is made, has the titanium alloy disk of porous coarse structure, cleaning
Titanium alloy disk obtained；
S5. 1-1.5ml acetic acid and 4-5ml ethyl alcohol are added in the chitosan/molybdenum disulfide disperse system solution configured to step S2, surpasses
Sound 1.5-2h, magnetic agitation 22-24h；
S6. the chitosan being stirred using in step S5/molybdenum disulfide disperse system solution is as electrodeposit liquid, made from step S4
Titanium alloy disk makees cathode, and platinum plate electrode makees anode, electrode distance 10mm, voltage 40-60V, sedimentation time 150-
300s；The titanium alloy disk that overlay film is taken out from the electrodeposit liquid sprays the titanium alloy disk surfaces with clear water, goes
It except the extra substance of adsorption, places into drying oven, goes moisture removal to get to chitosan/curing of titanium alloy surface
Molybdenum photocatalysis antibacterial coating；
The step S1 intermediate ion liquid is 1- butyl -3- methylimidazole hexafluorophosphates.
2. a kind of preparation method of chitosan according to claim 1/molybdenum disulfide photocatalysis antibacterial coating, feature exist
In the volume parts of each component are in the mixed acid solution of deionized water/nitric/hydrofluoric in the step S3：5 parts of ions
Water, 2-4 part nitric acid and 1-3 parts of hydrofluoric acid.
3. a kind of chitosan/molybdenum disulfide photocatalysis antibacterial coating according to any claim in claim 1-2
Preparation method, which is characterized in that the nitric acid is that analysis is pure；The hydrofluoric acid is that analysis is pure.
4. a kind of preparation method of chitosan according to claim 1/molybdenum disulfide photocatalysis antibacterial coating, feature exist
In drying oven setting temperature is 150 DEG C in the step S6, baking time 60min.
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| CN108392675B (en) * | 2018-03-05 | 2020-08-11 | 湖北大学 | Preparation method of near-infrared light response nano antibacterial coating based on molybdenum disulfide and photosensitizer |
| CN108816292B (en) * | 2018-06-05 | 2020-10-30 | 安徽大学 | Preparation method and application of polydopamine/nano molybdenum disulfide photocatalyst |
| CN109112474B (en) * | 2018-09-26 | 2020-09-04 | 湖北大学 | Preparation method of molybdenum disulfide biological functional coating based on magnetron sputtering of titanium sheet surface |
| CN112526120B (en) * | 2020-11-19 | 2024-05-14 | 山东省农业科学院农业质量标准与检测技术研究所 | Method for detecting salbutamol based on SPR technology |
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