CN114711251A - Titanium carbide-manganese sulfide composite bacteriostatic material, preparation method thereof and bacteriostatic method - Google Patents
Titanium carbide-manganese sulfide composite bacteriostatic material, preparation method thereof and bacteriostatic method Download PDFInfo
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Abstract
The invention discloses a titanium carbide-manganese sulfide composite antibacterial material and a preparation method thereof, namely an antibacterial method. The material is uniformly dispersed in sterile water, the titanium carbide-manganese sulfide composite material with a certain concentration is respectively placed in EP tubes of escherichia coli and staphylococcus aureus, near-infrared laser with the wavelength of 808nm is selected for irradiation, and the survival rate of bacteria is analyzed after the culture box stays overnight. The titanium carbide is added in the invention in order to utilize the excellent photo-thermal performance thereof to efficiently inhibit bacteria, and simultaneously, the dispersion performance of the titanium carbide in water is utilized; the prepared composite material has better photo-thermal conversion efficiency, thereby obtaining better antibacterial performance and having good inhibition effect on gram negative bacteria and gram positive bacteria.
Description
Technical Field
The invention relates to the technical field of bacteriostasis, and particularly relates to a titanium carbide-manganese sulfide composite bacteriostatic material, a preparation method thereof and a bacteriostasis method.
Background
In recent years, infectious diseases caused by bacteria have been increasing continuously, and have become one of the major problems threatening human health worldwide. Many traditional anti-infective treatments that rely on antibiotics gradually lose their effectiveness due to the emergence of resistant strains. Therefore, the development of novel antibacterial agents is important. Among them, new antibacterial therapies based on nanomaterials are receiving increasing attention, such as photothermal therapy (PTT), photodynamic therapy (PDT), and ultrasound. Of these therapies, ROS-based antimicrobial therapies have higher efficacy and fewer side effects. Research has shown that high concentration of ROS can destroy cell membrane, resulting in functional disorder of biomolecules such as nucleic acid and protein, and finally causing bacterial inactivation.
Some nanomaterials with native enzymatic activity (also called "nanoenzymes") can utilize their peroxide mimetic enzymatic activity to deliver low doses of H2O2Is converted into OH; or converting oxygen into superoxide anion O by using its oxidase activity2 -Finally, the level of ROS in bacterial cells is increased, so that bacteria are killed, and the anti-infection effect is enhanced. The nano enzyme can inhibit bacterial infection and is expected to overcome the defect of using high-concentration H2O2The defect of (2). However, it is difficult to completely eradicate drug-resistant bacteria efficiently by a single antibacterial therapy based on nano-enzyme catalytic antibacterial, and thus the antibacterial efficiency can be improved and the drug dosage can be reduced by combining a plurality of antibacterial treatment modes for synergistic treatment. Therefore, in order to ensure the bacteriostasis efficiency, the construction of the nano material which is based on the nano enzyme catalytic effect and has multiple antibacterial functions is particularly important.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to explore the antibacterial property of a new material.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of a titanium carbide-manganese sulfide composite antibacterial material comprises the following steps:
1) adding manganese acetate tetrahydrate into the titanium carbide dispersion liquid, and uniformly stirring to prepare a solution I;
2) dissolving L-cysteine in ultrapure water to prepare a solution II;
3) adding the solution II into the solution I, and stirring for 1h to prepare a solution III;
4) transferring the solution III into a high-pressure reaction kettle, and reacting for a certain time;
5) and after the solution is cooled, collecting the precipitate, respectively cleaning the precipitate with ultrapure water and absolute ethyl alcohol, and then drying the precipitate in vacuum to obtain the titanium carbide-manganese sulfide composite antibacterial material.
Preferably, the concentration of the titanium carbide in the step 1) is 0.5-1 mg/mL, and the mass of the added manganese acetate tetrahydrate is 0.122-0.490 g.
Preferably, the concentration of the L-cysteine solution in the step 2) is 0.01-0.05 mg/mL.
Preferably, the molar ratio of the L-cysteine to the manganese acetate tetrahydrate is 1: 1.
Preferably, the reaction conditions in the step 4) are a reaction temperature of 200 ℃ and a reaction time of 16 h.
The invention further provides the titanium carbide-manganese sulfide composite antibacterial material prepared by the preparation method.
The invention further provides a bacteriostatic method of the titanium carbide-manganese sulfide composite bacteriostatic material, which comprises the following steps:
a) adding sterile water into the titanium carbide-manganese sulfide composite antibacterial material to prepare an antibacterial material solution;
b) preparing an LB liquid culture medium: mixing peptone, sodium chloride and yeast according to the mass ratio of 2:2:1, fixing the volume to 25mg/mL with deionized water, and sterilizing at 120 ℃ under high temperature and high pressure for 15min to obtain the final product;
preparing LB solid medium plate: adding 2% agar powder on the basis of LB liquid culture medium, sterilizing at high temperature and high pressure, pouring into a bacteria culture dish in sterile environment, and cooling and solidifying the liquid to obtain the final product;
c) preparing bacterial liquid: diluting a proper amount of bacterial liquid to a proper concentration, uniformly coating the diluted bacterial liquid on an LB solid culture medium flat plate, then placing the flat plate in a constant-temperature incubator at 37 ℃ for overnight culture, storing the flat plate at 4 ℃, selecting a proper amount of monoclonal bacteria to be cultured in an LB liquid culture medium for 12 hours before an experiment, then taking a suspension to be diluted by 100 times by using a fresh LB liquid culture medium, and continuously culturing at 37 ℃ to obtain bacterial liquid for the experiment;
d) uniformly mixing the antibacterial material solution, the sodium acetate solution and the test bacterial liquid in a volume ratio of 1:8:1, irradiating for 8-10 min under the near-infrared laser, and continuously reacting for 30min to achieve the antibacterial effect.
Preferably, the concentration of the bacteriostatic material solution is 2.5mg/mL, and the pH value of the sodium acetate solution is 4.55.
Preferably, 808nm near-infrared laser irradiation is adopted in the step d), and the power is 2W/cm2。
Preferably, the bacterial liquid is gram negative/positive bacteria; more preferably E.coli or S.aureus.
Titanium carbide is a common two-dimensional layered material and has excellent photo-thermal performance and water solubility. Manganese sulfide as a nanoenzyme can exert dual enzyme activity, including Peroxidase (POD) and Oxidase (OXD). A one-step hydrothermal method is utilized to synthesize the titanium carbide-manganese sulfide composite antibacterial material, and tests prove that the nanometer material has good inhibition effect on gram-negative bacteria and gram-positive bacteria.
Compared with the prior art, the method is simple. The titanium carbide is added in the invention in order to utilize the excellent photo-thermal performance thereof to efficiently inhibit bacteria, and simultaneously, the defect that manganese sulfide is insoluble in water is improved by utilizing the good water solubility of the titanium carbide. The two-dimensional layered titanium carbide and the manganese sulfide are compounded to prepare a new material, so that the material has better photo-thermal conversion efficiency, further obtains better antibacterial performance, and has good inhibition effect on gram-negative bacteria and gram-positive bacteria.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
Fig. 1 is an SEM image of the titanium carbide-manganese sulfide composite bacteriostatic material prepared in example 1.
Fig. 2 is an XRD chart of the titanium carbide-manganese sulfide composite bacteriostatic material prepared in example 1.
FIG. 3 shows the laser power density of 2.0W/cm for the titanium carbide-manganese sulfide composite bacteriostatic material prepared in example 12Temperature rise profile.
FIG. 4 is a graph showing the survival rate of bacteria treated with Escherichia coli according to application examples 1 to 3.
FIG. 5 is a graph showing the survival rate of Staphylococcus aureus treated in application examples 4 to 6.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the accompanying drawings, and it should be understood that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Furthermore, the technical features involved in the different embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
Example 1:
the preparation method of the titanium carbide-manganese sulfide composite antibacterial material comprises the following steps:
(1) dispersing 30mg of titanium carbide in 30mL of ultrapure water to prepare a solution I;
(2) adding the solution I into 0.245g of manganese acetate tetrahydrate, and stirring to prepare a solution II;
(3) dissolving 0.121g L-cysteine in 5mL of ultrapure water to prepare a solution III;
(4) adding the solution III into the solution II, and stirring for 1h to prepare a solution IV;
(5) transferring the solution IV into a high-pressure reaction kettle, and reacting for 16h at 200 ℃;
(6) after the solution is cooled, collecting the precipitate, respectively cleaning the precipitate with ultrapure water and absolute ethyl alcohol for three times, and then carrying out vacuum drying at the temperature of 80 ℃ for 12 hours to obtain the titanium carbide-manganese sulfide composite antibacterial material.
It can be seen from fig. 1 and 2 that the layered titanium carbide-manganese sulfide composite material was successfully obtained. It is evident from the SEM image of fig. 1 that the nanoparticles are supported on the titanium carbide, indicating that the titanium carbide composite material was successfully prepared. The XRD pattern of fig. 2 shows strong characteristic peaks at 29.6 °, 34.3 °, 49.3 °, 58.6 °, 61.4 ° and 72.3 °, corresponding to (111), (200), (220), (311), (222) and (400) crystal planes (PDF #06-0518) of manganese sulfide, respectively, indicating successful loading of strong crystallinity manganese sulfide on titanium carbide.
FIG. 3 shows the laser power density of 2.0W/cm for the titanium carbide-manganese sulfide composite bacteriostatic material2Temperature rise curve below. The titanium carbide has good photo-thermal property, and the experiment on the in-vitro photo-thermal property of the titanium carbide-manganese sulfide shows that the bacteriostatic property of the bacteriostatic material can be further improved by introducing near-infrared laser. In FIG. 3, the solutions are 250. mu.g/mL, near infrared light (2.0W/cm)2808nm) was irradiated to the solution. It can be seen from the figure that the temperature rise of the titanium carbide and titanium carbide-manganese sulfide composite is higher after ten minutes of irradiation compared to water, pure manganese sulfide. Further illustrating the good photo-thermal properties of titanium carbide.
Application example: the bacteriostasis method of the titanium carbide-manganese sulfide composite bacteriostasis material is as follows
1) Preparing LB liquid and solid culture media: weighing 4g of peptone, 4g of sodium chloride and 2g of yeast, diluting to 400mL with deionized water, and sterilizing at 120 ℃ for 15min under high temperature and high pressure to obtain LB liquid culture medium for later use.
Adding 2% of agar powder into the solid culture medium, sterilizing at high temperature and high pressure, pouring into a bacterial culture dish in an aseptic environment, and cooling and solidifying the liquid to obtain the LB solid culture medium plate.
2) In the early stage of the experiment, a proper amount of bacterial liquid is taken to be diluted to a proper concentration, evenly coated on an LB solid culture medium plate, and then placed in a constant-temperature incubator at 37 ℃ for overnight culture and stored at 4 ℃. Before the experiment, a proper amount of monoclonal colonies are selected and cultured in an LB liquid culture medium for 12 hours, then the suspension is diluted by 100 times by using a fresh LB liquid culture medium, and the culture is continued at 37 ℃, so that the bacteria for the experiment are obtained.
3) Adding 100 μ L of the bacterial liquid into 900 μ L of sodium acetate buffer solution with pH 4.55, and adding 808nm 2W/cm2And (3) irradiating by using near-infrared laser for 8-10 min and reacting for 30 min.
4) Diluting the product of step 3) to 10-2、10-3、10-4、10-5、10-6Then 100. mu.L of each was applied evenly on LB medium plates, and the plates were incubated at 37 ℃ for 12 hours and counted.
5) Calculating bacterial survival rate ═ (C)0-C1)/C0×100％，C0Average number of CFU's of bacteria for Escherichia coli/Staphylococcus aureus test, C1The CFU processed by the step 3).
Bacterial survival rate ═ C0-C1)/C0。
Application example 1:
selecting Escherichia coli liquid as the bacterial liquid, and performing the antibacterial method, wherein the laser irradiation is performed for 8 min; the survival rate of the bacteria was calculated as (C)0-C1)/C0×100％＝81.82％。
Application example 2:
selecting escherichia coli liquid as the liquid, and carrying out the antibacterial treatment according to the antibacterial method, wherein the difference is that the treatment method in the step 3) comprises the following steps: taking 100 mu L of antibacterial material solution (adding titanium carbide-manganese sulfide composite antibacterial material into sterile water, dispersing uniformly to prepare 2.5mg/mL), adding 800 mu L of sodium acetate buffer solution with pH 4.55 and 100 mu L of bacterial solution, and reacting for 30 min. The survival rate of the bacteria was calculated as (C)0-C1)/C0×100％＝24.04％。
Application example 3:
bacterial liquid selectionSelecting an escherichia coli liquid, and carrying out the antibacterial treatment according to the antibacterial method, wherein the difference is that the treatment method in the step 3) comprises the following steps: adding 100 μ L of antibacterial material solution (prepared by adding titanium carbide-manganese sulfide composite antibacterial material into sterile water, dispersing uniformly to obtain 2.5mg/mL), adding 800 μ L of sodium acetate buffer solution with pH of 4.55 and 100 μ L of bacteria solution, and adding 808nm 2W/cm2Irradiating by near infrared laser for 8min, and reacting for 30 min. The survival rate of the bacteria was calculated as (C)0-C1)/C0×100％＝0.25％。
Application example 4:
selecting staphylococcus aureus liquid as the liquid, and performing the antibacterial method according to the liquid, wherein laser irradiation is performed for 10 min; the survival rate of the bacteria was calculated as (C)0-C1)/C0×100％＝44.54％。
Application example 5:
selecting staphylococcus aureus liquid as the liquid, and performing the antibacterial treatment according to the antibacterial method, wherein the difference is that the treatment method in the step 3) comprises the following steps: taking 100 mu L of antibacterial material solution (adding titanium carbide-manganese sulfide composite antibacterial material into sterile water, dispersing uniformly to prepare 2.5mg/mL), adding 800 mu L of sodium acetate buffer solution with pH 4.55 and 100 mu L of bacterial solution, and reacting for 30 min. The survival rate of the bacteria was calculated as (C)0-C1)/C0×100％＝33.31％。
Application example 6:
the bacterial liquid is staphylococcus aureus bacterial liquid, the bacterial liquid is processed according to the bacteriostasis method, and the difference is that the processing method in the step 3) comprises the following steps: adding 100 μ L of antibacterial material solution (prepared by adding titanium carbide-manganese sulfide composite antibacterial material into sterile water, dispersing uniformly to obtain 2.5mg/mL), adding 800 μ L of sodium acetate buffer solution with pH of 4.55 and 100 μ L of bacteria solution, and adding 808nm 2W/cm2Irradiating by near infrared laser for 10min, and reacting for 30 min. The survival rate of the bacteria was calculated as (C)0-C1)/C0×100％＝0.04％。
The bacteriostatic effects on E.coli and S.aureus are shown in FIGS. 4 and 5, respectively. FIG. 4 shows the bacteriostatic effect on E.coli under different conditions. From the figure, it can be seen that the survival rates of the bacteria are 81.82% and 21.04% respectively after 30min of cultivation under a single condition (illumination or titanium carbide-manganese sulfide composite). After the titanium carbide-manganese sulfide composite material is added, the survival rate of bacteria is obviously reduced, because the antibacterial material has certain activity of oxide mimic enzyme at room temperature, ROS can be generated to inhibit the activity of bacteria. In addition, after the escherichia coli is treated by the titanium carbide-manganese sulfide composite material for 8min by near infrared, the near infrared light source is removed, and the escherichia coli is continuously placed for 22min, so that the survival rate of bacteria is only 0.25%, and the escherichia coli is mainly benefited by the good photothermal conversion capability of the titanium carbide. FIG. 5 is a graph showing the bacteriostatic effect on Staphylococcus aureus under different conditions. After culturing for 30min under a single condition (illumination or titanium carbide-manganese sulfide composite), the bacterial activity is obviously reduced to 44.54 percent and 33.31 percent. In addition, after the titanium carbide-manganese sulfide composite material is added and treated for 10min by near infrared, a light source is removed and the composite material is placed for 20min, and the survival rate of bacteria is only 0.04 percent.
While embodiments of the invention have been described above, it is not limited to the applications set forth in the description and the embodiments, which are fully applicable in various fields of endeavor to which the invention pertains, and further modifications may readily be made by those skilled in the art, it being understood that the invention is not limited to the details shown and described herein without departing from the general concept defined by the appended claims and their equivalents.
Claims (10)
1. The preparation method of the titanium carbide-manganese sulfide composite antibacterial material is characterized by comprising the following steps of:
1) adding manganese acetate tetrahydrate into titanium carbide dispersion liquid, and uniformly stirring to obtain solution I;
2) dissolving L-cysteine in ultrapure water to prepare a solution II;
3) adding the solution II into the solution I, and stirring for 1h to prepare a solution III;
4) transferring the solution III into a high-pressure reaction kettle, and reacting for a certain time;
5) and after the solution is cooled, collecting the precipitate, respectively cleaning the precipitate with ultrapure water and absolute ethyl alcohol, and then drying the precipitate in vacuum to obtain the titanium carbide-manganese sulfide composite antibacterial material.
2. The preparation method of the titanium carbide-manganese sulfide composite bacteriostatic material according to claim 1, wherein the concentration of the titanium carbide in the step 1) is 0.5-1 mg/mL, and the mass of the added manganese acetate tetrahydrate is 0.122-0.490 g.
3. The preparation method of the titanium carbide-manganese sulfide composite bacteriostatic material according to claim 1, wherein the concentration of the L-cysteine solution in the step 2) is 0.01-0.05 mg/mL.
4. The method for preparing the titanium carbide-manganese sulfide composite bacteriostatic material according to claim 1, wherein the molar ratio of the L-cysteine to the manganese acetate tetrahydrate is 1: 1.
5. The preparation method of the titanium carbide-manganese sulfide composite bacteriostatic material according to claim 1, wherein the reaction conditions in the step 4) are 180-220 ℃ and the reaction time is 12-18 h.
6. The titanium carbide-manganese sulfide composite bacteriostatic material prepared by the preparation method of any one of claims 1-5.
7. The bacteriostasis method of the titanium carbide-manganese sulfide composite bacteriostasis material according to claim 5, which is characterized by comprising the following steps:
a) adding sterile water into the titanium carbide-manganese sulfide composite antibacterial material to prepare an antibacterial material solution;
b) preparing an LB liquid culture medium: mixing peptone, sodium chloride and yeast according to the mass ratio of 2:2:1, fixing the volume to 25mg/mL with deionized water, and sterilizing at 120 ℃ under high temperature and high pressure for 15min to obtain the final product;
preparing an LB solid medium plate: adding 2% agar powder on the basis of LB liquid culture medium, sterilizing at high temperature and high pressure, pouring into a bacteria culture dish in sterile environment, and cooling and solidifying the liquid to obtain the final product;
c) preparing bacterial liquid: diluting a proper amount of bacterial liquid to a proper concentration, uniformly coating the diluted bacterial liquid on an LB solid culture medium plate, then putting the LB solid culture medium plate in a constant-temperature incubator at 37 ℃ for overnight culture, preserving the LB solid culture medium plate at 4 ℃, selecting a proper amount of monoclonal bacterial colony to culture in an LB liquid culture medium for 12 hours before an experiment, then taking a suspension to dilute the suspension by 100 times by using a fresh LB liquid culture medium, and continuing to culture at 37 ℃ to obtain a bacterial liquid for the experiment;
d) uniformly mixing the antibacterial material solution, the sodium acetate solution and the test bacterial liquid in a volume ratio of 1:8:1, irradiating for 8-10 min under the near-infrared laser, and continuously reacting for 30min to achieve the antibacterial effect.
8. The method for inhibiting bacteria of the titanium carbide-manganese sulfide composite bacteriostatic material according to claim 7, wherein the concentration of the bacteriostatic material solution is 2.5mg/mL, and the pH value of the sodium acetate solution is 4.55.
9. The method for inhibiting bacteria of titanium carbide-manganese sulfide composite bacteriostatic material according to claim 7, wherein in the step d), 808nm near-infrared laser irradiation is adopted, and the power is 2W/cm2。
10. The method for inhibiting bacteria of the titanium carbide-manganese sulfide composite antibacterial material according to claim 7, wherein the bacterial liquid is gram-negative/positive bacteria.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20080112405A (en) * | 2008-11-21 | 2008-12-24 | 엔엠 테크 엘티디. 나노머티리얼스 앤드 마이크로디바이시스 테크놀로지 | Functional nanomaterials with antibacterial and antiviral activity |
| CN108735984A (en) * | 2018-04-11 | 2018-11-02 | 燕山大学 | A kind of preparation method of molybdenum disulfide/carbonization titanium composite material |
| CN111180694A (en) * | 2019-12-31 | 2020-05-19 | 广东工业大学 | MXene/metal sulfide composite material, negative electrode material, preparation and application |
| CN113016823A (en) * | 2021-02-02 | 2021-06-25 | 南京师范大学 | Preparation method of photo-thermal antibacterial near-infrared bimetallic nanoparticles |
-
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- 2022-03-25 CN CN202210297527.XA patent/CN114711251B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20080112405A (en) * | 2008-11-21 | 2008-12-24 | 엔엠 테크 엘티디. 나노머티리얼스 앤드 마이크로디바이시스 테크놀로지 | Functional nanomaterials with antibacterial and antiviral activity |
| CN108735984A (en) * | 2018-04-11 | 2018-11-02 | 燕山大学 | A kind of preparation method of molybdenum disulfide/carbonization titanium composite material |
| CN111180694A (en) * | 2019-12-31 | 2020-05-19 | 广东工业大学 | MXene/metal sulfide composite material, negative electrode material, preparation and application |
| CN113016823A (en) * | 2021-02-02 | 2021-06-25 | 南京师范大学 | Preparation method of photo-thermal antibacterial near-infrared bimetallic nanoparticles |
Non-Patent Citations (2)
| Title |
|---|
| FARBOD ALIMOHAMMADI等: ""Antimicrobial Properties of 2D MnO2 and MoS2 NanomaterialsVertically Aligned on Graphene Materials and Ti3C2 MXene"", 《LANGMUIR》, vol. 34, pages 7192 - 7200 * |
| KASHIF RASOOL等: ""Antibacterial Activity of Ti3C2Tx MXene"", 《ACS NANO》, vol. 10, pages 3674 - 3684, XP055381471, DOI: 10.1021/acsnano.6b00181 * |
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