CN113600827B - Au/Ga2O3/AuGa2Multiphase composite material and preparation method and application thereof - Google Patents
Au/Ga2O3/AuGa2Multiphase composite material and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides Au/Ga2O3/AuGa2The preparation method of the multiphase composite material comprises the following steps: adding liquid metal gallium into chloroauric acid solution, performing ultrasonic treatment, centrifuging, and drying to obtain Au/GaOOH/AuGa2A composite material; the obtained Au/GaOOH/AuGa is then used2The composite material is annealed to obtain Au/Ga2O3/AuGa2A multiphase composite material. The multiphase composite material prepared by the invention has remarkable antibacterial activity on escherichia coli and staphylococcus aureus. The preparation method has low cost, is simple and quick, and can directly realize Ga in the ultrasonic process2O3And the synthesis of Ga alloy provides a new thought for synthesizing gallium oxide based compound, and the method of the invention has high universality and can be used for synthesizing other liquid metal oxides and liquid metal alloy.
Description
Technical Field
The invention relates to Au/Ga2O3/AuGa2A multiphase composite material and a preparation method and application thereof belong to the technical field of liquid metal forming.
Background
Infectious diseases still remain a great challenge in human society so far, antibacterial materials can reduce cross infection of bacteria and are not easy to generate drug resistance, and especially inorganic antibacterial materials are paid attention by researchers and develop rapidly due to the advantages of high heat resistance, convenient use, good chemical stability, wide antibacterial spectrum, long effectiveness, no drug resistance and the like.
Inorganic substances widely studied at presentThe antibacterial material mainly comprises metals Ag, Cu, Zn and Ti and some rare metal elements and oxides thereof. As a result of the studies, Ga (NO)3)3Can effectively inhibit growth of Pseudomonas aeruginosa, inhibit formation of growth membrane, and has bactericidal activity. Gallium oxide belongs to a transparent metal oxide semiconductor, has chemical, photo-thermal, electronic, gas-sensitive, optical and photocatalytic characteristics, and has potential application in various fields. The nano gallium oxide is prepared by adopting a hydrothermal method in the Mager, and is characterized, and experiments show that gallium oxide (Ga)2O3) Has good antibacterial activity against staphylococcus aureus, escherichia coli and pseudomonas aeruginosa [ see: study on antibacterial Properties of Malachi inorganic gallium Compound [ D]Southwest university of transportation 2015.]. However, gallium oxide has low antibacterial properties and needs to be further improved.
Gallium is a low melting point metal, and the low melting point metal/alloy refers to a metal and an alloy thereof with a melting point below 300 ℃, generally 30-200 ℃, and the low melting point metal includes bismuth, tin, lead, indium, gallium, rubidium, cesium and the like. Such metals are also called liquid metals because of their low melting points and they are easily converted into a fluid form after heating, and liquid metals have been widely used in the fields of medical treatment, electronics, and the like because of their low melting points, high electrical conductivity, high fluidity, and the like. The liquid metal gallium has low toxicity and high chemical stability, and can be compounded with other materials to improve the performance of the liquid metal gallium due to excellent thermal conductivity, electrical conductivity, adjustable fluidity/rheological property, controllable surface chemistry and compatibility with various materials. The reorganization or functionalization of the self-limiting scale on the surface of the liquid metal nanomaterial can also better control the properties of the alloy. The liquid metal has the capability of being naturally alloyed with most metals such as Au, Ag, Al and the like, and the performance of the liquid metal nano material can be further widened by forming multi-metal, multi-phase and nano-structured particles.
Therefore, the development of a simple, convenient, environment-friendly and low-cost preparation method for preparing the Ga-based multiphase composite material with high antibacterial performance has important significance.
Disclosure of Invention
Aiming at the defects of the prior art, the inventionThe invention provides Au/Ga2O3/AuGa2Multiphase composite material and its preparation method and application. Au/Ga of the invention2O3/AuGa2The multiphase composite material has remarkable antibacterial activity, and the preparation method is simple, rapid, environment-friendly and low in cost.
The technical scheme of the invention is as follows:
Au/Ga2O3/AuGa2The preparation method of the multiphase composite material comprises the following steps:
adding liquid metal gallium into chloroauric acid solution, performing ultrasonic treatment, centrifuging, and drying to obtain Au/GaOOH/AuGa2A composite material; the obtained Au/GaOOH/AuGa is then used2The composite material is annealed to obtain Au/Ga2O3/AuGa2A multiphase composite material.
According to the invention, the concentration of the chloroauric acid solution is preferably 0.1-1mmol/L, more preferably 0.4-0.6mmol/L, and even more preferably 0.5 mmol/L.
According to the invention, the molar ratio of the liquid metal gallium to the gold element in the chloroauric acid is 25-60: 1.
According to the invention, the ultrasonic treatment time is 60-150min, the ultrasonic power is 80W, and the ultrasonic frequency is 20 KHz.
Preferably, the centrifugal speed is 15000-20000r/min, and the centrifugal time is 10-15 min.
According to the invention, the drying temperature is 80-100 ℃, and the drying time is 5-6 h.
According to the invention, the temperature of the annealing treatment is 500-600 ℃, and the time of the annealing treatment is 1.5-3 h.
The invention also provides Au/Ga prepared by the method2O3/AuGa2A multiphase composite material.
According to the invention, the Au/Ga2O3/AuGa2Use of a multiphase composite for antimicrobial; more preferably, the Au/Ga is2O3/AuGa2The multiphase composite material is used for resisting escherichia coli and staphylococcus aureus.
The invention has the following technical characteristics and beneficial effects:
1. the invention successfully synthesizes Au/Ga by utilizing ultrasonic and annealing technologies2O3/AuGa2The nano-rods are compounded, and the obtained material is a high-porosity multiphase nano-rod composite material. The antibacterial experiment shows that Au/Ga2O3/AuGa2The nanorod has remarkable antibacterial activity to escherichia coli and staphylococcus aureus, and the antibacterial efficiency of the nanorod is Ga2O3Over 1.5 times of the total amount of the active ingredients, and greatly improves the inhibition effect on escherichia coli and staphylococcus aureus.
2. Au/Ga of the invention2O3/AuGa2The preparation method of the multiphase composite material is low in cost, simple and quick, and can directly realize Ga in the ultrasonic process2O3And Ga alloy synthesis, the method of the invention needs to control the gallium-gold proportion, and AuGa can not be obtained if the added amount of gallium is less2Alloy, Au/Ga could not be synthesized successfully2O3/AuGa2A multiphase composite material. The preparation method is convenient and fast, and provides a new thought for synthesizing the gallium oxide-based compound; the method has high universality and can be used for synthesizing other liquid metal oxides and liquid metal alloys.
3. Au/Ga of the invention2O3/AuGa2The preparation method of the multiphase composite material is environment-friendly, the liquid metal gallium is non-toxic and low in cost, the multiphase material with a wide spectrum absorption range is synthesized by an ultrasonic method, and the method is simple, convenient, rapid, reliable, environment-friendly, free of interference and low in cost.
Drawings
FIG. 1 shows Au/Ga prepared in example 12O3/AuGa2SEM images of multiphase composites.
FIG. 2 shows Au/Ga prepared in example 12O3/AuGa2Particle size distribution profile of the multiphase composite.
FIG. 3 shows Au/Ga prepared in example 12O3/AuGa2Mapping graph of multiphase composite material.
FIG. 4 shows Au/Ga prepared in example 12O3/AuGa2Multiphase composite material, Au/GaOOH/AuGa2Composite material, Ga prepared in comparative example 12O3X-ray diffraction patterns of the material and the GaOOH material.
FIG. 5 shows Au/Ga prepared in example 12O3/AuGa2Multiphase composite and Ga prepared in comparative example 12O3Ultraviolet and visible absorption spectrum of the material.
FIG. 6 is Ga prepared in comparative example 12O3SEM image of material.
FIG. 7 shows Ga prepared in comparative example 12O3Particle size distribution profile of the material.
FIG. 8 is Au/Ga prepared in comparative example 22O3/AuGa2SEM images of multiphase composites.
FIG. 9 shows Au/Ga prepared in example 12O3/AuGa2Multiphase composite and Ga prepared in comparative example 12O3The inhibitory effect of the material on Escherichia coli and Staphylococcus aureus is shown.
Detailed Description
The present invention will be described in detail with reference to specific examples, but the invention is not limited thereto.
The experimental methods used in the examples are all conventional methods unless otherwise specified; the materials, reagents and the like used are commercially available unless otherwise specified.
Example 1
Au/Ga2O3/AuGa2The preparation method of the multiphase composite material comprises the following steps:
adding 0.1g of liquid metal gallium into 50mL of 0.5mmol/L chloroauric acid solution, carrying out ultrasonic treatment for 120min under the conditions of 80W of power and 20KHz of frequency, centrifuging the obtained reaction solution for 10min under the condition of 16000r/min of rotation speed, drying the product obtained by centrifuging at 80 ℃ for 5h to obtain Au/GaOOH/AuGa2A composite material; the obtained Au/GaOOH/AuGa is then used2Annealing the composite material at 500 ℃ for 2h in air atmosphere to obtain Au/Ga2O3/AuGa2A multiphase composite material.
Au/Ga prepared in this example2O3/AuGa2The SEM image of the multiphase composite material is shown in fig. 1, the particle size distribution is shown in fig. 2, and as can be seen from fig. 1 and 2, the micro-morphology of the obtained product is: spherical Au nanoparticles and spherical AuGa are uniformly dispersed on the surface2Ga of nanoparticles2O3Nanorods of Ga2O3The nanorod has a width of 200-250nm and a length of 400-600nm, and has spherical Au nanoparticles and spherical AuGa2The average particle size of the nanoparticles was 40 nm.
Au/Ga prepared in this example2O3/AuGa2The mapping pattern of the heterogeneous composite material is shown in FIG. 3, the XRD spectrum thereof is shown in FIG. 4, and it can be seen from FIG. 3 that gallium, oxygen and gold elements exist in the product, and the XRD spectrum of the obtained product comprises Au and Ga2O3And AuGa2The characteristic peak of (1), the element composition in mapping diagram is consistent with the XRD diagram of figure 4, Au and Ga are combined together to form AuGa2And Ga in the obtained product2O3Is alpha-Ga2O3。
Au/Ga prepared in this example was tested2O3/AuGa2The ultraviolet visible absorption spectrum of the multiphase composite material is that Xe lamp with 150W light source leads out light with 30 μ W optical power by a monochromator, and the obtained ultraviolet visible absorption spectrum is shown in figure 5, wherein, the absorption peak at 230nm corresponds to Ga2O3The absorption peak at 532nm is due to the plasmon resonance of Au, AuGa2Has a wide plasmon peak of 600nm-850nm, Au and AuGa2Presence of (B) broadens Ga2O3The light absorption range of (2) improves the performance of the optical fiber.
Example 2
Au/Ga2O3/AuGa2The preparation method of the multiphase composite material comprises the following steps:
adding 0.1g of liquid metal gallium into 50mL of 1mmol/L chloroauric acid solution, carrying out ultrasonic treatment for 120min under the conditions of power of 80W and frequency of 20KHz, centrifuging the obtained reaction solution for 10min under the condition of the rotating speed of 16000r/min, and drying the product obtained by centrifuging at 80 ℃ for 5h to obtain Au/GaOOH/AuGa2A composite material; the obtained Au/GaOOH/AuGa is then used2Annealing the composite material at 500 ℃ for 2h in air atmosphere to obtain Au/Ga2O3/AuGa2A multiphase composite material.
Comparative example 1
Ga2O3The preparation method of the material comprises the following steps:
adding 0.1g of liquid metal gallium into 50mL of water, carrying out ultrasonic treatment for 120min under the conditions of 80W power and 20KHz frequency, centrifuging the obtained reaction liquid for 10min under the condition of 16000r/min rotation speed, and drying the product obtained by centrifuging at 80 ℃ for 5h to obtain a GaOOH material; then annealing the obtained GaOOH material at 500 ℃ for 2h in the air atmosphere to obtain Ga2O3A material.
Ga prepared in this comparative example2O3The SEM image of the material is shown in fig. 6, and the particle size distribution diagram is shown in fig. 7. As can be seen from FIGS. 6 and 7, Ga2O3The width of the nano rod is 200-250nm, and the length is 400-600 nm.
Ga prepared in this comparative example2O3The UV-visible absorption spectrum of the material is shown in FIG. 5, and it can be seen from FIG. 5 that Ga is only present at 230nm2O3The absorption peak of the in-band transition of (2) has a narrow spectral absorption range.
Comparative example 2
Au/Ga2O3/AuGa2The multiphase composite was prepared as described in example 1, except that: the ultrasonic time is 1 h.
Au/Ga prepared by the comparative example2O3/AuGa2The SEM photograph of the heterogeneous composite is shown in FIG. 8, and it can be seen from FIG. 8 that the obtained Au nanoparticles and AuGa2The nano-particles are large and have uneven particle sizes, and the obtained material has bacteriostasisThe performance is poor.
Test examples
The materials prepared in example 1 and comparative example 1 were tested for bacteriostatic properties. The materials prepared in example 1 and comparative example 1 were tested for their bacteriostatic properties against escherichia coli and staphylococcus aureus under 808nm illumination.
The test procedure was as follows:
1. test of bacteriostatic property of escherichia coli
Control group
(1) Ultrasonically treating 990 μ L LB liquid culture medium at power of 21.6W for 3min to obtain solution A;
(2) taking logarithmic growth phase (OD)6000.5) of escherichia coli liquid according to a volume ratio of 1: 100 inoculating in LB liquid culture medium, shake culturing in shaking table at 37 deg.C for 8 hr, collecting bacterial liquid, mixing, diluting with LB liquid culture medium in gradient manner to obtain bacterial liquid with concentration of 1.0 × 108CFU·mL-1To obtain solution B.
(3) Mixing the 990 mu L A liquid with the 10 mu L B liquid to obtain a mixed liquid; selecting a 96-well plate, selecting 3 non-adjacent wells, adding 100 μ L of mixed solution into each well, and using power density of 2W/cm2The irradiation time of the near-infrared 808nm laser is 0min, 10min and 20min respectively for 3 holes.
(4) After the irradiation is completed, 100 mu LLB liquid culture medium is added into each well for dilution and uniform mixing, the mixture is spread on LB solid culture medium and cultured in an incubator at 37 ℃ for 12 hours, and then a flat plate is taken out, and the number of colonies is counted. This experiment was repeated in three groups.
Experimental group
Ga2O3Treatment group
(1) 2mg of Ga prepared in comparative example was added to 990. mu.L of LB liquid medium2O3Will contain Ga2O3Performing ultrasonic treatment on the LB liquid culture medium suspension for 3min under the condition that the power is 21.6W to obtain a solution A;
(2) - (4) same as control group.
Au/Ga2O3/AuGa2Treatment group
(1) At 990. mu.L of LB solution2mg of Au/Ga prepared in example were added to the culture medium2O3/AuGa2Will contain Au/Ga2O3/AuGa2Performing ultrasonic treatment on the LB liquid culture medium suspension for 3min under the condition that the power is 21.6W to obtain a solution A;
(2) - (4) the same as the control group.
2. Bacteriostatic property test on staphylococcus aureus
The specific test method is as described in the test method for the bacteriostatic property of escherichia coli, except that the escherichia coli is replaced by staphylococcus aureus.
The test results are shown in FIG. 9. from FIG. 9, it can be seen that Au/Ga prepared by the present invention2O3/AuGa2The multiphase composite material has remarkable antibacterial activity on escherichia coli and staphylococcus aureus, and the antibacterial efficiency of the multiphase composite material is Ga2O3The inhibition effect on escherichia coli and staphylococcus aureus is greatly improved by more than 2 times.
Claims (8)
1. Au/Ga2O3/AuGa2The preparation method of the multiphase composite material comprises the following steps:
adding liquid metal gallium into chloroauric acid solution, performing ultrasonic treatment, centrifuging, and drying to obtain Au/GaOOH/AuGa2A composite material; the obtained Au/GaOOH/AuGa is then used2The composite material is annealed to obtain Au/Ga2O3/AuGa2A multiphase composite material; the molar ratio of the liquid metal gallium to the gold element in the chloroauric acid is 25-60: 1;
the ultrasonic treatment time is 60-150min, the ultrasonic power is 80W, and the ultrasonic frequency is 20 KHz;
the temperature of the annealing treatment is 500-600 ℃, and the time of the annealing treatment is 1.5-3 h.
2. Au/Ga according to claim 12O3/AuGa2The preparation method of the multiphase composite material is characterized in that the concentration of the chloroauric acid solution is 0.1-1 mmol/L.
3. Au/Ga according to claim 22O3/AuGa2The preparation method of the multiphase composite material is characterized in that the concentration of the chloroauric acid solution is 0.4-0.6 mmol/L.
4. Au/Ga according to claim 32O3/AuGa2The preparation method of the multiphase composite material is characterized in that the concentration of the chloroauric acid solution is 0.5 mmol/L.
5. Au/Ga according to claim 12O3/AuGa2The preparation method of the multiphase composite material is characterized in that the centrifugal rotating speed is 15000-20000r/min, and the centrifugal time is 10-15 min; the drying temperature is 80-100 ℃, and the drying time is 5-6 h.
6. Au/Ga produced by the method of any one of claims 1 to 52O3/AuGa2A multiphase composite material.
7. Au/Ga according to claim 62O3/AuGa2Use of a multiphase composite for antimicrobial applications.
8. Use according to claim 7, wherein the Au/Ga2O3/AuGa2The multiphase composite material is used for resisting escherichia coli and staphylococcus aureus.
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| CN109414010A (en) * | 2016-05-04 | 2019-03-01 | 5D卫生防护集团有限公司 | Antimicrobial compositions |
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| CA2867787C (en) * | 2012-03-30 | 2022-01-04 | Dentsply Ih Ab | A medical device having a surface comprising antimicrobial metal |
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| CN107385372A (en) * | 2017-08-02 | 2017-11-24 | 山东大学 | A kind of preparation method of nano-structural transition metal film |
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| Au / Ga2O3 的制备及其催化还原芳香族;张燕辉等;《五邑大学学报（自然科学版）》;20170531;第31卷(第2期);第9-13页 * |
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