CN114984216A - Method for preparing nano gold/polyvinyl alcohol composite material by normal pressure plasma - Google Patents
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Abstract
The invention discloses a method for preparing a nano gold/polyvinyl alcohol composite material by normal pressure plasma, which comprises the following steps: s1, preparing a normal pressure plasma device; s2, preparing a solution; s3, carrying out plasma treatment; s4, dripping the nano gold/polyvinyl alcohol solution subjected to plasma jet treatment into different polytetrafluoroethylene molds, placing the molds into a blast drying oven, and drying for 2-4 hours at 60 ℃ to finally obtain the film-shaped nano gold/polyvinyl alcohol composite material. The invention has the advantages that: the preparation time is short, the process flow is simple and flexible, no strong reducing agent is needed to be added, no pollution is caused to the environment, and the nano gold particles with the size within the range of 10-20nm can be obtained through control.
Description
Technical Field
The invention relates to the technical field of nano material preparation, in particular to a method for preparing a nano gold/polyvinyl alcohol composite material by using normal pressure plasma.
Background
The nano gold refers to gold micro particles, the size of the gold micro particles is within the range of 1-100 nm, and the gold nano particles have photo-thermal characteristics which macroscopic simple substance gold does not have under the size, so the nano gold has wide application in the fields of chemistry, biology, medicines, foods and the like due to excellent small-size effect, special optical effect and biocompatibility.
Polyvinyl alcohol is a powdery organic compound which can be dissolved in water (above 95 ℃), and PVA hydrogel can be obtained through repeated cycles of freezing and thawing. Hydrogels are a class of very hydrophilic gels with a three-dimensional network structure that swell rapidly in water and retain a high water uptake without dissolving, and thus are able to retain a certain shape. Physical and chemical crosslinking effects among polymer chains have a vital influence on the water absorption capacity of the hydrogel, and meanwhile, the hydrogel is harmless to a human body and has good biocompatibility, and adverse reactions can be reduced by implanting the hydrogel into the human body, so that the PVA hydrogel is widely applied as excellent biomedical materials such as wound dressings and articular cartilages of the human body.
The main preparation methods of the existing nano gold can be divided into: sodium citrate reduction method, crystal seed growth method, two-phase method, electrochemical synthesis method and biological reduction method.
The method for preparing the spherical nano gold with the particle size of 10-50 nm is commonly used for preparing single nano gold, and is firstly proposed by Turkevich et al in 1951, namely a sodium citrate reduction method. However, it is difficult to prepare small-sized gold nanoparticles by this method, and the chemical interface of the gold nanoparticles prepared by this method is unclear, and in the patent of zhao et al (zhao, li crystal, yan bo, a method for preparing gold nanoparticles with echinoid shape by using seed-mediated method, china 201110251316.4), the gold nanoparticles crystal nuclei are first prepared by using weak reducing agent, so as to prepare nanoparticles with different particle sizes and shapes. Most importantly, the nano gold particles with the size of more than 20nm have obvious cytotoxicity, and the size of the nano gold particles synthesized by the normal-pressure plasma is 10-20nm, so that the harm of the nano gold particles to organisms is reduced to a certain extent.
Michael Faraday described for the first time the preparation of nanogold, and later zsignond incorporated its own new technology with the discovery of Faraday, thereby introducing the concept of crystal seed growth. The method is to take nano-gold particles with small size as the nucleation base point, and then add precursor aqueous solution containing gold ions in the presence of a reducing agent, thereby obtaining nano-gold particles with different shapes. However, in the process of preparing the nano gold, the particles have excessive secondary nucleation phenomenon.
In 1994, a two-phase process was developed by Brust and Schiffrin et al, which has great potential for the preparation of small-sized gold nanoparticles (e.g., 1-3nm) by transferring Au3+ ions from an aqueous precursor solution to an oil phase using tetraoctylammonium bromide (TOAB) as a phase transfer agent, and then reducing Au3+ to Au0 using NaBH4 as a reducing agent. Finally, centrifugal drying is carried out to obtain small-sized gold nanoparticles. In the preparation process, chemical medicines such as a strong reducing agent, a transfer agent and the like are required to be added, the preparation process is complex, the environment is polluted, and the purity of the obtained gold nanoparticles is influenced to a certain degree.
The electrochemical synthesis method is one of the potential methods for preparing the nano-gold at present, the method can effectively control the thickness, the surface appearance, the conductivity and other properties of nano-gold particles by changing the current density under the condition of controlling the same potential, and the preparation process flow is flexible and convenient and has no pollution to the environment. However, the electrochemical synthesis method requires a large amount of electric energy and is very costly.
According to the patent of (Tianbing, Lijiulong, a preparation method of nano-gold, nano-gold and application, China, 201710979975.7), radiation-resistant deinococcus thalli is crushed, supernatant liquid is extracted to prepare a nano-gold synthesis agent, and then the nano-gold synthesis agent is added into a solution containing Au3+ ions for continuous reaction, so that nano-gold particles with the size of about 51.72nm are obtained. The biological reduction method is considered as reduction reaction of organisms to metal ions or metabolism of the organisms, Au3+ in a precursor is reduced into Au0 through certain enzymes secreted by the organisms and having redox property, meanwhile, the organisms can also serve as crystal nuclei for growth of the nano gold particles, and the nano gold particles with different sizes and shapes can be prepared by regulating and controlling the extraction amount of the microorganisms. However, compared with the plasma synthesis method in the present invention, the method has the disadvantages of complicated extraction process, more process steps and longer time consumption.
Cancer is always a key factor influencing human life health, the number of people dying from various cancers worldwide increases year by year, cancer treatment is always a focus of attention of researchers, and for cancer, people always keep the consciousness concept of early discovery and early treatment, so that the search for an effective method for diagnosing and curing cancer becomes a research hotspot. The current common cancer treatment approaches: traditional operative treatment, drug therapy, radiation therapy, and novel photothermal treatment, the traditional operative treatment is very traumatic to patients, and the risk of the operation is very high, and a series of operative complications are caused. The drug treatment can generate obvious toxic reaction to normal tissues and organs of a human body while preventing the growth of cancer cells. Radiotherapy is a treatment method used in cancer treatment, which can kill diseased cancer cells directly or indirectly, but has a non-negligible effect on human body. In view of this, with the development of science and technology, the photothermal therapy of killing cancer cells by using the photothermal effect of nanogold gradually enters the field of view of the public, nanogold itself is used as a photosensitizer and has high photothermal conversion efficiency, and under the irradiation of laser with a specific wavelength, absorbed energy can be dissipated in the form of heat, so that the proteins and DNA of cancer cells are destroyed, and finally the purpose of killing cancer cells is achieved.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a method for preparing the nano gold/polyvinyl alcohol composite material by using the normal pressure plasma, which has the advantages of short preparation time, simple and flexible process flow, no need of adding a strong reducing agent, no pollution to the environment and capability of controlling and obtaining nano gold particles with the size within the range of 10-20 nm.
In order to solve the technical problems, the technical scheme provided by the invention is as follows: a method for preparing a nano gold/polyvinyl alcohol composite material by normal pressure plasma comprises the following steps:
s1, preparing a normal pressure plasma device, wherein the pressure plasma device is composed of an anode, a cathode, a mixed liquid, a workbench, a flow display instrument and a DC direct current power supply, the anode is a rod-shaped platinum electrode, the anode is immersed in the mixed liquid in a glass vessel and is externally connected with a DC direct current power supply anode, the cathode is a stainless steel tube with the inner diameter of 200-300 mu m, the stainless steel tube is vertically placed on the mixed liquid level for 1-2 mm, and the DC direct current power supply cathode is externally connected;
s2, preparing a solution, namely adding the solution A and the solution B into a prepared glass dish to prepare a mixed solution C, placing the mixed solution C on a magnetic stirrer until the mixed solution is uniformly stirred, wherein the solution A is a HAuCl4 solution with the concentration of 2.5 mu M-4 mM, the solution B is polyvinyl alcohol powder with the alcoholysis degree of 99% -99.4%, weighing the polyvinyl alcohol powder with certain mass by using a balance, pouring the polyvinyl alcohol powder into a conical flask, adding ultrapure water with certain mass, placing the conical flask on an 85-2A double-digital display constant-temperature magnetic stirrer, regulating the temperature to be within the range of 80-95 ℃, and stirring for about 20-40 minutes until the solution is clear, thereby preparing a sol solution with the mass fraction of 1% -10%;
s3, performing plasma treatment, before switching on a power supply, opening an air valve to introduce helium, adjusting the display number of a gas flow indicator to be 10-100 sccm, then switching on a DC (direct current) power supply, adjusting the current to be within a range of 3-6 mA to maintain the stability of plasma jet, then opening a magnetic stirrer on a workbench of the device to gently stir the mixed solution to keep the whole liquid level flat, and performing plasma jet treatment for 10-60 min to finally obtain the nanogold/polyvinyl alcohol solution which presents different colors such as pink, wine red, deep red and purple red;
s4, dripping the nano gold/polyvinyl alcohol solution subjected to plasma jet treatment into different polytetrafluoroethylene molds, placing the molds into a blast drying oven, and drying for 2-4 hours at 60 ℃ to finally obtain the film-shaped nano gold/polyvinyl alcohol composite material.
Further, the inside diameter of the stainless steel tube used for the cathode in S1 was selected to be 250 μm.
Further, the stainless steel tube used for the cathode in S1 maintained an interfacial distance of 1mm from the mixed solution.
Further, the solution A described in S2 was selected from HAuCl at a concentration of 2.5. mu.M, 0.05mM, 0.1mM, 0.2mM, 0.4mM, 0.6mM, 1.0mM, 2.0mM, respectively 4 And (3) solution.
Further, the solutions B described in S2 were prepared by weighing 1g, 4g, and 8g of polyvinyl alcohol powder, and dissolving in 99ml, 96ml, and 92ml of ultrapure water, respectively.
Further, the temperature of the constant-temperature magnetic stirrer in S2 is 90 ℃, the stirring time is controlled to be 30min, and finally PVA solutions with mass fractions of 1%, 4% and 8% are obtained.
Further, the gas flow rate display instrument described in S3 shows 50 sccm.
Further, the DC direct current power supply described in S3 has a current value of 5 mA.
Further, the treatment time of the plasma jet described in S3 was 10 min.
Further, the temperature of the forced air drying oven described in S4 was 60 ℃, and the drying time was 4 hours.
Compared with the prior art, the invention has the advantages that:
1. according to the invention, the Au3+ is reduced by utilizing electrons and active particles in the plasma jet, and the PVA hydrogel is used as a stabilizer, so that the agglomeration phenomenon of nano gold particles is effectively solved, the size of the nano gold particles is controlled within the range of 10-20nm, other strong reducing agents, phase-change agents and the like are not required to be added in the preparation process, the preparation process flow is simplified to a certain extent, the purity of the nano gold is improved, the energy is saved, the environment is protected, and the environment is not polluted;
2. the PVA hydrogel has biocompatibility and good water absorption, so that an application prospect is provided for a human wound dressing material, the nano-gold has good photo-thermal effect, the thermal effect of the nano-gold particles can be used for preventing the growth of cancer cells under the irradiation of specific wavelength, even killing the cancer cells, and simultaneously reducing the damage to normal tissues of a human body, the prepared nano-gold particles can be uniformly dispersed in the PVA three-dimensional grid, and besides the excellent thermal conversion efficiency of the nano-gold particles, the PVA hydrogel can improve the thermal stability of the nano-gold particles to a certain extent, so that the sustainability of nano-gold photo-thermal treatment is achieved.
Drawings
FIG. 1(a) is a graph of samples of AuNP/m-PVA at different concentrations;
FIG. 1(b) is a TEM and particle size characterization of AuNP/m-PVA at different concentrations;
FIG. 1(c) is a UV-VIS characterization of AuNP/m-PVA at different concentrations;
FIG. 2 is an FTIR characterization of AuNP/m-PVA at different concentrations;
FIG. 3 is an XPS characterization of different concentrations of AuNP/m-PVA;
FIGS. 4 and 5 are photothermal characterization of AuNP/m-PVA at different concentrations;
FIGS. 6 and 7 are the antibacterial characterization of AuNP/m-PVA at different concentrations;
Detailed Description
Example 1
Preparation of nano gold/polyvinyl alcohol
A method for preparing a nano gold/polyvinyl alcohol composite material by normal pressure plasma comprises the following steps:
5mL of 0.1mM HAuCl4 solution and 5mL of 4% PVA were added to the prepared glass plate to prepare 10mL of a mixture of 0.05mM HAuCl4+ 4% PVA, and then HAuCl4 solution of other concentration was prepared in the same manner.
Placing the prepared mixed solution on a magnetic stirrer, stirring until the mixed solution is uniform, then immersing a platinum electrode into the mixed solution, vertically placing a stainless steel tube filled with helium on the position 1mm above the liquid surface, introducing helium until a flow display is stabilized to 50sccm, turning on a DC (direct current) power supply to adjust the current to be stabilized to 5mA, connecting a circuit according to the steps of the device, and performing plasma treatment for 10min to obtain a mixed solution color comparison chart.
Example 2
The gold nanoparticles prepared in example 1 were examined
After AuNP with different concentrations is treated by plasma jet, the color of the sample solution sequentially changes from pink, wine red, dark red and purple (as shown in figure 1 a). It can be seen by TEM of nanogold (see fig. 1b) that the surface morphology of the prepared nanogold particles is mainly spherical, and the size of the particles is continuously increased along with the increase of the concentration of the precursor (HAuCl4), and is basically in the range of 10-20nm, and meanwhile, the nanogold particles can be uniformly dispersed in the three-dimensional grid of PVA. According to the UV-VIS spectrum of the sample (see FIG. 1c), the SPR peak of the solution mainly appears between 520-530nm, which indicates that Au3+ in the original solution has been reduced to Au0, and is mainly spherical nano-gold, and moreover, the SPR peak gradually appears in a red shift phenomenon with the increase of the concentration of HAuCl4, which indicates that the size of the nano-gold particles is gradually increased, and the results are consistent with the results presented in the TEM image.
The molecule of each substance has a certain molecular structure and energy level diagram, and it can be seen from the FTIR diagram of the sample (see figure 2) that the hydrogen bond enhancement in the PVA molecule may be caused by the existence of the chemical substance H2O2 generated by plasma induction and other active free radicals such as O, H, OH, but any change of the hydrogen bond environment will not cause the change of the corresponding FTIR peak of the PVA, the formation of the hydrogen bond is mainly shown at the broad peak, while the broad frequency band of 3200cm-1 to 3500cm-1 can be attributed to the stretching vibration of the-OH functional group in the PVA molecule, and the peaks around 2913cm-1, 1644cm-1 and 1084cm-1 can be associated with the bending of-CH 2 group.
It can be seen from sample XPS (see fig. 3) that the element Au4f in the sample can be well fitted with a double peak, where the binding energies of the two peaks are 83.6eV and 87.3eV, respectively. Moreover, the two element states of Au4f and the element state of Au0 are the same, so that it can be seen that after plasma treatment, Au3+ ions in the solution have been reduced to a simple substance of Au0, and the spectrum shows no peak of Au3+ ions, which indicates that the Au element exists in the sample in the form of a simple substance.
Example 3
The properties of the nanogold/polyvinyl alcohol material prepared in example 1 were evaluated by the following steps:
from photo-thermal experiments (see fig. 4) of samples, after 808nm and 0.8W cm-2 laser irradiation for 3min, the temperature of the samples is in a state of overall rising, but the CP-m-PVA used as a comparison has no obvious change under the laser irradiation, which shows that the sample material has higher photo-thermal conversion efficiency due to the existence of nano-gold, particularly, the highest temperature rising of the 2.0mM AuNP/m-PVA nano composite material under the near infrared spectrum of 0.8W cm-2 is within 30s, the temperature is over 45 ℃, and after 3min irradiation, the temperature is nearly 70 ℃, and the precondition requirement of photo-thermal antibiosis is far satisfied. After the sample is subjected to laser cyclic irradiation for 6min (see fig. 5), the temperature rise and the temperature decrease of the material show a stable trend, and due to the coating effect of the PVA hydrogel on the nano gold particles, the material has good thermal stability, meanwhile, the cyclic utilization of the material can be realized, and the application prospect of the material in the field of biomedicine is widened.
From the antibacterial experiments of the samples (see fig. 6 and 7), it can be seen that the 2.5 μ M AuNP/M-PVA, 0.2mM AuNP/M-PVA and 2.0mM AuNP/M-PVA without laser irradiation (power density of 0.8W · cm-2) have a bacteriostatic rate of-20% for escherichia coli and-15% for staphylococcus aureus, because of the tiny antibacterial property of AuNP, Au3+ ions can be adsorbed on the cell membrane of bacteria, thereby destroying the protein and DNA structure and finally causing bacterial cell damage. The sample irradiated by laser has obvious inhibition effect on escherichia coli and staphylococcus aureus, and particularly, the 2.0mM AuNP/m-PVA sample material has the inhibition rate of 97 percent on the escherichia coli and 100 percent on the staphylococcus aureus after near infrared radiation. Therefore, the nano-gold/polyvinyl alcohol composite material prepared by the method is expected to become a wound dressing and an antibacterial material in the field of bioengineering.
Although the present invention has been described in detail with reference to the above embodiments, it should be understood by those skilled in the art that: modifications and equivalents may be made thereto without departing from the spirit and scope of the invention and it is intended to cover in the claims the invention as defined in the appended claims.
Claims (10)
1. A method for preparing a nano gold/polyvinyl alcohol composite material by normal pressure plasma is characterized by comprising the following steps:
s1, preparing a normal pressure plasma device, wherein the pressure plasma device is composed of an anode, a cathode, a mixed liquid, a workbench, a flow display instrument and a DC direct current power supply, the anode is a rod-shaped platinum electrode, the anode is immersed in the mixed liquid in a glass vessel and is externally connected with a DC direct current power supply anode, the cathode is a stainless steel tube with the inner diameter of 200-300 mu m, the stainless steel tube is vertically placed on the mixed liquid level for 1-2 mm, and the DC direct current power supply cathode is externally connected;
s2, preparing a solution, namely adding the solution A and the solution B into a prepared glass dish to prepare a mixed solution C, placing the mixed solution C on a magnetic stirrer until the mixed solution is uniformly stirred, wherein the solution A is a HAuCl4 solution with the concentration of 2.5 mu M-4 mM, the solution B is polyvinyl alcohol powder with the alcoholysis degree of 99% -99.4%, weighing the polyvinyl alcohol powder with certain mass by using a balance, pouring the polyvinyl alcohol powder into a conical flask, adding ultrapure water with certain mass, placing the conical flask on an 85-2A double-digital display constant-temperature magnetic stirrer, regulating the temperature to be within the range of 80-95 ℃, and stirring for about 20-40 minutes until the solution is clear, thereby preparing a sol solution with the mass fraction of 1% -10%;
s3, performing plasma treatment, before switching on a power supply, opening an air valve to introduce helium, adjusting the display number of a gas flow indicator to be 10-100 sccm, then switching on a DC (direct current) power supply, adjusting the current to be within a range of 3-6 mA to maintain the stability of plasma jet, then opening a magnetic stirrer on a workbench of the device to gently stir the mixed solution to keep the whole liquid level flat, and performing plasma jet treatment for 10-60 min to finally obtain the nanogold/polyvinyl alcohol solution which presents different colors such as pink, wine red, deep red and purple red;
s4, dripping the nano gold/polyvinyl alcohol solution subjected to plasma jet treatment into different polytetrafluoroethylene molds, placing the molds into a blast drying oven, and drying for 2-4 hours at 60 ℃ to finally obtain the film-shaped nano gold/polyvinyl alcohol composite material.
2. The method for preparing the nano gold/polyvinyl alcohol composite material by the normal pressure plasma according to claim 1, wherein the method comprises the following steps: the inside diameter of the stainless steel tube used for the cathode in S1 was selected to be 250 μm.
3. The method for preparing the nano gold/polyvinyl alcohol composite material by the atmospheric pressure plasma according to claim 1, wherein the method comprises the following steps: the stainless steel tube used for the cathode in S1 maintained an interfacial distance of 1mm from the mixed solution.
4. The method for preparing the nano gold/polyvinyl alcohol composite material by the atmospheric pressure plasma according to claim 1, wherein the method comprises the following steps: the solution A described in S2 was HAuCl selected at a concentration of 2.5. mu.M, 0.05mM, 0.1mM, 0.2mM, 0.4mM, 0.6mM, 1.0mM, 2.0mM, respectively 4 And (3) solution.
5. The method for preparing the nano gold/polyvinyl alcohol composite material by the atmospheric pressure plasma according to claim 1, wherein the method comprises the following steps: the solution B described in S2 was prepared by weighing 1g, 4g, and 8g of polyvinyl alcohol powder, and dissolving in 99ml, 96ml, and 92ml of ultrapure water, respectively.
6. The method for preparing the nano gold/polyvinyl alcohol composite material by the atmospheric pressure plasma according to claim 1, wherein the method comprises the following steps: the temperature of the constant-temperature magnetic stirrer in the S2 is 90 ℃, the stirring time is controlled to be 30min, and PVA solutions with the mass fractions of 1%, 4% and 8% are finally obtained.
7. The method for preparing the nano gold/polyvinyl alcohol composite material by the atmospheric pressure plasma according to claim 1, wherein the method comprises the following steps: the gas flow rate display instrument described in S3 shows 50 sccm.
8. The method for preparing the nano gold/polyvinyl alcohol composite material by the atmospheric pressure plasma according to claim 1, wherein the method comprises the following steps: the DC power supply described in S3 has a current value of 5 mA.
9. The method for preparing the nano gold/polyvinyl alcohol composite material by the atmospheric pressure plasma according to claim 1, wherein the method comprises the following steps: the treatment time of the plasma jet described in S3 was 10 min.
10. The method for preparing the nano gold/polyvinyl alcohol composite material by the atmospheric pressure plasma according to claim 1, wherein the method comprises the following steps: the temperature of the air drying oven in the S4 is 60 ℃, and the drying time is 4 h.
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| CN115784314A (en) * | 2022-11-28 | 2023-03-14 | 昆明理工大学 | Method for preparing strontium manganate with assistance of jet plasma |
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| CN115784314A (en) * | 2022-11-28 | 2023-03-14 | 昆明理工大学 | Method for preparing strontium manganate with assistance of jet plasma |
| CN115784314B (en) * | 2022-11-28 | 2024-03-12 | 昆明理工大学 | Method for preparing strontium manganate with assistance of jet plasma |
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