CN115353161B - Preparation of palladium phosphorus sulfur micro-nano particles and application thereof in photo-thermal field - Google Patents
Preparation of palladium phosphorus sulfur micro-nano particles and application thereof in photo-thermal field Download PDFInfo
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Abstract
The invention belongs to the technical field of photo-thermal technology, and particularly relates to preparation of palladium phosphorus sulfur micro-nano particles and application of the palladium phosphorus sulfur micro-nano particles in the field of photo-thermal. In order to develop a high-performance palladium phosphorus sulfur micro-nano particle photo-thermal conversion material, the invention takes palladium phosphorus sulfur (PdPS) crystal powder as a material, adopts a laser liquid phase melting technology to carry out laser treatment, and prepares the palladium phosphorus sulfur micro-nano particle material after forming a micro-nano particle structure. The palladium phosphorus sulfur micro-nano particle material prepared by the invention has good biocompatibility, has very good electromagnetic wave absorption behavior in a very wide electromagnetic spectrum range (wavelength is 200nm-2000 nm), is in a macroscopic state of black powder, shows a photo-thermal conversion performance very close to that of a gold nano material in the photo-thermal conversion field, and can be applied to the technical field of photo-thermal.
Description
Technical Field
The invention belongs to the technical field of photo-thermal technology, and particularly relates to preparation of palladium phosphorus sulfur micro-nano particles and application of the palladium phosphorus sulfur micro-nano particles in the field of photo-thermal.
Background
In the field of photo-thermal technology, it is currently accepted that the photo-thermal material with the best performance is gold nanomaterial or carbon-containing inorganic or organic material taking carbon-based nanomaterial as a main body. The gold nano material can maximally convert electromagnetic oscillation of a specific wave band into heat energy by utilizing strong plasmon polarization behavior; the low-cost carbon-based nano materials are characterized in that electromagnetic oscillation of certain wave bands is maximally converted into thermal oscillation of the materials by utilizing the narrow-band structure and the multiple lattice vibration mode of the carbon-based materials, so that high-efficiency photo-thermal conversion behavior is realized in a wide-spectrum wave band. However, most of carbon-based nano materials do not have good biocompatibility, so that the photo-thermal technology based on the carbon-based nano materials can only be applied to the field of industrial photo-thermal conversion with lower added value; while gold nano-materials have good biocompatibility and higher photo-thermal conversion efficiency, and are greatly concerned in the fields of photo-thermal treatment and photo-thermal medicine related to biomedical technology, the plasmon polarization behavior of the gold nano-materials is greatly dependent on the morphological preparation of the gold nano-materials, so that the gold nano-materials are limited in practical application by high manufacturing control cost and complicated chemical purification treatment and are difficult to popularize. At present, most researchers still improve the preparation technology of gold nano materials or alloy other noble metals with the gold nano materials so as to increase the controllability of plasmon behaviors of the gold nano materials, thereby reducing the dependence on the morphological characteristics.
In addition, researchers have been working to find non-gold photothermal conversion nanomaterials with excellent properties, such as emerging two-dimensional materials. Among them, the noble metal palladium-containing compound is an important member of the current two-dimensional material research field, and as palladium which is noble metal together with gold, the noble metal palladium-containing compound should have better photo-thermal conversion behavior in theory. However, there are few reports of palladium-based photothermal conversion materials. Therefore, the preparation process of the palladium photo-thermal conversion material and the related micro-nano material with simple, high-efficiency and excellent performance are developed, so that the palladium photo-thermal conversion material can be applied to photo-thermal treatment of organisms instead of gold nano materials, and has good application prospect.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides a preparation method of a palladium phosphorus sulfur micro-nano particle material, and the prepared palladium phosphorus sulfur micro-nano particle material is a black powdery photo-thermal conversion material in a macroscopic manner, and has very good electromagnetic radiation absorption characteristics in a spectrum range of 200nm-2000nm, particularly in a range of visible light wave band to infrared wave band (500 nm-2000 nm), and is expected to be applied to the technical field of photo-thermal.
In order to achieve the above purpose, the present invention is realized by the following technical scheme:
the invention provides a preparation method of a palladium phosphorus sulfur micro-nano particle material, which comprises the following steps: the method is characterized in that palladium phosphorus sulfur crystal (PdPS) powder is used as a raw material, and is subjected to laser treatment by adopting a laser liquid phase melting technology, so that a micro-nano particle structure is formed.
As a preferred embodiment of the invention, the preparation method of the palladium phosphorus sulfur micro-nano particle material comprises the following steps:
s1, adding the ground palladium phosphorus sulfur crystal powder into a mixed solution of ethylene glycol and water, and fully dispersing to obtain palladium phosphorus sulfur crystal powder suspension;
s2, irradiating the palladium phosphorus sulfur crystal powder suspension in the step S1 by using pulse laser to form a micro-nano particle structure under the laser ablation effect, so as to prepare the palladium phosphorus sulfur micro-nano particle material.
The original palladium phosphorus sulfur crystal powder has substantially no photo-thermal conversion performance because its macroscopic morphology appears as a light gray crystal powder with a specific large optical band gap, and thus the electromagnetic radiation absorption efficiency is low. The invention adopts a laser liquid phase melting processing mode to act on palladium phosphorus sulfur (PdPS) crystal powder, and dissociates the crystal form of the palladium phosphorus sulfur crystal powder to prepare the unique palladium phosphorus sulfur micro-nano particles. The method breaks weaker chemical bonds in the original palladium phosphorus sulfur crystal material, so that P atoms and S atoms in the original palladium phosphorus sulfur crystal material are redistributed and recombined, thereby changing the conductivity and vibration characteristics of the palladium phosphorus sulfur material, and simultaneously, the laser effect also enables macroscopic crystal powder to be fused into a large number of tiny micro-nano particles, thereby greatly increasing the absorption behavior of the macroscopic crystal powder to electromagnetic wave oscillation and greatly improving the photo-thermal conversion performance of the product; and the mode of laser liquid phase melting technology can improve the thermal vibration performance of the prepared palladium phosphorus sulfur micro-nano particle material, exert the thermal efficiency of the photo-thermal conversion material to the maximum extent and realize the environment-friendly photo-thermal conversion behavior.
Preferably, in the palladium phosphorus sulfur crystal powder, the atomic weight ratio of palladium element, phosphorus element and sulfur element is 1:1:1.
Preferably, the volume ratio of the glycol to the water is (2-4): 1. More preferably, the volume ratio of the ethylene glycol to the water is 3:1.
Preferably, the concentration of the palladium phosphorus sulfur crystal powder in the mixed solution is (1-3) mg/(3-15) mL.
Preferably, the energy of the pulse laser is 100-1000mJ, the frequency is 1-50Hz, and the action time is 1-12h.
Preferably, a 355nm YAG laser and a 355nm total reflection mirror are used for irradiating pulse laser; or a 532nm YAG laser, 532nm total reflection mirror; or a 1064nm YAG laser and a 1064nm total reflection mirror.
The invention also discloses the palladium phosphorus sulfur micro-nano particle material prepared by the preparation method.
The palladium phosphorus sulfur micro-nano particle material prepared by the invention is a photo-thermal material with wide electromagnetic spectrum response, and shows stable electromagnetic wave absorption behavior in the electromagnetic spectrum range of 200nm-2000nm, wherein the photo-thermal conversion efficiency at 808nm is very close to that of gold nano particles, for example, the power density is 1W/cm 2 Under 808nm laser irradiation, the temperature of the 1mg/mL palladium phosphorus sulfur sample solution can be increased from room temperature to 85 ℃, and the high-temperature palladium phosphorus sulfur sample solution has strong photo-thermal conversion capability.
The invention also discloses application of the palladium phosphorus sulfur micro-nano particle material in the field of photo-heat.
The invention disperses palladium phosphorus sulfur (PdPS) crystal powder in a certain liquid environment and applies laser liquid phase melting corrosion to the crystal powder to form the palladium phosphorus sulfur micro-nano particle material. The prepared palladium phosphorus sulfur micro-nano particle material is a micro-nano particle structure, belongs to a high-efficiency photo-thermal conversion material, has better photo-thermal conversion behavior at normal temperature and normal pressure, has photo-thermal conversion performance comparable to that of gold nano particle photo-thermal materials reported in published documents (published documents are D' Acun to M, cioni P, gabellie E, presciiu tini G.explication gold nanoparticles for diagnosis and cancer technological aspects.nanotechnology.2021; 32 (19): 192001, or Nardine, S., abadeer, canine, J., murphy (2016) Recent Progress in Cancer Thermal Therapy Using Gold Nanoparticles. of Physical Chemistry C,120 (9)) and solves the problem of biocompatibility of carbon-based nano materials, and can be applied to the technical field of Yu Guangre, such as preparation of materials with photo-thermal conversion effect, even can be combined with the hydrogel and has wide application value in the aspect of specific application to photo-thermal systems.
It should be noted that the palladium phosphorus sulfur micro-nano particles of the present invention may also be synthesized by other means, such as hydrothermal method, and obtained by changing the compound used, such as other sulfide or phosphide or oxide. In addition, the palladium phosphorus sulfur micro-nano particles can be obtained by means of chemical vapor deposition and the like.
Compared with the prior art, the invention has the beneficial effects that:
the invention discloses a preparation method of a palladium phosphorus sulfur micro-nano particle material, which is used for developing a high-performance palladium phosphorus sulfur micro-nano particle photo-thermal conversion material. The palladium phosphorus sulfur micro-nano particle material prepared by the invention is a black powdery micro-nano material with good biocompatibility and good electromagnetic wave absorption behavior in a very wide electromagnetic spectrum range (wavelength 200nm-2000 nm), shows a photo-thermal conversion performance very close to that of a gold nano material in the photo-thermal conversion field, and can be applied to the technical field of photo-thermal.
Drawings
FIG. 1 is a TEM image of the palladium phosphorus sulfur micro-nano particle material prepared in example 1;
FIG. 2 is a TEM high resolution morphology of the palladium phosphorus sulfur micro-nano particle material prepared in example 1;
FIG. 3 is a graph showing the electromagnetic spectrum absorption contrast of a sample of palladium phosphorus sulfur micro-nano particle material and palladium phosphorus sulfur crystal raw powder;
FIG. 4 is a XRD powder diffraction contrast plot of a sample of palladium phosphorus sulfur micro-nano particulate material and palladium phosphorus sulfur crystal primary powder;
FIG. 5 shows that the Pd-P-S micro-nano particle material is 1W/cm 2 The photothermal performance in PBS solution (ph=7.4) under 808nm laser irradiation at 5 different concentration states;
FIG. 6 shows that the palladium phosphorus sulfur micro-nano particle material is modified by BSA at 1W/cm 2 The temperature rise of the photo-thermal performance in pure water under the irradiation of 808nm laser under 5 different concentration states is shown.
Detailed Description
The following describes the invention in more detail. The description of these embodiments is provided to assist understanding of the present invention, but is not intended to limit the present invention. In addition, the technical features of the embodiments of the present invention described below may be combined with each other as long as they do not collide with each other.
The experimental methods in the following examples, unless otherwise specified, are conventional, and the experimental materials used in the following examples, unless otherwise specified, are commercially available.
The laser irradiation treatment in the following examples was performed using a laser liquid phase etching apparatus, namely, a YAG laser, SPECTRA-PHYSICS LASERS, model PS201.
Example 1 preparation method of Palladium phosphorus Sulfur micro-nano particle Material
Firstly, putting 30mg of palladium phosphorus sulfur (PdPS) crystal particles (the mol ratio of Pd to P to S is 1:1:1) into an agate mortar for full grinding to form uniform light gray crystal powder, then dispersing the powder (PdPS powder) into 150mL of mixed solution consisting of IPA (ethylene glycol) and deionized water according to the volume ratio of 3:1, and carrying out ultrasonic dispersion for 10min at room temperature; the solution was then transferred to a 300mL glass bottle and fixed on a magnetic stirrer (magnetic stirrer rotation speed can be set at 100 rpm to 800 rpm). And using a 355nm YAG laser and a 355nm total reflection mirror to irradiate pulse laser into the mixed solution from the glass bottle mouth, wherein the energy of the pulse laser is 100mJ, the frequency is 50Hz, and the action time of the pulse laser is 2 hours, so that the palladium phosphorus sulfur micro-nano particle material is obtained.
Example 2 preparation method of Palladium phosphorus Sulfur micro-nano particle Material
Firstly, putting 10mg of palladium phosphorus sulfur crystal particles (the mol ratio of Pd to P to S is 1:1:1) into an agate mortar for full grinding to form uniform light gray crystal powder, then dispersing the powder (pdPS powder) into 50mL of mixed solution consisting of Ethanol and deionized water according to the volume ratio of 3:1, and carrying out ultrasonic dispersion for 15min at room temperature; the solution was then transferred to a 300mL glass bottle and fixed on a magnetic stirring apparatus. And (3) using a 532nm YAG laser and a 532nm total reflection mirror to irradiate pulse laser into the mixed solution from the glass bottle opening, wherein the energy of the pulse laser is 600mJ, the frequency is 10Hz, and the action time of the pulse laser is 3 hours, so that the palladium phosphorus sulfur micro-nano particle material is obtained.
Example 3 preparation method of Palladium phosphorus Sulfur micro-nano particle Material
Firstly, putting 30mg of palladium phosphorus sulfur crystal particles (the mol ratio of Pd to P to S is 1:1:1) into an agate mortar for full grinding to form uniform light gray crystal powder, then dispersing the powder (pdPS powder) into 30mL of mixed solution consisting of Ethanol and deionized water according to the volume ratio of 4:1, and carrying out ultrasonic dispersion for 30min at room temperature; the solution was then transferred to a 300mL glass bottle and fixed on a magnetic stirring apparatus. And (3) using a 1064nm YAG laser and a 1064nm total reflection mirror to irradiate pulse laser into the mixed solution from the glass bottle mouth, wherein the energy of the pulse laser is 1000mJ, the frequency is 50Hz, and the action time of the pulse laser is 3 hours, so as to obtain the palladium phosphorus sulfur micro-nano particle material.
Experimental example 1 Property and Performance analysis of Palladium phosphorus Sulfur micro-nano particle Material
(1) Transmission Electron Microscope (TEM) analysis
The palladium phosphorus sulfur micro-nano particles prepared in examples 1 to 3 were used as test samples, and were subjected to TEM analysis by a 300kV transmission electron microscope (FEI Tecnai G2F 30, FEI Co., U.S.A.), and in order to investigate the morphology of the nano particles, colloidal solutions of the palladium phosphorus sulfur micro-nano particles after laser action were dropped on a transmission electron microscope copper mesh, and dried under heating by an electric hot plate at 55℃and ethylene glycol was completely volatilized. The obtained TEM images are shown in fig. 1 and 2 (examples 2 and 3 are basically the same as example 1, and are not shown).
As can be seen from a TEM image, the prepared phosphothioate alloy micro-nano particles are not spherical, and all particles have uniform particle size and have a particle size scale of less than 10 nm.
(2) Ultraviolet-visible-near infrared absorption spectroscopy
The absorption spectra of the palladium phosphorus sulfur raw crystal powder and the palladium phosphorus sulfur micro-nano particles in the range of 200-2000nm were tested using a LIFM-ultraviolet-visible-near infrared spectrophotometer (UV-3600, shimadzu corporation) to predict the light absorption capacity thereof.
As can be seen from FIG. 3, the light absorption behavior of the palladium phosphorus sulfur micro-nano particles obtained after the laser action is obviously different from that of the original crystal, the palladium phosphorus sulfur nano particles show strong broadband absorption behavior in the infrared light wave band of 800-2000nm, and the absorption intensity is almost unchanged.
(3) Powder X-ray diffraction structure analysis
The change in crystal structure of the palladium phosphorus sulfur samples before and after the laser action was tested using a functional inorganic-X-ray powder diffractometer (D8 ADVANCE, bruk, germany). Wherein, the original crystal of palladium phosphorus sulfur is directly subjected to powder diffraction analysis; before diffraction analysis, the palladium phosphorus sulfur micro-nano particles are dispersed in glycol to prepare palladium phosphorus sulfur colloidal solution, and the palladium phosphorus sulfur colloidal solution is dripped on a quartz glass sheet, and then the test is carried out after the palladium phosphorus sulfur colloidal solution is fully dried.
As can be seen from fig. 4, the original palladium phosphorus sulfur crystal has a good crystal structure, and the palladium phosphorus sulfur nano-particles after laser action basically maintain the XRD peak of the original crystal, but have obvious bulge structures within the range of 2θ=15 ° -35 °, which indicates that the palladium phosphorus sulfur nano-particles have a certain degree of amorphization on the basis of the original palladium phosphorus sulfur crystal.
(4) Photothermal conversion Performance analysis
The photo-thermal conversion performance test depends on a photo-thermal performance test platform, and the test platform mainly comprises a 808nm laser, a thermal infrared imager and a laser power meter. The test procedure was as follows:
1) Drying the palladium phosphorus sulfur colloid solution after the laser action under vacuum to obtain palladium phosphorus sulfur micro-nano particles; after respectively carrying out ultrasonic dispersion on palladium phosphorus sulfur micro-nano particles and BSA (bovine serum albumin) in water or PBS (phosphate buffer solution, PH-7.4), fully mixing the palladium phosphorus sulfur micro-nano particles and the BSA (bovine serum albumin) in a sample cell, and obtaining sample solutions with palladium phosphorus sulfur concentration of 1mg/mL, 0.5mg/mL, 200 mug/mL, 50 mug/mL and 20 mug/mL respectively by adjusting the content of the palladium phosphorus sulfur micro-nano particles. The sample cell used in the test is a semitransparent plastic round box.
2) The distance between the 808nm laser fiber head and the sample cell is regulated to ensure that the laser spot just completely covers the surface of the sample cell, and the laser power density on the sample surface is 1W/cm by using an optical power meter 2 。
3) The change in temperature of the sample under laser irradiation was recorded using a thermal infrared imager, and the temperature value was recorded every 30 seconds.
The temperature change relationship with time of each group of samples under 808nm laser irradiation was obtained by the above method, and the results are shown in fig. 5 and 6. As can be seen, the initial temperature of the sample solution is about 25℃at 1W/cm 2 After the 808nm laser is irradiated for 5min, the temperature of sample solutions with the concentration of 1mg/mL, 0.5mg/mL, 200 mug/mL, 50 mug/mL and 20 mug/mL can be respectively increased to 84, 75, 70, 50 and 40 ℃, and the good photo-thermal conversion capability is shown, which indicates that the palladium phosphorus sulfur micro-nano particle material prepared by the method of the invention is a high-efficiency photo-thermal material and has excellent photo-thermal conversion performance under the conditions of normal temperature and normal pressure.
The embodiments of the present invention have been described in detail above, but the present invention is not limited to the described embodiments. It will be apparent to those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, and yet fall within the scope of the invention.
Claims (4)
1. The application of the palladium phosphorus sulfur micro-nano particle material in the field of photo-heat is characterized in that the preparation method of the palladium phosphorus sulfur micro-nano particle material comprises the following steps: taking palladium phosphorus sulfur crystal powder as a raw material, and carrying out laser treatment on the palladium phosphorus sulfur crystal powder by adopting a laser liquid phase melting technology to form a micro-nano particle structure; the preparation method of the palladium phosphorus sulfur micro-nano particle material specifically comprises the following steps:
s1, adding the ground palladium phosphorus sulfur crystal powder into a mixed solution of ethylene glycol and water, and fully dispersing to obtain a palladium phosphorus sulfur crystal powder suspension, wherein the atomic weight ratio of palladium element to phosphorus element to sulfur element in the palladium phosphorus sulfur crystal powder is 1:1:1;
s2, irradiating the palladium phosphorus sulfur crystal powder suspension in the step S1 by using pulse laser, wherein the energy during irradiation of the pulse laser is 100-1000mJ, the frequency is 10-50Hz, and the acting time is 2-3 hours, so that the palladium phosphorus sulfur crystal powder suspension forms a micro-nano particle structure under the action of laser ablation, and further the palladium phosphorus sulfur micro-nano particle material is prepared.
2. The use according to claim 1, wherein the volume ratio of ethylene glycol to water is (2-4): 1.
3. The use according to claim 1, wherein the concentration of the palladium phosphorus sulfur crystal powder in the mixed solution is (1-3) mg/(3-15) mL.
4. Use according to claim 1, characterized in that a 355nm yag laser and a 355nm total reflection mirror are used for the irradiation of the pulsed laser; or a 532nmYAG laser and a 532nm total reflection mirror; or a 1064nm YAG laser and a 1064nm total reflection mirror.
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| CN111468141A (en) * | 2019-11-21 | 2020-07-31 | 中山大学 | Preparation method and application of two-dimensional amorphous-crystalline heterojunction |
| CN112742423A (en) * | 2020-12-15 | 2021-05-04 | 中山大学 | Preparation of palladium-phosphorus-sulfur two-dimensional polycrystalline material and application thereof in electrochemical field |
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| CN111468141A (en) * | 2019-11-21 | 2020-07-31 | 中山大学 | Preparation method and application of two-dimensional amorphous-crystalline heterojunction |
| CN112742423A (en) * | 2020-12-15 | 2021-05-04 | 中山大学 | Preparation of palladium-phosphorus-sulfur two-dimensional polycrystalline material and application thereof in electrochemical field |
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