CN112588305B - Interface structure controllable silver nanoparticle/nano diamond composite material and preparation method thereof - Google Patents
Interface structure controllable silver nanoparticle/nano diamond composite material and preparation method thereof Download PDFInfo
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- 239000002113 nanodiamond Substances 0.000 title claims abstract description 58
- 239000002131 composite material Substances 0.000 title claims abstract description 23
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 22
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 17
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 16
- 239000004332 silver Substances 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000010438 heat treatment Methods 0.000 claims abstract description 22
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000002244 precipitate Substances 0.000 claims abstract description 10
- 101710134784 Agnoprotein Proteins 0.000 claims abstract description 9
- 239000002253 acid Substances 0.000 claims abstract description 8
- 238000010306 acid treatment Methods 0.000 claims abstract description 8
- 229910003460 diamond Inorganic materials 0.000 claims abstract description 8
- 239000010432 diamond Substances 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 6
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000010992 reflux Methods 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract description 3
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 12
- 238000009210 therapy by ultrasound Methods 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 2
- 230000001678 irradiating effect Effects 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 238000000034 method Methods 0.000 claims 1
- 239000000463 material Substances 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 239000002114 nanocomposite Substances 0.000 description 4
- 238000005660 chlorination reaction Methods 0.000 description 3
- IXCSERBJSXMMFS-UHFFFAOYSA-N hcl hcl Chemical compound Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 238000001291 vacuum drying Methods 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000004627 transmission electron microscopy Methods 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000012984 biological imaging Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 238000003745 diagnosis Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000002198 surface plasmon resonance spectroscopy Methods 0.000 description 1
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 1
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/06—Halogens; Compounds thereof
- B01J27/08—Halides
- B01J27/10—Chlorides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/48—Silver or gold
- B01J23/50—Silver
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
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- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract
The invention provides a silver nanoparticle/nano-diamond composite material with a controllable interface structure and a preparation method thereof, wherein the preparation method comprises the following steps: (1) heat treatment of the nano-diamond in air atmosphere; (2) carrying out acid treatment on the nano-diamond subjected to the heat treatment in the step (1); (3) the nano-diamond treated by the acid in the step (2) and SOCl 2 Mixing with dimethylformamide, heating and refluxing, cooling to room temperature, and centrifuging to precipitate; (4) washing the precipitate obtained in the step (3) with tetrahydrofuran, and drying in vacuum to obtain chlorinated diamond; (5) adding chlorinated diamond to AgNO 3 In the water solution, the silver nanoparticle/nano-diamond composite material is obtained by ultraviolet lamp irradiation.
Description
Technical Field
The invention relates to the technical field of photocatalytic materials, in particular to a silver nanoparticle/nano-diamond composite material with a controllable interface structure and a preparation method thereof.
Background
At present, nano materials are rapidly developed, particularly, the nano composite materials integrate the advantages of various materials, and have better application prospects in the fields of catalysis, sensors, biological imaging, medical diagnosis and the like. The interface structure and the appearance of the composite material, so that the controllable preparation of the nano composite material is favored by extensive researchers. However, developing simple protocols to synthesize multicomponent nanocomposites has been a challenge. At present, several novel nanocomposite structures such as core-shell nanostructures, segmented nanowires, coated nanoparticles, and anisotropic structured nanomaterials are reported in succession. These studies have been focused on developing nano-heterojunction materials with unique structures, but there are still more challenges to precisely control the nano-interface structure and thus regulate certain specific properties thereof. At present, although the Nano Diamond (ND) and the silver (Ag) are successfully synthesized, the Ag is mostly randomly deposited on the ND surface, so the interface structure is uncontrollable, and the properties and the repeatability of the prepared composite material are not ideal. At present, the research of precisely controlling the interface structure of ND and Ag by a certain technical means so as to control the photoelectric property of ND and Ag is not reported yet.
Disclosure of Invention
The invention provides an interface structure controllable silver nanoparticle/nano diamond composite material and a preparation method thereof, and solves the problem that the interface structure of the existing Ag/ND composite material is uncontrollable.
The technical scheme for realizing the invention is as follows:
the preparation method of the silver nanoparticle/nano-diamond composite material with the controllable interface structure comprises the following steps:
(1) heat treatment of the nano-diamond in air atmosphere;
(2) carrying out acid treatment on the nano-diamond subjected to the heat treatment in the step (1);
(3) the nano-diamond and SOCl treated by the acid in the step (2) 2 Mixing with dimethylformamide, heating and refluxing, cooling to room temperature, and centrifuging to precipitate;
(4) washing the precipitate obtained in the step (3) with tetrahydrofuran, and drying in vacuum to obtain chlorinated diamond;
(5) adding chlorinated diamond to AgNO 3 In the water solution, the silver nanoparticle/nano-diamond composite material is obtained by ultraviolet lamp irradiation.
In the step (1), the size of the nano-diamond is 5 nm, the heat treatment temperature is 420-.
In the step (2), the acid is hydrochloric acid with the mass fraction of 35-50%, the acid treatment temperature is 80-90 ℃, and the ultrasonic treatment is carried out for 12-48 h.
The reflux temperature in the step (3) is 65-80 ℃, and the treatment time is 20-48 h.
AgNO in the step (5) 3 The concentration of the aqueous solution is 0.5-4.0 mg/ml, and the diamond chloride and the AgNO are mixed 3 The mass-volume ratio of the aqueous solution is 1: 5.
and (5) irradiating for 10 min under an ultraviolet lamp of 365 nm.
The invention has the beneficial effects that: the invention achieves the performance of the precisely controlled composite material by effectively controlling the interface structure, and provides a surface modification method to control the interface structure of Ag and ND so as to accurately control the photoelectric performance of the Ag and ND.
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, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is an X-ray diffraction pattern (XRD) of a sample of the present invention;
FIG. 2 is a transmission electron microscopy ("TEM") spectrum of an Ag/ND composite;
fig. 3 is an ultraviolet-visible absorption spectrum of the sample.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art based on the embodiments of the present invention without inventive step, are within the scope of the present invention.
Example 1
The preparation method of the silver nanoparticle/nano-diamond composite material with the controllable interface structure comprises the following steps:
(1) commercially available nanodiamonds (size 5 Nm) (ND) were first heat treated in an air atmosphere: keeping the temperature at 420 ℃ for 30 min, wherein the heating rate is 5 ℃/min;
(2) taking 50 mg of ND subjected to heat treatment for acid treatment, and heating 100ml of hydrochloric acid (HCl) with the mass fraction of 40% to 80-90 ℃ with ultrasonic treatment for 24 hours;
(3) 30mg of acid-treated ND was taken and charged with 100ml of SOCl 2 And 2 ml of Dimethylformamide (DMF), heating to 75 ℃ and treating for 24 h; then cooling to room temperature, centrifuging at 8000rpm, and taking the precipitate;
(4) and (3) ND chlorination: washing the precipitate with tetrahydrofuran for 3 times, and vacuum drying for 24 hr;
(5) adding 50 ml AgNO into 10mg of chlorinated ND 3 In the water solution, the concentration is 2.0 mg/ml, and the solution is irradiated for 10 min under an ultraviolet lamp of 365 nm.
Fig. 1 is an X-ray diffraction pattern (XRD) of a sample, from which it is understood that characteristic diffraction peaks of both Ag and ND appear in the Ag/ND composite material. The two are better compounded together.
FIG. 2 is a transmission electron microscopy pattern of an Ag/ND composite with the Ag and ND particles intimately bonded together.
FIG. 3 is the UV-VIS absorption spectrum of the sample, in which the absorption packet in the Ag/ND composite material at 400-500 nm is caused by the surface plasmon resonance absorption of Ag nanoparticles.
Example 2
The preparation method of the silver nanoparticle/nano-diamond composite material with the controllable interface structure comprises the following steps:
(1) commercially available nanodiamonds (size 5 Nm) (ND) were first heat treated in an air atmosphere: keeping the temperature at 430 ℃ for 50 min, wherein the heating rate is 5 ℃/min;
(2) taking 50 mg of ND subjected to heat treatment for acid treatment, and heating 100ml of hydrochloric acid (HCl) with the mass fraction of 35% to 85 ℃ with ultrasonic treatment for 12 hours;
(3) 30mg of acid-treated ND was added to a solution containing 100ml of SOCl 2 And 2 ml of Dimethylformamide (DMF), heating to 65 ℃ and treating for 20 h; then cooling to room temperature, centrifuging at 8000rpm, and taking the precipitate;
(4) and (3) ND chlorination: washing the precipitate with tetrahydrofuran for 2 times, and vacuum drying for 12 hr;
(5) adding 50 ml AgNO into 10mg of chlorinated ND 3 In water solution, the concentration is 0.5.0 mg/ml, and the solution is irradiated for 10 min under 365 nm ultraviolet lamp.
Example 3
The preparation method of the silver nanoparticle/nano-diamond composite material with the controllable interface structure comprises the following steps:
(1) commercially available nanodiamonds (size 5 Nm) (ND) were first heat treated in an air atmosphere: keeping the temperature at 435 ℃ for 60 min, wherein the heating rate is 5 ℃/min;
(2) taking 50 mg of ND subjected to heat treatment for acid treatment, heating 100ml of hydrochloric acid (HCl) with the mass fraction of 50% to 90 ℃, and carrying out ultrasonic treatment for 48 hours;
(3) 30mg of acid-treated ND was added to a solution containing 100ml of SOCl 2 And 2 ml of Dimethylformamide (DMF), heated to 80 ℃ for 48 treatment); then cooling to room temperature, centrifuging at 8000rpm, and taking the precipitate;
(4) and (3) ND chlorination: washing the precipitate with tetrahydrofuran for 5 times, and vacuum drying for 48 hr;
(5) adding 50 ml AgNO into 10mg of chlorinated ND 3 In the water solution, the concentration is 4.0 mg/ml, and the solution is irradiated for 10 min under an ultraviolet lamp of 365 nm.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (3)
1. The preparation method of the interface structure controllable silver nanoparticle/nano diamond composite material is characterized by comprising the following steps:
(1) heat treatment of the nano-diamond in air atmosphere; the size of the nano diamond is 5 nm, the heat treatment temperature is 420-;
(2) carrying out acid treatment on the nano-diamond subjected to the heat treatment in the step (1); the acid is 35-50% hydrochloric acid by mass, the acid treatment temperature is 80-90 ℃, and the ultrasonic treatment is carried out for 12-48 h;
(3) the nano-diamond treated by the acid in the step (2) and SOCl 2 Mixing with dimethylformamide, heating and refluxing at 65-80 deg.C for 20-48 h, cooling to room temperature, and centrifuging to obtain precipitate;
(4) washing the precipitate obtained in the step (3) with tetrahydrofuran, and drying in vacuum to obtain chlorinated diamond;
(5) adding chlorinated diamond to AgNO 3 In the water solution, ultraviolet lamp irradiation is carried out to obtain the silver nanoparticle/nano diamond composite material; said step AgNO 3 The concentration of the aqueous solution is 0.5-4.0 mg/ml, and the diamond chloride and the AgNO are mixed 3 The mass-volume ratio of the aqueous solution is 1: 5.
2. the method for preparing the interface structure controllable silver nanoparticle/nanodiamond composite material according to claim 1, characterized in that: and (5) irradiating for 10 min under an ultraviolet lamp of 365 nm.
3. A silver nanoparticle/nanodiamond composite material produced by the production method according to claim 1 or 2.
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