CN113371695A - Preparation method of graphene and precious metal composite slurry - Google Patents
Preparation method of graphene and precious metal composite slurry Download PDFInfo
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- CN113371695A CN113371695A CN202110684673.3A CN202110684673A CN113371695A CN 113371695 A CN113371695 A CN 113371695A CN 202110684673 A CN202110684673 A CN 202110684673A CN 113371695 A CN113371695 A CN 113371695A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 67
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 67
- 239000002002 slurry Substances 0.000 title claims abstract description 17
- 239000002131 composite material Substances 0.000 title claims abstract description 13
- 239000010970 precious metal Substances 0.000 title claims abstract description 13
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 229910000510 noble metal Inorganic materials 0.000 claims abstract description 47
- 239000002905 metal composite material Substances 0.000 claims abstract description 24
- 239000002243 precursor Substances 0.000 claims abstract description 21
- 239000003960 organic solvent Substances 0.000 claims abstract description 15
- 239000002245 particle Substances 0.000 claims abstract description 7
- 150000003839 salts Chemical class 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims description 18
- 238000006243 chemical reaction Methods 0.000 claims description 17
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 12
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 9
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 9
- 229910017053 inorganic salt Inorganic materials 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 9
- 239000011159 matrix material Substances 0.000 claims description 7
- 239000012454 non-polar solvent Substances 0.000 claims description 7
- GQEZCXVZFLOKMC-UHFFFAOYSA-N 1-hexadecene Chemical compound CCCCCCCCCCCCCCC=C GQEZCXVZFLOKMC-UHFFFAOYSA-N 0.000 claims description 6
- BCKXLBQYZLBQEK-KVVVOXFISA-M Sodium oleate Chemical compound [Na+].CCCCCCCC\C=C/CCCCCCCC([O-])=O BCKXLBQYZLBQEK-KVVVOXFISA-M 0.000 claims description 6
- 239000012459 cleaning agent Substances 0.000 claims description 6
- 238000005342 ion exchange Methods 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 6
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 6
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 5
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 5
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 5
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 5
- 239000005642 Oleic acid Substances 0.000 claims description 5
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 4
- 238000010992 reflux Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 229920001577 copolymer Polymers 0.000 claims description 3
- 229920001971 elastomer Polymers 0.000 claims description 3
- 239000000839 emulsion Substances 0.000 claims description 3
- 239000003822 epoxy resin Substances 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 3
- 230000008020 evaporation Effects 0.000 claims description 3
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 claims description 3
- IZLAVFWQHMDDGK-UHFFFAOYSA-N gold(1+);cyanide Chemical compound [Au+].N#[C-] IZLAVFWQHMDDGK-UHFFFAOYSA-N 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- CCCMONHAUSKTEQ-UHFFFAOYSA-N octadecene Natural products CCCCCCCCCCCCCCCCC=C CCCMONHAUSKTEQ-UHFFFAOYSA-N 0.000 claims description 3
- 229920000647 polyepoxide Polymers 0.000 claims description 3
- 239000004814 polyurethane Substances 0.000 claims description 3
- 229920002635 polyurethane Polymers 0.000 claims description 3
- 229940096017 silver fluoride Drugs 0.000 claims description 3
- REYHXKZHIMGNSE-UHFFFAOYSA-M silver monofluoride Chemical compound [F-].[Ag+] REYHXKZHIMGNSE-UHFFFAOYSA-M 0.000 claims description 3
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 238000011946 reduction process Methods 0.000 abstract description 5
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 3
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 abstract description 2
- 239000006185 dispersion Substances 0.000 abstract description 2
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 abstract description 2
- 231100000252 nontoxic Toxicity 0.000 abstract description 2
- 230000003000 nontoxic effect Effects 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 231100000331 toxic Toxicity 0.000 abstract description 2
- 230000002588 toxic effect Effects 0.000 abstract description 2
- 230000035945 sensitivity Effects 0.000 description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 5
- 239000011889 copper foil Substances 0.000 description 4
- 230000010354 integration Effects 0.000 description 4
- 239000002105 nanoparticle Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 3
- 239000004926 polymethyl methacrylate Substances 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000000149 argon plasma sintering Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000002059 diagnostic imaging Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002082 metal nanoparticle Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- -1 oleic acid modified graphene Chemical class 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
Abstract
The invention relates to the technical field of graphene, in particular to a preparation method of graphene precious metal composite slurry. The preparation method sequentially comprises the steps of preparing a graphene oxide/noble metal salt precursor, preparing graphene noble metal composite particles and preparing graphene noble metal composite slurry. The graphene precious metal composite material with uniform dispersion is obtained, the preparation process is environment-friendly, the operation is simple, the cost is low, and the graphene precious metal composite material is suitable for large-scale production, and particularly, a nontoxic high-temperature organic solvent is adopted in the reduction process of graphene oxide, so that the use of toxic and harmful substances such as hydrazine hydrate and the like in the traditional reduction process is avoided.
Description
Technical Field
The invention relates to a method for preparing graphene and precious metal composite slurry.
Background
The CMOS image sensor is one of the basic devices for modern visual information acquisition, can realize the rapid acquisition and conversion of light intensity information and provide the rapid change information of a light field in time and space dimensions, and is widely applied to the fields of machine vision, industrial detection, medical imaging and the like. CMOS image sensors typically output an electrical signal in a carrier integration mode, the strength of which is proportional to the device sensitivity and integration time. In order to obtain clear images, the CMOS image sensor has a remarkable characteristic of allowing integration time to be extremely short, on the order of μ s or even ns, when applied to ultra-high-speed measurement. For example, in ultra-high speed processing, aiming at a high-speed spindle, the requirement of 20000-60000 r/min for absolute position measurement and positioning is met, and an absolute circular grating encoder with the highest rotating speed of 36000r/min is provided by Renyshao corporation in England by customizing measures such as a CMOS image sensor; to prevent blurring of the encoder image at high motion speeds, the allowable integration time of a CMOS image sensor is within 50 ns. To ensure the output signal strength, improving the sensitivity of the device becomes one of the key problems in developing a CMOS image sensor for ultra-high speed measurement.
The sensitivity of a CMOS image sensor is determined by the fill factor and quantum efficiency. The fill factor is mainly determined by the structure of the CMOS image sensor; quantum efficiency is defined as the percentage of photons received by the photosensitive surface that are converted into electron-hole pairs, and is primarily determined by the material of the photosensitive unit. The conventional CMOS image sensor has a light sensing unit made of silicon, and the light reflection rate of silicon is about 30%, which greatly limits the sensitivity of the CMOS image sensor. The research and development for improving the sensitivity of the CMOS image sensor include improvement and development of both structure and material.
To further improve CMOS sensitivity, higher trapping efficiency can be achieved by surface plasmon effect and light scattering effect of the nanoparticles. However, the traditional micro-nano processing technology has more steps and a complex production process, a layer of PMMA needs to be spin-coated on a copper foil, a PMMA/copper foil array is obtained through electron beam exposure, then graphene is deposited on the PMMA/copper foil array through CVD, and finally a final graphene/gold nanoparticle/copper foil finished product is obtained through doping of gold nanoparticles so as to enhance the sensitivity of the device.
In summary, in the prior art, the graphene precious metal composite material has the disadvantages of poor matrix combination, poor dispersibility, complex preparation process and the like. Therefore, a method which has the advantages of good binding force between graphene and noble metal, uniform dispersion of graphene, simple process, low cost, convenient material component design and suitability for large-scale production needs to be developed in the field.
Disclosure of Invention
The invention aims to solve the defects and provides a preparation method of graphene and precious metal composite slurry.
In order to overcome the defects in the background art, the technical scheme adopted by the invention for solving the technical problems is as follows: the preparation method of the graphene precious metal composite slurry comprises the following steps:
firstly, preparing a graphene oxide/noble metal salt precursor:
mixing graphene oxide, noble metal inorganic salt and sodium oleate in water and ethanol, adding a nonpolar solvent, stirring, heating, reacting under a reflux condition, standing the solution after the reaction is finished, taking the upper layer oil phase liquid, heating to remove the organic solvent, and vacuum-drying to obtain a viscous graphene oxide/noble metal organic salt precursor;
step two, preparing graphene noble metal composite particles:
adding the precursor prepared in the first step into an organic solvent in an inert atmosphere, and heating and dissolving to uniformly disperse the precursor; transferring the organic solvent to a high-temperature reaction kettle, heating to react for a period of time, cooling to room temperature after the reaction is finished, adding a cleaning agent to wash and centrifuge, and pouring out upper-layer liquid to obtain graphene noble metal composite particles;
step three, preparing graphene precious metal composite slurry:
and dispersing the precursor prepared in the second step in an organic matrix as required to obtain the required graphene noble metal composite slurry.
According to another embodiment of the present invention, further comprising the mole ratio of the noble metal inorganic salt, graphene oxide and sodium oleate in the first step is in the range of 1: (0.005-2.5): (1-2).
According to another embodiment of the present invention, further comprising that the noble metal inorganic salt in the first step is one or two of silver nitrate, silver fluoride, gold chloride, gold cyanide, chloroplatinic acid; the nonpolar solvent is one of n-hexane, toluene, benzene and acetone; .
According to another embodiment of the present invention, it further comprises that the reaction temperature of the ion exchange in the first step is 60 to 100 ℃ and the reaction time of the ion exchange is 0.5 to 5 hours.
According to another embodiment of the present invention, further comprising heating the oil-phase liquid in the first step at a temperature of 100 ℃ and 150 ℃ for an evaporation time of 0.5 to 2 hours.
According to another embodiment of the present invention, the organic solvent in the second step is one or more of octadecene, hexadecene, oleylamine, and oleic acid; the cleaning agent comprises n-hexane, acetone or ethanol.
According to another embodiment of the present invention, the second step further comprises heating to dissolve the precursor at a temperature of 80 to 120 ℃ for a dissolution time of 5 to 30 min.
According to another embodiment of the present invention, it further comprises that the reaction temperature of the reactor in the second step is 120 to 280 ℃ and the reaction time is 30 to 120 min.
According to another embodiment of the present invention, the organic matrix further comprising in the third step comprises epoxy resin, polyurethane, vinylidene chloride copolymer emulsion, chlorinated rubber.
According to another embodiment of the present invention, the graphene noble metal composite slurry in the third step further has a solid content of 1% to 45%.
The invention has the beneficial effects that:
1. introducing graphene oxide firstly in the process of preparing a noble metal precursor, wherein the surface of the graphene oxide has more hydrophilic functional groups and can be dispersed in a water phase, covalent bond modification can be carried out on the graphene oxide and oleic acid at a water-ethanol-nonpolar solvent three-phase interface under a condensation reflux state to obtain oleic acid modified graphene oxide, and in the subsequent thermal reduction process, unsaturated bonds in a high-temperature organic solvent have reducibility and can reduce the graphene oxide into graphene, and meanwhile, the noble metal precursor connected by the covalent bonds is reduced in situ to obtain noble metal nanoparticles to obtain a uniformly dispersed graphene noble metal composite material;
2. according to the invention, the homogeneous reactor is used for carrying out thermal reduction reaction instead of traditional direct stirring, because the graphene is light in density and the noble metal is high in density, the graphene is difficult to be uniformly dispersed in the traditional stirring reaction, and the homogeneous reactor rotates back and forth due to the reactor, so that the dispersibility of the graphene and the noble metal can be improved, the graphene is prevented from floating on the upper layer of the solvent, and the copper is prevented from floating on the lower layer of the solvent;
3. the preparation process is environment-friendly, simple to operate and low in cost, is suitable for large-scale production, and particularly adopts a non-toxic high-temperature organic solvent in the reduction process of the graphene oxide, so that the use of toxic and harmful substances such as hydrazine hydrate and the like in the traditional reduction process is avoided.
Drawings
The invention is further illustrated with reference to the following figures and examples.
Fig. 1 is a field emission scanning electron microscope image of noble metal graphene nanoparticles of example 1.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious 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.
The preparation method comprises the following steps:
firstly, preparing a graphene oxide/noble metal salt precursor:
mixing graphene oxide, noble metal inorganic salt and sodium oleate in water and ethanol, adding a nonpolar solvent, stirring, heating, reacting under a reflux condition, standing the solution after the reaction is finished, taking the upper layer oil phase liquid, heating to remove the organic solvent, and vacuum-drying to obtain a viscous graphene oxide/noble metal organic salt precursor;
step two, preparing graphene noble metal composite particles:
adding the precursor prepared in the first step into an organic solvent in an inert atmosphere, and heating and dissolving to uniformly disperse the precursor; transferring the organic solvent to a high-temperature reaction kettle, heating to react for a period of time, cooling to room temperature after the reaction is finished, adding a cleaning agent to wash and centrifuge, and pouring out upper-layer liquid to obtain graphene noble metal composite particles;
step three, preparing graphene precious metal composite slurry:
and dispersing the precursor prepared in the second step in an organic matrix as required to obtain the required graphene noble metal composite slurry.
Further, in the first step:
the mole ratio of the noble metal inorganic salt to the graphene oxide to the sodium oleate is 1: (0.005-2.5): (1-2);
the noble metal inorganic salt is one or two of silver nitrate, silver fluoride, gold chloride, gold cyanide and chloroplatinic acid;
the nonpolar solvent is one of n-hexane, toluene, benzene and acetone;
the reaction temperature of the ion exchange is 60-100 ℃, and the reaction time of the ion exchange is 0.5-5 hours;
the temperature of the heating oil phase liquid is 100-150 ℃, and the evaporation time is 0.5-2 hours.
Further, in the second step:
the organic solvent is one or more of octadecene, hexadecene, oleylamine and oleic acid; the cleaning agent comprises n-hexane, acetone or ethanol;
heating to dissolve the precursor at 80-120 deg.c for 5-30 min;
the reaction temperature of the reactor is 120-280 ℃, and the reaction time is 30-120 min.
Further, in the third step:
the organic matrix comprises epoxy resin, polyurethane, chloro-meta-copolymer emulsion and chlorinated rubber;
the solid content of the graphene noble metal composite slurry is 1% -45%.
The experimental data in each example are shown in the following table:
the above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (10)
1. A preparation method of graphene and precious metal composite slurry is characterized by comprising the following steps:
firstly, preparing a graphene oxide/noble metal salt precursor:
mixing graphene oxide, noble metal inorganic salt and sodium oleate in water and ethanol, adding a nonpolar solvent, stirring, heating, reacting under a reflux condition, standing the solution after the reaction is finished, taking the upper layer oil phase liquid, heating to remove the organic solvent, and vacuum-drying to obtain a viscous graphene oxide/noble metal organic salt precursor;
step two, preparing graphene noble metal composite particles:
adding the precursor prepared in the first step into an organic solvent in an inert atmosphere, and heating and dissolving to uniformly disperse the precursor; transferring the organic solvent to a high-temperature reaction kettle, heating to react for a period of time, cooling to room temperature after the reaction is finished, adding a cleaning agent to wash and centrifuge, and pouring out upper-layer liquid to obtain graphene noble metal composite particles;
step three, preparing graphene precious metal composite slurry:
and dispersing the precursor prepared in the second step in an organic matrix as required to obtain the required graphene noble metal composite slurry.
2. The method for preparing a graphene noble metal composite paste according to claim 1, wherein: the mole ratio of the noble metal inorganic salt, the graphene oxide and the sodium oleate in the first step is 1: (0.005-2.5): (1-2).
3. The method for preparing a graphene noble metal composite paste according to claim 1, wherein: the noble metal inorganic salt in the first step is one or two of silver nitrate, silver fluoride, gold chloride, gold cyanide and chloroplatinic acid; the nonpolar solvent is one of n-hexane, toluene, benzene and acetone.
4. The method for preparing a graphene noble metal composite paste according to claim 1, wherein: the reaction temperature of the ion exchange in the first step is 60-100 ℃, and the reaction time of the ion exchange is 0.5-5 hours.
5. The method for preparing a graphene noble metal composite paste according to claim 1, wherein: the temperature of the heating oil phase liquid in the first step is 100-150 ℃, and the evaporation time is 0.5-2 hours.
6. The method for preparing a graphene noble metal composite paste according to claim 1, wherein: the organic solvent in the second step is one or more of octadecene, hexadecene, oleylamine and oleic acid; the cleaning agent comprises n-hexane, acetone or ethanol.
7. The method for preparing a graphene noble metal composite paste according to claim 1, wherein: the temperature for heating and dissolving the precursor in the second step is 80-120 ℃, and the dissolving time is 5-30 min.
8. The method for preparing a graphene noble metal composite paste according to claim 1, wherein: the reaction temperature of the reactor in the second step is 120-280 ℃, and the reaction time is 30-120 min.
9. The method for preparing a graphene noble metal composite paste according to claim 1, wherein: the organic matrix in the third step comprises epoxy resin, polyurethane, chloro-meta-copolymer emulsion and chlorinated rubber.
10. The method for preparing a graphene noble metal composite paste according to claim 1, wherein: the solid content of the graphene noble metal composite slurry in the third step is 1% -45%.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106268631A (en) * | 2015-06-04 | 2017-01-04 | 中国科学院上海应用物理研究所 | Graphene-noble metal nano particles Compound Water, aeroge and preparation method thereof, application |
| CN107433402A (en) * | 2017-08-30 | 2017-12-05 | 桂林电子科技大学 | A kind of preparation method and applications of graphene nano silver paste |
| CN109852835A (en) * | 2019-01-23 | 2019-06-07 | 南京工业大学 | A kind of preparation method of graphene/copper nanocomposite |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106268631A (en) * | 2015-06-04 | 2017-01-04 | 中国科学院上海应用物理研究所 | Graphene-noble metal nano particles Compound Water, aeroge and preparation method thereof, application |
| CN107433402A (en) * | 2017-08-30 | 2017-12-05 | 桂林电子科技大学 | A kind of preparation method and applications of graphene nano silver paste |
| CN109852835A (en) * | 2019-01-23 | 2019-06-07 | 南京工业大学 | A kind of preparation method of graphene/copper nanocomposite |
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Application publication date: 20210910 |