CN105181773A - Precious metal composition and application thereof - Google Patents
Precious metal composition and application thereof Download PDFInfo
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- CN105181773A CN105181773A CN201510567167.0A CN201510567167A CN105181773A CN 105181773 A CN105181773 A CN 105181773A CN 201510567167 A CN201510567167 A CN 201510567167A CN 105181773 A CN105181773 A CN 105181773A
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Abstract
The invention discloses a precious metal composition and an application thereof. The precious metal composition is formed by adopting nano precious metal, polylactic acid modified polycarbonate (PPC/PLA) and graphene oxide as main components and is used for preparing an electrode. According to the precious metal composition and the electrode prepared by adopting the precious metal composition as the basis, the advantages of the nano precious metal and the advantages of graphene are combined, so that the precious metal composition has advantages of good conducting performance, low resistance and the like, the precision of an electrochemical sensor is further improved, and the development is directed.
Description
Technical field
The present invention relates to a kind of precious metal composition and application thereof, relate to a kind of precious metal composition that can be used for preparing electrochemical sensor electrodes further, belong to electrochemical field.
Background technology
Obvious to the catalytic oxidation of organic molecule on the precious metal material such as gold, silver, platinum electrode, therefore, noble metal electrode is commonly used for the detection of organic molecule.The electrochemical sensor in order to noble metal electrode being working electrode is when detecting trace organic molecule, and have detection speed soon, the features such as detectability is low, facilitate many, but testing result are consistent than liquid phase chromatography.
In " surface nature of noble metal nano structure and electrode and SERS research ", Xu Minmin points out that nano-noble metal is due to surface effect, and have very large specific surface area, catalysis can accelerate chemical reaction.Therefore, when nano-noble metal is used as electrode, reaction efficiency can be higher, but greatly reduced by the precious metal atom bunch fusing point that small size limits, sometimes even can not stable existence.
Nano-noble metal, in the process being coated to carrier making electrode, accurately, equably can not apply, thus cause the huge waste of noble metal, can not play it better and reduce resistance, improves the effect of electrochemical sensor efficiency.
Summary of the invention
Based on the defect of prior art, the first object of the present invention is, provides a kind of precious metal composition.
A kind of precious metal composition, comprises noble metal, polylactic acid modified Copolycarbonate (PPC/PLA), graphene oxide.
Described noble metal is a kind of or its multiple alloy in Au Ag Pt Pd, osmium, iridium.
The particle diameter of described noble metal is 10 ~ 500nm, preferably 50 ~ 250nm, more preferably 100nm, object is the electrical efficiency increasing electrode, the too little meeting of particle diameter makes nano level metallic particles fusing point reduce, thus melts in redox graphene process, can not keep its original particle diameter.
The weight-average molecular weight of described PPC/PLA is: Mw=10,000 ~ 800,000; Preferably, Mw=60,000 ~ 500,000; More preferably, Mw=300,000.It is by pyrolytic, noble metal is dispersed for adding PPC/PLA object, thus obtains the low electrode of resistivity.
Recording PPC/PLA heat decomposition temperature is: 90 ~ 320 DEG C.
Add graphene oxide in composition, object is reduced to Graphene, strengthens conductive effect, promote that the PPC/PLA do not decomposed completely decomposes completely simultaneously by reduction reaction by increasing conduction specific surface area and being combined with part nano-noble metal.
The present invention also provides the degree of each composition in precious metal composition, various composition weight percentage is: noble metal 10 ~ 20%, polylactic acid modified Copolycarbonate (PPC/PLA) 40 ~ 60%, graphene oxide 20 ~ 50%.
Preferably, various composition weight percentage is: noble metal 12 ~ 18%, polylactic acid modified Copolycarbonate (PPC/PLA) 45 ~ 55%, graphene oxide 27 ~ 43%.
Still more preferably, various composition weight percentage is: noble metal 16%, polylactic acid modified Copolycarbonate (PPC/PLA) 50%, graphene oxide 34%.
The second object of the present invention is to provide a kind of application process of precious metal composition, and described composition under given conditions, can be attached on electrode holder, thus modifies and modified electrode.
V-Mixer is utilized to be 10 by the noble metal granule of mean grain size 10 ~ 500nm and weight-average molecular weight (Mw), 000 ~ 800, the polylactic acid modified Copolycarbonate (PPC/PLA) of 000 mixes, high frequency induction thermal plasma device is utilized to be discarded in plasma atmosphere under argon atmosphere this mixed-powder, utilize filtrator to reclaim the micro mist produced, namely obtain composite particle.In composite particle, add graphene oxide, utilize planetary mill fully to mix, obtain mixed-powder.After mixed-powder drying; heat 0.5 ~ 2.5 hour at 500 ~ 950 DEG C; concrete mode is: muffle furnace is first heated to more than 950 DEG C; cool to design temperature again; under the protection of argon gas, add graphene oxide, period pours argon gas incessantly, in course of reaction; electrode holder can be placed in exit as required, with the electrode of obtained different size in good time.
The consumption of described noble metal, PPC/PLA, graphene oxide carrys out proportioning by the weight percentage of above-mentioned precious metal composition.
Described preferred temperature of reaction is 700 ~ 920 DEG C, and further preferred temperature is 850 DEG C.
The described preferred heat time is 1 ~ 2h, and further the preferred heat time is 1.5h.
The third object of the present invention is to provide the electrochemical sensor that a kind of electrode be made up of the precious metal composition that the present invention relates to builds.
The grain size that precious metal composition involved in the present invention controls nano-noble metal prevents its at high temperature melting, maintains its nano-meter characteristic.The present invention decreases the consumption of noble metal in electrode production process, improve the utilization ratio of noble metal, the polylactic acid modified Copolycarbonate (PPC/PLA) being mixed with nano-noble metal and graphene oxide passes through pyrolytic, a part of noble metal is coated on electrode holder equably, another part noble metal is coated on the graphene oxide (Graphene) after reduction equably, gives full play to the advantage such as high-specific surface area and satisfactory electrical conductivity of Graphene.
Nano-noble metal combines with the advantage of Graphene by the present invention, has prepared the electrode that electric conductivity is good, resistance is low, for the precision improving electrochemical sensor further provides developing direction.
Embodiment
Below by specific embodiment, further technical scheme of the present invention is specifically described.Should be appreciated that, the following examples just as illustrating, and do not limit the scope of the invention, and the apparent change made according to the present invention of those skilled in the art simultaneously and modification are also contained within the scope of the invention.
Embodiment 1
V-Mixer is utilized to be 10 by the nanogold particle 10% of mean grain size 10nm and weight-average molecular weight (Mw), the polylactic acid modified Copolycarbonate (PPC/PLA) 40% of 000 mixes, high frequency induction thermal plasma device is utilized to be discarded in plasma atmosphere under argon atmosphere this mixed-powder, utilize filtrator to reclaim the micro mist produced, namely obtain composite particle.In composite particle, add graphene oxide 50%, utilize planetary mill fully to mix, obtain mixed-powder.After mixed-powder drying, heat 0.8 hour at 900 DEG C, concrete mode is: muffle furnace is first heated to more than 950 DEG C; cool to 900 DEG C again, under the protection of argon gas, add precious metal composition, period pours argon gas incessantly; electrode holder is placed in reactor, obtains described electrode.
Embodiment 2
V-Mixer is utilized to be 60 by the nanoparticle palladium 12% of mean grain size 50nm and weight-average molecular weight (Mw), the polylactic acid modified Copolycarbonate (PPC/PLA) 45% of 000 mixes, high frequency induction thermal plasma device is utilized to be discarded in plasma atmosphere under argon atmosphere this mixed-powder, utilize filtrator to reclaim the micro mist produced, namely obtain composite particle.In composite particle, add graphene oxide 43%, utilize planetary mill fully to mix, obtain mixed-powder.After mixed-powder drying, heat 0.5 hour at 950 DEG C, concrete mode is: muffle furnace is first heated to more than 950 DEG C, then lowers the temperature back 950 DEG C, and under the protection of argon gas, add precious metal composition, period pours argon gas incessantly, obtains described electrode.
Embodiment 3
V-Mixer is utilized to be 100 by the nano-Ag particles 15% of mean grain size 170nm and weight-average molecular weight (Mw), the polylactic acid modified Copolycarbonate (PPC/PLA) 52% of 000 mixes, high frequency induction thermal plasma device is utilized to be discarded in plasma atmosphere under argon atmosphere this mixed-powder, utilize filtrator to reclaim the micro mist produced, namely obtain composite particle.In composite particle, add graphene oxide 33%, utilize planetary mill fully to mix, obtain mixed-powder.After mixed-powder drying, heat 2.5 hours at 500 DEG C, concrete mode is: muffle furnace is first heated to more than 950 DEG C, then lowers the temperature back 500 DEG C, and under the protection of argon gas, add precious metal composition, period pours argon gas incessantly, obtains described electrode.
Embodiment 4
V-Mixer is utilized to be 300 by the nano-platinum particle 16% of mean grain size 100nm and weight-average molecular weight (Mw), the polylactic acid modified Copolycarbonate (PPC/PLA) 50% of 0000 mixes, high frequency induction thermal plasma device is utilized to be discarded in plasma atmosphere under argon atmosphere this mixed-powder, utilize filtrator to reclaim the micro mist produced, namely obtain composite particle.In composite particle, add graphene oxide 34%, utilize planetary mill fully to mix, obtain mixed-powder.After mixed-powder drying, heat 1.5 hours at 850 DEG C, concrete mode is: muffle furnace is first heated to more than 950 DEG C, then cools to 850 DEG C, and under the protection of argon gas, add precious metal composition, period pours argon gas incessantly, and reaction terminates, and obtains electrode.
Embodiment 5
V-Mixer is utilized to be 500 by the nm of gold of mean grain size 250nm/iridium alloy particle 18% and weight-average molecular weight (Mw), the polylactic acid modified Copolycarbonate (PPC/PLA) 55% of 000 mixes, high frequency induction thermal plasma device is utilized to be discarded in plasma atmosphere under argon atmosphere this mixed-powder, utilize filtrator to reclaim the micro mist produced, namely obtain composite particle.In composite particle, add graphene oxide 27%, utilize planetary mill fully to mix, obtain mixed-powder.After mixed-powder drying, heat 1 hour at 920 DEG C, concrete mode is: muffle furnace is first heated to more than 950 DEG C, then cools to 920 DEG C, and under the protection of argon gas, add precious metal composition, period pours argon gas incessantly, obtains described electrode.
Embodiment 6
V-Mixer is utilized to be 200 by the nano-platinum particle 19% of mean grain size 200nm and weight-average molecular weight (Mw), the polylactic acid modified Copolycarbonate (PPC/PLA) 47% of 000 mixes, high frequency induction thermal plasma device is utilized to be discarded in plasma atmosphere under argon atmosphere this mixed-powder, utilize filtrator to reclaim the micro mist produced, namely obtain composite particle.In composite particle, add graphene oxide 34%, utilize planetary mill fully to mix, obtain mixed-powder.After mixed-powder drying, heat 2.3 hours at 700 DEG C, concrete mode is: muffle furnace is first heated to more than 950 DEG C, then cools to 700 DEG C, and under the protection of argon gas, add precious metal composition, period pours argon gas incessantly, obtains described electrode.
Embodiment 7
V-Mixer is utilized to be 800 by the nanoparticle palladium 20% of mean grain size 500nm and weight-average molecular weight (Mw), the polylactic acid modified Copolycarbonate (PPC/PLA) 60% of 000 mixes, high frequency induction thermal plasma device is utilized to be discarded in plasma atmosphere under argon atmosphere this mixed-powder, utilize filtrator to reclaim the micro mist produced, namely obtain composite particle.In composite particle, add graphene oxide 20%, utilize planetary mill fully to mix, obtain mixed-powder.After mixed-powder drying, heat 2 hours at 620 DEG C, concrete mode is: muffle furnace is first heated to more than 950 DEG C, then cools to 620 DEG C, and under the protection of argon gas, add precious metal composition, period pours argon gas incessantly, and reaction end obtains electrode.
Carry out specific insulation measurement to embodiment 1 ~ 7, result is as shown in [table one].
[table]
Claims (10)
1. a precious metal composition, base is characterised in that: comprise noble metal, polylactic acid modified Copolycarbonate (PPC/PLA), graphene oxide;
Wherein, each composition weight percentage in described precious metal composition: noble metal 10 ~ 20%, polylactic acid modified Copolycarbonate (PPC/PLA) 40 ~ 60%, graphene oxide 20 ~ 50%;
Described noble metal is a kind of or its multiple alloy in Au Ag Pt Pd, osmium, iridium.
2. precious metal composition according to claim 1, it is characterized in that: each composition weight percentage in described precious metal composition: noble metal 12 ~ 18%, polylactic acid modified Copolycarbonate (PPC/PLA) 45 ~ 55%, graphene oxide 27 ~ 43%.
3. precious metal composition according to claim 1, it is characterized in that: each composition weight percentage in described precious metal composition: noble metal 16%, polylactic acid modified Copolycarbonate (PPC/PLA) 50%, graphene oxide 34%.
4. arbitrary precious metal composition according to claims 1 to 3, is characterized in that: the particle diameter of described noble metal is 10 ~ 500nm, and the weight-average molecular weight of described PPC/PLA is: Mw=10,000 ~ 800,000.
5. precious metal composition according to claim 4, is characterized in that: the particle diameter of described noble metal is 50 ~ 250nm, and the weight-average molecular weight of described PPC/PLA is: Mw=60,000 ~ 500,000.
6. precious metal composition according to claim 4, is characterized in that: the particle diameter of described noble metal is 100nm, and the weight-average molecular weight of described PPC/PLA is: Mw=300,000.
7. a preparation method for electrode, described electrode is based on precious metal composition arbitrary described in claim 1 ~ 6, and its preparation process is as follows:
(1) V-Mixer is utilized to be 10 by the noble metal granule of mean grain size 10 ~ 500nm and weight-average molecular weight, 000 ~ 800, the polylactic acid modified Copolycarbonate of 000 mixes, high frequency induction thermal plasma device is utilized to be discarded in plasma atmosphere under argon atmosphere this mixed-powder, utilize filtrator to reclaim the micro mist produced, namely obtain composite particle;
(2) in composite particle, add graphene oxide, utilize planetary mill fully to mix, obtain mixed-powder;
(3) by after mixed-powder drying; and heat 0.5 ~ 2.5 hour at 500 ~ 950 DEG C; concrete mode is: muffle furnace is first heated to more than 950 DEG C; cool to design temperature again; under the protection of argon gas, add graphene oxide, period pours argon gas incessantly, in course of reaction; electrode holder is placed in exit, obtained described electrode.
8. the preparation method of electrode according to claim 7, it is characterized in that: described temperature of reaction is 700 ~ 920 DEG C, the described heat time is 1 ~ 2h.
9. the preparation method of electrode according to claim 8, it is characterized in that: described temperature of reaction is 850 DEG C, the described heat time is 1.5h.
10. an electrochemical sensor, is characterized in that: described electrochemical sensor is prepared from based on the arbitrary precious metal composition described in claim 1 ~ 6.
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| CN108414591B (en) | 2020-07-17 |
| CN108414591A (en) | 2018-08-17 |
| CN105181773B (en) | 2018-09-11 |
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