CN101649477A - Preparation method of metal carbon aerogel composite material - Google Patents
Preparation method of metal carbon aerogel composite material Download PDFInfo
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- CN101649477A CN101649477A CN200910306868A CN200910306868A CN101649477A CN 101649477 A CN101649477 A CN 101649477A CN 200910306868 A CN200910306868 A CN 200910306868A CN 200910306868 A CN200910306868 A CN 200910306868A CN 101649477 A CN101649477 A CN 101649477A
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Abstract
The invention provides a preparation method of a metal carbon aerogel composite material. The preparation method comprises the following steps: firstly immerging carbon aerogel in an electroplate liquid of a metal to be plated, processing the aerogel by ultrasonic treatment and impregnation to be used as a cathode, taking a platinum plate as an anode, and controlling the technical parameters of the metal to be plated, such as the pulse frequency, the duty ratio, the temperature, the cathode current density and the plating time, and finally obtaining a metal carbon aerogel composite material. The metal carbon aerogel composite material with micro-pores prepared by the preparation method can be applied to a gas absorption material, a super-capacitor material, a laser inertial confinement fusion target material, a civil hydrogen storage material and other nano materials, and also can be applied to the associated technical field.
Description
Technical field
The invention belongs to the preparation field of metal carbon aerogel composite material, be specifically related to a kind of preparation method of metal carbon aerogel composite material.
Background technology
Carbon aerogels is a kind of novel nano porous material, have many excellent properties, as the specific surface area height, mass density is low, the continuous hole of nano level, constructional features such as nano level skeleton carbon particulate, controllable structure and size adjustable can be used as a kind of good porous support, and various active adulterants are loaded in the carbon aerogels.By with metal-doped in carbon aerogels, can improve the aerogel structure, optimize the performance of aerogel.Metal carbon aerogel composite material can be used for gas adsorption material, super capacitor material, hydrogen storage material, laser inertial confinement fusion target material and other and nano material and technology association area also significant application value.
The preparation method of metal current carbon aerogel composite material mainly contains pickling process, ion exchange method, sol-gel method and out-phase settling process.Pickling process is that the method that the organic aerogel of employing constant pressure and dry floods in the water-soluble metal salts solution prepares metal-doped carbon aerogels.The carbon aerogels material of the loaded metal of immersion process for preparing reunite owing to some metal ion in steeping process easily reduces to grow, thereby metallics size homogeneity is slightly poor.
The patent No. is the patent application material of 99113224.6 " a kind of technology at plating flexible graphite products with thick silver layer ", introduced and adopted electrochemical plating to prepare a kind of method of metal graphite composite material, but because the inside of graphite does not have hole, only limited to the outside surface of graphite by electroplated metal particulate deposition position, graphite inside does not form the compound of graphite and silver, and the matrix material that forms of graphite and silver do not belong to the category of nano material, is difficult to satisfy the application demand of specific occasion at the nano material with a series of excellent specific properties.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of preparation method of metal carbon aerogel composite material.
The preparation method of metal carbon aerogel composite material of the present invention in turn includes the following steps:
(a) electroplate liquid of preparation electroplate liquid preparation plating metal;
(b) under the preparation of carbon aerogels and the pre-treatment room temperature, will be synthetic by sol-gel, the carbon aerogels made of aging, the supercritical drying of exchange of solvent, pickling and high temperature cabonization process puts into the electroplate liquid of the plating metal that step a prepares, behind supersound process 10～30min, flooded again 3～5 days;
(c) electroplating process with the impregnated plating piece carbon aerogels of step b as negative electrode, the platinum plate is made anode, negative electrode and anode are hung in the coating bath that holds plating metal electroplate liquid among the step a together, then coating bath is put into heat collecting type thermostatically heating magnetic stirring apparatus; Characteristic according to plating metal on the pulse plating supply unit is provided with the corresponding techniques parameter, connects power supply then, electroplates under magnetic agitation, produces adulterated carbon aerogels;
(d) clean the doping carbon aerogel washed with de-ionized water for preparing among the step c, be neutral up to washing lotion pH value;
(e) dry the doping carbon aerogel that cleaned in the steps d is put into the vacuum drying oven vacuum drying treatment, vacuum tightness is-0.1MPa, and temperature is controlled at 80～150 ℃ and be incubated 4h, obtains metal carbon aerogel composite material.
Plating metal among the described step a is palladium, copper, iron and silver.
When the plating metal described in the present invention is palladium, the consisting of of electroplate liquid:
Ammonium chloride 15～20ml/L
NH
4OH(25％) 35～40ml/L
Regulate pH value 8.5～9.2 with ammoniacal liquor
According to the characteristic of plating metal palladium, the corresponding techniques parameter be set on the pulse plating supply unit be:
Pulse-repetition 500Hz
Cathode current density 0.2～0.6A/dm
2
Dutycycle 1: 4～1: 1
25 ℃ of temperature.
When the plating metal described in the present invention is copper, the consisting of of electroplate liquid:
Copper sulfate 150～250g/L
According to the characteristic of plating metal copper, the corresponding techniques parameter be set on the pulse plating supply unit be:
Pulse-repetition 500Hz
Cathode current density 1～3A/dm
2
Dutycycle 1: 1
20～40 ℃ of temperature.
When the plating metal described in the present invention is iron, the consisting of of electroplate liquid:
PH value 4.0～5.5
According to the characteristic of plating metal iron, the corresponding techniques parameter be set on the pulse plating supply unit be:
Pulse-repetition 500Hz
Cathode current density 1.5～2.0A/dm
2
Dutycycle 1: 1
20～30 ℃ of temperature.
Plating metal described in the present invention is when silver, the consisting of of electroplate liquid:
Imino-diacetic ammonium sulphonate 90～120g/L
Ammonium sulfate 110～140g/L
Ammonium citrate 2～6g/L
PH value 8.5～9.0
According to the characteristic of plating metal silver, the corresponding techniques parameter be set on the pulse plating supply unit be:
Pulse-repetition 500Hz
Current density 0.2～0.4A/dm
2
Dutycycle 1: 1
15～30 ℃ of temperature.
Carbon aerogels among the step b described in the present invention is a kind of in Resorcinol-formaldehyde carbon aerogels, P-F carbon aerogels, Resorcinol-formaldehyde carbon aerogels or the Phloroglucinol-formaldehyde carbon aerogels.
Anode among the step c described in the present invention adopts palladium plate, graphite or carbon aerogels to substitute.
The preparation method of metal carbon aerogel composite material of the present invention, earlier carbon aerogels is immersed in the plating metal electroplate liquid, through supersound process and the dipping after as negative electrode, anode is selected the platinum plate, technical parameter by the control plated metal, pulse-repetition, dutycycle, temperature, cathode current density and electroplating time are being connected power supply and electroplate liquid are being carried out under the situation of magnetic agitation, meeting metal refining in cathode surface and internal void.It is for electroplate liquid fully is immersed in the network hole of carbon aerogels that carbon aerogels is immersed in the plating metal solution, adopt ultrasonic wave can quicken the migration of electroplate liquid in carbon aerogels inside, it is in order to guarantee the homogeneity of plating bath in electroplating process that using magnetic force stirs.
The specific surface area of the metal carbon aerogel composite material that the present invention obtains is 700m
2/ g～1000m
2/ g, final sedimentary metal particle size is less than 80nm in its internal void.Adopt the preparation method of the present invention can be according to the size of carbon aerogels internal void, control the metal doping amount by control current density and electroplating time, and preparation method's reaction conditions of the present invention is gentle, be easy to control, uniform doping, doping is big, and reaction product stability at normal temperatures is high.Adopt the metal carbon aerogel composite material that has micropore of the present invention's preparation to can be used for gas adsorption material, super capacitor material, laser inertial confinement fusion target material, civilian hydrogen storage material and other nano material and technology association area.
Description of drawings
Fig. 1 is the sem photograph of the palladium carbon aerogel composite material section of employing the present invention preparation.
The palladium carbon aerogel composite material that Fig. 2 prepares for employing the present invention removes the X-ray diffractogram behind the outside surface coating.
The copper carbon aerogel composite material that Fig. 3 prepares for employing the present invention removes the X-ray diffractogram behind the outside surface coating.
Embodiment
Further specify the present invention below in conjunction with the drawings and specific embodiments.
The preparation of embodiment 1 palladium carbon aerogel composite material
At first prepare palladium electroplating liquid, electroplate liquid consists of: palladium 10g/L, ammonium chloride 15ml/L, 25% NH
4OH 35ml/L, regulate pH value to 9.2 with ammoniacal liquor, then will put into palladium electroplating liquid by Resorcinol-formaldehyde carbon aerogels that Resorcinol and formaldehyde make, ultrasonic 10min and flood 5 days after, do negative electrode with this carbon aerogels of handling, the palladium plate is done anode, characteristic according to the plating metal palladium on the pulse plating supply unit is provided with the corresponding techniques parameter, pulse-repetition is 500Hz, and dutycycle is 1: 4, and current density is 0.38A/dm
2, electroplating time is 5min, temperature is 25 ℃, connects power supply then, and carries out magnetic agitation simultaneously, the doping carbon aerogel after obtaining to electroplate.Then with this doping carbon aerogel washed with de-ionized water, be neutrality to washing lotion pH value after, put into the vacuum drying oven vacuum drying treatment, vacuum tightness is-0.1MPa that controlled temperature is 80 ℃ and is incubated 4h, makes the palladium carbon aerogel composite material.Palladium metal particle size in the palladium carbon aerogel composite material is less than 40nm, and the specific surface area of palladium carbon aerogel composite material is 880m
2/ g, doping is 2.3wt%, the sem photograph of palladium carbon aerogel composite material section removes X-ray diffractogram behind the outside surface coating shown in curve b among Fig. 2 as shown in Figure 1.
The preparation of embodiment 2 palladium carbon aerogel composite materials
According to the preparation process of embodiment 1 described palladium carbon aerogel composite material, different is that the electroplating time in the technical parameter is 10min.Palladium metal particle size in the palladium carbon aerogel composite material is 27nm, and the specific surface area of palladium carbon aerogel composite material is 850m
2/ g, doping is 5.0wt%, the palladium carbon aerogel composite material removes X-ray diffractogram behind the outside surface coating shown in curve c among Fig. 2.
The preparation of embodiment 3 palladium carbon aerogel composite materials
According to the preparation process of embodiment 1 described palladium carbon aerogel composite material, different is that the electroplating time in the technical parameter is 20min.Palladium metal particle size in the palladium carbon aerogel composite material is 39nm, and the specific surface area of palladium carbon aerogel composite material is 800m
2/ g, doping is 9.4wt%, the palladium carbon aerogel composite material removes X-ray diffractogram behind the outside surface coating shown in curve d among Fig. 2.
The preparation of embodiment 4 palladium carbon aerogel composite materials
According to the preparation process of embodiment 1 described palladium carbon aerogel composite material, different is that the electroplating time in the technical parameter is 30min.Palladium metal particle size in the palladium carbon aerogel composite material is 34nm, and the specific surface area of palladium carbon aerogel composite material is 720m
2/ g, doping is 16.8wt%, the palladium carbon aerogel composite material removes X-ray diffractogram behind the outside surface coating shown in curve e among Fig. 2.
The preparation of embodiment 5 palladium carbon aerogel composite materials
According to the preparation process of embodiment 1 described palladium carbon aerogel composite material, different is that the electroplating time in the technical parameter is 60min.Palladium metal particle size in the palladium carbon aerogel composite material is 27nm, and the specific surface area of palladium carbon aerogel composite material is 820m
2/ g, doping is 27.3wt%, the palladium carbon aerogel composite material removes X-ray diffractogram behind the outside surface coating shown in curve f among Fig. 2.
The preparation of embodiment 6 palladium carbon aerogel composite materials
According to the preparation process of embodiment 1 described palladium carbon aerogel composite material, different is that the electroplating time in the technical parameter is 90min.Palladium metal particle size 27nm in the palladium carbon aerogel composite material, the specific surface area of palladium carbon aerogel composite material is 920m
2/ g, doping is 31.0wt%.
The preparation of embodiment 7 palladium carbon aerogel composite materials
According to the preparation process of embodiment 1 described palladium carbon aerogel composite material, different is that electroplate liquid consists of: palladium 20g/L, ammonium chloride 20ml/L, 25% NH
4OH 40ml/L regulates pH value to 8.5 with ammoniacal liquor, and the current density in the technical parameter is 0.2A/dm
2, dutycycle is 1: 1, electroplating time is 10min.Palladium metal particle size in the palladium carbon aerogel composite material is 25nm, and the specific surface area of palladium carbon aerogel composite material is 830m
2/ g, doping is 3.0wt%.
The preparation of embodiment 8 palladium carbon aerogel composite materials
According to the preparation process of embodiment 1 described palladium carbon aerogel composite material, different is that electroplate liquid consists of: palladium 20g/L, ammonium chloride 20ml/L, 25% NH
4OH 40ml/L regulates pH value to 8.5 with ammoniacal liquor, and the current density in the technical parameter is 0.6A/dm
2, dutycycle is 1: 1, electroplating time is 10min.Palladium metal particle size in the palladium carbon aerogel composite material is 28nm, and the specific surface area of palladium carbon aerogel composite material is 880m
2/ g, doping is 9.0wt%.
The preparation of embodiment 9 bronze medal carbon aerogel composite materials
At first prepare copper electroplating liquid, copper electroplating liquid consists of: copper sulfate 150g/L, sulfuric acid 50g/L, then will put into copper electroplating liquid by Resorcinol-formaldehyde carbon aerogels that Resorcinol and formaldehyde make, ultrasonic 20min and flood 3 days after, do negative electrode with this carbon aerogels of handling, the platinum plate is done anode, characteristic according to plating metal copper on the pulse plating supply unit is provided with the corresponding techniques parameter, and pulse-repetition is 500Hz, and cathode current density is 1.0A/dm
2, dutycycle is 1: 1, and electroplating time is 10min, and temperature is 25 ℃, connects power supply then, and carries out magnetic agitation simultaneously, the doping carbon aerogel after obtaining to electroplate.Then with this doping carbon aerogel washed with de-ionized water, be neutrality to washing lotion pH value after, put into the vacuum drying oven vacuum drying treatment, vacuum tightness is-0.1MPa that controlled temperature is 80 ℃ and is incubated 4h, makes the copper carbon aerogel composite material.Metallic copper particle in the copper carbon aerogel composite material is of a size of 28nm, and the specific surface area of copper carbon aerogel composite material is 900m
2/ g, doping is 20.0wt%, X-ray diffractogram was as shown in Figure 3 after the copper carbon aerogel composite material removed outside surface coating.
The preparation of embodiment 10 bronze medal carbon aerogel composite materials
According to the preparation process of embodiment 9 described copper carbon aerogel composite materials, different is that copper electroplating liquid consists of: copper sulfate 250g/L, and sulfuric acid 80g/L, the cathode current density in the technical parameter is 3.0A/dm
2Metallic copper particle in the copper carbon aerogel composite material is of a size of 28nm, and the specific surface area of copper carbon aerogel composite material is 1000m
2/ g, doping is 30.0wt%.
The preparation of embodiment 11 iron carbon aerogel composite materials
At first prepare ferroelectric plating bath, ferroelectric plating bath consists of: ferrous sulfate 200g/L, ammonium sulfate 100g/L, pH value 4.0 then will be put into ferroelectric plating bath by Resorcinol-formaldehyde carbon aerogels that Resorcinol and formaldehyde make, ultrasonic 20min and flood 5 days after, do negative electrode with this carbon aerogels of handling, the platinum plate is done anode, and the characteristic according to plating metal copper on the pulse plating supply unit is provided with the corresponding techniques parameter, pulse-repetition is 500Hz, and cathode current density is 1.5A/dm
2, dutycycle is 1: 1, and electroplating time is 10min, and temperature is 20 ℃, connects power supply then, and carries out magnetic agitation simultaneously, the doping carbon aerogel after obtaining to electroplate.Then with this doping carbon aerogel washed with de-ionized water, be neutrality to washing lotion pH value after, put into the vacuum drying oven vacuum drying treatment, vacuum tightness is-0.1MPa that controlled temperature is 80 ℃ and is incubated 4h, makes the iron carbon aerogel composite material.Iron granule in the iron carbon aerogel composite material is of a size of 37nm, and the specific surface area of iron carbon aerogel composite material is 960m
2/ g, doping is 24.0wt%.
The preparation of embodiment 12 iron carbon aerogel composite materials
According to the preparation process of embodiment 11 described iron carbon aerogel composite materials, different is that ferroelectric plating bath consists of: ferrous sulfate 260g/L, ammonium sulfate 130g/L, pH value 5.5.Cathode current density in the technical parameter is 2.0A/dm
2, temperature is 30 ℃.Iron granule in the iron carbon aerogel composite material is of a size of 40nm, and the specific surface area of iron carbon aerogel composite material is 1000m
2/ g, doping is 28.0wt%.
The preparation of embodiment 13 silver medal carbon aerogel composite materials
At first prepare plating solution for silver-plating, plating solution for silver-plating consists of: Silver Nitrate 30g/L, imino-diacetic ammonium sulphonate 90g/L, ammonium sulfate 110g/L, ammonium citrate 2g/L, pH value 8.5, then will put into plating solution for silver-plating by Resorcinol-formaldehyde carbon aerogels that Resorcinol and formaldehyde make, ultrasonic 30min and flood 3 days after, do negative electrode with this carbon aerogels of handling, the platinum plate is done anode, and the characteristic according to plating metal copper on the pulse plating supply unit is provided with the corresponding techniques parameter, pulse-repetition is 500Hz, and cathode current density is 0.2A/dm
2, dutycycle is 1: 1, and electroplating time is 10min, and temperature is 15 ℃, connects power supply then, and carries out magnetic agitation simultaneously, the doping carbon aerogel after obtaining to electroplate.Then with this doping carbon aerogel washed with de-ionized water, be neutrality to washing lotion pH value after, put into the vacuum drying oven vacuum drying treatment, vacuum tightness is-0.1MPa that controlled temperature is 150 ℃ and is incubated 4h, makes silver-colored carbon aerogel composite material.Metallic silver particles in the silver carbon aerogel composite material is of a size of 37nm, the specific surface area 850m of silver-colored carbon aerogel composite material
2/ g, doping 10.0wt%.
The preparation of embodiment 14 silver medal carbon aerogel composite materials
According to the preparation process of embodiment 13 described silver-colored carbon aerogel composite materials, different is that plating solution for silver-plating consists of: Silver Nitrate 40g/L, imino-diacetic ammonium sulphonate 120g/L, ammonium sulfate 140g/L, ammonium citrate 6g/L, pH value 9.0.Cathode current density in the technical parameter is 0.4A/dm
2, temperature is 30 ℃.Metallic silver particles in the silver carbon aerogel composite material is of a size of 40nm, the specific surface area 900m of silver-colored carbon aerogel composite material
2/ g, doping 15.0wt%.
Claims (8)
1. the preparation method of a metal carbon aerogel composite material in turn includes the following steps:
(a) electroplate liquid of preparation electroplate liquid preparation plating metal;
(b) under the preparation of carbon aerogels and the pre-treatment room temperature, will be synthetic by sol-gel, the carbon aerogels made of aging, the supercritical drying of exchange of solvent, pickling and high temperature cabonization process puts into the electroplate liquid of the plating metal that step a prepares, behind supersound process 10～30min, flooded again 3～5 days;
(c) as negative electrode, the platinum plate is made anode to electroplating process with the impregnated plating piece carbon aerogels of step b, and negative electrode and anode are hung in the coating bath that holds plating metal electroplate liquid among the step a together, then coating bath is put into heat collecting type thermostatically heating magnetic stirring apparatus; Characteristic according to plating metal on the pulse plating supply unit is provided with the corresponding techniques parameter, connects power supply then, electroplates under magnetic agitation, produces adulterated carbon aerogels;
(d) clean the doping carbon aerogel washed with de-ionized water for preparing among the step c, be neutral up to washing lotion pH value;
(e) dry the doping carbon aerogel that cleaned in the steps d is put into the vacuum drying oven vacuum drying treatment, vacuum tightness is-0.1MPa, and temperature is controlled at 80～150 ℃ and be incubated 4h, obtains metal carbon aerogel composite material.
2. the preparation method of a kind of metal carbon aerogel composite material according to claim 1 is characterized in that, the plating metal among the described step a is palladium, copper, iron and silver.
3. the preparation method of a kind of metal carbon aerogel composite material according to claim 2 is characterized in that, when described plating metal is palladium, and the consisting of of electroplate liquid:
Palladium 10～20g/L
Ammonium chloride 15～20ml/L
NH4OH(25％) 35～40ml/L
Regulate pH value 8.5～9.2 with ammoniacal liquor
According to the characteristic of plating metal palladium the corresponding techniques parameter being set on the pulse plating supply unit is:
Pulse-repetition 500Hz
Cathode current density 0.2～0.6A/dm2
Dutycycle 1: 4～1: 1
25 ℃ of temperature
4. the preparation method of a kind of metal carbon aerogel composite material according to claim 2 is characterized in that, when described plating metal is copper, and the consisting of of electroplate liquid:
Copper sulfate 150～250g/L
Sulfuric acid 50～80g/L
According to the characteristic of plating metal copper the corresponding techniques parameter being set on the pulse plating supply unit is:
Pulse-repetition 500Hz
Cathode current density 1～3A/dm2
Dutycycle 1: 1
20～40 ℃ of temperature
5. the preparation method of a kind of metal carbon aerogel composite material according to claim 2 is characterized in that, when described plating metal is iron, and the consisting of of electroplate liquid:
Ferrous sulfate 200～260g/L
Ammonium sulfate 100～130g/L
PH value 4.0～5.5
According to the characteristic of plating metal iron the corresponding techniques parameter being set on the pulse plating supply unit is:
Pulse-repetition 500Hz
Cathode current density 1.5～2.0A/dm2
Dutycycle 1: 1
20～30 ℃ of temperature
6. the preparation method of a kind of metal carbon aerogel composite material according to claim 2 is characterized in that, described plating metal is when silver, the consisting of of electroplate liquid:
Silver Nitrate 30～40g/L
Imino-diacetic ammonium sulphonate 90～120g/L
Ammonium sulfate 110～140g/L
Ammonium citrate 2～6g/L
PH value 8.5～9.0
According to the characteristic of plating metal silver the corresponding techniques parameter being set on the pulse plating supply unit is:
Pulse-repetition 500Hz
Current density 0.2～0.4A/dm2
Dutycycle 1: 1
15～30 ℃ of temperature
7. the preparation method of a kind of metal carbon aerogel composite material according to claim 1, it is characterized in that the carbon aerogels among the described step b is a kind of in resorcinol formaldehyde carbon aerogels, phenol formaldehyde (PF) carbon aerogels, Resorcinol formaldehyde carbon aerogels or the Phloroglucinol formaldehyde carbon aerogels.
8. the preparation method of a kind of metal carbon aerogel composite material according to claim 1 is characterized in that, the anode among the described step c adopts palladium plate, graphite or carbon aerogels to substitute.
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| CN107761124A (en) * | 2017-10-23 | 2018-03-06 | 大连理工大学 | A kind of preparation method and application for carrying silver-colored carbon aerogels |
| CN107761124B (en) * | 2017-10-23 | 2019-06-07 | 大连理工大学 | A kind of preparation method and application carrying silver-colored carbon aerogels |
| CN111101172A (en) * | 2019-12-31 | 2020-05-05 | 新疆烯金石墨烯科技有限公司 | Graphene-aluminum composite material and preparation method thereof |
| CN111101172B (en) * | 2019-12-31 | 2021-02-09 | 新疆烯金石墨烯科技有限公司 | Graphene-aluminum composite material and preparation method thereof |
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| CN112264628B (en) * | 2020-10-28 | 2022-03-25 | 中国工程物理研究院激光聚变研究中心 | Preparation method of gold aerogel |
| CN114774981A (en) * | 2022-05-18 | 2022-07-22 | 浙江工业大学 | Preparation method and application of ruthenium-based boron-doped carbon aerogel deuterium evolution catalyst |
| CN114774981B (en) * | 2022-05-18 | 2023-12-12 | 浙江工业大学 | Preparation method and application of ruthenium-based boron-doped carbon aerogel deuterium-precipitating catalyst |
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