CN102903537A - Preparation method of multi-walled carbon nanotube loaded high-density high-dispersion nano platinum counter electrode - Google Patents
Preparation method of multi-walled carbon nanotube loaded high-density high-dispersion nano platinum counter electrode Download PDFInfo
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Abstract
The invention discloses a preparation method of a multi-walled carbon nanotube loaded high-density high-dispersion nano platinum counter electrode. The method comprises the main steps of: preprocessing a multi-walled carbon nanotube through mixed acid, dispersing into chloroplatinic acid-ethylene glycol solution with a certain concentration, and adding appropriate polyvinylpyrrolidone; carrying out ultrasonic agitation and hydro-thermal treatment to obtain a complex of a multi-walled carbon nanotube loaded platinum; after being subjected to multiple washing, centrifugal separation and drying, uniformly mixing the complex with a certain amount of terpineol, ethyl cellulose, triton and the like to obtain complex slurry; and coating the slurry onto a conductive glass substrate through a coating method, and obtaining the counter electrode through sintering at high temperature. The counter electrode material prepared by the method has the advantages that the specific surface area is large, the catalytic activity is high, the operation is simple, the preparation cost is low, and the like.
Description
Technical field
The invention belongs to the new energy materials technical field, particularly a kind of DSSC based on multiple-wall carbon nanotube loaded with nano platinum is to the preparation method of electrode.
Background technology
Dye-sensitized solar cells (DSSC) is a kind of third generation thin-film solar cells of the nano photoelectric functional materials such as electrode being got up as base growth take nano crystal semiconductor, organic photosensitive dyestuff, electrolyte and high catalytic activity.Wherein, be one of important component part of DSSC to electrode, its Main Function has: collect and transmission electronic (1), the oxidized electrolyte of (2) catalytic reduction.Traditional mainly is the platinum plating conductive glass electrode to electrode, and wherein platinum has good conductivity and efficient catalytic activity.But platinum belongs to noble metal, and preparation and use cost are higher, are unfavorable for that this kind is to the large-scale application of electrode.In recent years, CNT (carbon nano-tube) has a wide range of applications at aspects such as opto-electronic conversion, photocatalysis and electrochemical sensings with its good conductivity, higher catalytic activity and the larger premium properties such as specific area.Use separately CNT (carbon nano-tube) as to electrode material the time in DSSC, its catalytic activity is far below platinum, thereby greatly reduces the photoelectric conversion efficiency of DSSC.Adopt the nano-carbon tube load metal platinum to substitute when using platinum or CNT (carbon nano-tube) separately, can either effectively reduce the platinum use amount, can strengthen again the electro catalytic activity of CNT (carbon nano-tube).At present, mainly prepare nano-carbon tube load platinum combined counter electrode by methods such as electrophoresis, rotary coatings at electro-conductive glass.Yet, these class methods can not be controlled platinum effectively in load capacity, dispersiveness and the granular size on CNT (carbon nano-tube) surface, and these class methods itself are difficult to realize large-scale production, to such an extent as to affected the electro catalytic activity of combined counter electrode in DSSC, thereby can not effectively improve the photoelectric conversion efficiency of DSSC.
Summary of the invention
Technical problem: the purpose of this invention is to provide a kind of DSSC of preparation to the method for electrode, it is low-cost, high efficiency to electrode to be conducive to controlled preparation.The method is take chloroplatinic acid and multiple-wall carbon nanotube as primary raw material, and by the proportioning of control chloroplatinic acid and multiple-wall carbon nanotube, and level of inhibitor and hydrothermal reaction condition are realized controlled preparation.At first prepare multiple-wall carbon nanotube Supported Pt Nanoparticles compound, again by knife coating with composite coated in the electro-conductive glass substrate, prepare multiple-wall carbon nanotube load high density, high dispersancy nano platinum combined counter electrode through high-temperature process.
Technical scheme: preparation method's method of multiple-wall carbon nanotube load high density of the present invention, high dispersancy nano platinum combined counter electrode realizes by following approach:
The first step, the preliminary treatment of multiple-wall carbon nanotube: multiple-wall carbon nanotube is mixed in the ratio of 1-2mg/mL with nitration mixture, behind the ultrasonic processing 4-6h, centrifugation, repeatedly be washed to neutrality, at 70-80 ℃ of lower vacuumize 10-12h, obtain acid-treated multiple-wall carbon nanotube after the grinding;
Second step, multiple-wall carbon nanotube loaded with nano platinum composite manufacture: take ethylene glycol as solvent, above-mentioned ethylene glycol solution and the ethylene glycol that obtains acid-treated multiple-wall carbon nanotube, polymerization inhibitor, 0.01mol/L chloroplatinic acid is mixed; Wherein the mixed proportion of multiple-wall carbon nanotube is 0.25-1.25mg/ml, and the mixed proportion of polymerization inhibitor is 0.025-0.05mg/ml, and the mixed proportion of chloroplatinic acid is 0.25-0.5ml/ml; Transfer in the hydrothermal reaction kettle 120-160 ℃ of lower reaction 4-8h after ultrasonic agitation is even; React complete rear gained solution centrifugal and separate, washed several times with water is to neutral, and 70-80 ℃ of lower vacuumize 10-12h grinds, and namely gets multiple-wall carbon nanotube loaded with nano platinum composite material, and be for subsequent use;
The 3rd step is to the preparation of electrode: take terpinol as dispersant, with the above-mentioned composite material that makes, Yi base Xian Wei Su ﹑ song draws logical and terpinol mixes; Wherein the mixed proportion of composite material is 25-50mg/ml, and the mixed proportion of ethyl cellulose is 5-10mg/ml, and the mixed proportion of Qu Latong is 0.005-0.01ml/ml; Ultrasonic agitation makes the homogeneous slurry, and knife coating is coated to cleaned dried conductive substrates surface, and 300-450 ℃ of lower calcining 1-2h is cooled to room temperature, obtain preparing to electrode.
Described polymerization inhibitor is PVP K30, and the mass ratio of itself and multiple-wall carbon nanotube is 1/50~1/5.The mass ratio of described ethyl cellulose and multiple-wall carbon nanotube loaded with nano platinum composite material is 1/10~2/5.Described nitration mixture is the mixed acid that the concentrated sulfuric acid and red fuming nitric acid (RFNA) form, and the volume ratio of the concentrated sulfuric acid and red fuming nitric acid (RFNA) is 1/3~3/1.
Beneficial effect: the present invention at the nano-platinum particle through nitration mixture pretreated multiple-wall carbon nanotube area load high density, polymolecularity, and prepares DSSC to electrode with this compound by hydro thermal method.What the method was prepared not only can reduce the consumption of noble metal platinum to electrode, utilize strong conduction and the auxiliary catalysis ability of multiple-wall carbon nanotube, and can effectively by the control hydrothermal reaction condition, regulate and control Platinum Nanoparticles in multiple-wall carbon nanotube surface coverage, decentralization and particle size.Thereby realize scale prepare high efficiency, cheaply to electrode.
Description of drawings
Fig. 1 is the transmission electron microscope picture of multiple-wall carbon nanotube loaded with nano platinum complexes.
Embodiment
The first step, the preliminary treatment of multiple-wall carbon nanotube: multiple-wall carbon nanotube is mixed in the ratio of 1-2mg/mL with nitration mixture, behind the ultrasonic dispersion 4-6h, centrifugation, through repeatedly being washed to neutrality, at 70-80 ℃ of lower vacuumize 10-12h, grind into powder, for subsequent use;
Second step, the preparation of multiple-wall carbon nanotube Supported Pt Nanoparticles compound: chloroplatinic acid aqueous solution and the 1-2mg polymerization inhibitor of getting the pretreated Duo wall Na of 0.05g rice Tan Guan ﹑ 10-20mL0.01mol/L join in the 40ml ethylene glycol, ultrasonic dispersion, transfer in the hydrothermal reaction kettle after stirring; At 120-160 ℃ of lower reaction 4-8h; It is extremely neutral through centrifugation and washed several times with water to react complete rear gained solution; At 70-80 ℃ of lower vacuumize 10-12h, grind into powder namely gets compound;
The 3rd step, to the preparation of electrode: after getting the above-mentioned compound of 0.05g and 0.01-0.02g Yi base Xian Wei Su ﹑ 2-3ml terpinol and 0.01-0.02ml song and drawing logical the mixing, through ultrasonic, stir and obtain finely dispersed slurry; Be coated to clean conductive substrates surface by knife coating, through 300-450 ℃ of lower calcining 1-2h, be cooled to room temperature, obtain compound to electrode.
The pipe range 5-15 μ m that described multiple-wall carbon nanotube is, aperture 10-30nm.
Described nitration mixture is that volume ratio is about the concentrated sulfuric acid of 3:1 and the nitration mixture of red fuming nitric acid (RFNA).
Described polymerization inhibitor is PVP K30.
Described reactor is corrosion-resistant reactor, and reaction is carried out in thermostatic drying chamber.
Describedly lead the substrate of electro-conductive glass electricity for mixing the fluorine electro-conductive glass, the face resistance is 8-15 Ω/cm
2
The present invention is described in further detail below in conjunction with embodiment, but the working of an invention mode is not limited to this.
Embodiment 1:
Get the nitration mixture (volume ratio of sulfuric acid and nitric acid is 3:1) that the 0.15g multiple-wall carbon nanotube joins 100mL sulfuric acid and nitric acid, behind the ultrasonic processing 4h, centrifugation repeatedly is washed to neutrality, and 80 ℃ of lower vacuumize 10h grind, and are for subsequent use;
The platinum acid chloride solution of getting the Duo wall Na rice Tan Guan ﹑ 10mL0.01mol/L after the 0.05g nitration mixture is processed joins in the 40ml ethylene glycol, transfers in the hydrothermal reaction kettle 120 ℃ of lower reaction 6h after ultrasonic agitation is even; React complete rear gained solution centrifugal and separate, washed several times with water is to neutral, and 80 ℃ of lower vacuumize 10h grind, and namely get multiple-wall carbon nanotube loaded with nano platinum composite material, and are for subsequent use;
Get the above-mentioned composite material that makes of 0.05g and 0.01g Yi base Xian Wei Su ﹑ 2ml terpinol and 0.01ml song and draw logical the mixing, ultrasonic agitation makes the homogeneous slurry, and knife coating is coated to cleaned dried conductive substrates surface, 300 ℃ of lower calcining 1h, be cooled to room temperature, obtain preparing to electrode.
The load capacity of platinum is the 20.3%(mass ratio in the combined counter electrode that the method makes), the particle average grain diameter is 7.6nm, is assembled into battery and has obtained 2.8% electricity conversion.
Embodiment 2:
Get the nitration mixture (volume ratio of sulfuric acid and nitric acid is 3:1) that the 0.15g multiple-wall carbon nanotube joins 100mL sulfuric acid and nitric acid, behind the ultrasonic processing 4h, centrifugation repeatedly is washed to neutrality, and 80 ℃ of lower vacuumize 10h grind, and are for subsequent use;
The platinum acid chloride solution of Duo wall Na rice Tan Guan ﹑ 20mL0.01mol/L after getting the 0.05g nitration mixture and processing and joining in the 40ml ethylene glycol, ultrasonic agitation are transferred in the hydrothermal reaction kettle 120 ℃ of lower reaction 6h after evenly; React complete rear gained solution centrifugal and separate, washed several times with water is to neutral, and 80 ℃ of lower vacuumize 10h grind, and namely get multiple-wall carbon nanotube loaded with nano platinum composite material, and are for subsequent use;
Get the above-mentioned composite material that makes of 0.05g and 0.01g Yi base Xian Wei Su ﹑ 2ml terpinol and 0.01ml song and draw logical the mixing, ultrasonic agitation makes the homogeneous slurry, and knife coating is coated to cleaned dried conductive substrates surface, 300 ℃ of lower calcining 1h, be cooled to room temperature, obtain preparing to electrode.
The load capacity of platinum is the 36.1%(mass ratio in the combined counter electrode that the method makes), the particle average grain diameter is 6.2nm, is assembled into battery and has obtained 4.3% electricity conversion.
Embodiment 3:
Get the nitration mixture (volume ratio of sulfuric acid and nitric acid is 3:1) that the 0.15g multiple-wall carbon nanotube joins 100mL sulfuric acid and nitric acid, behind the ultrasonic processing 4h, centrifugation repeatedly is washed to neutrality, and 80 ℃ of lower vacuumize 10h grind, and are for subsequent use;
Platinum acid chloride solution and the 0.0015g polyvinylpyrrolidone of getting the Duo wall Na rice Tan Guan ﹑ 20mL0.01mol/L after the 0.05g nitration mixture is processed join in the 40ml ethylene glycol, transfer in the hydrothermal reaction kettle 120 ℃ of lower reaction 6h after ultrasonic agitation is even; React complete rear gained solution centrifugal and separate, washed several times with water is to neutral, and 80 ℃ of lower vacuumize 10h grind, and namely get multiple-wall carbon nanotube loaded with nano platinum composite material, and are for subsequent use;
Get the above-mentioned composite material that makes of 0.05g and 0.01g Yi base Xian Wei Su ﹑ 2ml terpinol and 0.01ml song and draw logical the mixing, ultrasonic agitation makes the homogeneous slurry, and knife coating is coated to cleaned dried conductive substrates surface, 300 ℃ of lower calcining 1h, be cooled to room temperature, obtain preparing to electrode.
The load capacity of platinum is the 38.7%(mass ratio in the combined counter electrode that the method makes), the particle average grain diameter is 4.9nm, is assembled into battery and has obtained 5.5% electricity conversion.
Embodiment 4:
Get the nitration mixture (volume ratio of sulfuric acid and nitric acid is 3:1) that the 0.15g multiple-wall carbon nanotube joins 100mL sulfuric acid and nitric acid, behind the ultrasonic processing 4h, centrifugation repeatedly is washed to neutrality, and 80 ℃ of lower vacuumize 10h grind, and are for subsequent use;
Platinum acid chloride solution and the 0.0015g polyvinylpyrrolidone of getting the Duo wall Na rice Tan Guan ﹑ 20mL0.01mol/L after the 0.05g nitration mixture is processed join in the 40ml ethylene glycol, transfer in the hydrothermal reaction kettle 160 ℃ of lower reaction 6h after ultrasonic agitation is even; React complete rear gained solution centrifugal and separate, washed several times with water is to neutral, and 80 ℃ of lower vacuumize 10h grind, and namely get multiple-wall carbon nanotube loaded with nano platinum composite material, and are for subsequent use;
Get the above-mentioned composite material that makes of 0.05g and 0.02g Yi base Xian Wei Su ﹑ 2ml terpinol and 0.01ml song and draw logical the mixing, ultrasonic agitation makes the homogeneous slurry, and knife coating is coated to cleaned dried conductive substrates surface, 300 ℃ of lower calcining 1h, be cooled to room temperature, obtain preparing to electrode.
The load capacity of platinum is the 44.6%(mass ratio in the combined counter electrode that the method makes), the particle average grain diameter is that 3.5nm(sees accompanying drawing), be assembled into battery and obtained 6.4% electricity conversion.
Embodiment 5:
Get the nitration mixture (volume ratio of sulfuric acid and nitric acid is 3:1) that the 0.15g multiple-wall carbon nanotube joins 100mL sulfuric acid and nitric acid, behind the ultrasonic processing 4h, centrifugation repeatedly is washed to neutrality, and 80 ℃ of lower vacuumize 10h grind, and are for subsequent use;
Platinum acid chloride solution and the 0.0015g polyvinylpyrrolidone of getting the Duo wall Na rice Tan Guan ﹑ 20mL0.01mol/L after the 0.05g nitration mixture is processed join in the 40ml ethylene glycol, transfer in the hydrothermal reaction kettle 160 ℃ of lower reaction 6h after ultrasonic agitation is even; React complete rear gained solution centrifugal and separate, washed several times with water is to neutral, and 80 ℃ of lower vacuumize 10h grind, and namely get multiple-wall carbon nanotube loaded with nano platinum composite material, and are for subsequent use;
Get the above-mentioned composite material that makes of 0.05g and 0.02g Yi base Xian Wei Su ﹑ 3ml terpinol and 0.02ml song and draw logical the mixing, ultrasonic agitation makes the homogeneous slurry, and knife coating is coated to cleaned dried conductive substrates surface, 450 ℃ of lower calcining 1h, be cooled to room temperature, obtain preparing to electrode.
The load capacity of platinum is the 44.6%(mass ratio in the combined counter electrode that the method makes), the particle average grain diameter is 12.8nm, is assembled into battery and has obtained 4.6% electricity conversion.
Claims (4)
1. a multiple-wall carbon nanotube load high density high dispersancy nano platinum is characterized in that to the preparation method of electrode the method realizes by following approach:
The first step, the preliminary treatment of multiple-wall carbon nanotube: multiple-wall carbon nanotube is mixed in the ratio of 1-2mg/mL with nitration mixture, behind the ultrasonic processing 4-6h, centrifugation, repeatedly be washed to neutrality, at 70-80 ℃ of lower vacuumize 10-12h, obtain acid-treated multiple-wall carbon nanotube after the grinding;
Second step, multiple-wall carbon nanotube loaded with nano platinum composite manufacture: take ethylene glycol as solvent, above-mentioned ethylene glycol solution and the ethylene glycol that obtains acid-treated multiple-wall carbon nanotube, polymerization inhibitor, 0.01mol/L chloroplatinic acid is mixed; Wherein the mixed proportion of multiple-wall carbon nanotube is 0.25-1.25mg/ml, and the mixed proportion of polymerization inhibitor is 0.025-0.05mg/ml, and the mixed proportion of chloroplatinic acid is 0.25-0.5ml/ml; Transfer in the hydrothermal reaction kettle 120-160 ℃ of lower reaction 4-8h after ultrasonic agitation is even; React complete rear gained solution centrifugal and separate, washed several times with water is to neutral, and 70-80 ℃ of lower vacuumize 10-12h grinds, and namely gets multiple-wall carbon nanotube loaded with nano platinum composite material, and be for subsequent use;
The 3rd step is to the preparation of electrode: take terpinol as dispersant, with the above-mentioned composite material that makes, Yi base Xian Wei Su ﹑ song draws logical and terpinol mixes; Wherein the mixed proportion of composite material is 25-50mg/ml, and the mixed proportion of ethyl cellulose is 5-10mg/ml, and the mixed proportion of Qu Latong is 0.005-0.01ml/ml; Ultrasonic agitation makes the homogeneous slurry, and knife coating is coated to cleaned dried conductive substrates surface, and 300-450 ℃ of lower calcining 1-2h is cooled to room temperature, obtain preparing to electrode.
2. multiple-wall carbon nanotube load high density high dispersancy nano platinum according to claim 1 is characterized in that to the preparation method of electrode described polymerization inhibitor is PVP K30, and the mass ratio of itself and multiple-wall carbon nanotube is 1/50~1/5.
3. multiple-wall carbon nanotube load high density high dispersancy nano platinum according to claim 1 is characterized in that to the preparation method of electrode the mass ratio of described ethyl cellulose and multiple-wall carbon nanotube loaded with nano platinum composite material is 1/10~2/5.
4. multiple-wall carbon nanotube load high density high dispersancy nano platinum according to claim 1 is characterized in that to the preparation method of electrode described nitration mixture is the mixed acid that the concentrated sulfuric acid and red fuming nitric acid (RFNA) form, and the volume ratio of the concentrated sulfuric acid and red fuming nitric acid (RFNA) is 1/3~3/1.
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