CN113421716B - Method for regulating and controlling growth mechanism of platinum nanowires in carrier mesoporous controllable growth mechanism - Google Patents
Method for regulating and controlling growth mechanism of platinum nanowires in carrier mesoporous controllable growth mechanism Download PDFInfo
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Abstract
The invention discloses a method for regulating and controlling a mesoporous controllable growth mechanism of a platinum nanowire in a carrier, which comprises the following steps: taking materials; step two, distilling; step three, dispersing; step four, mixing; step five, stirring; step six, growing; step seven, drying; according to the invention, the concentration of ethylene glycol in the growth base liquid is regulated, the temperature in the high-pressure reaction kettle is regulated, the growth of a dominant crystal face of the platinum nanowire is ensured, the regulation mode is simple, the working reliability of the platinum nanowire growing on the mesoporous metal oxide @ titanium nitride after regulation is improved, impurities in N, N-dimethylformamide are removed through a distillation step, the influence of the impurities on the growth mechanism of the platinum nanowire during growth is reduced, the regulation precision is improved, the uniform distribution of the metal oxide @ titanium nitride carrier is ensured through ultrasonic dispersion, and the conductivity of the platinum nanowire growing on the mesoporous metal oxide @ titanium nitride after regulation is further improved.
Description
Technical Field
The invention relates to the technical field of platinum nanowires, in particular to a method for regulating and controlling a mesoporous controllable growth mechanism of a platinum nanowire in a carrier.
Background
The platinum nanowire has special physicochemical properties, has wide prospects in the application of fields such as biomedicine, sensors, conductive materials and chemical catalysts, and the like, and the crystal surface structure of the platinum nanowire growing in the mesoporous of the carrier and the structural characteristics of the nanowire determine the electrocatalytic activity and stability of the mesoporous metal oxide @ titanium nitride loading the platinum nanowire, but the original method for preparing the platinum nanowire by hydrothermal reaction regulation still has the following problems that firstly, in the original process for preparing the platinum nanowire by regulation, the growth state of the platinum nanowire cannot be accurately regulated, so that the special physicochemical properties of the prepared platinum nanowire are influenced, and further the working reliability of the platinum nanowire growing on the mesoporous metal oxide @ titanium nitride is influenced; secondly, impurities in the growth base liquid are not removed firstly in the original regulation and control process, the original growth mechanism of the platinum nanowires is influenced in the regulation and control process, and therefore the regulation and control accuracy is reduced; thirdly, in the original regulation and control process, the metal oxide @ titanium nitride carrier is not fully mixed in the growth base liquid, so that the electric conductivity of the platinum nanowire growing on the mesoporous metal oxide @ titanium nitride after the regulation and control preparation is influenced.
Disclosure of Invention
The invention aims to provide a method for regulating and controlling a controllable growth mechanism of a platinum nanowire in a carrier mesoporous, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a method for regulating and controlling a controllable growth mechanism of a platinum nanowire in a carrier mesopore comprises the following steps: taking materials; step two, distillation; step three, dispersing; step four, mixing; step five, stirring; step six, growing; step seven, drying;
in the first step, 290-310 parts of N, N-dimethylformamide, 8-12 parts of ethylene glycol, 8-10 parts of metal oxide @ titanium nitride carrier, 4-6 parts of sodium hydroxide, 7-9 parts of anhydrous copper sulfate and 8-12 parts of chloroplatinic acid are respectively weighed according to the parts by weight of the components and are respectively placed for later use;
in the second step, the N, N-dimethylformamide prepared in the first step is put into a container, then the prepared anhydrous copper sulfate is added, the mixture is placed still and poured into a distillation flask, and the pure N, N-dimethylformamide is obtained after low-pressure distillation;
in the third step, the pure N, N-dimethylformamide obtained in the second step is poured into an ultrasonic dispersion machine, the metal oxide @ titanium nitride carrier prepared in the first step and ethylene glycol are added, and the metal oxide @ titanium nitride carrier and the ethylene glycol are uniformly dispersed in the pure N, N-dimethylformamide by utilizing ultrasonic oscillation to obtain a growth base solution;
in the fourth step, the growth base solution obtained in the third step is poured into a magnetic stirrer, the sodium hydroxide and the chloroplatinic acid prepared in the first step are added while stirring at a low speed, and the mixture is sealed and kept stand after stirring to obtain a primary mixed solution;
pouring the preliminary mixed liquid obtained in the fourth step into a magnetic stirrer for high-speed stirring, and fully stirring to obtain a complete mixed liquid;
in the sixth step, the completely mixed solution obtained in the fifth step is put into a polytetrafluoroethylene-lined high-pressure reaction kettle and heated at high temperature to obtain a mixture loaded with platinum nanowires;
and in the seventh step, the mixture loaded by the platinum nanowires obtained in the sixth step is poured into a container to be sealed and placed still, the mixture is repeatedly washed by ethanol after being filtered, and the mixture is dried in an oven after being washed, so that the platinum nanowires growing on the mesoporous metal oxide @ titanium nitride are obtained.
Preferably, in the second step, the standing temperature is 25-30 ℃, the standing time is 0.2-0.3 h, the pressure of low-pressure distillation is 2.2-2.7 KPa, the distillation temperature is 120-140 ℃, and the distillation time is 0.5-0.8 h.
Preferably, in the third step, the working frequency of the ultrasonic dispersion machine is 5 to 13kHz, and the dispersion time is 3.5 to 4.5 hours.
Preferably, in the fourth step, the stirring speed of the magnetic stirrer is 30-60 r/min, the stirring time is 1.5-2.5 h, the temperature of sealing and standing is 25-30 ℃, and the standing time is 0.2-0.3 h.
Preferably, in the fifth step, the stirring speed of the magnetic stirrer is 250-330 r/min, and the stirring time is 23-25 h.
Preferably, in the sixth step, the pressure of the polytetrafluoroethylene-lined high-pressure reaction kettle is 2500-3500 KPa, the temperature is 150-190 ℃, and the reaction time is 6-12 h.
Preferably, in the seventh step, the sealing and standing temperature is 25-30 ℃, the standing time is 0.8-1.2 h, the filter is washed by ethanol every 0.5h, the operation is repeated for four times, the filter is placed in an oven at the temperature of 45-50 ℃, and the baking time is 1.5-2 h.
Compared with the prior art, the invention has the beneficial effects that: according to the method for regulating the controllable growth mechanism of the platinum nanowires in the carrier mesopores, the growth base liquid is regulated in advance before preparation, the concentration of a reducing agent in the growth base liquid is regulated, so that the aim of regulating the growth of the platinum nanowires is fulfilled, the growth of the platinum nanowires is further regulated by regulating and controlling the temperature in a polytetrafluoroethylene-lined high-pressure reaction kettle, so that the platinum nanowires grow to have dominant crystal faces, the regulation and the control are simple, and the working reliability of the platinum nanowires growing on the mesoporous metal oxide @ titanium nitride after the regulation and the preparation is guaranteed; the N, N-dimethylformamide is distilled before regulation, so that impurities in the growth base liquid are removed, the influence of the impurities on the regulation is eliminated, and the regulation accuracy is improved; by ultrasonic dispersion treatment, the uniform distribution of the metal oxide @ titanium nitride carrier in the growth base solution is ensured, the chloroplatinic acid is in full contact with the metal oxide @ titanium nitride carrier in the process of regulating and controlling the platinum nanowire, and the conductivity of the platinum nanowire growing on the mesoporous metal oxide @ titanium nitride after regulation and control is improved.
Drawings
FIG. 1 is a flow chart of the method of the present invention.
Detailed Description
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 only a part of the embodiments of the present invention, and not all of the embodiments. 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.
Referring to fig. 1, a technical solution provided by the present invention:
example 1:
a method for regulating and controlling a controllable growth mechanism of a platinum nanowire in a carrier mesopore comprises the following steps: taking materials; step two, distilling; step three, dispersing; step four, mixing; step five, stirring; step six, growing; step seven, drying;
in the first step, 300 parts of N, N-dimethylformamide, 8 parts of ethylene glycol, 9 parts of metal oxide @ titanium nitride carrier, 5 parts of sodium hydroxide, 8 parts of anhydrous copper sulfate and 10 parts of chloroplatinic acid are respectively weighed according to the parts by weight of the components and are respectively placed for later use;
in the second step, the N, N-dimethylformamide prepared in the first step is placed into a container, then the prepared anhydrous copper sulfate is added, the mixture is kept stand for 0.2 hour at the temperature of 25 ℃, the mixture is poured into a distillation flask after the mixture is kept stand, the pressure is adjusted to be 2.5KPa, the temperature is 135 ℃, the mixture is distilled for 0.6 hour, and pure N, N-dimethylformamide is obtained after low-pressure distillation;
in the third step, the pure N, N-dimethylformamide obtained in the second step is poured into an ultrasonic dispersion machine, and the metal oxide @ titanium nitride carrier prepared in the first step and ethylene glycol are added, wherein the working frequency of the ultrasonic dispersion machine is 8kHz, and the dispersion time is 4 hours, so that a growth base solution is obtained;
in the fourth step, the growth base solution obtained in the third step is poured into a magnetic stirrer, the sodium hydroxide and the chloroplatinic acid prepared in the first step are added while stirring at a low speed, the stirring speed of the magnetic stirrer is 50r/min, the stirring time is 2 hours, the mixture is sealed and kept stand for 0.3 hour after stirring, the temperature of the sealed and kept stand is 28 ℃, and a primary mixed solution is obtained after the mixture is kept stand;
pouring the preliminary mixed liquid obtained in the fourth step into a magnetic stirrer for high-speed stirring, wherein the stirring speed of the magnetic stirrer is 275r/min, the stirring time is 24 hours, and fully stirring to obtain complete mixed liquid;
in the sixth step, the completely mixed solution obtained in the fifth step is put into a polytetrafluoroethylene-lined high-pressure reaction kettle, the pressure of the high-pressure reaction kettle is 3000KPa, the temperature is 150 ℃, the reaction time is 7 hours, and the mixture loaded with the platinum nanowires is obtained after continuous heating at high temperature;
and seventhly, pouring the mixture loaded with the platinum nanowires obtained in the sixth step into a container, sealing and standing for 1h at the sealing and standing temperature of 27 ℃, standing and filtering, washing with ethanol every 0.5h after filtering, repeating the operation for four times, washing, baking in an oven for 2h at the baking temperature of 50 ℃, and baking to obtain the platinum nanowires growing on the mesoporous metal oxide @ titanium nitride.
Example 2:
a method for regulating and controlling a controllable growth mechanism of a platinum nanowire in a carrier mesopore comprises the following steps: taking materials; step two, distillation; step three, dispersing; step four, mixing; step five, stirring; step six, growing; step seven, drying;
in the first step, 300 parts of N, N-dimethylformamide, 12 parts of ethylene glycol, 9 parts of metal oxide @ titanium nitride carrier, 6 parts of sodium hydroxide, 7 parts of anhydrous copper sulfate and 12 parts of chloroplatinic acid are respectively weighed according to the parts by weight of the components and are respectively placed for later use;
in the second step, the N, N-dimethylformamide prepared in the first step is placed into a container, then the prepared anhydrous copper sulfate is added, the mixture is kept stand for 0.2h at the temperature of 28 ℃, the mixture is poured into a distillation flask after the mixture is kept stand, the pressure is adjusted to be 2.5KPa, the temperature is 130 ℃, the mixture is distilled for 0.6h, and pure N, N-dimethylformamide is obtained after low-pressure distillation;
in the third step, the pure N, N-dimethylformamide obtained in the second step is poured into an ultrasonic dispersion machine, and the metal oxide @ titanium nitride carrier prepared in the first step and ethylene glycol are added, wherein the working frequency of the ultrasonic dispersion machine is 10kHz, and the dispersion time is 4 hours, so that a growth base solution is obtained;
in the fourth step, the growth base solution obtained in the third step is poured into a magnetic stirrer, the sodium hydroxide and the chloroplatinic acid prepared in the first step are added while stirring at a low speed, the stirring speed of the magnetic stirrer is 45r/min, the stirring time is 2 hours, the mixture is sealed and kept stand for 0.4 hour after stirring, the sealed and kept stand temperature is 27 ℃, and a primary mixed solution is obtained after keeping stand;
pouring the preliminary mixed liquid obtained in the fourth step into a magnetic stirrer for high-speed stirring, wherein the stirring speed of the magnetic stirrer is 250r/min, the stirring time is 24 hours, and fully stirring to obtain a complete mixed liquid;
in the sixth step, the completely mixed solution obtained in the fifth step is put into a polytetrafluoroethylene-lined high-pressure reaction kettle, the pressure of the high-pressure reaction kettle is 3000KPa, the temperature is 160 ℃, the reaction time is 10 hours, and the mixture loaded with the platinum nanowires is obtained after continuous heating at high temperature;
and seventhly, pouring the mixture loaded with the platinum nanowires obtained in the sixth step into a container, sealing and standing for 0.8h at the sealing and standing temperature of 27 ℃, standing and filtering, washing with ethanol every 0.5h after filtering, repeating the operation for four times, washing, baking in an oven for 2h at the baking temperature of 47 ℃, and baking to obtain the platinum nanowires growing on the mesoporous metal oxide @ titanium nitride.
Example 3:
a method for regulating and controlling a controllable growth mechanism of a platinum nanowire in a carrier mesopore comprises the following steps: taking materials; step two, distillation; step three, dispersing; step four, mixing; step five, stirring; step six, growing; step seven, drying;
in the first step, 300 parts of N, N-dimethylformamide, 9 parts of ethylene glycol, 9 parts of metal oxide @ titanium nitride carrier, 5 parts of sodium hydroxide, 9 parts of anhydrous copper sulfate and 8 parts of chloroplatinic acid are respectively weighed according to the parts by weight of the components and are respectively placed for later use;
in the second step, the N, N-dimethylformamide prepared in the first step is placed into a container, then the prepared anhydrous copper sulfate is added, the mixture is kept stand for 0.3 hour at the temperature of 27 ℃, the mixture is poured into a distillation flask after the mixture is kept stand, the pressure is adjusted to be 2.5KPa, the temperature is 135 ℃, the mixture is distilled for 0.8 hour, and pure N, N-dimethylformamide is obtained after low-pressure distillation;
in the third step, the pure N, N-dimethylformamide obtained in the second step is poured into an ultrasonic dispersion machine, and the metal oxide @ titanium nitride carrier prepared in the first step and ethylene glycol are added, wherein the working frequency of the ultrasonic dispersion machine is 9kHz, and the dispersion time is 4 hours, so that a growth base solution is obtained;
in the fourth step, the growth base solution obtained in the third step is poured into a magnetic stirrer, the sodium hydroxide and the chloroplatinic acid prepared in the first step are added while stirring at a low speed, the stirring speed of the magnetic stirrer is 45r/min, the stirring time is 2 hours, the mixture is sealed and kept stand for 0.3 hour after stirring, the temperature of the sealed and kept stand is 28 ℃, and a primary mixed solution is obtained after the mixture is kept stand;
pouring the preliminary mixed liquid obtained in the fourth step into a magnetic stirrer for high-speed stirring, wherein the stirring speed of the magnetic stirrer is 330r/min, the stirring time is 24 hours, and fully stirring to obtain complete mixed liquid;
in the sixth step, the completely mixed solution obtained in the fifth step is put into a polytetrafluoroethylene-lined high-pressure reaction kettle, the pressure of the high-pressure reaction kettle is 3200KPa, the temperature is 170 ℃, the reaction time is 8 hours, and the mixture loaded with the platinum nanowires is obtained after continuous heating at high temperature;
and seventhly, pouring the mixture loaded with the platinum nanowires obtained in the sixth step into a container, sealing and standing for 1h at the sealing and standing temperature of 27 ℃, standing and filtering, washing with ethanol every 0.5h after filtering, repeating the operation for four times, washing, baking in an oven for 2h at the baking temperature of 47 ℃, and baking to obtain the platinum nanowires growing on the mesoporous metal oxide @ titanium nitride.
The platinum nanowires grown on the mesoporous metal oxide @ titanium nitride obtained in the above embodiments are respectively subjected to performance detection, and compared with the platinum nanowires grown on the mesoporous metal oxide @ titanium nitride obtained after general regulation, and the obtained results are as follows:
based on the above, the method has the advantages that the method regulates and controls the crystal face structure of the platinum nanowire by regulating and controlling the concentration of the reducing agent ethylene glycol in the growth base liquid and regulating the temperature in the polytetrafluoroethylene-lined high-pressure reaction kettle, and the regulation and control mode is simple, so that the working reliability of the platinum nanowire growing on the mesoporous metal oxide @ titanium nitride after the regulation and control preparation is ensured; the N, N-dimethylformamide is purified by the added distillation step, so that impurities in the growth base liquid are removed, and the regulation and control accuracy is improved; through ultrasonic dispersion treatment, the metal oxide @ titanium nitride carrier is uniformly distributed in the growth base solution, so that the conductivity of the platinum nanowire grown on the mesoporous metal oxide @ titanium nitride after preparation is regulated and controlled is improved.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (6)
1. A method for regulating and controlling a controllable growth mechanism of a platinum nanowire in a carrier mesopore comprises the following steps: taking materials; step two, distillation; step three, dispersing; step four, mixing; step five, stirring; step six, growing; step seven, drying; the method is characterized in that:
in the first step, 290-310 parts of N, N-dimethylformamide, 8-12 parts of ethylene glycol, 8-10 parts of metal oxide @ titanium nitride carrier, 4-6 parts of sodium hydroxide, 7-9 parts of anhydrous copper sulfate and 8-12 parts of chloroplatinic acid are respectively weighed according to the parts by weight of the components and are respectively placed for later use;
in the second step, the N, N-dimethylformamide prepared in the first step is put into a container, then the prepared anhydrous copper sulfate is added, the mixture is placed still and poured into a distillation flask, and the pure N, N-dimethylformamide is obtained after low-pressure distillation;
in the third step, the pure N, N-dimethylformamide obtained in the second step is poured into an ultrasonic dispersion machine, the metal oxide @ titanium nitride carrier prepared in the first step and ethylene glycol are added, and the metal oxide @ titanium nitride carrier and the ethylene glycol are uniformly dispersed in the pure N, N-dimethylformamide by utilizing ultrasonic oscillation to obtain a growth base solution;
in the fourth step, the growth base solution obtained in the third step is poured into a magnetic stirrer, the sodium hydroxide and the chloroplatinic acid prepared in the first step are added while stirring at a low speed, and the mixture is sealed and kept stand after stirring to obtain a primary mixed solution;
pouring the preliminary mixed liquid obtained in the fourth step into a magnetic stirrer for high-speed stirring, and fully stirring to obtain a complete mixed liquid;
in the sixth step, the complete mixed solution obtained in the fifth step is put into a polytetrafluoroethylene-lined high-pressure reaction kettle, the pressure of the polytetrafluoroethylene-lined high-pressure reaction kettle is 2500-3500 KPa, the temperature is 150-190 ℃, the reaction time is 6-12 h, and the mixture loaded with the platinum nanowires is obtained after high-temperature heating;
and in the seventh step, pouring the mixture loaded with the platinum nanowires obtained in the sixth step into a container, sealing and standing, filtering, repeatedly washing with ethanol, washing, and drying in an oven to obtain the platinum nanowires growing on the mesoporous metal oxide @ titanium nitride.
2. The method for regulating the controllable growth mechanism of the platinum nanowires in the mesoporous of the carrier according to claim 1, wherein the method comprises the following steps: in the second step, the standing temperature is 25-30 ℃, the standing time is 0.2-0.3 h, the pressure of low-pressure distillation is 2.2-2.7 KPa, the distillation temperature is 120-140 ℃, and the distillation time is 0.5-0.8 h.
3. The method for regulating the mesoporous controllable growth mechanism of the platinum nanowire on the carrier according to claim 1, wherein the method comprises the following steps: in the third step, the working frequency of the ultrasonic dispersion machine is 5-13 kHz, and the dispersion time is 3.5-4.5 h.
4. The method for regulating the mesoporous controllable growth mechanism of the platinum nanowire on the carrier according to claim 1, wherein the method comprises the following steps: in the fourth step, the stirring speed of the magnetic stirrer is 30-60 r/min, the stirring time is 1.5-2.5 h, the sealing and standing temperature is 25-30 ℃, and the standing time is 0.2-0.3 h.
5. The method for regulating the mesoporous controllable growth mechanism of the platinum nanowire on the carrier according to claim 1, wherein the method comprises the following steps: in the fifth step, the stirring speed of the magnetic stirrer is 250-330 r/min, and the stirring time is 23-25 h.
6. The method for regulating the mesoporous controllable growth mechanism of the platinum nanowire on the carrier according to claim 1, wherein the method comprises the following steps: and seventhly, sealing and standing at the temperature of 25-30 ℃ for 0.8-1.2 h, washing with ethanol every 0.5h after filtering, repeating the operation for four times, putting the filter material into a baking oven at the temperature of 45-50 ℃ and baking for 1.5-2 h.
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