CN113421716B - Method for regulating and controlling growth mechanism of platinum nanowires in carrier mesoporous controllable growth mechanism - Google Patents

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

A control method for the controllable growth mechanism of platinum nanowires in carrier mesopores

technical field

The invention relates to the technical field of platinum nanowires, in particular to a method for regulating the controllable growth mechanism of platinum nanowires in carrier mesopores.

Background technique

Platinum nanowires have special physical and chemical properties, and have broad prospects for application in the fields of biomedicine, sensors, conductive materials, and chemical catalysts. At the same time, the crystal plane structure and structural characteristics of platinum nanowires grown in the carrier mesopores It determines the electrocatalytic activity and stability of mesoporous metal oxide@titanium nitride loaded with platinum nanowires, but the original method of hydrothermal reaction regulation and preparation of platinum nanowires still has the following problems. First, in the original regulation In the process of preparing platinum nanowires, the growth state of platinum nanowires cannot be accurately regulated, which affects the special physical and chemical properties of the prepared platinum nanowires, which in turn affects the growth of mesoporous metal oxide@titanium nitride. The working reliability of platinum nanowires; second, the original regulation process did not remove the impurities in the growth base liquid first, which affected the original growth mechanism of platinum nanowires during the regulation process, thereby reducing the accuracy of regulation; third , In the original regulation process, the metal oxide@titanium nitride carrier was not sufficiently mixed in the growth base solution, which affected the conductivity of the platinum nanowires grown on the mesoporous metal oxide@titanium nitride after the regulation and preparation.

Contents of the invention

The purpose of the present invention is to provide a method for regulating the controllable growth mechanism of platinum nanowires in carrier mesopores, so as to solve the problems raised in the above-mentioned background technology.

In order to achieve the above object, the present invention provides the following technical scheme: a method for controlling the growth mechanism of platinum nanowires in the carrier mesopore, comprising the following steps: step 1, taking material; step 2, distillation; step 3, dispersing; step Four, mixing; step five, stirring; step six, growing; step seven, drying;

Wherein in the above step 1, according to the parts by weight of each component, weigh 290-310 parts of N,N-dimethylformamide, 8-12 parts of ethylene glycol, and 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 placed separately for later use;

Among them, in the above step two, put the N,N-dimethylformamide prepared in step one into the container, then add the prepared anhydrous copper sulfate, pour it into the distillation bottle after standing still, and after low-pressure distillation Obtain pure N,N-dimethylformamide;

In the above step three, pour the pure N,N-dimethylformamide obtained in step two into an ultrasonic disperser, and add the metal oxide @titanium nitride carrier and ethylene glycol prepared in step one , using ultrasonic vibration to uniformly disperse the metal oxide@titanium nitride carrier and ethylene glycol in pure N,N-dimethylformamide to obtain the growth base solution;

Wherein in the above step 4, pour the growth base liquid obtained in step 3 into a magnetic stirrer, add sodium hydroxide and chloroplatinic acid prepared in step 1 while stirring at a low speed, seal and stand still after stirring to obtain a preliminary mixed solution ;

Wherein in the above-mentioned step 5, the preliminary mixed solution obtained in the step 4 is poured into a magnetic stirrer for high-speed stirring, and a complete mixed solution is obtained after fully stirring;

Wherein in the above step six, the complete mixed solution obtained in the step five is put into a polytetrafluoroethylene-lined high-pressure reactor, and the mixture loaded with platinum nanowires is obtained after heating at a high temperature;

Wherein in the above-mentioned step 7, pour the platinum nanowire-loaded mixture obtained in step 6 into a container, seal it and let it stand, filter and wash it repeatedly with ethanol, put it into an oven after washing, and dry it in an oven to obtain a mesoporous metal oxide Platinum nanowires grown on titanium nitride.

Preferably, in said step 2, the standing temperature is 25-30°C, the standing time is 0.2-0.3h, the pressure of low-pressure distillation is 2.2-2.7KPa, the distillation temperature is 120-140°C, and the distillation time is 0.5- 0.8h.

Preferably, in the third step, the working frequency of the ultrasonic disperser is 5-13kHz, and the dispersion time is 3.5-4.5h.

Preferably, in the step 4, the stirring speed of the magnetic stirrer is 30-60r/min, the stirring time is 1.5-2.5h, the temperature for sealing and standing is 25-30°C, and the standing time is 0.2-0.3h.

Preferably, in the step five, the stirring speed of the magnetic stirrer is 250-330r/min, and the stirring time is 23-25h.

Preferably, in the step six, the pressure of the polytetrafluoroethylene-lined high-pressure reactor is 2500-3500KPa, the temperature is 150-190°C, and the reaction time is 6-12h.

Preferably, in the step seven, the sealing temperature is 25-30°C, and the standing time is 0.8-1.2h. After filtering, it is washed with ethanol every 0.5h, and the operation is repeated four times. The temperature in the oven is 45～50℃, the baking time is 1.5～2h.

Compared with the prior art, the beneficial effect of the present invention is: the regulation method of the controllable growth mechanism of platinum nanowires in the mesopores of the carrier, by preparing the growth base liquid in advance before preparation, the reduction of the reducing agent in the growth base liquid Control the concentration of platinum nanowires to achieve the purpose of regulating the growth of platinum nanowires, and then further regulate the growth of platinum nanowires by regulating the temperature in the polytetrafluoroethylene-lined high-pressure reactor, so that platinum nanowires grow out of dominant crystal planes, and control the growth of platinum nanowires. It is simple and ensures the reliability of platinum nanowires grown on mesoporous metal oxide@titanium nitride after regulation and preparation; by distilling N,N-dimethylformamide before regulation, the growth substrate is removed Impurities in the liquid eliminate the influence of impurities on the regulation, thereby improving the accuracy of regulation; through ultrasonic dispersion treatment, the uniform distribution of the metal oxide@titanium nitride carrier in the growth base liquid is ensured, which is conducive to the regulation of platinum During the process of nanowires, chloroplatinic acid is in full contact with the metal oxide@titanium nitride carrier, which improves the conductivity of platinum nanowires grown on mesoporous metal oxide@titanium nitride after preparation.

Description of drawings

Fig. 1 is a flow chart of the method of the present invention.

Detailed ways

The following will clearly and completely describe the technical solutions in the embodiments of the present invention with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only some, not all, embodiments of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by persons of ordinary skill in the art without making creative efforts belong to the protection scope of the present invention.

Please refer to Fig. 1, a kind of technical scheme provided by the present invention:

Example 1:

A method for controlling the controllable growth mechanism of platinum nanowires in carrier mesopores, comprising the following steps: Step 1, taking material; Step 2, distillation; Step 3, dispersing; Step 4, mixing; Step 5, stirring; Step 6, growing; step seven, drying;

In the above step 1, 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 placed for subsequent use;

Wherein in the above step 2, put the N,N-dimethylformamide prepared in the step 1 into the container, then add the prepared anhydrous copper sulfate, let stand for 0.2h, the stand temperature is 25°C, After standing still, pour it into a distillation bottle, adjust the pressure to 2.5KPa, the temperature to 135°C, distill for 0.6h, and obtain pure N,N-dimethylformamide after low-pressure distillation;

In the above step three, pour the pure N,N-dimethylformamide obtained in step two into an ultrasonic disperser, and add the metal oxide @titanium nitride carrier and ethylene glycol prepared in step one , the operating frequency of the ultrasonic disperser is 8kHz, the dispersion time is 4h, and the growth base liquid is obtained;

Wherein in the above-mentioned step 4, the growth base solution obtained in the step 3 is poured into the magnetic stirrer, and the sodium hydroxide and chloroplatinic acid prepared in the step 1 are added while stirring at a low speed, and the stirring speed of the magnetic stirrer is 50r/min , the stirring time is 2h, and after stirring, it is sealed and stood for 0.3h, and the temperature of sealing and standing is 28°C, and the preliminary mixed solution is obtained after standing;

Wherein in the above-mentioned step five, the preliminary mixed solution obtained in the step four is poured into a magnetic stirrer for high-speed stirring, the stirring speed of the magnetic stirrer is 275r/min, and the stirring time is 24h, and a complete mixed solution is obtained after fully stirring;

In the above step six, put the complete mixture obtained in step five into a polytetrafluoroethylene-lined autoclave, the pressure of the autoclave is 3000KPa, the temperature is 150°C, the reaction time is 7h, after continuous heating at high temperature A mixture of supported platinum nanowires is obtained;

Wherein in the above step 7, pour the platinum nanowire-loaded mixture obtained in step 6 into a container and seal it for 1 hour. The sealed temperature is 27° C., filter after standing, and rinse with ethanol every 0.5 hours after filtering , repeated the operation four times, after washing, put it into an oven and bake for 2 hours at a temperature of 50° C. After baking, platinum nanowires grown on mesoporous metal oxide@titanium nitride were obtained.

Example 2:

A method for controlling the controllable growth mechanism of platinum nanowires in carrier mesopores, comprising the following steps: Step 1, taking material; Step 2, distillation; Step 3, dispersing; Step 4, mixing; Step 5, stirring; Step 6, growing; step seven, drying;

Wherein in the above step 1, according to the parts by weight of each component, 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 placed separately for subsequent use;

Wherein in the above step 2, put the N,N-dimethylformamide prepared in the step 1 into the container, then add the prepared anhydrous copper sulfate, let stand for 0.2h, the stand temperature is 28°C, After standing still, pour it into a distillation bottle, adjust the pressure to 2.5KPa, the temperature to 130°C, distill for 0.6h, and obtain pure N,N-dimethylformamide after low-pressure distillation;

In the above step three, pour the pure N,N-dimethylformamide obtained in step two into an ultrasonic disperser, and add the metal oxide @titanium nitride carrier and ethylene glycol prepared in step one , the operating frequency of the ultrasonic disperser is 10kHz, the dispersion time is 4h, and the growth base liquid is obtained;

Wherein in the above-mentioned step 4, the growth base liquid obtained in the step 3 is poured into the magnetic stirrer, and the sodium hydroxide and chloroplatinic acid prepared in the step 1 are added while stirring at a low speed, and the stirring speed of the magnetic stirrer is 45r/min , the stirring time is 2h, and after stirring, it is sealed and stood for 0.4h, and the temperature of sealing and standing is 27°C, and the preliminary mixed solution is obtained after standing;

Wherein in the above-mentioned step five, the preliminary mixed solution obtained in the step four is poured into a magnetic stirrer for high-speed stirring, the stirring speed of the magnetic stirrer is 250r/min, and the stirring time is 24h, and a complete mixed solution is obtained after fully stirring;

Wherein in the above step six, put the complete mixture obtained in step five into a polytetrafluoroethylene-lined autoclave, the pressure of the autoclave is 3000KPa, the temperature is 160°C, the reaction time is 10h, after continuous heating at high temperature A mixture of supported platinum nanowires is obtained;

Among them, in the above step seven, pour the platinum nanowire-loaded mixture obtained in step six into a container and seal it for 0.8 hours. Rinse and repeat the operation four times. After washing, put it into an oven and bake for 2 hours at a temperature of 47° C. After baking, platinum nanowires grown on mesoporous metal oxide@titanium nitride are obtained.

Example 3:

A method for controlling the controllable growth mechanism of platinum nanowires in carrier mesopores, comprising the following steps: Step 1, taking material; Step 2, distillation; Step 3, dispersing; Step 4, mixing; Step 5, stirring; Step 6, growing; step seven, drying;

Wherein in the above step 1, according to the parts by weight of each component, 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 placed for subsequent use;

Wherein in the above step 2, put the N,N-dimethylformamide prepared in the step 1 into the container, then add the prepared anhydrous copper sulfate, let stand for 0.3h, the stand temperature is 27°C, After standing still, pour it into a distillation bottle, adjust the pressure to 2.5KPa, the temperature to 135°C, distill for 0.8h, and obtain pure N,N-dimethylformamide after low-pressure distillation;

In the above step three, pour the pure N,N-dimethylformamide obtained in step two into an ultrasonic disperser, and add the metal oxide @titanium nitride carrier and ethylene glycol prepared in step one , the operating frequency of the ultrasonic disperser is 9kHz, and the dispersion time is 4h to obtain the growth base liquid;

Wherein in the above-mentioned step 4, the growth base liquid obtained in the step 3 is poured into the magnetic stirrer, and the sodium hydroxide and chloroplatinic acid prepared in the step 1 are added while stirring at a low speed, and the stirring speed of the magnetic stirrer is 45r/min , the stirring time is 2h, and after stirring, it is sealed and stood for 0.3h, and the temperature of sealing and standing is 28°C, and the preliminary mixed solution is obtained after standing;

Wherein in the above-mentioned step five, the preliminary mixed solution obtained in the step four is poured into a magnetic stirrer for high-speed stirring, the stirring speed of the magnetic stirrer is 330r/min, and the stirring time is 24h, and a complete mixed solution is obtained after fully stirring;

In the above step six, put the complete mixture obtained in step five into a polytetrafluoroethylene-lined autoclave, the pressure of the autoclave is 3200KPa, the temperature is 170°C, the reaction time is 8h, after continuous heating at high temperature A mixture of supported platinum nanowires is obtained;

Wherein in the above step 7, pour the platinum nanowire-loaded mixture obtained in step 6 into a container and seal it for 1 hour. The sealed temperature is 27° C., filter after standing, and rinse with ethanol every 0.5 hours after filtering , repeated the operation four times, after washing, put it into an oven and bake for 2 hours at a temperature of 47° C. After baking, platinum nanowires grown on mesoporous metal oxide@titanium nitride were obtained.

The performance of the platinum nanowires grown on mesoporous metal oxide@titanium nitride obtained in the above examples was tested separately, and compared with the platinum nanowires grown on mesoporous metal oxide@titanium nitride obtained after general regulation. For comparison, the results obtained are as follows:

Based on the above, the advantage of the present invention is that the invention regulates the crystal plane structure of platinum nanowires by regulating the concentration of the reducing agent ethylene glycol contained in the growth base liquid and regulating the temperature in the polytetrafluoroethylene-lined high-pressure reactor. , the control method is simple, thus ensuring the reliability of the platinum nanowires grown on the mesoporous metal oxide@titanium nitride after the control and preparation; the N,N-dimethylformamide is purified by the added distillation step , the impurities in the growth base liquid were removed, thereby increasing the control accuracy; through ultrasonic dispersion treatment, the metal oxide@titanium nitride carrier was evenly distributed in the growth base liquid, thereby improving the mesoporous Conductivity of platinum nanowires grown on metal oxide@titanium nitride.

It will be apparent to those skilled in the art that the invention is not limited to the details of the above-described exemplary embodiments, but that the invention can be embodied in other specific forms without departing from the spirit or essential characteristics of the invention. Accordingly, the embodiments should be regarded in all points of view as exemplary and not restrictive, the scope of the invention being defined by the appended claims rather than the foregoing description, and it is therefore intended that the scope of the invention be defined by the appended claims rather than by the foregoing description. All changes within the meaning and range of equivalents of the elements are embraced in the present invention. 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.

Images