CN112194180A - Modification method for enhancing mechanical property of aerogel - Google Patents
Modification method for enhancing mechanical property of aerogel Download PDFInfo
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- CN112194180A CN112194180A CN202011098149.XA CN202011098149A CN112194180A CN 112194180 A CN112194180 A CN 112194180A CN 202011098149 A CN202011098149 A CN 202011098149A CN 112194180 A CN112194180 A CN 112194180A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G25/00—Compounds of zirconium
- C01G25/006—Compounds containing, besides zirconium, two or more other elements, with the exception of oxygen or hydrogen
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0091—Preparation of aerogels, e.g. xerogels
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/168—After-treatment
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Abstract
The invention relates to a modification method for enhancing the mechanical property of aerogel. Lead acetate trihydrate is used as a lead source, tetrabutyl titanate is used as a titanium source, zirconium n-propoxide is used as a zirconium source, and ethylene glycol monomethyl ether is used as a solvent. The method comprises the steps of forming a lead zirconate titanate precursor solution through a water-bath heating reaction, adding deionized water, standing for hydrolysis for 1-3 days, then adding deionized water, propylene oxide and carbon nanotubes to prepare a carbon nanotube-doped lead zirconate titanate sol, covering a layer of organic solvent on the surface of the prepared wet gel, aging and standing for 1-3 days to form the wet gel with a stable network structure. After aging, the wet gel was replaced in ethanol solvent. And finally, performing supercritical drying on the displaced wet gel to obtain the composite aerogel with more excellent heat-insulating property, mechanical property and piezoelectric property.
Description
Technical Field
The invention belongs to the technical field of preparation of inorganic nano porous materials, and relates to a modification method for enhancing the mechanical property of aerogel.
Background
Aerogel is a kind of nano particles mutually polymerized to form a highly dispersed porous solid material. Aerogel materials generally have a large specific surface area, good thermal insulation properties, high porosity, very low apparent density, high optical transparency, low thermal conductivity. These unique structures provide the aerogel with unusual properties in mechanical, electromagnetic, thermal, optical, acoustical, etc. However, the structural skeleton of the aerogel is brittle, and the strength of the aerogel is low due to the fact that the aerogel is arranged in a dispersed manner, the application of the aerogel in the aspect of bearing is limited due to the defects, and in addition, the mechanical property of the aerogel is poor due to high porosity and low solid content of the aerogel. The poor mechanical properties of the aerogel affect the processability of the aerogel in the practical application process. Therefore, it is very important to improve the mechanical properties of the aerogel. At present, the improvement of the mechanical properties of the aerogel is mainly realized by selecting a proper precursor, preparing flexible aerogel or compounding the flexible aerogel with a fiber woven body, and preparing composite aerogel.
Researches find that various fiber composite reinforced aerogel composite materials can well achieve the purpose of enhancing the mechanical strength of the aerogel and well meet the requirements of practical application. However, the fiber-reinforced aerogel composite material still has some problems, wherein the size of the composite fiber is micron-sized, the composite fiber and the nano-sized aerogel particles have obvious interface effect in the composite process, the combination is not very tight, the crack defect is easily generated, once the material is damaged, the stress transmission can be locally failed, and the heat insulation performance and the piezoelectric performance of the material are destructively influenced. The carbon nano tube is a nano material with good mechanical strength, is more tightly combined with the nanometer skeleton particles of the aerogel on a microstructure, and is beneficial to the mechanical stability of the material. Ajayan and the like firstly add carbon nanotubes as fillers into a polymer to reinforce and modify the polymer, and the modified polymer is called a polymer resin-carbon nanotube composite material, and researches show that the material has good mechanical properties. Many researchers at home and abroad also compound PZT aerogel, but the preparation of the aerogel with good piezoelectric property, mechanical property and heat insulation property is difficult.
Disclosure of Invention
The invention aims to enhance the mechanical property of the PZT aerogel through simple doping modification. In order to achieve the purpose of the invention, the technical scheme adopted by the invention is as follows:
the method comprises the following steps: 16.25ml of ethylene glycol methyl ether and 2.9875g of lead acetate trihydrate were put into a beaker and heated in a water bath at 60 ℃ with stirring for 0.5 to 1 hour. When the lead acetate trihydrate had dissolved sufficiently, the solution was taken out and cooled to room temperature.
Step two: slowly dripping 1.23ml of tetrabutyl titanate solution along the wall of the cup, stirring while dripping, and continuously stirring for 0.5-1 hour after dripping to fully mix the solution. After the mixture was mixed well, 1.725ml of zirconium n-propoxide solution was added to the solution along the wall of the cup, and the mixture was stirred while dropping, and then stirred for 3 to 5 minutes after dropping, thereby forming a lead zirconate titanate precursor solution.
Step three: 2ml of deionized water was added to the lead zirconate titanate precursor solution, and the mixture was stirred while adding the deionized water, to hydrolyze the lead zirconate titanate precursor solution. Then it was left to stand for 2-3 days.
Step four: standing for 2-3 days, adding 2ml of deionized water while stirring, fully mixing, adding 4.2ml of propylene oxide, and stirring for 3-5 minutes. After being mixed evenly, the carbon nano tubes are added for 2 to 4 times, the mass fractions of the carbon nano tubes are respectively 0 percent, 1 percent, 2 percent, 3 percent and 4 percent, and the carbon nano tubes are stirred for 3 to 5 minutes each time. The mixture was then sealed and placed in an oven at 60 ℃ to allow it to gel.
Step five: covering a layer of ethylene glycol monomethyl ether on the surface of the wet gel, and aging for 1-3 days at 10-30 ℃.
Step six: after aging, the wet gel is placed in an ethanol solvent for replacement for 1-2 weeks, and the ethanol is replaced every 12 hours.
Step seven: and (3) drying the displaced wet gel by a supercritical drying process, wherein the drying medium is carbon dioxide, the supercritical temperature is finally 45 ℃, the air pressure is 7.5MPa, and the drying time is 1-2 hours. And finally obtaining the lead zirconate titanate carbon nanotube aerogel.
Detailed Description
Example 1
16.25ml of ethylene glycol methyl ether and 2.9875g of lead acetate trihydrate were put into a beaker and heated in a water bath at 60 ℃ with stirring for 0.5 to 1 hour. When the lead acetate trihydrate had dissolved sufficiently, the solution was taken out and cooled to room temperature. Slowly dripping 1.23ml of tetrabutyl titanate solution along the wall of the cup, stirring while dripping, and continuously stirring for 0.5-1 hour after dripping to fully mix the solution. After the mixture was mixed well, 1.725ml of zirconium n-propoxide solution was added to the solution along the wall of the cup, and the mixture was stirred while dropping, and then stirred for 3 to 5 minutes after dropping, thereby forming a lead zirconate titanate precursor solution. 2ml of deionized water was added to the lead zirconate titanate precursor solution, and the mixture was stirred while adding the deionized water, to hydrolyze the lead zirconate titanate precursor solution. Then it was left to stand for 2-3 days. Standing for 2-3 days, adding 2ml of deionized water while stirring, fully mixing, adding 4.2ml of propylene oxide, and stirring for 3-5 minutes. The mixture was then sealed and placed in an oven at 60 ℃ to allow it to gel. Covering a layer of ethylene glycol monomethyl ether on the surface of the wet gel, and aging for 1-3 days at 10-30 ℃. After aging, the wet gel is placed in an ethanol solvent for replacement for 1-2 weeks, and the ethanol is replaced every 12 hours. And (3) drying the displaced wet gel by a supercritical drying process, wherein the drying medium is carbon dioxide, the supercritical temperature is finally 45 ℃, the air pressure is 7.5MPa, and the drying time is 1-2 hours. And finally obtaining the lead zirconate titanate aerogel.
Example 2
16.25ml of ethylene glycol methyl ether and 2.9875g of lead acetate trihydrate were put into a beaker and heated in a water bath at 60 ℃ with stirring for 0.5 to 1 hour. When the lead acetate trihydrate had dissolved sufficiently, the solution was taken out and cooled to room temperature. Slowly dripping 1.23ml of tetrabutyl titanate solution along the wall of the cup, stirring while dripping, and continuously stirring for 0.5-1 hour after dripping to fully mix the solution. After the mixture was mixed well, 1.725ml of zirconium n-propoxide solution was added to the solution along the wall of the cup, and the mixture was stirred while dropping, and then stirred for 3 to 5 minutes after dropping, thereby forming a lead zirconate titanate precursor solution. 2ml of deionized water was added to the lead zirconate titanate precursor solution, and the mixture was stirred while adding the deionized water, to hydrolyze the lead zirconate titanate precursor solution. Then it was left to stand for 2-3 days. Standing for 2-3 days, adding 2ml of deionized water while stirring, fully mixing, adding 4.2ml of propylene oxide, and stirring for 3-5 minutes. After mixing evenly, 0.0566g of carbon nano tube is added in 2 to 4 times and stirred for 3 to 5 minutes. The mixture was then sealed and placed in an oven at 60 ℃ to allow it to gel. Covering a layer of ethylene glycol monomethyl ether on the surface of the wet gel, and aging for 1-3 days at 10-30 ℃. After aging, the wet gel is placed in an ethanol solvent for replacement for 1-2 weeks, and the ethanol is replaced every 12 hours. And (3) drying the displaced wet gel by a supercritical drying process, wherein the drying medium is carbon dioxide, the supercritical temperature is finally 45 ℃, the air pressure is 7.5MPa, and the drying time is 1-2 hours. And finally obtaining the lead zirconate titanate carbon nanotube composite aerogel.
Example 3
16.25ml of ethylene glycol methyl ether and 2.9875g of lead acetate trihydrate were put into a beaker and heated in a water bath at 60 ℃ with stirring for 0.5 to 1 hour. When the lead acetate trihydrate had dissolved sufficiently, the solution was taken out and cooled to room temperature. Slowly dripping 1.23ml of tetrabutyl titanate solution along the wall of the cup, stirring while dripping, and continuously stirring for 0.5-1 hour after dripping to fully mix the solution. After the mixture was mixed well, 1.725ml of zirconium n-propoxide solution was added to the solution along the wall of the cup, and the mixture was stirred while dropping, and then stirred for 3 to 5 minutes after dropping, thereby forming a lead zirconate titanate precursor solution. 2ml of deionized water was added to the lead zirconate titanate precursor solution, and the mixture was stirred while adding the deionized water, to hydrolyze the lead zirconate titanate precursor solution. Then it was left to stand for 2-3 days. Standing for 2-3 days, adding 2ml of deionized water while stirring, fully mixing, adding 4.2ml of propylene oxide, and stirring for 3-5 minutes. After mixing evenly, 0.1144g of carbon nano tube is added in 2-4 times and stirred for 3-5 minutes. The mixture was then sealed and placed in an oven at 60 ℃ to allow it to gel. Covering a layer of ethylene glycol monomethyl ether on the surface of the wet gel, and aging for 1-3 days at 10-30 ℃. After aging, the wet gel is placed in an ethanol solvent for replacement for 1-2 weeks, and the ethanol is replaced every 12 hours. And (3) drying the displaced wet gel by a supercritical drying process, wherein the drying medium is carbon dioxide, the supercritical temperature is finally 45 ℃, the air pressure is 7.5MPa, and the drying time is 1-2 hours. And finally obtaining the lead zirconate titanate carbon nanotube composite aerogel.
Example 4
16.25ml of ethylene glycol methyl ether and 2.9875g of lead acetate trihydrate were put into a beaker and heated in a water bath at 60 ℃ with stirring for 0.5 to 1 hour. When the lead acetate trihydrate had dissolved sufficiently, the solution was taken out and cooled to room temperature. Slowly dripping 1.23ml of tetrabutyl titanate solution along the wall of the cup, stirring while dripping, and continuously stirring for 0.5-1 hour after dripping to fully mix the solution. After the mixture was mixed well, 1.725ml of zirconium n-propoxide solution was added to the solution along the wall of the cup, and the mixture was stirred while dropping, and then stirred for 3 to 5 minutes after dropping, thereby forming a lead zirconate titanate precursor solution. 2ml of deionized water was added to the lead zirconate titanate precursor solution, and the mixture was stirred while adding the deionized water, to hydrolyze the lead zirconate titanate precursor solution. Then it was left to stand for 2-3 days. Standing for 2-3 days, adding 2ml of deionized water while stirring, fully mixing, adding 4.2ml of propylene oxide, and stirring for 3-5 minutes. After mixing evenly, 0.1733g of carbon nano tube is added in 2-4 times and stirred for 3-5 minutes. The mixture was then sealed and placed in an oven at 60 ℃ to allow it to gel. Covering a layer of ethylene glycol monomethyl ether on the surface of the wet gel, and aging for 1-3 days at 10-30 ℃. After aging, the wet gel is placed in an ethanol solvent for replacement for 1-2 weeks, and the ethanol is replaced every 12 hours. And (3) drying the displaced wet gel by a supercritical drying process, wherein the drying medium is carbon dioxide, the supercritical temperature is finally 45 ℃, the air pressure is 7.5MPa, and the drying time is 1-2 hours. And finally obtaining the lead zirconate titanate carbon nanotube composite aerogel.
Example 5
16.25ml of ethylene glycol methyl ether and 2.9875g of lead acetate trihydrate were put into a beaker and heated in a water bath at 60 ℃ with stirring for 0.5 to 1 hour. When the lead acetate trihydrate had dissolved sufficiently, the solution was taken out and cooled to room temperature. Slowly dripping 1.23ml of tetrabutyl titanate solution along the wall of the cup, stirring while dripping, and continuously stirring for 0.5-1 hour after dripping to fully mix the solution. After the mixture was mixed well, 1.725ml of zirconium n-propoxide solution was added to the solution along the wall of the cup, and the mixture was stirred while dropping, and then stirred for 3 to 5 minutes after dropping, thereby forming a lead zirconate titanate precursor solution. 2ml of deionized water was added to the lead zirconate titanate precursor solution, and the mixture was stirred while adding the deionized water, to hydrolyze the lead zirconate titanate precursor solution. Then it was left to stand for 2-3 days. Standing for 2-3 days, adding 2ml of deionized water while stirring, fully mixing, adding 4.2ml of propylene oxide, and stirring for 3-5 minutes. After mixing evenly, 0.2335g of carbon nano tube is added in 2-4 times and stirred for 3-5 minutes. The mixture was then sealed and placed in an oven at 60 ℃ to allow it to gel. Covering a layer of ethylene glycol monomethyl ether on the surface of the wet gel, and aging for 1-3 days at 10-30 ℃. After aging, the wet gel is placed in an ethanol solvent for replacement for 1-2 weeks, and the ethanol is replaced every 12 hours. And (3) drying the displaced wet gel by a supercritical drying process, wherein the drying medium is carbon dioxide, the supercritical temperature is finally 45 ℃, the air pressure is 7.5MPa, and the drying time is 1-2 hours. And finally obtaining the lead zirconate titanate carbon nanotube composite aerogel.
Claims (4)
1. A modification method for enhancing the mechanical property of aerogel is characterized by comprising the following steps:
the method comprises the following steps: putting ethylene glycol monomethyl ether and lead acetate trihydrate into a beaker, heating and stirring in a water bath at 60 ℃ for 0.5-1 hour, and taking out the solution and cooling to room temperature after the lead acetate trihydrate is fully dissolved;
step two: slowly dripping tetrabutyl titanate solution along the wall of the cup, stirring while dripping, continuously stirring for 0.5-1 hour after dripping to fully mix the tetrabutyl titanate solution, adding normal zirconium propoxide solution into the solution along the wall of the cup while stirring after fully mixing, and continuously stirring for 3-5 minutes after dripping to form lead zirconate titanate precursor solution;
step three: adding deionized water into the lead zirconate titanate precursor solution, stirring while adding, hydrolyzing, and standing for 2-3 days;
step four: standing for 2-3 days, adding deionized water while stirring, adding propylene oxide after fully mixing, stirring for 3-5 minutes, adding carbon nanotubes after uniformly mixing, stirring for 3-5 minutes, and sealing the mixed solution in a heater to make the mixed solution gel;
step five: covering a layer of organic solvent on the surface of the wet gel, and aging for 1-3 days;
step six: after aging, placing the wet gel in an ethanol solvent for replacement for 1-2 weeks, and replacing the ethanol every 12 hours;
step seven: and drying the displaced wet gel through a supercritical drying process to finally obtain the lead zirconate titanate carbon nanotube aerogel.
2. The modification method for enhancing the mechanical property of the aerogel according to claim 1, wherein the modification method comprises the following steps: and step four, adding the carbon nano tubes in batches according to the mass fractions of 0%, 1%, 2%, 3% and 4% in sequence, fully mixing, and putting the mixture into a 60 ℃ oven to rapidly gel.
3. The modification method for enhancing the mechanical property of the aerogel according to claim 1, wherein the modification method comprises the following steps: the organic solvent in the fifth step is ethylene glycol monomethyl ether, and the aging temperature is 10-30 ℃.
4. The modification method for enhancing the mechanical property of the aerogel according to claim 1, wherein the modification method comprises the following steps: and seventhly, selecting carbon dioxide as a drying medium for supercritical drying, wherein the supercritical temperature is finally 45 ℃, the air pressure is 7.5MPa, and the drying time is 1-2 hours.
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