CN109718910B - Preparation method of high-temperature-resistant surface disordered nano material - Google Patents
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Abstract
The invention provides a preparation method of a high-temperature-resistant surface disordered nano material, which comprises the following steps: carrying out ball milling on the semiconductor nano material and a lithium-containing compound, and then carrying out heat treatment to obtain a surface disordered nano material; the heat treatment temperature is 600-1500 ℃, and the heat treatment atmosphere is oxygen-containing atmosphere. The invention prepares the surface disordered nano material by a ball milling method, catalyzes the diffusion reaction of the nano material and a lithium compound by controlling the ball milling condition and utilizing high energy provided by instantaneous impact of a milling ball on a sample in the ball milling process, enhances the diffusion by heat treatment, and finally prepares the high-temperature-resistant surface disordered core-shell structure nano material. The preparation method of the invention can use no hydrogen, thus having no flammable and explosive danger; the experimental conditions are easy to realize, the preparation period is short, and the batch production can be realized. The surface disordered nano material provided by the invention is prepared under the high-temperature condition, and has good high-temperature resistance.
Description
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to a preparation method of a high-temperature-resistant surface disordered nano material.
Background
Through surface lattice disorder, the method is a universal and effective energy band engineering adjusting means for oxide semiconductors. Researches find that the oxide nanoparticles treated by the surface disorder technology have high-efficiency microwave absorption capacity, and the surface disorder technology is expected to be used for developing novel high-performance microwave stealth materials.
The semiconductor "Disorder Engineering" concept was originally proposed in 2004 by liberal institute of optical and mechanical institute of catharanthus of china academy of sciences and professor dawn in dawn wave of usa (Science, 331, 746(2011)), that is, spatial separation of semiconductor electrons and holes was achieved by constructing an ordered/disordered core-shell structure through surface lattice Disorder control of semiconductor nanoparticles. The method is initially used in the field of photocatalysis, and subsequent research shows that plasma formed by space separation of electrons and holes can oscillate under the action of a microwave field, and conventional microwave transparent materials ZnO and TiO can be prepared by utilizing a disorder engineering technology2The microwave absorption efficiency is improved to 99.999 percent. An oxide semiconductor which does not have microwave absorbing ability is subjected to a disorder treatment to obtain high microwave absorbing efficiency.
The metal oxide semiconductor has the economic advantages of rich source, low preparation cost and the like, has the inherent conditions of no toxicity, environmental protection and the like, is suitable for large-scale production and application, and is expected to develop a low-cost high-performance microwave stealth material. Therefore, the preparation of semiconductor materials with disordered surfaces is of great significance.
At present, the core-shell structure nano particles with disordered surfaces are mainly obtained by hydrogenation treatment in disorder engineering, but the method has harsh experimental conditions, hydrogen has flammable and explosive hidden dangers, and the material cannot be used in a high-temperature environment because hydrogen is easy to escape at high temperature, so that the application of the material in special occasions such as high temperature is limited. Therefore, the key to the preparation of the novel concept material is to develop a preparation method of the surface disordered material which is safe, easy to realize, capable of mass production and good in thermal stability.
Disclosure of Invention
In view of the above, the technical problem to be solved by the present invention is to provide a method for preparing a high temperature resistant surface disordered nanomaterial, the method provided by the present invention is safe and can be used for mass production, and the prepared surface disordered nanomaterial has good thermal stability.
The invention provides a preparation method of a high-temperature-resistant surface disordered nano material, which comprises the following steps:
carrying out ball milling on the semiconductor nano material and a lithium-containing compound, and then carrying out heat treatment to obtain a surface disordered nano material;
the heat treatment temperature is 600-1500 ℃, and the heat treatment atmosphere is oxygen-containing atmosphere.
Preferably, the lithium-containing compound is selected from one or more of lithium carbonate, lithium oxide, lithium hydroxide, lithium chloride and lithium nitrate.
Preferably, the semiconductor nano material is selected from one or more of titanium dioxide, zinc oxide, zirconium dioxide, barium titanate, strontium titanate and calcium titanate; the average particle size of the semiconductor nano material is 5-100 nm.
Preferably, the molar ratio of the semiconductor nano material to the lithium-containing compound is 1 (0.01-2).
Preferably, the rotation speed of the ball milling is 200-1000 r/min, and the time is 2-12 hours.
Preferably, the rotation speed of the ball mill is 400-800 r/min, and the time is 2-6 hours.
Preferably, the mass ratio of the ball materials subjected to ball milling is (10-20) to 1; the volume ratio of the ball-milled grinding balls to the ball-milling tank is 1/3-3/4.
Preferably, the oxygen-containing atmosphere is selected from the group consisting of oxygen, air, an oxygen-argon mixed gas, an oxygen-nitrogen mixed gas, an oxygen-helium mixed gas, an oxygen-neon mixed gas, and a mixed gas of the above gases.
Preferably, the time of the heat treatment is 0.5 to 4 hours.
Preferably, the temperature of the heat treatment is 800-1200 ℃.
Compared with the prior art, the invention provides a preparation method of a high-temperature-resistant surface disordered nano material, which comprises the following steps: carrying out ball milling on the semiconductor nano material and a lithium-containing compound, and then carrying out heat treatment to obtain a surface disordered nano material; the heat treatment temperature is 600-1500 ℃, and the heat treatment atmosphere is oxygen-containing atmosphere. The invention prepares the surface disordered nano material by a ball milling method, catalyzes the diffusion reaction of the nano material and a lithium compound by controlling the ball milling condition and utilizing high energy provided by instantaneous impact of a milling ball on a sample in the ball milling process, enhances the diffusion by heat treatment, and finally prepares the high-temperature-resistant surface disordered core-shell structure nano material. Compared with the traditional high-temperature high-pressure hydrogenation method, the preparation method of the invention can not use hydrogen, thus having no flammable and explosive danger; the experimental conditions are easy to realize, the preparation period is short, and the batch production can be realized. In addition, the surface disordered nano material provided by the invention is prepared under the high-temperature condition, and has good high-temperature resistance.
Drawings
FIG. 1a shows the nano TiO raw material in example 12XRD pattern of (a);
FIG. 1b is an XRD pattern of a sample obtained after addition of a lithium-containing compound and ball milling and heat treatment in example 1.
Detailed Description
The invention provides a preparation method of a high-temperature-resistant surface disordered nano material, which comprises the following steps:
carrying out ball milling on the semiconductor nano material and a lithium-containing compound, and then carrying out heat treatment to obtain a surface disordered nano material;
the heat treatment temperature is 600-1500 ℃, and the heat treatment atmosphere is oxygen-containing atmosphere.
The invention prepares the high-temperature resistant surface disordered nano material by ball milling and subsequent heat treatment, catalyzes the reaction of the nano material and a lithium compound by controlling the ball milling condition and utilizing high energy provided by instantaneous impact of a grinding ball on a sample in the ball milling process, enhances the diffusion of lithium atoms to semiconductor nano particles by subsequent heat treatment, and extrudes each position or gap position of a semiconductor to obtain the high-temperature resistant surface disordered structure. Compared with the traditional high-temperature high-pressure hydrogenation method, the preparation method disclosed by the invention does not use hydrogen, has no flammable and explosive hazards, is easy to realize preparation conditions, is short in preparation period, and can realize batch production.
The present invention is not limited to the kind of the semiconductor nanomaterial, and the semiconductor nanomaterial known to those skilled in the art may be used. The semiconductor nano material is preferably one or more of titanium dioxide, zinc oxide, zirconium dioxide, barium titanate, strontium titanate and calcium titanate; more preferably titanium dioxide. The source of the nanomaterial is not particularly limited in the present invention, and the nanomaterial can be obtained as a general commercial product or according to a preparation method well known to those skilled in the art.
In the invention, the average particle size of the semiconductor nano material is preferably 3-100 nm, and more preferably 5-20 nm. In the above particle size range, the nano material with better surface disorder effect can be obtained, the microwave absorption performance of the nano material can reach the best, if the particle size is less than 3nm, the nano material is easy to be completely disordered, the core-shell structure material with surface disorder/internal order is difficult to obtain, and if the particle size is more than 100nm, the microwave absorption wave band of the obtained surface disorder nano material does not meet the existing requirement. For the nano material with the granularity of 3-100 nm, if the granularity is controlled to be 5-20 nm, the surface disordered core-shell structure material can be obtained more easily, and the photocatalysis and microwave absorption effects of the material are further improved obviously.
In the present invention, the lithium-containing compound is selected from one or more of lithium carbonate, lithium oxide, lithium hydroxide, lithium chloride, and lithium nitrate, and preferably lithium carbonate or lithium hydroxide.
The molar ratio of the semiconductor nano material to the lithium-containing compound is 1 (0.01-2), and preferably 1: (0.1 to 1).
The invention mixes the semiconductor nano material and the lithium-containing compound for ball milling, and the invention has no special limitation on the temperature and the gas environment of the ball milling. Under the condition of normal temperature, the air atmosphere can be used. In the present invention, the normal temperature is defined as 25 ± 5 ℃.
In the invention, the rotation speed of the ball milling is preferably 200-1000 r/min, and more preferably 400-800 r/min. The surface disorder material can be well obtained in the rotating speed range, if the rotating speed is lower than 200r/min, the surface disorder effect is not obvious, and if the rotating speed is higher than 1000r/min, excessive ball milling is easily caused. In the invention, the time for ball milling is preferably 2 to 12 hours, and more preferably 2 to 6 hours.
In the invention, the mass ratio of the ball materials subjected to ball milling is preferably (10-20) to 1, and is preferably (12-18) to 1.
In the invention, the volume ratio of the ball-milled grinding balls to the ball-milling tank is preferably 1/3-3/4, and more preferably 1/3-1/2.
In some embodiments, the shell of the ball milling tank for ball milling is made of stainless steel, and the lining of the ball milling tank and the milling balls are made of silicon nitride or zirconia.
The semiconductor nano material and the lithium-containing compound are subjected to heat treatment after ball milling, and in the invention, the heat treatment temperature is 600-1500 ℃, and more preferably 800-1200 ℃. The atmosphere of the heat treatment is oxygen-containing atmosphere. The oxygen-containing atmosphere is selected from oxygen, air, oxygen-argon mixed gas, oxygen-nitrogen mixed gas, oxygen-helium mixed gas, oxygen-neon mixed gas and mixed gas of the above gases. In the present invention, the gas is preferably a mixture of air and oxygen and argon.
The heat treatment time in the invention is 0.5-4 hours, preferably 1-3 hours.
Compared with the traditional high-temperature high-pressure hydrogenation method and the hydrogen atmosphere ball milling hydrogenation technology, the method utilizes the power of high-energy ball milling instantaneous grinding to promote the semiconductor nano material to react with a lithium-containing compound, lithium atoms occupy the semiconductor crystal lattice under the action of high-energy impact of grinding balls, and diffusion is further enhanced through heat treatment, so that the surface disordered nano material is obtained. Compared with high-temperature high-pressure hydrogenation treatment, the method can prepare the surface disordered nano-crystal under a mild pressure environment, and can process the nano-material on a large scale by increasing the capacity of the ball milling tank to prepare the surface disordered nano-material in batches. Compared with the method for preparing the surface disordered nano material by hydrogen atmosphere ball milling, the method does not use hydrogen and has no danger of flammability and explosiveness. The surface disordered nano material prepared by the invention has wide application prospect in the field of novel high-temperature-resistant microwave absorbing materials.
For further understanding of the present invention, the following examples are provided to illustrate the preparation method of the high temperature resistant surface disordered nanomaterial provided by the present invention, and the scope of the present invention is not limited by the following examples.
In the following examples, the nanomaterial materials are commercially available or obtained according to conventional preparation methods in the art, for example, the nanomaterial materials are prepared by a conventional hydrothermal method, the nanomaterial materials are prepared by a sol-gel method or a thermal oxidation method, and the nanomaterial materials are prepared by a hydrothermal method.
Example 1
1.1 preparation of samples
5g of nano titanium dioxide (TiO)2Average particle size of 10nm) and 0.5g of lithium carbonate are put into a 45m L ball milling tank, grinding balls accounting for one third of the capacity of the ball milling tank are added, the number ratio of the grinding balls to the grinding balls is 7: 18: 180, the mass ratio of the grinding balls to the grinding balls is 14: 1, the lining of the ball milling tank and the grinding balls are made of silicon nitride, the ball milling is carried out for 6 hours at the rotating speed of 600r/min, samples are taken out, the samples are moved into a quartz boat and sent into a tubular furnace, oxygen and argon mixed gas is introduced, the volume ratio of the oxygen and the argon is 1:2, the flow rate is 50m L/min.
1.2 testing of the samples
(1) Respectively carrying out XRD test on the primary sample and the sample obtained after ball milling heat treatment, and increasing the half-height width of a 25-degree diffraction peak of the sample from 0.73 degrees to 1.2 degrees after ball milling and heat treatment. Since the 10nm particle size could not be further reduced by both the ball milling and the heat treatment, it was found that the increase in the half height width of XRD was caused by disorder of the crystal grains. Referring to FIGS. 1a and 1b, FIG. 1a shows the nano TiO as the raw material in example 12XRD pattern of (a); FIG. 1b is an XRD pattern of a sample obtained after addition of a lithium-containing compound and ball milling and heat treatment in example 1.
(2) Respectively carrying out electromagnetic property tests on the primary sample and the sample obtained after ball milling heat treatment, substituting the measured dielectric constant into a reflection loss R L formula to obtain the sample with poor microwave reflection loss absorption effect, the peak value is about-2 dB, after ball milling and heat treatment, the sample generates excellent microwave absorption performance, the microwave reflection loss R L peak value reaches-26 dB and is positioned at 16.5GHz, and the microwave absorption efficiency peak value is-10 dB and the bandwidth is 7GHz (11-18 GHz).
Example 2
2.1 preparation of samples
Putting 5g of nano zinc oxide (ZnO, the average particle size is 15nm) and 0.5g of lithium hydroxide into a 45m L ball milling tank, adding grinding balls accounting for one third of the capacity of the ball milling tank, wherein the number ratio of the grinding balls is 10mm balls to 5mm balls to 3mm balls is 7: 18: 180, the mass ratio of ball materials is 14: 1, the lining of the ball milling tank and the grinding balls are made of silicon nitride, carrying out ball milling at the rotating speed of 600r/min for 6 hours, taking out a sample, moving the sample into a quartz boat, feeding the quartz boat into a tubular furnace, introducing oxygen-argon mixed gas, wherein the oxygen-argon ratio is 1:4, the flow rate is 50m L/min, the heat treatment temperature is 800 ℃, the heat treatment time is 2 hours, and naturally cooling and then taking out the sample.
2.2 testing of the samples
(1) XRD tests are respectively carried out on the primary sample and the sample obtained after ball milling heat treatment, and the results show that the 002 diffraction peak of the sample is increased from 0.6 degree to 1 degree after ball milling and heat treatment.
(2) The primary sample and the sample obtained after the ball milling heat treatment are respectively subjected to the electromagnetic property test of the 1-18GHz frequency band according to the method of the embodiment 1, the dielectric constant data is substituted into the reflection loss R L formula, and the microwave reflection loss R L peak value of the sample obtained through calculation reaches-22 dB and is located at the 16.0GHz position.
Example 3
3.1 preparation of samples
Taking 10g of nano barium titanate (BaTiO)3Average grain diameter of 10nm) and 0.5g of lithium carbonate are put into a 80m L ball milling tank, grinding balls accounting for one third of the capacity of the ball milling tank are added, the ratio of the grinding balls to the grinding balls is 20mm balls to 15mm balls to 10mm balls to 5mm balls, the ratio of the grinding balls to the grinding balls is 1: 2: 5: 50, the mass ratio of the grinding balls to the grinding balls is 20: 1, the lining and the grinding balls of the ball milling tank are made of silicon nitride, the ball milling tank is ball milled for 6 hours at the rotating speed of 800r/min, the lithium carbonateAnd (3) taking out the sample, moving the sample into a quartz boat, sending the quartz boat into a tube furnace, introducing dry air at the flow rate of 100m L/min, at the heat treatment temperature of 900 ℃, for 2 hours, naturally cooling, and taking out the sample.
3.2 testing of the samples
(1) XRD tests are respectively carried out on the primary sample and the sample obtained after ball milling heat treatment, and the results show that the 110 diffraction peak of the sample is increased from 0.5 degree to 0.8 degree after ball milling and heat treatment.
(2) The primary sample and the sample obtained after the ball milling heat treatment are respectively subjected to the electromagnetic property test of the 1-18GHz frequency band according to the method in the embodiment 1, the dielectric constant data is substituted into the reflection loss R L formula, and the microwave reflection loss R L peak value of the sample obtained through calculation reaches-25 dB and is located at the 16GHz position.
Example 4
4.1 preparation of samples
5g of nano zinc titanate (ZnTiO) is taken320nm in average particle size) and 0.2g of lithium hydroxide are put into a 45m L ball milling pot, grinding balls accounting for one third of the capacity of the ball milling pot are added, the number ratio of the grinding balls to the grinding balls is 7: 18: 180, the mass ratio of the grinding balls to the grinding balls is 14: 1, the lining of the ball milling pot and the grinding balls are made of silicon nitride, the ball milling is carried out for 6 hours at the rotating speed of 600r/min, a sample is taken out, the sample is moved into a quartz boat and is sent into a tubular furnace, oxygen and argon mixed gas is introduced, the volume ratio of the oxygen and the argon is 1:4, the flow is 50m L/min, the heat treatment temperature is 800 ℃, the heat treatment time is 2.
4.2 testing of the samples
(1) XRD tests are respectively carried out on the primary sample and the sample obtained after ball milling heat treatment, and the results show that the 311 diffraction peak of the sample is increased from 0.5 degree to 0.8 degree after ball milling and heat treatment.
(2) And (2) respectively carrying out electromagnetic property tests of 1-18GHz frequency bands on the primary sample and the sample obtained after ball milling heat treatment according to the method in the embodiment 1, substituting the dielectric constant data into a reflection loss R L formula, and calculating that the peak value of the microwave reflection loss R L of the obtained sample reaches-24 dB.
Comparative example 1
L1.1.1 preparation of sample
Putting 5g of nano titanium dioxide (TiO2, with the average particle size of 10nm) into a 45m L ball milling tank, adding grinding balls accounting for one third of the capacity of the ball milling tank, wherein the number ratio of the grinding balls to the grinding balls is 10mm to 5mm to 3mm is 7 to 18 to 180, the mass ratio of ball materials is 14 to 1, the lining of the ball milling tank and the grinding balls are made of silicon nitride, carrying out ball milling at the rotating speed of 600r/min for 6 hours, taking out a sample, moving the sample into a quartz boat, feeding the quartz boat into a tubular furnace, introducing oxygen-argon mixed gas, wherein the volume ratio of oxygen to argon is 1 to 2, the flow rate is 50m L/min, the heat treatment temperature is 800 ℃, the heat treatment time is 2 hours, naturally cooling, and taking out the sample.
L1.2.2 testing of samples
Compared with the primary sample, the microwave absorption performance of the ball milling and heat treatment sample is slightly improved, but the peak value is not more than-3 dB, the microwave absorption performance is 16GHz, the absorption peak is narrow, and the half-height width is not more than 1 GHz
Comparative example 2
L2.1.1 preparation of sample
Putting 5g of nano titanium dioxide (TiO2, with the average particle size of 10nm) and 0.5g of lithium carbonate into a 45m L ball milling tank, adding grinding balls accounting for one third of the capacity of the ball milling tank, wherein the number ratio of the grinding balls to the grinding balls is 10mm to 5mm to 3mm is 7 to 18 to 180, the mass ratio of ball materials is 14 to 1, the lining and the grinding balls of the ball milling tank are made of silicon nitride, carrying out ball milling at the rotating speed of 600r/min for 6 hours, taking out a sample, moving the sample into a quartz boat, feeding the quartz boat into a tubular furnace, introducing oxygen-argon mixed gas, wherein the volume ratio of oxygen to argon is 1 to 2, the flow rate is 50m L/min, the heat treatment temperature is 400 ℃, the heat treatment time is 2 hours, and naturally cooling and then taking out the.
L2.2.2, the sample obtained after ball milling heat treatment is subjected to electromagnetic property test, and the microwave reflection loss spectrogram of the sample is obtained by substituting the measured dielectric constant into a reflection loss R L formula.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (8)
1. A preparation method of a high-temperature-resistant surface disordered nano material is characterized by comprising the following steps:
carrying out ball milling on the semiconductor nano material and a lithium-containing compound, and then carrying out heat treatment to obtain a surface disordered nano material;
the heat treatment temperature is 800-1200 ℃, and the heat treatment atmosphere is oxygen-containing atmosphere; the oxygen-containing atmosphere is selected from oxygen, air, oxygen-argon mixed gas, oxygen-nitrogen mixed gas, oxygen-helium mixed gas, oxygen-neon mixed gas and mixed gas of the oxygen-argon mixed gas and the oxygen-neon mixed gas;
the preparation method does not use hydrogen.
2. The method according to claim 1, wherein the lithium-containing compound is one or more selected from the group consisting of lithium carbonate, lithium oxide, lithium hydroxide, lithium chloride, and lithium nitrate.
3. The preparation method according to claim 1, wherein the semiconductor nanomaterial is selected from one or more of titanium dioxide, zinc oxide, zirconium dioxide, barium titanate, strontium titanate, and calcium titanate; the average particle size of the semiconductor nano material is 5-100 nm.
4. The preparation method according to claim 1, wherein the molar ratio of the semiconductor nano material to the lithium-containing compound is 1 (0.01-2).
5. The preparation method of claim 1, wherein the rotation speed of the ball mill is 200-1000 r/min, and the time is 2-12 hours.
6. The preparation method of claim 1, wherein the rotation speed of the ball mill is 400-800 r/min, and the time is 2-6 hours.
7. The preparation method of claim 1, wherein the ball-milled ball material mass ratio is (10-20): 1; the volume ratio of the ball-milled grinding balls to the ball-milling tank is 1/3-3/4.
8. The method according to claim 1, wherein the heat treatment is carried out for 0.5 to 4 hours.
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