CN102167980B - Inorganic liquid crystal based on anatase type TiO2 nano rod and application thereof - Google Patents
Inorganic liquid crystal based on anatase type TiO2 nano rod and application thereof Download PDFInfo
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- CN102167980B CN102167980B CN 201110056031 CN201110056031A CN102167980B CN 102167980 B CN102167980 B CN 102167980B CN 201110056031 CN201110056031 CN 201110056031 CN 201110056031 A CN201110056031 A CN 201110056031A CN 102167980 B CN102167980 B CN 102167980B
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Abstract
The invention discloses an inorganic liquid crystal based on an anatase type TiO2 nano rod and application thereof. The inorganic liquid crystal has a concentration of 0.1-0.3M and consists of an anatase type TiO2 nano rod which has a diameter of 1-2nm and a length of 20-40nm and an oleic acid solvent. The phase of the liquid crystal with a concentration of 0.1-0.16M is a nematic phase. The phase of the liquid crystal with a concentration of 0.17-0.24M is a spherocrystal phase. The phase of the liquid crystal with a concentration of 0.25-0.3M is a smectic phase. The inorganic liquid crystal based on an anatase type TiO2 nano rod is used for making shift/pressure sensors and temperature sensors. The range of the inorganic liquid crystal is broadened to include the anatase type TiO2 nano rod for the first time. The liquid crystal not only can be applied in the field of traditional liquid crystal displays, but also can be applied in the fields of shift/pressure sensors and temperature sensors.
Description
Technical field
The present invention relates to the Inorganic Liquid Crystals of semiconductor nano, relate in particular to a kind of based on Detitanium-ore-type TiO
2Inorganic Liquid Crystals of nanometer rod and uses thereof.
Background technology
Liquid crystal material is a kind of very important photoelectric functional material of modern society, and find the liquid crystal of courage Zi alcohol benzoic ether and acetic ester since F.Reinitzer since, scientist has had been found that nearly 100,000 kinds of organic lcd materials.Along with the development of science and technology, also more and more higher to the requirement of liquid crystal material, organic lcd material commonly used has shown limitation gradually.Compare with organic lcd, Inorganic Liquid Crystals also has the characteristic of electron rich except having strong anisotropy and birefringent character, and this makes it that character such as special optics, electricity and magnetics be arranged.Nineteen twenty-five, Germany scientist Zocher is at V
2O
5In found first the liquid crystal behavior of inorganic nanoparticles colloidal sol up to now, to be only had V by the Inorganic Liquid Crystals material of Complete Characterization
2O
5, gibbsite (Al (OH)
3, tens of kinds of β-FeOOH etc.
Along with going deep into of research, higher than quantum dot, this just makes its surface form the transfer rate of more highdensity surface reaction activity point and higher interfacial charge current carrier due to the specific surface area of nanometer rod; Electronics can be along the long axis direction transmission of monodimension nano stick in nanometer rod, the remarkable delocalization effect of consequent current carrier in nanometer rod can reduce the recombination probability in electronics, hole, thereby part makes up the generation of surface trap attitude with excellent characteristics such as the more efficient carrier separation efficient of assurance, so concentrate on semiconductor nanorods Inorganic Liquid Crystals direction for the research of Inorganic Liquid Crystals material.But up to the present, scientists has only been found CdSe, SnO
2, ZnO, CdTe and rutile TiO
2The Inorganic Liquid Crystals of nanometer rod.The present invention is extended to Detitanium-ore-type TiO with the scope of Inorganic Liquid Crystals first
2Nanometer rod.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, provide a kind of based on Detitanium-ore-type TiO
2Inorganic Liquid Crystals of nanometer rod and uses thereof.
Based on Detitanium-ore-type TiO
2The Inorganic Liquid Crystals of nanometer rod is to be that 1～2 nm, length are the Detitanium-ore-type TiO of 20～40 nm by diameter
2Nanometer rod and oleic acid solvent consist of concentration: the Inorganic Liquid Crystals of 0. 1～0.3M.Described concentration is that the mesomorphic phase of 0.1～0.16M is nematic phase; Concentration is that the mesomorphic phase of 0.17～0.24M is the spherocrystal phase; Concentration is that the mesomorphic phase of 0.25～0.3M is smectic phase.
Based on Detitanium-ore-type TiO
2The Inorganic Liquid Crystals of nanometer rod is used for making displacement/pressure transmitter and temperature sensor.
The beneficial effect that the present invention compared with prior art has: based on Detitanium-ore-type TiO
2The Inorganic Liquid Crystals of nanometer rod cleans more, cheapness, and environmentally safe.Based on based on Detitanium-ore-type TiO
2The Inorganic Liquid Crystals of nanometer rod need not to carry out surface modification treatment for what directly synthesize.Detitanium-ore-type TiO
2The spherulite size that nanometer rod forms is convenient to screen in actual applications and separate about 20～50 μ m.TiO
2The periphery of the spherocrystal that nanometer rod forms is the TiO by lower concentration
2The thread formation mutually that the nanometer rod self-assembly forms, thereby have great specific surface area, can adsorb a large amount of toxic substances and organism.Detitanium-ore-type TiO
2A kind of splendid photocatalyst material, Detitanium-ore-type TiO
2The structure of the spherocrystal that nanometer rod forms can improve Detitanium-ore-type TiO widely
2Light-catalysed performance.Therefore, we can think, Detitanium-ore-type TiO
2The spherocrystal that nanometer rod forms is having broad prospects as the research in the high-efficiency adsorbent of the carrier of extraordinary enzyme, toxic substance and novel fields such as high-efficiency photocatalysis material with in using.
Description of drawings
Fig. 1 adopts the microemulsion method, utilizes aminolysis technique, the TiO that directly prepares
2The TEM picture of nanometer rod;
Fig. 2 adopts the microemulsion method, utilizes aminolysis technique, the TiO that directly prepares
2The XRD figure spectrum of nanometer rod;
Fig. 3 is that concentration is the Detitanium-ore-type TiO of 0.120M
2The polarisation photo of the Inorganic Liquid Crystals of nanometer rod and oleic acid;
Fig. 4 is that concentration is the Detitanium-ore-type TiO of 0.189M
2The polarisation photo of the Inorganic Liquid Crystals of nanometer rod and oleic acid;
Fig. 5 is that concentration is the Detitanium-ore-type TiO of 0.231M
2The polarisation photo of the Inorganic Liquid Crystals of nanometer rod and oleic acid;
Fig. 6 is that concentration is the Detitanium-ore-type TiO of 0.231M
2The schematic diagram of the polarisation photo of the spherocrystal of nanometer rod and oleic acid and negative spherocrystal thereof and black cross delustring;
Fig. 7 is that concentration is the Detitanium-ore-type TiO of 0.231M
2The spherocrystal of nanometer rod and oleic acid should be used as the polarisation photo of displacement, pressure transmitter;
Fig. 8 is that concentration is the Detitanium-ore-type TiO of 0.231M
2The spherocrystal of nanometer and oleic acid should be as the polarisation photo of temperature sensor;
Fig. 9 is that concentration is the Detitanium-ore-type TiO of 0.262M
2The polarisation photo of the Inorganic Liquid Crystals of nanometer rod and oleic acid;
Figure 10 is that concentration is the Detitanium-ore-type TiO of 0.284M
2The polarisation photo of the Inorganic Liquid Crystals of nanometer rod and oleic acid.
Embodiment
Case study on implementation 1:
Under room temperature, oleic acid (1.6mL, 5 mmol) is added in vaccenic acid (6 mL), stir.Then temperature is added to 80 ℃, kept 1 hour in argon atmospher, remove water and oxygen remaining in solution.Tetrabutyl titanate (0.24 mL, 1 mmol) is injected into above-mentioned mixing solutions, continues insulation 20 minutes under 80 ℃.In this process, can find that solution becomes light yellowly by colourless at leisure, shows the formation that the oleic acid titanium is arranged in this process.This reaction system is heated to 260 ℃ to be kept 10 minutes.Then oleyl amine (0.48mL, 1.5mmol) is injected into this reaction system fast, inspires " aminolysis " reaction, be accompanied by strong stirring, insulation is 90 minutes under the condition of 260 ℃.Reaction finishes, and preserving the theoretical concentration that synthesizes is the Detitanium-ore-type TiO of 0.120M
2The Inorganic Liquid Crystals of nanometer and oleic acid.Adopting saturating, the anti-dual-purpose polarizing microscope of NIKON ECLIPSE E600POL, is that 20 ℃, enlargement ratio are that under 200 state, observation concentration is the Detitanium-ore-type TiO of 0.120M adding sharp colorimetric compensation device, experimental temperature
2The Inorganic Liquid Crystals of nanometer rod and oleic acid.(as shown in Figure 3).
Toluene (6 mL) and acetone (3 mL) are joined respectively the Detitanium-ore-type TiO that concentration is 0.120M
2In the Inorganic Liquid Crystals of nanometer rod and oleic acid, with the rotating speed of 5000 rev/mins centrifugal 30 minutes.After centrifugal end, have yellow TiO
2Precipitation, remove supernatant liquor, non-polar solvent n-hexane dissolution precipitation with 10mL, after ultrasonic 0.5h processes, get a treatment solution and drop on the copper mesh that is covered with the carbon supporting film, adopt at last JEM-1200 transmission electron microscope (acceleration voltage 80kV) to describe the microscopic appearance (as shown in Figure 1) of sample.The crystal formation of sample adopts Philip PW1050 powder diffractometer to analyze, and the operation wavelength of diffractometer is CuK
α, take measurement of an angle 20 °～80 ° (as shown in Figure 2).It is almost consistent and possess the Detitanium-ore-type TiO of self-assembly characteristic that experiment has synthesized size homogeneous, diameter
2Nanometer rod (diameter 1.2 nm, length 20～32nm).
Case study on implementation 2:
Under room temperature, oleic acid (3.2mL, 10 mmol) is added in vaccenic acid (6 mL), stir.Then temperature is added to 80 ℃, kept 1 hour in argon atmospher, remove water and oxygen remaining in solution.Tetrabutyl titanate (0.48 mL, 2mmol) is injected into above-mentioned mixing solutions, continues insulation 20 minutes under 80 ℃.In this process, can find that solution becomes light yellowly by colourless at leisure, shows the formation that the oleic acid titanium is arranged in this process.This reaction system is heated to 260 ℃ to be kept 10 minutes.Then oleyl amine (0.96mL, 3mmol) is injected into this reaction system fast, inspires " aminolysis " reaction, be accompanied by strong stirring, insulation is 90 minutes under the condition of 260 ℃.Reaction finishes, and preserving the theoretical concentration that synthesizes is the Detitanium-ore-type TiO of 0.189M
2The Inorganic Liquid Crystals of nanometer and oleic acid.Adopting saturating, the anti-dual-purpose polarizing microscope of NIKON ECLIPSE E600POL, is that 20 ℃, enlargement ratio are that under 200 state, observation concentration is the Detitanium-ore-type TiO of 0.189M adding sharp colorimetric compensation device, experimental temperature
2The Inorganic Liquid Crystals of nanometer rod and oleic acid.(as shown in Figure 4).
Toluene (12mL) and acetone (6 mL) are joined respectively the Detitanium-ore-type TiO that concentration is 0.189M
2In the Inorganic Liquid Crystals of nanometer rod and oleic acid, with the rotating speed of 5000 rev/mins centrifugal 30 minutes.After centrifugal end, have yellow TiO
2Precipitation, remove supernatant liquor, with the non-polar solvent n-hexane dissolution precipitation of 10mL, after ultrasonic 0.5h processes, get a treatment solution and drop on the copper mesh that is covered with the carbon supporting film, adopt at last JEM-1200 transmission electron microscope (acceleration voltage 80kV) to describe the microscopic appearance of sample.The crystal formation of sample adopts Philip PW1050 powder diffractometer to analyze, and the operation wavelength of diffractometer is CuK
α, take measurement of an angle 20 °～80 °.It is almost consistent and possess the Detitanium-ore-type TiO of self-assembly characteristic that experiment has synthesized size homogeneous, diameter
2Nanometer rod (diameter 1.4nm, length 22～35nm).
Case study on implementation 3:
Under room temperature, oleic acid (4.8mL, 15 mmol) is added in vaccenic acid (6 mL), stir.Then temperature is added to 80 ℃, kept 1 hour in argon atmospher, remove water and oxygen remaining in solution.Tetrabutyl titanate (0.72 mL, 3mmol) is injected into above-mentioned mixing solutions, continues insulation 20 minutes under 80 ℃.In this process, can find that solution becomes light yellowly by colourless at leisure, shows the formation that the oleic acid titanium is arranged in this process.This reaction system is heated to 260 ℃ to be kept 10 minutes.Then oleyl amine (1.28mL, 4.5mmol) is injected into this reaction system fast, inspires " aminolysis " reaction, be accompanied by strong stirring, insulation is 90 minutes under the condition of 260 ℃.Reaction finishes, and preserving the theoretical concentration that synthesizes is the Detitanium-ore-type TiO of 0.231M
2The Inorganic Liquid Crystals of nanometer and oleic acid.Adopting saturating, the anti-dual-purpose polarizing microscope of NIKON ECLIPSE E600POL, is that 20 ℃, enlargement ratio are that under 200 state, observation concentration is the Detitanium-ore-type TiO of 0.231M adding sharp colorimetric compensation device, experimental temperature
2The Inorganic Liquid Crystals of nanometer rod and oleic acid.(as Fig. 5, shown in Figure 6).
Toluene (18 mL) and acetone (9 mL) are joined respectively the Detitanium-ore-type TiO that concentration is 0.231M
2In the Inorganic Liquid Crystals of nanometer rod and oleic acid, with the rotating speed of 5000 rev/mins centrifugal 30 minutes.After centrifugal end, have yellow TiO
2Precipitation, remove supernatant liquor, with the non-polar solvent n-hexane dissolution precipitation of 10mL, after ultrasonic 0.5h processes, get a treatment solution and drop on the copper mesh that is covered with the carbon supporting film, adopt at last JEM-1200 transmission electron microscope (acceleration voltage 80kV) to describe the microscopic appearance of sample.The crystal formation of sample adopts Philip PW1050 powder diffractometer to analyze, and the operation wavelength of diffractometer is CuK
α, take measurement of an angle 20 ° ~ 80 °.
Utilizing two diameters is that the glass fibre of 125 μ m is controlled the distance between the slide glass of two of up and down, observation have, concentration under the two states of supreme slide glass is the Detitanium-ore-type TiO of 0.231M
2The spherocrystal of nanometer rod and oleic acid; Under the condition of not controlling the distance between the slide glass of two of up and down, by upper slide glass being applied respectively the pressure of 2N, 50N, observation concentration is the Detitanium-ore-type TiO of 0.231M
2The spherocrystal of nanometer rod and oleic acid (as shown in Figure 7).
Adopt NIKON saturating, the anti-dual-purpose polarizing microscope of ECLIPSE E600POL (being with hot platform), be under the condition of 200 state adding sharp colorimetric compensation device, enlargement ratio, with 20 ℃ as starting temperature, with temperature rise rate and the rate of temperature fall of 1 ℃/min, observation concentration under different temperature condition is the Detitanium-ore-type TiO of 0.231M
2The spherocrystal of nanometer rod and oleic acid (as shown in Figure 8).
Case study on implementation 4:
Under room temperature, oleic acid (6.4mL, 20 mmol) is added in vaccenic acid (6 mL), stir.Then temperature is added to 80 ℃, kept 1 hour in argon atmospher, remove water and oxygen remaining in solution.Tetrabutyl titanate (0.96 mL, 4mmol) is injected into above-mentioned mixing solutions, continues insulation 20 minutes under 80 ℃.In this process, can find that solution becomes light yellowly by colourless at leisure, shows the formation that the oleic acid titanium is arranged in this process.This reaction system is heated to 260 ℃ to be kept 10 minutes.Then oleyl amine (1.6mL, 6mmol) is injected into this reaction system fast, inspires " aminolysis " reaction, be accompanied by strong stirring, insulation is 90 minutes under the condition of 260 ℃.Reaction finishes, and preserving the theoretical concentration that synthesizes is the Detitanium-ore-type TiO of 0.262M
2The Inorganic Liquid Crystals of nanometer and oleic acid.Adopting saturating, the anti-dual-purpose polarizing microscope of NIKON ECLIPSE E600POL, is that 20 ℃, enlargement ratio are that under 200 state, observation concentration is the Detitanium-ore-type TiO of 0.262M adding sharp colorimetric compensation device, experimental temperature
2The Inorganic Liquid Crystals of nanometer rod and oleic acid.(as shown in Figure 9).
Toluene (24 mL) and acetone (12 mL) are joined respectively the Detitanium-ore-type TiO that concentration is 0.262M
2In the Inorganic Liquid Crystals of nanometer rod and oleic acid, with the rotating speed of 5000 rev/mins centrifugal 30 minutes.After centrifugal end, have yellow TiO
2Precipitation, remove supernatant liquor, with the non-polar solvent n-hexane dissolution precipitation of 10mL, after ultrasonic 0.5h processes, get a treatment solution and drop on the copper mesh that is covered with the carbon supporting film, adopt at last JEM-1200 transmission electron microscope (acceleration voltage 80kV) to describe the microscopic appearance of sample.The crystal formation of sample adopts Philip PW1050 powder diffractometer to analyze, and the operation wavelength of diffractometer is CuK
α, take measurement of an angle 20 °～80 °.It is almost consistent and possess the Detitanium-ore-type TiO of self-assembly characteristic that experiment has synthesized size homogeneous, diameter
2Nanometer rod (diameter 1.7nm, length 26～37nm).
Case study on implementation 5:
Under room temperature, oleic acid (8mL, 25 mmol) is added in vaccenic acid (6 mL), stir.Then temperature is added to 80 ℃, kept 1 hour in argon atmospher, remove water and oxygen remaining in solution.Tetrabutyl titanate (1.2 mL, 5mmol) is injected into above-mentioned mixing solutions, continues insulation 20 minutes under 80 ℃.In this process, can find that solution becomes light yellowly by colourless at leisure, shows the formation that the oleic acid titanium is arranged in this process.This reaction system is heated to 260 ℃ to be kept 10 minutes.Then oleyl amine (2.08mL, 7.5mmol) is injected into this reaction system fast, inspires " aminolysis " reaction, be accompanied by strong stirring, insulation is 90 minutes under the condition of 260 ℃.Reaction finishes, and preserving the theoretical concentration that synthesizes is the Detitanium-ore-type TiO of 0.284M
2The Inorganic Liquid Crystals of nanometer and oleic acid.Adopting saturating, the anti-dual-purpose polarizing microscope of NIKON ECLIPSE E600POL, is that 20 ℃, enlargement ratio are that under 200 state, observation concentration is the Detitanium-ore-type TiO of 0.284M adding sharp colorimetric compensation device, experimental temperature
2The Inorganic Liquid Crystals of nanometer rod and oleic acid.(as shown in figure 10).
Toluene (30 mL) and acetone (15 mL) are joined respectively the Detitanium-ore-type TiO that concentration is 0.284M
2In the Inorganic Liquid Crystals of nanometer rod and oleic acid, with the rotating speed of 5000 rev/mins centrifugal 30 minutes.After centrifugal end, have yellow TiO
2Precipitation, remove supernatant liquor, with the non-polar solvent n-hexane dissolution precipitation of 10mL, after ultrasonic 0.5h processes, get a treatment solution and drop on the copper mesh that is covered with the carbon supporting film, adopt at last JEM-1200 transmission electron microscope (acceleration voltage 80kV) to describe the microscopic appearance of sample.The crystal formation of sample adopts Philip PW1050 powder diffractometer to analyze, and the operation wavelength of diffractometer is CuK
α, take measurement of an angle 20 °～80 °.It is almost consistent and possess the Detitanium-ore-type TiO of self-assembly characteristic that experiment has synthesized size homogeneous, diameter
2Nanometer rod (diameter 1.9nm, length 28～40nm).
Claims (2)
1. one kind based on Detitanium-ore-type TiO
2The Inorganic Liquid Crystals of nanometer rod is characterized in that it is is that 1～2 nm, length are the Detitanium-ore-type TiO of 20～40 nm by diameter
2Nanometer rod and oleic acid solvent consist of concentration: the Inorganic Liquid Crystals of 0.17～0.24M, mesomorphic phase are the spherocrystal phase.
2. one kind according to claim 1 based on Detitanium-ore-type TiO
2The purposes of the Inorganic Liquid Crystals of nanometer rod is characterized in that for making displacement/pressure transmitter and temperature sensor.
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| CN107815320A (en) * | 2017-10-22 | 2018-03-20 | 清华-伯克利深圳学院筹备办公室 | A kind of New Liquid Crystal material and preparation method thereof and optical modulator |
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Non-Patent Citations (6)
| Title |
|---|
| 叶波.锐钛矿相单分散TiO2纳米棒的合成及其自组装特性研究.《中国优秀硕士学位论文全文数据库工程科技I辑》.2010, |
| 崔叔茂等.无机液晶的研究进展.《材料导报》.2007,第21卷(第5期),10-13. |
| 张洁等.无机溶致液晶研究进展.《化学通报》.2004,(第7期),487-491. |
| 无机液晶的研究进展;崔叔茂等;《材料导报》;20070531;第21卷(第5期);10-13 * |
| 无机溶致液晶研究进展;张洁等;《化学通报》;20040731(第7期);487-491 * |
| 锐钛矿相单分散TiO2纳米棒的合成及其自组装特性研究;叶波;《中国优秀硕士学位论文全文数据库工程科技I辑》;20100815;第2-4章 * |
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