CN110849846A - Method and system for detecting concentration of gaseous compound based on polymer dispersed liquid crystal - Google Patents
Method and system for detecting concentration of gaseous compound based on polymer dispersed liquid crystal Download PDFInfo
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Abstract
The invention discloses a method and a system for detecting the concentration of a gaseous compound. The method comprises the following steps: providing a light source; exposing a detection unit to a gaseous compound to be detected and irradiating the detection unit by a light source, wherein the detection unit comprises a transparent substrate and a polymer dispersed liquid crystal film arranged on the transparent substrate, and the polymer dispersed liquid crystal film comprises a polymer and a liquid crystal material dispersed in the polymer; testing the optical performance of the detection unit; and collecting data for analysis, and converting the optical property of the detection unit into the concentration of the gaseous compound according to the corresponding relationship between the optical property of the detection unit and the concentration of the gaseous compound, which is measured in advance. The invention can realize the rapid real-time and accurate detection of the concentration of the gaseous compound by using the detection unit containing the polymer dispersed liquid crystal film, and simultaneously improve the detection reliability.
Description
Technical Field
The invention relates to a method for detecting the concentration of a gaseous compound, in particular to an optical detection method and a detection system based on a polymer dispersed liquid crystal film.
Background
Most organic gases have high volatility, toxicity and flammability, are seriously harmful to organisms exposed to the organic gases, and are more likely to cause serious pollution to the ecological environment. Today, the detection of harmful gases is of paramount social importance in the world facing severe industrial, atmospheric and environmental pollution. The existing organic gas measuring method is generally used for detecting the existence of harmful gas, but the real-time accurate detection of gas concentration still has problems, a sample to be detected needs to be sent to an analysis laboratory or a detection center, and a complex instrument is used for further detection, so that the detection cost is increased, and meanwhile, the data delay and inaccuracy caused by transportation are caused.
The liquid crystal may undergo some changes in alignment to external stimuli (e.g., electric field, temperature, chemicals, etc.), thereby changing optical characteristics. The response of the liquid crystal to these external stimuli can be used to produce corresponding sensors. The liquid crystal/polyvinylpyrrolidone composite fiber is prepared by electrostatic spinning technology such as Catherineg. Reyes, etc. and is used for detecting toluene gas. However, as the polyvinylpyrrolidone used as the skin layer of the composite fiber is a water-soluble polymer, the sensitivity of the composite fiber to humidity is increased, and the detection result is easily influenced by the environment. The patent CN103018174B uses the principle that when a liquid crystal composite material containing cholesteric liquid crystal and conductive material meets organic gas, the color and resistance change simultaneously to detect the existence of the organic gas and its concentration. The patent CN105223138B uses cholesteric liquid crystal coated on a transparent substrate with an alignment layer, and the detection is achieved by utilizing the principle that the pitch of cholesteric liquid crystal changes under different gases and concentrations, thereby affecting the spectrum of reflected light. However, in these patents, the cholesteric liquid crystal as the detection unit is in a flowing state and is easily affected by external vibration, thereby causing uncertainty and inaccuracy of detection.
Therefore, it is desirable to provide a liquid crystal-based detection method that is less affected by the environment and has reliable test results. Meanwhile, the detection method is small and portable, and can quickly, sensitively and real-timely detect the gaseous compound and the concentration thereof.
Disclosure of Invention
To meet the above need, the present invention provides a method for detecting the concentration of a gaseous compound, the method comprising: providing a light source; exposing a detection unit to a gaseous compound to be detected and irradiating the detection unit by a light source, wherein the detection unit comprises a transparent substrate and a polymer dispersed liquid crystal film arranged on the transparent substrate, and the polymer dispersed liquid crystal film comprises a polymer and a liquid crystal material dispersed in the polymer; testing the optical performance of the detection unit; and collecting data for analysis, and converting the change of the optical property of the detection unit into the concentration of the gaseous compound according to the predicted correspondence between the optical property of the detection unit and the concentration of the gaseous compound. In a preferred embodiment, the gaseous compound is a volatile organic compound. In some embodiments, the liquid crystal material comprises at least one nematic liquid crystal.
In some embodiments, the optical properties of the detection cell are mutated above and below a characteristic concentration of the gaseous compound. In some embodiments, the characteristic concentration of the gaseous compound varies with the composition and proportion of the liquid crystal material in the polymer dispersed liquid crystal film. In other embodiments, the optical properties of the detection cell are linear with respect to the concentration of the gaseous compound.
In a preferred embodiment, the optical property is the transmitted light intensity of the light emitted by the light source through the detection cell. In a preferred embodiment, the transmitted light includes direct transmitted light and scattered transmitted light.
In some embodiments, the detection unit comprises a plurality of different polymer-dispersed liquid crystal films laid on the transparent substrate, the plurality of different polymer-dispersed liquid crystal films producing different changes in optical properties for different concentrations of the gaseous compound to be detected.
Another aspect of the invention provides a system for detecting a concentration of a gaseous compound, the system comprising: a light source device; a detection cell device exposed to the gaseous compound and illuminated by the light source device; and data collection and analysis unit means for collecting optical detection signals passing through the detection unit means and converting the optical detection signals into concentration information of the gaseous compound.
The invention discloses a method for detecting a gaseous compound, which is characterized in that a detection unit containing a polymer dispersed liquid crystal film is used for detecting the concentration of the gaseous compound, and a liquid crystal material serving as a detection element is wrapped in a polymer, so that the detection result is slightly influenced by the environment, and the detection reliability is improved. Meanwhile, the detection unit is small and portable, can realize quick real-time and accurate detection, and has wider application range.
Drawings
The invention may be better understood by reference to the following description of embodiments of the invention taken in conjunction with the accompanying drawings, in which:
fig. 1 is a schematic structural diagram of a detection unit disclosed by the invention.
FIG. 2 is a schematic diagram of the working principle of liquid crystal droplets in a polymer dispersed liquid crystal film of the present invention changing their conformation with a gaseous compound.
Fig. 3 is a schematic structural diagram of the detection device for the concentration of a gaseous compound disclosed in the present invention.
Fig. 4 is an optical performance/concentration curve tested according to an embodiment of the invention.
Fig. 5 is an optical performance/concentration curve tested according to an embodiment of the invention.
Fig. 6 is an optical performance/concentration curve tested according to an embodiment of the invention.
Fig. 7 is an optical performance/concentration curve tested according to an embodiment of the invention.
Fig. 8 is an optical performance/concentration curve tested according to an embodiment of the invention.
Fig. 9 is an optical performance/concentration curve tested according to an embodiment of the invention.
Detailed Description
In the following description, for purposes of explanation, numerous specific details are set forth in order to provide a thorough understanding of the present invention, however, it will be apparent to those skilled in the art that the present invention may be practiced without these specific details. In other instances, well-known structures and devices are shown in block diagram form. In this regard, the illustrated example embodiments are provided for purposes of illustration only and are not intended to be limiting of the invention. Therefore, it is intended that the scope of the invention be limited not by this detailed description, but rather by the claims appended hereto.
The present invention provides a method for detecting the concentration of gaseous compounds, including all gaseous compounds that interact with liquid crystal materials to cause liquid crystal molecules to respond and thereby produce a change in optical properties, particularly volatile gaseous organic compounds such as acetone, ethanol, toluene, and the like. Here, the gaseous compound in the present invention means a compound that is gaseous at the time of detection, and does not mean a compound that is gaseous at normal temperature. The specific detection procedure is described below.
In a first step, a light source is provided for generating light for detection. The light emitted by the light source may be natural light, polarized light, light of a particular wavelength, or other light of a particular requirement.
In a second step, the detection unit is exposed to the gaseous compound to be detected and illuminated by a light source. As shown in fig. 1, the detection unit includes a transparent substrate 1 and a polymer dispersed liquid crystal film 2 disposed on the transparent substrate. The polymer dispersed liquid crystal film comprises a polymer 21 and a liquid crystal material 22, wherein the liquid crystal material 22 is dispersed in the polymer 21 in the form of droplets. The polymer 21 may be a polymer material commonly used in Polymer Dispersed Liquid Crystal (PDLC) technology, such as epoxy resins, polyacrylates, polystyrene, and the like. The liquid crystal material 22 is a commonly used thermotropic liquid crystal including nematic, cholesteric, and smectic liquid crystals. Preferably, the liquid crystal material 22 comprises at least one nematic liquid crystal, such as the commercially available single-component nematic liquid crystal 5CB, nematic liquid crystal mixture E7, MBBA, etc. The transparent substrate 1 may be rigid transparent glass, or may be flexible transparent polymer material, such as PET, PEN, PC, etc., but the present invention is not limited thereto; other materials with a desired transmittance may also be used. In the following examples, transparent glass is used as the transparent substrate 1.
The polymer dispersed liquid crystal film can be prepared by a conventional phase separation method, i.e., mixing a liquid crystal material and a polymer or a prepolymer uniformly at a certain temperature range or in a certain solvent to form an isotropic system, and then performing phase separation by polymerization, heating or solvent volatilization to gradually form liquid crystal droplets, thereby finally obtaining a polymer dispersed liquid crystal, wherein the solvent can be a volatile organic solvent capable of completely dissolving a high molecular material and the liquid crystal material, such as chloroform, acetone, chloroform and mixtures thereof, but is not limited thereto, and for example, when the polymer is a water-soluble polymer, the solvent can also be water. The phase separation method may include polymerization-induced phase separation, thermal process-induced phase separation, solvent volatilization-induced phase separation, and the like, and in the following examples, the polymer dispersed liquid crystal film is prepared by a solvent volatilization-induced phase separation method and a polymerization-induced phase separation method.
And thirdly, testing the change of the optical performance of the detection unit. As shown in fig. 2, in the polymer dispersed liquid crystal film, liquid crystal molecules 201 tend to be aligned in the liquid crystal droplets due to anchoring action of the surfaces of the liquid crystal droplets, and the optical axis orientation of the liquid crystal droplets is random in the polymer dispersed film, causing anisotropy in refractive index, and thus scattering occurs when light is irradiated onto the polymer dispersed film. When the detected gas molecules 202 enter the liquid crystal droplets through the polymer, the anchoring conditions of the liquid crystal molecules are changed, the ordered arrangement of the liquid crystal molecules is disturbed, and the refractive index of the liquid crystal droplets tends to be isotropic, so that the scattering of the transmitted light is reduced, and the optical performance of the polymer dispersed liquid crystal film is finally changed. And the degree of change in this ordered arrangement varies with the number of gas molecules 202 (i.e., gas concentration) entering the liquid crystal droplets, resulting in a varying degree of optical properties of the polymer dispersed liquid crystal film. Such a change in optical properties exhibits different behavior depending on the liquid crystal material in the polymer dispersed liquid crystal film. One way is that the optical properties of the polymer dispersed liquid crystal film are mutated above and below the characteristic concentration of the gas molecules, and the characteristic concentration varies with the composition and proportion of the liquid crystal material; in another mode, the optical properties of the polymer dispersed liquid crystal film gradually change with the concentration of the gas molecules, and some changes in the optical properties are linear with the gas concentration.
The detection unit may further comprise a plurality of different polymer dispersed liquid crystal films laid on the transparent substrate. When the optical properties of the polymer-dispersed liquid crystal films are changed in the first manner, each polymer-dispersed liquid crystal film is sensitive to a different concentration range of the gaseous compound to be detected, so that the detection range of the detection unit can be expanded.
The optical property change of the detection unit is reversible, when the gas molecules leave the polymer dispersed liquid crystal film, the liquid crystal molecules can return to the ordered arrangement state under the action of the anchoring energy of the polymer and the surface of the liquid crystal microdroplet, and the detection can be carried out again. The optical properties include transmitted light intensity, transmittance, reflectance, reflection and absorption spectra, haze, birefringence, etc. of the detection cell. Preferably, the optical property of the detection unit is the intensity of transmitted light through the detection unit, wherein the transmitted light comprises direct transmitted light and scattered transmitted light.
And fourthly, collecting data for analysis, and converting the change of the optical property into the concentration of the gaseous compound according to the predicted corresponding relation between the optical property of the detection unit and the concentration of the gaseous compound, thereby obtaining the instant concentration of the gaseous compound. According to the type of the gaseous compound and the optical performance to be tested, the corresponding optical performance/gas concentration relation is different, and the detection unit comprising different polymer dispersed liquid crystal films and the optical performance to be tested can be selected according to the requirement to achieve one-to-one correspondence.
The invention also provides a system for detecting the gaseous compound, which comprises a light source device 2, a detection unit device 1 and a data collection and analysis unit device 3. The light source device 2 provides light required for detection, and may be in various forms such as natural light, polarized light, light with a specific wavelength, or other light with special requirements. The data collection and analysis unit means 3 collects the optical detection signal passing through the detection unit means 1, and converts the optical detection signal into readable information on the concentration of the gaseous compound. Depending on the optical properties to be tested, the light source device 2 and the data collection and analysis unit device 3 may be located on opposite sides of the detection unit device 1, as shown in FIG. 3, or on the same side (not shown) of the detection unit device 1.
The detection method will be described in detail with reference to specific examples. In the following examples, the percentages are by mass unless otherwise specified.
In the following examples, the light source is a helium-neon laser emitting red light at 635nm, and the probe of the data collection and analysis unit apparatus is a silicon detector capable of measuring the light intensity per unit area. In the detection process, the gas to be detected is mixed with the nitrogen, and the nitrogen molecules cannot influence the ordered arrangement of the liquid crystal molecules and cannot change the optical performance of the liquid crystal molecules, so that the light intensity measured under the condition of only nitrogen is basically consistent with the light intensity measured in the air. The light intensity measured in the case of only nitrogen gas is set to 1 in the embodiment, thereby converting the absolute intensity of the detected transmitted light into the relative transmitted light intensity, i.e., the relative transmittance of the detection unit.
Example 1
The liquid crystal, polymer and organic solvent (5CB: polylactic acid: chloroform: 6:88) were mixed in proportion to form a homogeneous solution. The homogeneous solution was coated on a transparent glass substrate with a film coater to form a film having a thickness of 0.1 mm. Then, the two phases were separated and the polymer was solidified by the volatilization of the solvent at room temperature, and finally a polymer dispersed liquid crystal film of about 10 μm was formed on the transparent glass substrate, thereby producing a detection cell.
The test unit is placed in a transparent sealed box, and the light source and the probe are placed on both sides of the test unit and on a straight line, as shown in fig. 3. The nitrogen gas mixed with acetone gas of various concentrations was continuously introduced, and the intensity of transmitted light passing through the detection unit was measured. After the test was completed, the gas was turned off, and after several minutes of recovery, the test procedure was repeated again. The results of the two tests are shown in fig. 4. As seen from the figure, the relative transmitted light intensity by the detection unit does not substantially vary with the concentration around the concentration of the acetone gas of about 2.4% (characteristic concentration), but varies greatly around the concentration of the acetone gas of about 2.4%, and can be easily detected. Meanwhile, the data of the two tests are basically consistent, which shows that the repeatability and the reliability of the test result and the detection method are good.
Example 2
The liquid crystal, which may be 5CB, E7, or a mixture of the two (1:1), is mixed with the polymer and the organic solvent in a ratio (liquid crystal: polylactic acid: chloroform: 6:88) to form a homogeneous solution. The homogeneous solution was coated on a transparent glass substrate with a film coater to form a film having a thickness of 0.1 mm. Then, the two phases were separated and the polymer was solidified by the volatilization of the solvent at room temperature, and finally a polymer dispersed liquid crystal film of about 10 μm was formed on the transparent glass substrate, thereby producing a detection cell.
The test unit is placed in a transparent sealed box, and the light source and the probe are placed on both sides of the test unit and on a straight line, as shown in fig. 3. The nitrogen gas mixed with acetone gas of various concentrations was continuously introduced, and the intensity of transmitted light passing through the test cell was measured, and the results are shown in FIG. 5. As can be seen from the figure, the detection units containing different polymer dispersed liquid crystal films all have a characteristic concentration for acetone gas, around which there is a sudden change in optical properties. Meanwhile, these characteristic concentrations continuously vary (from 2.4% to 11%) with the variation of the liquid crystal composition and the ratio in the polymer dispersed liquid crystal film, which further increases the detection range of the detection unit.
Example 3
A homogeneous solution was formed by mixing the liquid crystal at a ratio of 1:1 with a prepolymer, commercially available as UV optical adhesive NOA65, wherein the liquid crystal was a mixture of 5CB and E7 (1: 1). The homogeneous solution was sandwiched between a release film and a transparent glass substrate to form a film having a thickness of 0.1 mm. Then irradiated with UV light (365nm, intensity 20 mW/cm) at room temperature2) Irradiating for 5 minutes to cure the prepolymerPhase separation occurs and a polymer dispersed liquid crystal film is finally formed on the transparent glass substrate. Before the test, the release film was peeled off, thereby producing a detection unit.
The test unit is placed in a transparent sealed box, and the light source and the probe are placed on both sides of the test unit and on a straight line, as shown in fig. 3. The nitrogen gas mixed with acetone gas of various concentrations was continuously introduced, and the intensity of transmitted light passing through the test cell was measured, and the results are shown in FIG. 6. As seen from the figure, the detecting unit in this example had a similar tendency of variation in optical properties to the detecting unit in example 1, but the concentration of the features whose optical properties were changed abruptly was different depending on the polymer in the polymer dispersed liquid crystal film.
Example 4
The liquid crystal, polymer and organic solvent (5CB: polylactic acid: chloroform: 6:88) were mixed in proportion to form a homogeneous solution. The homogeneous solution was coated on a transparent glass substrate with a film coater to form a film having a thickness of 0.1 mm. Then, the two phases were separated and the polymer was solidified by the volatilization of the solvent at room temperature, and finally a polymer dispersed liquid crystal film of about 10 μm was formed on the transparent glass substrate, thereby producing a detection cell.
The test unit is placed in a transparent sealed box, and the light source and the probe are placed on both sides of the test unit and on a straight line, as shown in fig. 3. The nitrogen gas mixed with ethanol gas of various concentrations was continuously introduced, and the intensity of transmitted light passing through the test cell was measured, and the results are shown in FIG. 7. For ethanol gas, the optical properties of the detection cell had a similar trend with concentration as for acetone gas, indicating that this detection method is equally applicable to ethanol gas.
Example 5
The liquid crystal, polymer and organic solvent (MBBA: polylactic acid: chloroform: 6:88) were mixed in proportion to form a homogeneous solution. The homogeneous solution was coated on a transparent glass substrate with a film coater to form a film having a thickness of 0.1 mm. Then, the two phases were separated and the polymer was solidified by the volatilization of the solvent at room temperature, and finally a polymer dispersed liquid crystal film of about 10 μm was formed on the transparent glass substrate, thereby producing a detection cell.
The test unit is placed in a transparent sealed box, and the light source and the probe are placed on both sides of the test unit and on a straight line, as shown in fig. 3. The nitrogen gas mixed with acetone gas of various concentrations was continuously introduced, and the intensity of transmitted light passing through the test cell was measured, and the results are shown in FIG. 8. As can be seen from the figure, for the polymer dispersed liquid crystal film in the present embodiment, when the concentration of acetone gas is within a certain range (> 4%), the concentration of the gaseous compound to be measured can be further accurately measured by the linear relationship between the light intensity of the transmitted light of the polymer dispersed liquid crystal film and the gas concentration.
Example 6
The liquid crystal, polymer and organic solvent (5CB: polylactic acid: chloroform: 6:88) were mixed in proportion to form a homogeneous solution. The homogeneous solution was coated on a transparent glass substrate with a film coater to form a film having a thickness of 0.2 mm. Then, the two phases were separated and the polymer was solidified by the volatilization of the solvent at room temperature, and finally a polymer dispersed liquid crystal film of about 20 μm was formed on the transparent glass substrate, thereby producing a detection cell.
The test unit is placed in a transparent sealed box, and the light source and the probe are placed on both sides of the test unit and on a straight line, as shown in fig. 3. The nitrogen gas mixed with acetone gas of different concentrations was continuously introduced, and the light intensity of the direct transmission light passing through the detection unit was measured. The probe was then moved 1 cm from the straight position to test the scattered transmitted light passing through the detection cell, the test result being shown in figure 9. As can be seen from the graph, the light intensity of the transmitted light passing through the detection unit is corresponding to the concentration variation trend of the acetone gas regardless of direct incidence and scattering, and the characteristic concentration of the acetone gas with the abrupt change of the optical property is basically consistent, which shows that the detection result is not influenced by the detection position.
Although several exemplary embodiments have been described above in detail, the disclosed embodiments are merely exemplary and not limiting, and those skilled in the art will readily appreciate that many other modifications, adaptations, and/or alternatives are possible in the exemplary embodiments without materially departing from the novel teachings and advantages of the present disclosure. Accordingly, all such modifications, adaptations, and/or alternatives are intended to be included within the scope of the present disclosure as defined by the following claims.
Claims (10)
1. A method of detecting a concentration of a gaseous compound, the method comprising:
providing a light source;
exposing a detection cell to the gaseous compound and illuminated by the light source, wherein the detection cell comprises a transparent substrate and a polymer dispersed liquid crystal film disposed on the transparent substrate, the polymer dispersed liquid crystal film comprising a polymer and a liquid crystal material dispersed in the polymer;
testing the optical performance of the detection unit; and
data analysis is collected and the optical properties of the detection unit are converted into the concentration of the gaseous compound according to a correspondence between the optical properties of the detection unit and the concentration of the gaseous compound measured in advance.
2. The method of claim 1, wherein the liquid crystal material comprises at least one nematic liquid crystal.
3. The method of claim 1, wherein the gaseous compound is a volatile organic compound.
4. The method of claim 1, wherein the optical properties of the detection cell are mutated above and below a characteristic concentration of the gaseous compound.
5. The method of claim 1, wherein the optical performance of the detection cell is linear with the concentration of the gaseous compound.
6. The method of claim 4 or 5, wherein the optical property is the intensity of transmitted light from the light source through the detection cell.
7. The method of claim 6, wherein the transmitted light comprises direct transmitted light and scattered transmitted light.
8. The method of claim 4, wherein the characteristic concentration of the gaseous compound varies with the composition and proportion of the liquid crystal material.
9. The method of claim 1, wherein the detection unit comprises a plurality of different polymer-dispersed liquid crystal films laid out on the transparent substrate, the plurality of different polymer-dispersed liquid crystal films producing variations in optical properties for different concentrations of the gaseous compound to be detected.
10. A system for detecting a concentration of a gaseous compound, the system comprising:
a light source device;
a detection cell device exposed to the gaseous compound and illuminated by the light source device; and
data collection and analysis unit means for collecting optical detection signals passing through the detection unit means and converting the optical detection signals into information on the concentration of the gaseous compound.
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