CN110801807B - TiO with self-cleaning property2Preparation method of molecular pollution adsorption material with film-coated zeolite molecular sieve and adsorption device - Google Patents
TiO with self-cleaning property2Preparation method of molecular pollution adsorption material with film-coated zeolite molecular sieve and adsorption device Download PDFInfo
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Abstract
TiO with self-cleaning property2A preparation method of a molecular pollution adsorption material with a film-coated zeolite molecular sieve and an adsorption device belong to the technical field of molecular cleaning. The invention aims to solve the problem that the existing space molecule pollutants can be condensed and deposited on the surface of each sensitive element, so that the full play of the functions of the sensitive elements is influenced and even the sensitive elements are out of work. The invention takes zeolite molecular sieve as the core, TiO prepared by atomic layer deposition method2The film is a shell to obtain TiO2The film layer is coated on the molecular pollution adsorption material of the zeolite molecular sieve. The film layer has good three-dimensional shape retention and wrapping property, improves the structural stability of the zeolite molecular sieve, and simultaneously has TiO2The shell layer has good photocatalytic performance and shows good self-cleaning capability under ultraviolet light. The adsorption capacity of the molecular pollution adsorption material prepared by the invention on the aerospace pollutants reaches 13.5 mg.g‑1The excellent pollutant treatment capacity can be widely applied to the fields of automobile exhaust treatment, green spraying and the like.
Description
Technical Field
The invention relates to TiO with self-cleaning performance2A preparation method of a molecular pollution adsorption material with a film-coated zeolite molecular sieve and an adsorption device belong to the technical field of molecular cleaning.
Background
With the development of spacecraft towards high performance, high reliability and long service life, rigorous requirements on the precision and sensitivity of effective load are provided, and the influence and prevention and control of space molecular pollution on the load sensitive surface are greatly concerned. The space molecule contaminant can condense and deposit on the sensitive surface of each load, affecting the full functioning thereof and even leading to the failure of the load. Therefore, it is imperative to adopt appropriate means and measures to control the formation of the pollution and reduce its impact on the spacecraft. Therefore, it is necessary to provide a molecular contamination adsorbing material having self-cleaning property.
Disclosure of Invention
The invention provides a TiO with self-cleaning property, aiming at solving the problems that the existing space molecule pollutants can be condensed and deposited on the surfaces of all sensitive elements to influence the full play of the functions of the sensitive elements and even cause failure2A preparation method of a molecular pollution adsorption material with a film layer coated with a zeolite molecular sieve and an adsorption device.
The technical scheme of the invention is as follows:
TiO with self-cleaning property2The preparation method of the molecular pollution adsorption material of the membrane-coated zeolite molecular sieve comprises the following operation steps:
wherein, the operation process of each atomic layer deposition growth cycle is as follows: 1) injecting water source into the deposition cavity of the atomic layer deposition instrument in a pulse mode with pulse time t1Is 0.02s to 0.04 s; 2) opening of inlet and exhaust valvesPurging with nitrogen for a time t2Is 30s to 60 s; 3) injecting a titanium source into a deposition cavity of the atomic layer deposition instrument in a pulse mode for a pulse time t3Is 0.2s to 0.4 s; 4) opening the air inlet valve and the air outlet valve, purging by using nitrogen, and purging for time t4Is 30s to 60 s;
Preferably: the operation process of heating and drying the spherical zeolite molecular sieve in the step 1 is as follows: and (3) putting the zeolite molecular sieve into a tube furnace for heating, heating to 200 ℃ within 0.5h, vacuumizing to-0.1 MPa, preserving the heat for 2h, and naturally cooling to room temperature.
Preferably: the temperature of the water source in the step 2 is room temperature, and the temperature of the titanium source is 50-100 ℃.
Most preferably: the titanium source is titanium (C) tetraisopropoxide12H28O4Ti), and the water source is deionized water.
Preferably: and the carrier gas in the step 2 is high-purity nitrogen.
Preferably: in the step 3, the step 2 is plated with TiO2The heat treatment conditions of the zeolite molecular sieve of the membrane layer are as follows: will be coated with TiO2And (3) heating the zeolite molecular sieve of the membrane layer in a tube furnace, heating to 200 ℃ within 0.5h, vacuumizing to-0.1 MPa, preserving the heat for 2h, and naturally cooling to room temperature.
Preferably: the spherical zeolite molecular sieve has the model of 5A, 10X or 13X, the particle size of 3-5 mm and micropores and/or mesoporous channels with the pore diameter of less than 20 nm.
Preferably: the obtained TiO of the molecular contamination adsorbing material2The thickness of the film layer is 5 nm-10 nm.
TiO obtained by applying the preparation method2The using device of the molecular pollution adsorption material of the film-coated zeolite molecular sieve comprises a support frame 1, a heat insulation layer 2, a bearing box 3, a limiting strip 4 and a molecular pollution adsorption material 5, wherein the support frame 1 is a polygonal box body, the upper cover of the box body is a removable cover plate, and the removable cover plate is communicated with a box body main bodyConnecting in an over-pressure buckling mode; a plurality of cavities are uniformly divided in the support frame 1 by arranging a plurality of limiting strips, and the bearing box 3 is arranged in the cavities; the heat insulating layer 2 is fixed between the supporting frame 1 and the carrying box 3 in an adhesion mode, and the carrying box 3 is filled with a molecular pollution adsorbing material 5.
Preferably: the supporting frame 1 is made of aluminum magnesium alloy, and a heat conducting coating is coated on the surface of the supporting frame 1; the heat insulating layer 2 is made of polyimide, foam plastic or foam rubber material; the bearing box is an 80-mesh metal aluminum mesh bag.
The invention has the following beneficial effects: the invention constructs TiO integrated with structural stability, adsorption selectivity and adsorption efficiency on the surface of the spherical 5A zeolite molecular sieve with strong adsorption capacity, strong regenerability and high selective adsorption by using Atomic Layer Deposition (ALD)2The film layer has good wrapping performance and can effectively solve the problem that dust of the zeolite molecular sieve falls. TiO prepared by the method2The molecular pollution adsorption material with the zeolite molecular sieve coated by the film layer has better catalytic performance and self-cleaning capability under the irradiation of ultraviolet light, so that the adsorption and catalysis of volatile organic gas molecules by the material are facilitated, and the environment in a spacecraft is purified. The molecular pollution adsorption device has the advantages of low cost, convenient disassembly, safe use and light weight, and can reduce the load of a large instrument. The semi-open design is beneficial to the contact of volatile organic gas and the adsorption material, is more beneficial to the improvement of the adsorption performance, and achieves the aim of quickly removing polluted gas molecules.
Drawings
FIG. 1 is an XPS spectrum of the surface layer of the molecular contamination adsorbing material prepared by the present invention, wherein a) is a full spectrum, b) is a Ti 2p spectrum, and c) is an O1s spectrum;
FIG. 2 is a photograph of a TFM of the surface layer of the adsorbent material with molecular contamination prepared by the present invention;
FIG. 3 is an infrared spectrum of the molecular contamination adsorbing material prepared by the present invention;
FIG. 4 is a schematic diagram of the adsorption amount of the molecular contamination adsorbent material on the contaminant prepared by the present invention;
FIG. 5 is a schematic view showing the structure of the molecular contamination adsorbing device of the present invention.
Detailed Description
The experimental procedures used in the following examples are conventional unless otherwise specified. The materials, reagents, methods and apparatus used, unless otherwise specified, are conventional in the art and are commercially available to those skilled in the art.
Embodiment mode 1: TiO 22Preparation of membrane-coated zeolite molecular sieve molecular pollution adsorption material
Step one, 50g of spherical 5A zeolite molecular sieve with the particle size of 30-50 nm is placed in a tubular furnace, redundant water vapor in the zeolite is discharged, meanwhile, rapid air suction in the atomic layer deposition process is facilitated, the specific operation is that the temperature of the furnace is raised to 200 ℃ within 0.5h, heat preservation is carried out, the furnace is pumped to vacuum for 2h, then natural cooling is carried out until the normal temperature is recovered, and the furnace is placed in a drying dish for standby.
Step two, the spherical 5A zeolite molecular sieve to be used obtained by the treatment of the step is put into a deposition cavity of an atomic layer deposition instrument, and the deposition cavity is pumped to 5 multiplied by 10-3Torr, introducing nitrogen until the pressure of the chamber is 0.1Torr, and the temperature in the deposition chamber is 200 ℃; then carrying out TiO on the surface of the zeolite molecular sieve2Film atomic layer cycle deposition growth, repeatedly executing 200 growth deposition cycles to obtain the TiO plated film2Zeolite molecular sieve of the membranous layer; the operation process of each atomic layer deposition growth cycle comprises the following steps: 1) injecting a water source into a deposition cavity of the atomic layer deposition instrument in a pulse mode, wherein the water source is deionized water, the temperature is room temperature, and the pulse time t1Is 0.02 s; 2) opening the air inlet valve and the air outlet valve, purging by using nitrogen, and purging for time t2Is 40 s; 3) injecting a titanium source into a deposition cavity of the atomic layer deposition instrument in a pulse mode, wherein the titanium source is titanium tetraisopropoxide, the temperature is 75 ℃, and the pulse time t is3Is 0.2 s; 4) opening the air inlet valve and the air outlet valve, purging by using nitrogen, and purging for time t4Was 40 s.
Step three, the obtained TiO plating2Heating the zeolite molecular sieve in the membrane layer in a tube furnace to 200 deg.C within 0.5h, and pumpingKeeping the temperature for 2h after the vacuum is reduced to-0.1 MPa, naturally cooling to room temperature to obtain a molecular contamination adsorbing material, and measuring the TiO of the molecular contamination adsorbing material by using an ellipsometer2The thickness of the film layer is 6 nm.
The detection test was performed on the molecular contamination adsorbent obtained above, and the results were as follows.
Fig. 1 is an XPS spectrum of the molecular contamination adsorbing material surface layer material, which is shown by a in fig. 1 and is a full spectrum of the XPS spectrum of the molecular contamination adsorbing material surface layer material, and the molecular contamination adsorbing material surface layer material is composed of three elements of Ti, O and C, wherein the element C exists because titanium tetraisopropoxide is a metal organic substance which is not completely reacted on the surface of the substrate 5A zeolite molecular sieve. Wherein the reaction equation of each growth and deposition period is as follows:
Ti(OCH(CH3)2)4+TiO2-OH*→HOCH(CH3)2+TiO2-O-Ti(OCH(CH3)2)3* TiO2-O-Ti(OCH(CH3)2)3*+2H2O→TiO2-TiO2-OH*+3(HOCH(CH3)2)。
the graph b in FIG. 1 is a 2p spectrogram of Ti, and it can be seen from the graph that two peaks can be fitted at two positions of 464.2eV and 458.5eV, which correspond to Ti 2p1/2And Ti 2p3/2The difference of the binding energy is 5.7eV, which proves that Ti element in the surface layer material of the molecular contamination adsorption material is Ti4+The form exists. The 1s spectrum of O in FIG. 1 is plotted as c, and it can be seen that two peaks can be fitted at 529.7eV and 531.2eV, where the peak at 529.7eV is typical of Ti-O bonds and the peak at 531.2eV corresponds to the Ti-OH species at the surface. According to the XPS manual, the molecular contamination adsorbing material surface layer material is TiO2。
FIG. 2 is an AFM photograph of a surface layer material of a molecular contamination adsorbent, and it can be seen that TiO prepared in embodiment 12The microcosmic appearance of the titanium tetraisopropoxide is nano island-shaped and the surface is compact and uniform, because the titanium tetraisopropoxide molecule is slow in adsorption speed and thermal movement capacity on the substrate, slow in molecular diffusion and between islands under the deposition condition of the titanium tetraisopropoxide nano island-shaped nano titanium tetraisopropoxide nano titanium substrateThe distance is large so that the film is extremely flat, and the root mean square roughness is calculated to be only 0.754. The lower roughness causes water contacting the surface to flow into the gaps of the structure rapidly, fills the gaps and spreads to form a stable water film, the water contact angle under the air environment is 13.52 degrees, and the hydrophilic performance is realized. The adsorption material is more favorable for the adsorption of the molecular pollution adsorption material on nonpolar volatile organic gas molecules, and is more favorable for ensuring the environment in the spacecraft.
The molecular contamination adsorbing material prepared in embodiment 1 and the zeolite molecular sieve were subjected to mechanical property test under the same conditions. The method comprises the following specific steps: respectively placing the molecular pollutant adsorption material and the zeolite molecular sieve on a vibration test bed, vibrating for 10min at the frequency of 50Hz, then taking out the molecular pollutant adsorption material and the zeolite molecular sieve, and screening to check whether micro powder particles are generated. The test result shows that about 2% of micro powder of the untreated spherical 5A zeolite molecular sieve occurs due to the conditions of cracks and breakage of the zeolite molecular sieve caused by molecular sieve collision in the vibration process, and the molecular pollution adsorbing material prepared in the specific embodiment 1 has no micro powder after the test, so that the film layer on the surface of the zeolite molecular sieve plays a great role in protecting the zeolite molecular sieve, and the mechanical property of the molecular pollution adsorbing material is improved.
The molecular contamination adsorbing material prepared in the specific embodiment 1 is subjected to a UV irradiation self-cleaning test, and the test process is as follows: (1) infrared spectroscopy is performed on the molecular contamination adsorbing material prepared in the specific embodiment 1to characterize the chemical functional groups of the molecular contamination adsorbing material. (2) Immersing the molecular pollution adsorption material in a beaker filled with normal hexane for 15min, taking out two parts, and characterizing the chemical functional group of the molecular pollution adsorption material by using infrared spectroscopy on one part. And irradiating the other part for 15min by using an ultraviolet lamp, and then performing infrared spectrum to characterize chemical functional groups of the molecular pollution adsorption material. The above results are shown in FIG. 3 at 2600cm-1To 3400cm-1In the range, the infrared spectrum of the original space molecular pollution adsorbing material has no characteristic peak, and the infrared spectrum is 2987cm after being polluted by n-hexane-1And 2900cm-1Is represented by-CH2-and-CH3Two characteristic peaks disappear after UV irradiation, and the original molecule is pollutedThe infrared characterization results of the dye adsorption materials are consistent. The molecular pollution adsorbing material can eliminate pollutants on the surface of the material through ultraviolet irradiation after the molecular pollution adsorbing material adsorbs n-hexane, and has self-cleaning performance under the ultraviolet irradiation. This is due to TiO2The internal oxygen atom and Ti form Ti-O bond in a three-degree coordination mode, the oxygen atom on the surface and Ti combine in a two-degree coordination mode to form bridge oxygen, but the stability of the bridge oxygen is poor due to low coordination degree, and under the irradiation of UV, TiO2The lattice bond between the oxygen at the bridge site and Ti is weakened, and the electron of VB is excited to CB, so that TiO2Photoelectrons (e) generated at the web surface-) And a cavity (h)+) Photoelectrons with Ti4+Reaction to produce Ti3+The cavity reacts with the bridge site oxygen to form oxygen vacancies, H2O combines with oxygen vacancy to generate OH, and enhances TiO2Hydrophilicity of the omentum. At the same time, under the action of the cavity, H2O is oxidized to hydroxyl radical and H+Oxygen in the air is photo-electronically reduced to superoxide radicals, which react with TiO2Organic contaminants on the omentum surface, such as n-hexane, are oxidized to CO2、H2O, etc. inorganic substance, so-CH2-and-CH3The characteristic peak of (a) disappears after UV irradiation.
The adsorption experiment was performed on the molecular contamination adsorbent prepared in embodiment 1. The experimental process is as follows: the molecular contamination adsorbing material and a piece of 703 silicon rubber with the weight of 1g are placed in a sealed tank, the sealed tank is heated to 200 ℃, the mass change of the molecular contamination adsorbing device is tested, and the average value of the adsorption quantity is obtained (under the condition that the temperature of the 703 silicon rubber is 100-200 ℃, gases such as organic siloxane, methane, n-butene and the like are released). As a result, as shown in FIG. 4, it was found that the adsorption amount of the molecular contamination adsorbent was 5.2mg g-1～13.5mg·g-1And the adsorption capacity is strong within 4 h.
In conclusion, the molecular pollution adsorption material can be used as a space pollution adsorption material to be applied to a spacecraft, can realize a self-cleaning function while adsorbing organic gas in the spacecraft, and meets the requirement of the spacecraft on pollution control.
Embodiment mode 2: using TiO2Use device of molecular pollution adsorption material of membrane-coated zeolite molecular sieve
As shown in fig. 5, the device comprises a supporting frame 1, a heat insulating layer 2, a bearing box 3, a limiting strip 4 and a molecular pollution adsorbing material 5, wherein the supporting frame 1 is a regular hexagon box body made of aluminum-magnesium alloy, the upper cover of the box body is a movable cover plate, and the movable cover plate is connected with a box body main body in a pressing and buckling mode; 6 triangular cavities are evenly divided from the interior of the support frame 1 by arranging 6 limiting strips, and the bearing box 3 is arranged in the cavities; the heat insulating layer 2 is fixed between the supporting frame 1 and the carrying box 3 by means of adhesion, and the carrying box 3 is an 80-mesh metal aluminum mesh bag, as shown in fig. 4. TiO prepared by the embodiment 12The molecular contamination adsorbing material of the membrane layer coated zeolite molecular sieve is put into a using device of the molecular contamination adsorbing material as a molecular contamination adsorbing material 5. The molecular pollution adsorption material device can be fixed on a sensitive element and can adsorb organic gas of a large instrument, and meanwhile, the molecular pollution adsorption material in the adsorption device is easy to replace and can meet the requirement of the large instrument on pollution control.
Claims (6)
1. TiO with self-cleaning property2The preparation method of the molecular pollution adsorption material of the membrane-coated zeolite molecular sieve is characterized by comprising the following steps: the method comprises the following operation steps:
step 1, heating and drying a spherical zeolite molecular sieve; the spherical zeolite molecular sieve is 5A in model number;
step 2, placing the zeolite molecular sieve processed in the step 1 in a deposition cavity of an atomic layer deposition instrument, and pumping the deposition cavity to 5 multiplied by 10-3 Torr, then introducing carrier gas until the pressure of the chamber is 0.1Torr, and the temperature in the deposition chamber is 200 ℃; then carrying out TiO on the surface of the zeolite molecular sieve2The film atomic layer is periodically deposited and grown, and 200 deposition growth periods are repeatedly executed to obtain the film coated with TiO2Zeolite molecular sieve of the membranous layer;
wherein, the operation process of each atomic layer deposition growth cycle is as follows: 1) pulsing into a deposition chamber of an atomic layer deposition apparatusInjecting water source, pulse time t1Is 0.02 s; 2) opening the air inlet valve and the air outlet valve, purging by using nitrogen, and purging for time t2Is 40 s; 3) injecting a titanium source into a deposition cavity of the atomic layer deposition instrument in a pulse mode for a pulse time t3Is 0.2 s; 4) opening the air inlet valve and the air outlet valve, purging by using nitrogen, and purging for time t4Is 40 s;
step 3, the TiO plating obtained in the step 2 is carried out2Carrying out heat treatment on the zeolite molecular sieve of the membrane layer to obtain a molecular pollution adsorption material; TiO of the molecular contamination adsorption material2The microscopic morphology of the film layer presents a nano island shape, the surface is compact and uniform, the film layer is extremely flat, and the root-mean-square roughness of the film layer is 0.754;
the titanium source is titanium tetraisopropoxide, and the water source is deionized water;
the temperature of the water source in the step 2 is room temperature, and the temperature of the titanium source is 75 ℃;
in the step 3, the step 2 is plated with TiO2The heat treatment conditions of the zeolite molecular sieve of the membrane layer are as follows: will be coated with TiO2And (3) heating the zeolite molecular sieve of the membrane layer in a tube furnace, heating to 200 ℃ within 0.5h, vacuumizing to-0.1 MPa, preserving the heat for 2h, and naturally cooling to room temperature.
2. TiO with self-cleaning properties according to claim 12The preparation method of the molecular pollution adsorption material of the membrane-coated zeolite molecular sieve is characterized by comprising the following steps: the operation process of heating and drying the spherical zeolite molecular sieve in the step 1 is as follows: and (3) putting the zeolite molecular sieve into a tube furnace for heating, heating to 200 ℃ within 0.5h, vacuumizing to-0.1 MPa, preserving the heat for 2h, and naturally cooling to room temperature.
3. TiO with self-cleaning properties according to claim 12The preparation method of the molecular pollution adsorption material of the membrane-coated zeolite molecular sieve is characterized by comprising the following steps: the carrier gas in the step 2 is nitrogen.
4. According to claim1A TiO with self-cleaning properties2The preparation method of the molecular pollution adsorption material of the membrane-coated zeolite molecular sieve is characterized by comprising the following steps: TiO of the obtained molecular contamination adsorbing material2The thickness of the film layer is 6 nm.
5. An adsorption device comprising the TiO produced by the method of any one of claims 1to 4 having self-cleaning properties2The molecular pollution adsorbing material of the film-coated zeolite molecular sieve is characterized in that: the device comprises a supporting frame (1), a heat insulating layer (2), a bearing box (3), a limiting strip (4) and a molecular pollution adsorption material (5), wherein the supporting frame (1) is a polygonal box body, the upper cover of the box body is a movable cover plate, and the movable cover plate is connected with a box body main body in a pressing and buckling mode; a plurality of cavities are uniformly divided by arranging a plurality of limiting strips (4) in the supporting frame (1), and the bearing box (3) is arranged in the cavities; the heat insulating layer (2) is fixed between the supporting frame (1) and the bearing box (3) in an adhesion mode, and the bearing box (3) is internally provided with a molecular pollution adsorption material (5).
6. The adsorption device of claim 5, wherein: the supporting frame (1) is made of aluminum magnesium alloy, and a heat conducting coating is coated on the surface of the supporting frame (1); the heat insulating layer (2) is made of polyimide, foam plastic or foam rubber material; the bearing box (3) is an 80-mesh metal aluminum mesh bag.
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