CN111704733B - Full-automatic peristaltic pump type film preparation device - Google Patents
Full-automatic peristaltic pump type film preparation device Download PDFInfo
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- CN111704733B CN111704733B CN201910204821.XA CN201910204821A CN111704733B CN 111704733 B CN111704733 B CN 111704733B CN 201910204821 A CN201910204821 A CN 201910204821A CN 111704733 B CN111704733 B CN 111704733B
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- 230000002572 peristaltic effect Effects 0.000 title claims abstract description 88
- 238000002360 preparation method Methods 0.000 title abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 69
- 239000000758 substrate Substances 0.000 claims abstract description 50
- 238000000034 method Methods 0.000 claims abstract description 34
- 239000000463 material Substances 0.000 claims abstract description 13
- 239000007791 liquid phase Substances 0.000 claims abstract description 7
- 239000000243 solution Substances 0.000 claims description 54
- 239000007788 liquid Substances 0.000 claims description 37
- 239000011248 coating agent Substances 0.000 claims description 27
- 238000000576 coating method Methods 0.000 claims description 27
- 238000002791 soaking Methods 0.000 claims description 18
- 239000010410 layer Substances 0.000 claims description 17
- 239000002184 metal Substances 0.000 claims description 10
- 229910052751 metal Inorganic materials 0.000 claims description 10
- 239000011521 glass Substances 0.000 claims description 9
- 239000012621 metal-organic framework Substances 0.000 claims description 8
- 239000013110 organic ligand Substances 0.000 claims description 8
- 239000012266 salt solution Substances 0.000 claims description 8
- 238000002474 experimental method Methods 0.000 claims description 7
- 239000002699 waste material Substances 0.000 claims description 7
- -1 amino, sulfhydryl Chemical group 0.000 claims description 6
- 230000004048 modification Effects 0.000 claims description 5
- 238000012986 modification Methods 0.000 claims description 5
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 4
- 125000000962 organic group Chemical group 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- 239000002356 single layer Substances 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 2
- 239000000919 ceramic Substances 0.000 claims description 2
- 230000008859 change Effects 0.000 claims description 2
- 125000002883 imidazolyl group Chemical group 0.000 claims description 2
- 238000005259 measurement Methods 0.000 claims description 2
- 239000006262 metallic foam Substances 0.000 claims description 2
- 239000010445 mica Substances 0.000 claims description 2
- 229910052618 mica group Inorganic materials 0.000 claims description 2
- 239000004033 plastic Substances 0.000 claims description 2
- 229920000307 polymer substrate Polymers 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- 229910001220 stainless steel Inorganic materials 0.000 claims description 2
- 239000010935 stainless steel Substances 0.000 claims description 2
- 125000004076 pyridyl group Chemical group 0.000 claims 1
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 53
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 13
- 239000010409 thin film Substances 0.000 description 8
- GZTBKEOTCAVWNJ-UHFFFAOYSA-L C(C)O.C(C)(=O)[O-].[Cu+2].C(C)(=O)[O-] Chemical compound C(C)O.C(C)(=O)[O-].[Cu+2].C(C)(=O)[O-] GZTBKEOTCAVWNJ-UHFFFAOYSA-L 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- HSSYVKMJJLDTKZ-UHFFFAOYSA-N 3-phenylphthalic acid Chemical compound OC(=O)C1=CC=CC(C=2C=CC=CC=2)=C1C(O)=O HSSYVKMJJLDTKZ-UHFFFAOYSA-N 0.000 description 3
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 235000019441 ethanol Nutrition 0.000 description 3
- 238000007747 plating Methods 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000004528 spin coating Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 229940076286 cupric acetate Drugs 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000004943 liquid phase epitaxy Methods 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G83/00—Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
- C08G83/008—Supramolecular polymers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2387/00—Characterised by the use of unspecified macromolecular compounds, obtained otherwise than by polymerisation reactions only involving unsaturated carbon-to-carbon bonds
Abstract
The invention provides a device for preparing a film by a full-automatic peristaltic pump, which is a device for preparing the film on a substrate by a liquid phase epitaxial growth method by utilizing a peristaltic pump full-automatic control system. The device comprises a constant temperature circulator, a peristaltic pump, a control system, a reaction container and a solution bottle, wherein corresponding parameters can be set for the control system according to requirements, the running and stopping time of the peristaltic pump and the circulation times and the temperature in the reaction container are precisely controlled, so that high-quality film materials can be automatically, accurately, efficiently and effectively prepared by saving manpower, and the device has the advantages of high synthesis speed, high preparation efficiency, controllable reaction temperature, controllable film thickness, low cost, simplicity in operation and the like.
Description
Technical Field
The invention belongs to the technical field of full-automatic peristaltic pump devices, and particularly relates to a full-automatic peristaltic pump type device for preparing a film.
Background
The film material has wide application in the biological field and various storage, separation and sensors. Particularly, the film material obtained by layer-by-layer self-assembly has better surface morphology and adjustable film thickness, and is of great interest in the fields of optics, electricity, magnetism, catalysis and the like. The liquid phase epitaxy method is to grow a thin film in a step-by-step assembly manner, and can prepare a uniform, heterogeneous and thickness-controllable thin film. However, how to effectively prepare layer-by-layer self-assembled thin film materials using this method remains a great challenge. The methods commonly used at present are a manual soaking method, a spin coating method and the like. However, the manual soaking method is difficult to accurately control the preparation time, and is time-consuming and labor-consuming; the spin coating method is difficult to obtain a layer-by-layer self-assembled film with a flat and uniform surface, and the preparation is easily influenced by the external environment temperature. Therefore, a device for fully automatically preparing a film is needed to replace manual soaking work, so that the defects of large soaking time error, few assembly layers, large influence from external environment and the like are overcome.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides a device for preparing a film by a full-automatic peristaltic pump, which is a device for preparing the film on a substrate by a liquid phase epitaxial growth method by utilizing a full-automatic peristaltic pump control system.
According to the invention, the device comprises a constant temperature circulator, a peristaltic pump, a control system, a reaction container and a solution bottle;
the constant temperature circulator is arranged on one side of the reaction container, and the other side of the reaction container is connected with the peristaltic pump; the constant temperature circulator is used for controlling the temperature of the reaction container, realizing high-precision temperature control and measurement of an external system, and enabling the reaction container to prepare a film within the temperature change range of-20 ℃ to 150 ℃, such as 50 ℃;
the control system is connected with the peristaltic pump and is used for receiving the instruction signal and converting the instruction signal into a motion for instructing the peristaltic pump to start and stop;
the solution bottle is a container for containing coating solution and is connected with the peristaltic pump, and the connection can be realized through a peristaltic pump hose;
the peristaltic pump is used for introducing the coating liquid in the solution bottle into the reaction container or discharging the waste liquid in the reaction container according to a certain sequence by the instruction of the control system;
the reaction container is a container for containing the coating liquid led in by the peristaltic pump and a substrate, and can enable circulating liquid of the constant temperature circulator to circulate, so that the temperature of the reaction container is kept constant, and the influence of external conditions (such as temperature) on the film growth process is reduced.
According to the embodiment of the invention, the appearance structure of the reaction container can be selected according to the requirement of film growth, so that the substrate is conveniently and completely soaked in the film plating liquid, the film growth is convenient, the solution temperature in the reaction container can be kept, and the appearance structure of the film plating liquid is convenient to empty.
Preferably, the reaction vessel is of a double-layer glass structure; illustratively, the reaction vessel may employ a double glass bent bottle structure.
According to an embodiment of the present invention, the control system employs a programmable controller (PLC), such as a memory employing a programmable program, and stores therein instructions for performing operations such as logic operations, sequence control, timing, counting, and arithmetic operations, and selects and controls the running time, stop time, and number of cycles, etc. of the peristaltic pump through digital and analog inputs and outputs.
According to the embodiment of the invention, the size and the material of the solution bottle can be selected according to the properties of reaction raw materials and experimental requirements. The volume of the solution bottle can be 100-2000 mL; the material of the solution bottle can be any one of glass, stainless steel, plastic and ceramic.
According to the embodiment of the invention, the coating liquid can be one or more of metal salt solution, organic ligand solution and solvent.
According to an embodiment of the present invention, the material of the substrate may be any one of a metal substrate, a silicon substrate, a mica substrate, a glass substrate, a quartz glass substrate, a metal foam substrate, a polymer substrate, and the like.
Preferably, the substrate is a modified substrate, the modification may be modification of an organic group, and the organic group may be one or more of hydroxyl, carboxyl, amino, mercapto, pyridyl, carbenyl, and imidazolyl; illustratively, the substrate is a quartz glass substrate that has been modified with hydroxyl groups.
According to embodiments of the present invention, the device may be sized according to the purpose of preparing the film, the size of the operating space, and the needs of the operator. The aspect ratio of the constant temperature circulator may be, for example, 8:5:12, for example, 40×25×60cm (length/width/height); the peristaltic pump may have an aspect ratio of, for example, 5.6:2:3, for example, 28 x 10 x 15cm (length/width/height).
The invention also provides a method for preparing the film, which is a device for preparing the film based on the full-automatic peristaltic pump; the method comprises the following steps:
1) Starting a constant temperature circulator, and adjusting to the temperature required by the experiment;
2) Preparing coating liquid, placing the coating liquid in a solution bottle, and connecting the solution bottle with a peristaltic pump through a peristaltic pump hose;
3) Placing a substrate in a reaction vessel;
4) And controlling the running time, the stopping time and the circulation times of the peristaltic pump by a control system, so that the substrate is soaked in the coating liquid in the reaction container in the step 3), and the film is prepared.
The invention also provides a method for preparing the layer-by-layer self-assembled film, which is a device for preparing the film based on the full-automatic peristaltic pump; the method comprises the following steps:
1) Starting a constant temperature circulator, and adjusting to the temperature required by the experiment;
2) Preparing coating liquid, placing the coating liquid in a solution bottle, and connecting the solution bottle with a peristaltic pump through a peristaltic pump hose;
3) Placing a substrate in a reaction vessel;
4) Controlling the running time, the stopping time and the circulation times of the peristaltic pump through a control system, soaking a substrate in the coating liquid in the reaction container in the step 3), and forming a self-assembled film with a single-layer structure through a liquid phase epitaxial growth method;
5) And (3) repeating the step (4) to prepare the layer-by-layer self-assembled film.
According to an embodiment of the invention, the method comprises the steps of:
s1, starting a constant temperature circulator, and adjusting to the temperature required by an experiment;
s2, preparing a metal salt solution and an organic ligand solution, respectively placing the metal salt solution and the organic ligand solution in solution bottles, and respectively connecting the solution bottles with corresponding peristaltic pumps through peristaltic pump hoses;
s3, placing the substrate in a reaction container;
s4, controlling the running time, the stopping time and the circulation times of the peristaltic pump through a control system, sequentially soaking the substrate in the metal salt solution and the organic ligand solution in the reaction container in S3, and forming a metal organic framework film with a single-layer structure through a liquid phase epitaxial growth method;
and S5, repeating the step S4 to obtain the metal organic framework film self-assembled layer by layer.
According to the embodiment of the invention, in the method, the operation time of the peristaltic pump is controlled, and is determined according to the flow rate of the peristaltic pump, the shape and size of the reaction container, the placement mode of the substrate and the like, so that the coating liquid is suitable to completely permeate the substrate; the stop time of the peristaltic pump (i.e., the soaking time of the substrate) is determined according to the type of the reaction solution and the growth quality of the film; the temperature of the constant temperature circulator is set according to experimental requirements.
The invention has the beneficial effects that:
1. the invention provides a device for preparing a film by a full-automatic peristaltic pump. The device can set corresponding parameters for the control system according to the requirement to control the running time of the peristaltic pump, so that the substrate is completely immersed in the coating liquid in the reaction container; the soaking residence time of the substrate in the reaction vessel can be controlled to ensure the quality guarantee growth of the film; the reaction temperature can be controlled, and the influence of the external temperature on the reaction is reduced; the number of cycles of the entire operation can be further controlled to thereby produce films of different thicknesses.
2. The full-automatic peristaltic pump type film preparation device provided by the invention can accurately control the thickness and the reaction temperature of the film in the preparation process, and the film plating solution is self-assembled on the substrate layer by layer according to a certain sequence in a constant temperature state, so that the time and the labor are greatly saved, the film, especially the layer-by-layer self-assembled film material, is effectively prepared, and the quality and the efficiency of the film material are greatly improved. And can automatically, accurately, efficiently, and with little effort, produce high quality thin film materials, such as Metal Organic Framework (MOF) thin film materials, based on operator set parameters and commands issued to the control system.
3. The full-automatic peristaltic pump type film preparation device provided by the invention is a full-automatic film preparation device, overcomes various defects of manual soaking work, such as reduction of the problems of large soaking time error, uneven assembly thickness and the like, and has the capability of preparing films in complex environments.
4. The full-automatic peristaltic pump type film preparation device provided by the invention can complete the operation task of soaking and preparing the film through programming, has the advantages of people and machines in terms of construction and performance, and particularly reflects the intelligence and adaptability of people. The peristaltic pump has the advantages of working accuracy and no limitation to the environment (especially when prepared by adopting solvent reaction harmful to human bodies), and has wide development prospect in the field of film preparation.
5. The device for preparing the film by the full-automatic peristaltic pump has the advantages of high synthesis speed, high preparation efficiency, controllable reaction temperature, controllable film thickness, low cost, simple operation and the like.
Drawings
FIG. 1 is an operator panel view of a control system of an apparatus according to a preferred embodiment of the present invention;
FIG. 2 is a schematic view of the structure of the apparatus according to a preferred embodiment of the present invention;
FIG. 3 is a schematic view of the components of the apparatus according to a preferred embodiment of the present invention;
FIG. 4 is an XRD spectrum of the MOF Cu (BPDC) film prepared in example 2;
FIG. 5 is an SEM image of a MOF Cu (BPDC) film prepared in example 2;
the reference numerals in fig. 3 are as follows:
1-a constant temperature circulator; 2-a reaction vessel; 3-peristaltic pump; 4-a control system; 5-solution bottle.
Detailed Description
The preparation method of the present invention will be described in further detail with reference to specific examples. It is to be understood that the following examples are illustrative only and are not to be construed as limiting the scope of the invention. All techniques implemented based on the above description of the invention are intended to be included within the scope of the invention.
The process of preparing a MOF Cu (BPDC) film by the apparatus of the present invention is described in detail below by way of exemplary embodiments, and the advantageous effects of the present invention are further described. These examples should not be construed as limiting the scope of the invention. All techniques implemented based on the above description of the invention are intended to be included within the scope of the invention.
The experimental methods used in the following examples are all conventional methods unless otherwise specified; the reagents, materials, etc. used in the examples described below are commercially available unless otherwise specified.
In the description of the present invention, it should be noted that the terms "first," "second," and the like are used for descriptive purposes only and are not indicative or implying relative importance.
Example 1
The embodiment provides a device for preparing a film by a full-automatic peristaltic pump, which comprises a constant-temperature circulator, a peristaltic pump, a control system, a reaction container and a solution bottle, wherein the structure schematic diagram of the device is shown in figure 2, and the schematic diagram of each component is shown in figure 3;
the constant temperature circulator is arranged on one side of the reaction container, and the other side of the reaction container is connected with the peristaltic pump; the constant temperature circulator is used for controlling the temperature of the reaction vessel;
the control system is connected with the peristaltic pump and is used for receiving the command signal and converting the command signal into a motion for commanding the peristaltic pump to start and stop;
the peristaltic pump is used for introducing coating liquid into the reaction container or discharging waste liquid in the reaction container according to a certain sequence by an instruction of the control system;
the reaction container is a container for containing coating liquid and a modified substrate, and can enable circulating liquid of the constant temperature circulator to circulate, so that the temperature of the reaction device is kept constant, and the influence of external conditions (such as temperature) on the film growth process is reduced.
The control system adopts a programmable controller (PLC), such as a memory adopting a programmable program, and stores instructions for executing operations such as logic operation, sequential control, timing, counting, arithmetic operation and the like in the memory, and inputs and outputs the instructions through digital and analog modes. The control system can control the running time, the circulation times and the like of the peristaltic pump to prepare the film, and the schematic diagram of an operation panel is shown in fig. 1.
Example 2
A metal organic framework (exemplified by MOF Cu (BPDC)) film was prepared using the apparatus described in example 1 above, which was sized as 40 x 25 x 60cm (length/width/height) according to laboratory setup; peristaltic pumps are 28 x 10 x 15cm (length/width/height) in size, and the number of peristaltic pumps is set according to experimental requirements; meanwhile, the reaction vessel is a simple and convenient double-layer glass bent bottle, which comprises the following steps:
the constant temperature circulator was turned on and the temperature was set at 50 ℃.
Weighing copper acetate and biphenyl dicarboxylic acid (H) 2 BPDC), each of them was dissolved in absolute ethanol to prepare 500mL of solutions having concentrations of 1mmol/L and 0.4mmol/L, respectively, and 500mL of absolute ethanol was separately taken.
The prepared cupric acetate ethanol solution, the prepared biphenyl dicarboxylic acid ethanol solution and the prepared absolute ethanol are respectively placed in solution bottles, and then each solution bottle is connected with a peristaltic pump corresponding to the solution bottle through peristaltic pump hoses.
Then, quartz glass modified with hydroxyl groups was used as a growth substrate and was fixed in a reaction vessel.
Finally, according to the corresponding placement positions of the solution and the peristaltic pump and the requirement of experimental steps, parameter setting (such as peristaltic pump running time, peristaltic pump stopping time, circulation times and the like) is carried out on the control system, and after setting is completed, a 'start circulation' button is clicked.
The specific parameters are as follows:
1. the running time of the peristaltic pump corresponding to the copper acetate ethanol solution is 30 seconds, so that the copper acetate ethanol solution in the reaction container can completely submerge the quartz glass substrate, and the stopping time is 600 seconds, namely, the soaking reaction is 600 seconds;
2. after the copper acetate ethanol solution is soaked and reacts, a peristaltic pump corresponding to the waste liquid runs for 30 seconds to pump the waste liquid in the reaction container;
3. running a peristaltic pump corresponding to the absolute ethyl alcohol for 30 seconds, and soaking for 60 seconds to remove residual copper acetate ethanol solution;
4. the running time of a peristaltic pump corresponding to the ethanol solution of the biphenyl dicarboxylic acid is 30 seconds, and the soaking reaction time is 1200 seconds;
5. after the soaking reaction of the ethanol solution of the biphenyl dicarboxylic acid is finished, a peristaltic pump corresponding to the waste liquid is operated for 30 seconds to pump the waste liquid out of the reaction container;
6. running a peristaltic pump corresponding to the absolute ethyl alcohol for 30 seconds, and soaking for 60 seconds to remove residual biphenyl dicarboxylic acid ethanol solution;
7. the operations 1 to 6 were repeated 30 times to obtain Cu (BPDC) metal organic frameworks (MOF Cu (BPDC) films) of corresponding thickness.
The running time of the peristaltic pump is controlled, and is determined according to the flow of the peristaltic pump, the shape and size of the reaction container, the placement mode of the substrate and the like, and the coating liquid is suitable for completely submerging the substrate; the stop time of the peristaltic pump (namely the residence time of the coating liquid) is determined according to the type of the reaction solution and the growth quality of the film; the temperature of the constant temperature circulator is set according to experimental requirements.
Wherein, fig. 4 is an XRD spectrum of the MOF Cu (BPDC) thin film prepared in example 2; FIG. 5 is an SEM image of a MOF Cu (BPDC) film prepared in example 2; the spectrogram can be seen, the thin film with a good morphology structure can be prepared by adopting the device, and the device can completely replace manual operation to form a process for preparing the thin film in batches.
The embodiments of the present invention have been described above. However, the present invention is not limited to the above embodiment. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (11)
1. A full-automatic peristaltic pump type device for preparing a film is a device for preparing the film on a substrate by a liquid phase epitaxial growth method by utilizing a peristaltic pump full-automatic control system;
the device comprises a constant temperature circulator, a peristaltic pump, a control system, a reaction container and a solution bottle;
the constant temperature circulator is arranged on one side of the reaction container, and the other side of the reaction container is connected with the peristaltic pump; the constant temperature circulator is used for controlling the temperature of the reaction container, so that high-precision temperature control and measurement of an external system are realized;
the control system is connected with the peristaltic pump and is used for receiving the instruction signal and converting the instruction signal into a motion for instructing the peristaltic pump to start and stop;
the solution bottle is a container for containing coating solution and is connected with the peristaltic pump, and the connection is realized through a peristaltic pump hose;
the peristaltic pump is used for introducing the coating liquid in the solution bottle into the reaction container or discharging the waste liquid in the reaction container according to a certain sequence by the instruction of the control system;
the reaction container is a container for containing the coating liquid led in by the peristaltic pump and a substrate, and can enable the circulating liquid of the constant temperature circulator to circulate, so that the temperature of the reaction container is kept constant, and the influence of external conditions on the film growth process is reduced;
the constant temperature circulator enables the reaction container to prepare a film within the temperature change range of-20 ℃ to 150 ℃;
the aspect ratio of the thermostatic circulator is 8:5:12, and the aspect ratio of the peristaltic pump is 5.6:2:3.
2. The apparatus of claim 1, wherein the reaction vessel is a double glass structure.
3. The apparatus of claim 2, wherein the reaction vessel is a double glass bent bottle structure.
4. A device according to any one of claims 1-3, wherein the control system employs a programmable controller having stored therein instructions for performing logical operations, sequential control, timing, counting and arithmetic operations, and selecting and controlling the running time, stopping time and number of cycles of the peristaltic pump by digital, analog inputs and outputs.
5. A device according to any one of claims 1 to 3, wherein the solution bottle has a volume of 100 to 2000mL;
the material of the solution bottle is any one of glass, stainless steel, plastic and ceramic;
the coating liquid is one or more of metal salt solution, organic ligand solution and solvent.
6. A device according to any one of claims 1 to 3, wherein the substrate is any one of a metal substrate, a silicon substrate, a mica substrate, a glass substrate, a metal foam substrate, and a polymer substrate.
7. The device of claim 6, wherein the substrate is a modified substrate, the modification being an organic group modification, the organic group being one or more of hydroxyl, carboxyl, amino, sulfhydryl, pyridyl, carbenyl, imidazolyl.
8. A method of preparing a film, the method being based on the apparatus of any one of claims 1-7, the method comprising the steps of:
1) Starting the constant temperature circulator and adjusting to the temperature required by the experiment;
2) Preparing the coating liquid, placing the coating liquid in the solution bottle, and connecting the solution bottle with the peristaltic pump through a peristaltic pump hose;
3) Placing the substrate in the reaction vessel;
4) And controlling the running time, the stopping time and the circulation times of the peristaltic pump through the control system, so that the substrate is soaked in the coating liquid in the reaction container in the step 3), and the film is prepared.
9. A method of preparing a layer-by-layer self-assembled film, the method being based on the apparatus of any one of claims 1-7, the method comprising the steps of:
1) Starting the constant temperature circulator and adjusting to the temperature required by the experiment;
2) Preparing the coating liquid, placing the coating liquid in the solution bottle, and connecting the solution bottle with the peristaltic pump through a peristaltic pump hose;
3) Placing the substrate in the reaction vessel;
4) Controlling the running time, the stopping time and the circulation times of the peristaltic pump through the control system, soaking the substrate in the coating liquid in the reaction container in the step 3), and forming a self-assembled film with a single-layer structure through a liquid phase epitaxial growth method;
5) And (3) repeating the step (4) to prepare the layer-by-layer self-assembled film.
10. The method according to claim 9, characterized in that it comprises the steps of:
s1, starting the constant temperature circulator, and adjusting to the temperature required by an experiment;
s2, preparing a metal salt solution and an organic ligand solution, respectively placing the metal salt solution and the organic ligand solution in the solution bottles, and respectively connecting the solution bottles with the corresponding peristaltic pumps through peristaltic pump hoses;
s3, placing the substrate in the reaction container;
s4, controlling the running time, the stopping time and the circulation times of the peristaltic pump through the control system, sequentially soaking the substrate in the metal salt solution and the organic ligand solution in the reaction container in the step S3, and forming a metal organic framework film with a single-layer structure through a liquid phase epitaxial growth method;
and S5, repeating the step S4 to obtain the metal organic framework film self-assembled layer by layer.
11. The method according to claim 10, wherein the operation time of the peristaltic pump is determined according to the flow rate of the peristaltic pump, the shape of the reaction vessel, the placement mode of the substrate, etc., and the coating liquid is preferably completely immersed in the substrate; the stop time of the peristaltic pump is determined according to the type of the reaction solution and the growth quality of the film; the temperature of the constant temperature circulator is set according to experimental requirements.
Priority Applications (1)
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| CN203055971U (en) * | 2013-01-24 | 2013-07-10 | 北京大学 | Production equipment for preparing semiconductor film on tubular substrate |
| WO2019014306A2 (en) * | 2017-07-13 | 2019-01-17 | Argos Therapeutics, Inc. | Automated processing systems, apparatus, methods and related devices |
| CN210261614U (en) * | 2019-03-18 | 2020-04-07 | 中国科学院福建物质结构研究所 | Full-automatic peristaltic pump type device for preparing film |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN203055971U (en) * | 2013-01-24 | 2013-07-10 | 北京大学 | Production equipment for preparing semiconductor film on tubular substrate |
| WO2019014306A2 (en) * | 2017-07-13 | 2019-01-17 | Argos Therapeutics, Inc. | Automated processing systems, apparatus, methods and related devices |
| CN210261614U (en) * | 2019-03-18 | 2020-04-07 | 中国科学院福建物质结构研究所 | Full-automatic peristaltic pump type device for preparing film |
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