CN210261614U - Full-automatic peristaltic pump type device for preparing film - Google Patents
Full-automatic peristaltic pump type device for preparing film Download PDFInfo
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- CN210261614U CN210261614U CN201920341539.1U CN201920341539U CN210261614U CN 210261614 U CN210261614 U CN 210261614U CN 201920341539 U CN201920341539 U CN 201920341539U CN 210261614 U CN210261614 U CN 210261614U
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Abstract
The utility model provides a device of film is prepared to full-automatic peristaltic pump formula, the device utilizes the full automatic control system of peristaltic pump, adopts the device of liquid phase epitaxial growth method preparation film on the basement. The device comprises a constant-temperature circulator, a peristaltic pump, a control system, a reaction container and a solution bottle, corresponding parameters can be set for the control system according to requirements, and the operation and stop time, the cycle times and the temperature in the reaction container of the peristaltic pump can be accurately controlled, so that high-quality thin film materials can be automatically, accurately and efficiently prepared in a labor-saving manner, 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 utility model belongs to the technical field of full-automatic peristaltic pump device, concretely relates to device of full-automatic peristaltic pump formula preparation film.
Background
The thin film material has wide application in the biological field and various storage, separation and sensors. Particularly, the thin film material obtained by layer-by-layer self-assembly has better surface appearance and adjustable thin film thickness, and is concerned about in the fields of optics, electrics, magnetics, catalysis and the like. The liquid phase epitaxy method is a method for growing a thin film by one-step assembly, and can prepare a uniform, heterogeneous and thickness-controllable thin film. However, how to effectively prepare the layer-by-layer self-assembled film material by using the method still has a great challenge. The current common methods are a manual dipping method, a spin coating method and the like. However, the manual soaking method is difficult to accurately control the preparation time, and consumes time and labor; 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 preparing films in a fully automatic manner is needed to replace manual soaking work so as to overcome the defects of large soaking time error, few assembly layers, large influence of external environment and the like.
SUMMERY OF THE UTILITY MODEL
In order to improve the not enough of existence among the prior art, the utility model provides a device of full-automatic peristaltic pump formula preparation film, the device utilizes the full automatic control system of peristaltic pump, adopts the device of liquid phase epitaxial growth method preparation film on the basement.
According to the utility model, 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 variation range of-20-150 ℃, such as 50 ℃;
the control system is connected with the peristaltic pump and used for receiving an 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 liquid 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 through an instruction of the control system;
the reaction container is used for containing the coating liquid introduced by the peristaltic pump and a container for placing the substrate, and the circulating liquid of the constant-temperature circulator can 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 utility model discloses an embodiment, reaction vessel's appearance structure can be selected according to the needs that the membrane grows, and the basement of being convenient for soaks completely in coating film liquid, and the film of being convenient for grows, can keep solution temperature among the reaction vessel, and the appearance structure of the evacuation coating film liquid of being convenient for can.
Preferably, the reaction vessel is of a double-layer glass structure; illustratively, the reaction vessel may adopt a double-glass curved bottle structure.
According to the utility model discloses an embodiment, control system adopts Programmable Logic Controller (PLC), like the memory that adopts the programmable program to in its inside storage carry out the instruction of operation such as logical operation, sequence control, timing, count and arithmetic operation, and through the input and the output of digital, analog type, select and control the operating time of peristaltic pump, off-time and cycle number etc..
According to the utility model discloses an embodiment, size, the material of solution bottle can be selected according to the nature of reaction raw materials, experiment requirement and put. The volume of the solution bottle can be 100-2000 mL; the material of the solution bottle may be any one of glass, stainless steel, plastic, and ceramic.
According to the embodiment of the present invention, the coating solution may be one or more of a metal salt solution, an organic ligand solution, and a 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 can be organic group modification, and the organic group can be one or more of hydroxyl, carboxyl, amino, sulfydryl, pyridyl, carbinyl and imidazolyl; illustratively, the substrate is a quartz glass substrate that has been modified with hydroxyl groups.
According to an embodiment of the present invention, the size of the apparatus may be designed according to the purpose of preparing the thin film, the size of the space of the operation site, and the operator's needs. Wherein the length-to-width-to-height ratio of the thermostatic circulator may be exemplarily 8:5:12, for example, 40 × 25 × 60cm (length/width/height); the peristaltic pump may illustratively have a length to width to height ratio of 5.6:2:3, for example 28 x 10 x 15cm (length/width/height).
The utility model 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 a 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 (3) controlling the running time, the stopping time and the cycle number 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 preparing to obtain the film.
The utility model also provides a method for preparing the layer-by-layer self-assembled film, which is based on the device for preparing the film by 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 a 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 cycle number of the peristaltic pump by a 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 by a liquid phase epitaxial growth method;
5) and (5) 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 the 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 cycle number of a peristaltic pump through a control system, sequentially soaking the substrate in the metal salt solution and the organic ligand solution in the reaction container of S3, and forming the 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 layer-by-layer self-assembled metal-organic framework film.
According to the embodiment of the present invention, in the above method, the operation time of the peristaltic pump is controlled according to the flow rate of the peristaltic pump, the shape and size of the reaction vessel, the placing mode of the substrate, and the like, preferably, the coating liquid completely submerges the substrate; the stop time of the peristaltic pump (namely 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 the experimental requirement.
The utility model has the advantages that:
1. the utility model provides a device of full-automatic peristaltic pump formula preparation film. 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 vessel; the soaking residence time of the substrate in the reaction vessel can be controlled to ensure the quality-guaranteeing growth of the film; the reaction temperature can be controlled, and the influence of the external temperature on the reaction is reduced; the cycle number of the whole operation can be further controlled, so that films with different thicknesses can be prepared.
2. The utility model provides a device of full-automatic peristaltic pump formula preparation film can be under homothermal state with coating film liquid, according to certain order one deck self-assembling in the basement at the thickness and the reaction temperature of preparation in-process control film accurately, has greatly saved time and manpower to prepare the film effectively, especially layer upon layer self-assembling film material, improved film material's quality and efficiency greatly. And can automatically, accurately, efficiently and manpower-effectively prepare high-quality film materials, such as Metal Organic Framework (MOF) film materials, based on the parameters set by an operator and the commands given by the operator to the control system.
3. The utility model provides a device of full-automatic peristaltic pump formula preparation film is full-automatic film preparation device, has compensatied the manual work and has carried out soaking work's all sorts of not enough, if reduced that the soak time error is big, the inhomogeneous scheduling problem of equipment thickness, has the ability of preparing the film in the complex environment.
4. The utility model provides a device accessible programming of full-automatic peristaltic pump formula preparation film accomplishes the operation task of soaking preparation film, has the advantage of people and machine concurrently in structure and performance, has especially embodied people's intelligence and adaptability. The peristaltic pump has the advantages of working accuracy and no limitation to the environment (especially when the peristaltic pump is prepared by adopting a solvent reaction harmful to a human body), and has wide development prospect in the field of film preparation.
5. Adopt the utility model provides a device preparation film of full-automatic peristaltic pump formula preparation film has advantages such as synthetic speed is fast, preparation efficiency is high, reaction temperature is controllable, film thickness is controllable, with low costs and easy operation.
Drawings
Fig. 1 is an operation panel diagram of a control system of an apparatus according to a preferred embodiment of the present invention;
FIG. 2 is a schematic structural view of an 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 MOFCCu (BPDC) thin film prepared in example 2;
FIG. 5 is an SEM image of a MOFCCu (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-a peristaltic pump; 4-a control system; 5-solution bottle.
Detailed Description
The following will explain the preparation method of the present invention in 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 the technologies realized based on the above mentioned contents of the present invention are covered in the protection scope of the present invention.
The following detailed description of the process for preparing MOF Cu (BPDC) film by the apparatus of the present invention is provided by way of illustrative specific examples, which further illustrate the beneficial effects of the present invention. These examples should not be construed as limiting the scope of the invention. All the technologies realized based on the above mentioned contents of the present invention are covered in the protection scope of the present invention.
The experimental methods used in the following examples are all conventional methods unless otherwise specified; reagents, materials and the like used in the following examples are commercially available unless otherwise specified.
In the description of the present invention, it should be noted that the terms "first", "second", etc. are used for descriptive purposes only and do not indicate or imply relative importance.
Example 1
The embodiment provides a full-automatic peristaltic pump type device for preparing a film, which comprises a constant-temperature circulator, a peristaltic pump, a control system, a reaction container and a solution bottle, wherein the structural schematic diagram of the device is shown in fig. 2, and the schematic diagrams of all the components are shown in fig. 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 container;
the control system is connected with the peristaltic pump and used for receiving the instruction signal and converting the instruction signal into a motion for instructing 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 through an instruction of the control system;
the reaction container is used for containing the coating liquid and the modified substrate, and the circulating liquid of the constant-temperature circulator can 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 employs a programmable controller (PLC), such as a memory employing a programmable program, and stores therein instructions for performing operations such as logical operations, sequence control, timing, counting, and arithmetic operations, and inputs and outputs by digital and analog types. The control system can carry out the preparation of the film by controlling the running time, the cycle number and the like of the peristaltic pump, and the schematic view of an operation panel of the control system is shown in figure 1.
Example 2
A metal organic framework (exemplified by mofcu (BPDC)) thin film was prepared using the apparatus described in example 1 above, with a constant temperature circulator of dimensions such as 40 x 25 x 60cm (length/width/height) depending on the laboratory setting; peristaltic pump size such as 28 x 10 x 15cm (length/width/height), the number of sets according to the experiment needs; meanwhile, the reaction container is simply and conveniently selected from a double-layer glass bent bottle, and the method specifically comprises the following steps:
the constant temperature circulator was turned on and the temperature was set to 50 ℃.
Copper acetate and biphenyldicarboxylic acid (H) were weighed2BPDC), mixing themRespectively dissolving the above raw materials in anhydrous ethanol to prepare solutions with the concentrations of 1mmol/L and 0.4mmol/L, 500mL respectively, and taking 500mL of anhydrous ethanol.
Respectively placing the prepared copper acetate ethanol solution, the prepared biphenyldicarboxylic acid ethanol solution and the prepared absolute ethyl alcohol into solution bottles, and connecting each solution bottle with a corresponding peristaltic pump through a peristaltic pump hose.
Then, the quartz glass modified with hydroxyl groups was fixed in a reaction vessel as a growth substrate.
And finally, according to the corresponding arrangement positions of the solution and the peristaltic pump and the requirements of the experimental steps, parameter setting (such as the running time of the peristaltic pump, the stop time of the peristaltic pump, the cycle times and the like) is carried out on the control system, and a 'start cycle' button is clicked after the setting is finished.
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 ketone acetate ethanol solution in the reaction container can completely immerse 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 reacted, a peristaltic pump corresponding to the waste liquid operates for 30 seconds to pump the waste liquid in the reaction container;
3. operating a peristaltic pump corresponding to the absolute ethyl alcohol for 30 seconds, and soaking for 60 seconds to remove the residual copper acetate ethanol solution;
4. the running time of a peristaltic pump corresponding to the biphenyldicarboxylic acid ethanol solution is 30 seconds, and the soaking reaction time is 1200 seconds;
5. after the biphenyl diformic acid ethanol solution is soaked and reacted, a peristaltic pump corresponding to the waste liquid operates for 30 seconds to pump out the waste liquid in the reaction container;
6. operating a peristaltic pump corresponding to the absolute ethyl alcohol for 30 seconds, and soaking for 60 seconds to remove the residual ethyl biphenyldicarboxylate solution;
7. repeating the operation 1-6 times for 30 times to obtain a Cu (BPDC) metal-organic framework (MOFCu (BPDC)) film with a corresponding thickness.
The running time of the peristaltic pump is controlled according to the flow of the peristaltic pump, the shape and the size of the reaction container, the placing mode of the substrate and the like, and the coating liquid is preferably completely submerged in 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 the experimental requirement.
Wherein, FIG. 4 is an XRD spectrum of MOFCCu (BPDC) thin film prepared in example 2; FIG. 5 is an SEM image of a MOFCCu (BPDC) film prepared in example 2; the spectrogram shows that the device can be used for preparing the film with a good morphology structure, and the device can completely replace manual operation to form a batch film preparation process.
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, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. A full-automatic peristaltic pump type device for preparing a film is a device for preparing a film on a substrate by a liquid phase epitaxial growth method by utilizing a full-automatic control system of a peristaltic pump;
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 and realizing high-precision temperature control and measurement of an external system;
the control system is connected with the peristaltic pump and used for receiving an 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 liquid and is connected with the peristaltic pump;
the peristaltic pump is used for introducing the film coating liquid in the solution bottle into the reaction container or discharging waste liquid in the reaction container according to a certain sequence through an instruction of the control system;
the reaction container is used for containing the coating liquid introduced by the peristaltic pump and a substrate, and circulating liquid of the constant-temperature circulator can circulate, so that the temperature of the reaction container is kept constant, and the influence of external conditions on the growth process of the film is reduced.
2. The apparatus of claim 1, wherein the constant temperature circulator allows the reaction vessel to produce a thin film over a temperature range of-20 ℃ to 150 ℃.
3. The apparatus of claim 1, wherein the reaction vessel is a double-glazed structure.
4. The apparatus of claim 3, wherein the reaction vessel is a double-glass curved bottle structure.
5. The apparatus according to any one of claims 1 to 4, wherein the control system employs a programmable controller, in which instructions for performing logical operations, sequence control, timing, counting and arithmetic operations are stored, and selects and controls the operation time, stop time and cycle number of the peristaltic pump through digital, analog input and output.
6. The device according to any one of claims 1 to 4, wherein the volume of the solution bottle is 100 to 2000 mL.
7. The device according to any one of claims 1 to 4, wherein the connection of the solution bottle to the peristaltic pump is achieved by a peristaltic pump hose.
8. The device of any one of claims 1-4, wherein the device has a ratio of length to width to height of the thermostatic circulator of 8:5: 12.
9. The device of any one of claims 1-4, wherein the peristaltic pump has a ratio of 5.6:2:3 in length to width.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111437790A (en) * | 2020-04-15 | 2020-07-24 | 河南科技大学 | Differential pressure type liquid phase timing reaction device for laboratory |
| CN111704733A (en) * | 2019-03-18 | 2020-09-25 | 中国科学院福建物质结构研究所 | Full-automatic peristaltic pump type device for preparing film |
| CN113968983A (en) * | 2020-07-24 | 2022-01-25 | 中国科学院福建物质结构研究所 | Layer-by-layer brushing preparation method of film |
-
2019
- 2019-03-18 CN CN201920341539.1U patent/CN210261614U/en active Active
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111704733A (en) * | 2019-03-18 | 2020-09-25 | 中国科学院福建物质结构研究所 | Full-automatic peristaltic pump type device for preparing film |
| CN111704733B (en) * | 2019-03-18 | 2024-04-12 | 中国科学院福建物质结构研究所 | Full-automatic peristaltic pump type film preparation device |
| CN111437790A (en) * | 2020-04-15 | 2020-07-24 | 河南科技大学 | Differential pressure type liquid phase timing reaction device for laboratory |
| CN113968983A (en) * | 2020-07-24 | 2022-01-25 | 中国科学院福建物质结构研究所 | Layer-by-layer brushing preparation method of film |
| CN113968983B (en) * | 2020-07-24 | 2022-12-06 | 中国科学院福建物质结构研究所 | Layer-by-layer brushing preparation method of film |
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