CN113571862B - Rapid manufacturing method of flexible filter - Google Patents
Rapid manufacturing method of flexible filter Download PDFInfo
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- CN113571862B CN113571862B CN202110508169.8A CN202110508169A CN113571862B CN 113571862 B CN113571862 B CN 113571862B CN 202110508169 A CN202110508169 A CN 202110508169A CN 113571862 B CN113571862 B CN 113571862B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01P—WAVEGUIDES; RESONATORS, LINES, OR OTHER DEVICES OF THE WAVEGUIDE TYPE
- H01P11/00—Apparatus or processes specially adapted for manufacturing waveguides or resonators, lines, or other devices of the waveguide type
- H01P11/007—Manufacturing frequency-selective devices
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
- G01R31/00—Arrangements for testing electric properties; Arrangements for locating electric faults; Arrangements for electrical testing characterised by what is being tested not provided for elsewhere
Abstract
A method for rapid manufacturing of a flexible filter, comprising the steps of: (1) adopting a computer to carry out simulation design on the flexible microwave filter to obtain theoretical structure size parameters of the flexible microwave filter; (2) preparing the flexible microwave filter with the structural design completed in the step (1) by adopting a normal-temperature wet process; (3) carrying out electrical performance test and/or mechanical performance test on the flexible band-pass filter obtained in the step (2), if the test result deviates from the expected value, adjusting parameters, returning to the step (1) and/or the step (2), and remanufacturing the flexible microwave filter; and (3) if the test result meets the expected value, fixing the parameters in the steps (1) and (2) and carrying out batch production on the flexible microwave filter. The efficiency of researching the manufacturing process parameters of the flexible microwave filter is greatly improved, the optimal process parameters can be obtained only by trial production of one sample, and the labor cost of scientific research personnel is greatly reduced.
Description
The application is a divisional application of a manufacturing method of a flexible microwave filter, and the application date of the application is as follows: 2020.07.06, application No. 202010640641.9, entitled: a method for manufacturing a flexible microwave filter.
Technical Field
The invention relates to a rapid manufacturing method of a flexible microwave filter, which is a divisional application of CN 2020106406419.
Background
In practical application, flexible filters are usually required to be adapted to different occasions, and only some existing researches on electrical and mechanical properties cannot completely meet practical requirements. A filter is a device that allows only waves in a particular frequency band to pass through and shields other unwanted signal transmission frequency bands. Compared with a rigid filter, the flexible filter generally has the advantages of small volume, conformality, light weight and the like, and is widely applied to equipment or systems such as aerospace, mobile communication, satellite communication and the like. As a key component of a wireless communication system, the performance of a flexible filter directly affects the operation of the system.
The relevant background art documents (without limitation) are listed below:
[1]Zhang X，Grajal J，Vazquez-Roy J L，et al.Two-dimensional MoS2-enabled flexible rectenna for Wi-Fi-band wireless energy harvesting[J].Nature，2019，566(7744)：368-372.
[2]Jiang Y，Zhao Y，Zhang L，et al.Flexible film bulk acoustic wave filters toward radiofrequency wireless communication[J].Small，2018，14(20)：1703644.
[3]Xu S X，Liu W，Hu B M，et al.Circuit-integratable high-frequency micro supercapacitors with filter/oscillator demonstrations[J].Nano Energy，2019，58：803-810.
[4]Nikoobakht A，Aghaei J，Khatami R，et al.Stochastic flexible transmission operation for coordinated integration of plug-in electric vehicles and renewable energy sources[J].Applied Energy，2019，238：225-238.
[5]Pan T S，Dai L L，Chen S H，et al.Low-impedance flexible archimedean-equiangular spiral antenna[J].IEEE Antennas and Wireless Propagation Letters，2019，18(9)：1789-1793.
[6] application study of the baxizhuang, weiweiping, multiband filtering technique in partial discharge detection [ J ] technological propagation, 2016 (2): 104-105.
[7] Design of DGS-based UWB filter [ D ]. harbin: harbin engineering university, 2014: 5-15.
[8] Yaanpinti, research and design of ultra wide band microwave filter [ D ]. Nanjing: nanjing university of aerospace, 2009: 6-14.
The present patent application is a divisional application of the parent CN 2020106406419, and is proposed to overcome the problems pointed out by the first examination opinions of examiners.
Disclosure of Invention
An object of the present invention is to provide a method of manufacturing a flexible microwave filter. Another object of the present invention is to provide a method for rapidly optimizing a manufacturing process of a flexible microwave filter.
The specific technical scheme for realizing the purpose of the invention is as follows:
a method of manufacturing a flexible microwave filter, comprising the steps of:
(1) research on flexible substrate material
LCP (liquid crystal polymer) and PI (polyimide) are flexible filter substrates that are commonly used at present. LCP has the defects of higher cost and lower yield, and PI is cheaper than LCP. Besides, the substrate of the flexible filter is selected from polyimide materials in consideration of the advantages of extremely high thermal stability, excellent mechanical properties, stable chemical properties and the like of the PI.
(2) Design of flexible microwave filter
Compared with microstrip lines, a Coplanar Waveguide (CPW) has the characteristics of small size, high design flexibility, and low manufacturing difficulty. Meanwhile, because the signal line and the ground wire of the coplanar waveguide structure are on the same side, the single-side preparation requirement of the flexible substrate can be met, and therefore the coplanar waveguide structure is selected to be used for designing the filter. The design methods of the filter mainly include two types, namely a distributed parameter method and a lumped parameter method, but the structural design and calculation of the two methods are usually complicated. To solve the above problems, the present invention proposes an inverted converter structure. The structure can meet the requirement of series connection or parallel connection at the same point, and makes up the defects of two common methods.
(3) Performance study of Flexible filters
Firstly, the improved normal-temperature wet process is used for preparing the flexible band-pass filter with the finished structure design. Next, in order to demonstrate the feasibility of using this process to fabricate flexible filters, filter performance was tested and studied. Since the application environment of the flexible filter is variable, it is not possible to fully satisfy the application requirement of the flexible filter only by studying the performance of the filter in the flat or curved state. Therefore, in addition to the straight and bending test of the flexible filter, the performance of the flexible filter in a series of states of different folding, bending, curling and the like is also researched.
Before the flexible microwave filter is formally manufactured, the flexible microwave filter is firstly designed and simulated according to expected performance indexes. The specific design flow is shown in fig. 2.
The traditional process for preparing the flexible filter is easy to have the problems of low bonding force between the metal layer and the surface of the thin film, expensive used equipment and the like[53]. In order to solve the above problems, the present invention proposes to use a normal temperature wet process. The process realizes the surface metallization of the polyimide film, can prepare the flexible microwave filter meeting the circuit requirements, does not depend on expensive equipment, and can carry out the preparation process under the conditions of normal temperature and normal pressure.
The normal temperature wet process utilizes the characteristic that the polyimide film is not hydrolysis-resistant in an alkaline environment, and forms a surface ring-opened modified layer by treating the strong alkaline solution on the surface of the film; secondly, the etched film is placed in silver salt solution and passes through Ag+Diffusing, ion exchanging with active group on the surface of PI to make Ag+Entering a molecular chain; finally, the film is chemically reduced to lead the Ag+Reducing and gathering at the surface of the film to prepare the PI/Ag composite film with high conductivity and high reflectivity. The whole process of the process is carried out at normal temperature and normal pressure, and high-temperature thermal annealing and vacuum preparation conditions do not need to depend on expensive equipment. The invention confirms the proper process flow for preparing the PI/Ag composite film through experiments.
The complete flow is shown in fig. 1:
(1) adopting a computer to carry out simulation design on the flexible microwave filter to obtain theoretical structure size parameters of the flexible microwave filter;
(2) preparing the flexible microwave filter with the structural design completed in the step (1) by adopting a normal-temperature wet process;
(3) carrying out electrical performance test on the flexible band-pass filter obtained in the step (2), if the test result deviates from the expected value, adjusting parameters, returning to the step (1) and/or the step (2), and remanufacturing the flexible microwave filter; and (3) if the test result meets the expected value, fixing the parameters in the steps (1) and (2) and carrying out mass production on the flexible microwave filter.
The specific manufacturing process of the flexible microwave filter based on the normal temperature wet process provided by the invention is shown in fig. 3. Step (3) in fig. 3 is a pattern of the flexible microwave filter required for inkjet printing, and step (4) is a cleaning step; the steps (1), (2) and (4) are hydrolysis reaction, ion exchange reaction and reduction reaction processes respectively.
The invention uses potassium hydroxide solution as strong alkali solution to modify the surface, uses silver ammonia solution to realize ion exchange, and uses hydrogen peroxide as reducing agent. Fig. 4 shows the main chemical reaction equation of the PI film in the process of surface metallization. As can be seen from fig. 4, the surface of the polyimide is firstly reacted with KOH solution, and after the amide bond is attacked, the amide bond is opened to form polyamic acid salt (poly (amic acid), PAA), so as to modify the surface of the thin film; and finally, carrying out reduction treatment by hydrogen peroxide, wherein the silver ions adsorbed on the surface of the film are reduced into metallic silver, and simultaneously, a large amount of oxygen is generated.
The three chemical reaction equations in fig. 4 correspond to the chemical reactions of steps (1) (2) (4) in fig. 3 in sequence.
The three chemical reaction equations relate to three process parameters of the flexible microwave filter: (I) the effect of KOH solution treatment time on resistivity; (II) Ag (NH)3)2The effect of OH solution treatment time on resistivity; (III) H2O2Solution treatment time pairThe effect of the resistivity. The resistivity refers to the resistivity of the metal layer of the flexible microwave filter.
In order to obtain the optimal values of the three process parameters, the invention also provides a manufacturing process parameter optimization research method. Namely:
and a dripping device is adopted, so that the liquid level of the solution in the container is lowered at a constant speed, the polyimide film is vertically placed in the container, and when the solution starts dripping, a timer is used for timing. And when the solution is dripped, stopping timing by the timer to obtain the consumed time of the whole reaction process.
In the technical scheme of the invention, as the liquid level height of the solution in the container is reduced at a constant speed, different heights of the polyimide film from the initial liquid level linearly represent the solution processing time, and finally the resistivity of the polyimide film at different heights is measured, namely the influence of the solution processing time on the resistivity can be correspondingly obtained.
The invention has the beneficial effects that:
the filter preparation technology based on the normal-temperature wet process provided by the invention does not need expensive equipment and harsh environment control, makes up for the defects of the traditional process at present, and can still keep the performance of a manufactured device better. The developed flexible filter can be applied to various working occasions and is expected to become a component of future flexible equipment.
According to the method, the efficiency of researching the manufacturing process parameters of the flexible microwave filter is greatly improved, the optimal process parameters can be obtained only by completing the trial production of one sample, and the labor cost of scientific research personnel is greatly reduced; the method is completely different from the traditional research method, and the traditional research method needs to trial-produce a large number of samples to obtain proper process parameters. Because the method of the present invention, the liquid level in the container is continuously and linearly decreased, and the whole process is continuous, the resistivity at any height of the measured polyimide film corresponds to one solution processing time. Theoretically, the process parameter influence curve obtained in the process of trial production of one sample is equivalent to the process parameter influence curve obtained only by trial production of samples by an infinite number of traditional methods. This further highlights the advantages of the invention.
Drawings
Fig. 1 is a complete flow of the manufacture of a flexible microwave filter.
Fig. 2 is a specific design flow of the flexible microwave filter.
Fig. 3 is a specific manufacturing flow of the flexible microwave filter based on the normal temperature wet process.
Fig. 4 is three chemical reaction equations successively involved in the normal temperature wet process based on fig. 3.
FIG. 5 shows a test apparatus according to the present invention.
Fig. 6 is a graph showing the thickness measurements of the silver layer at different positions of the flexible microwave filter obtained in one example.
Fig. 7 is an SEM image of the flexible microwave filter obtained in one example.
Detailed Description
For the convenience of understanding, the technical scheme of the invention is specifically described by combining the examples.
The main raw materials adopted in the manufacturing process of the invention are shown in table 1, and the reagents and raw materials used in the experimental process are all common experimental reagents.
TABLE 1 Main test reagents and raw materials
The whole process of the manufacturing process is carried out at normal temperature and normal pressure, and the main process steps are as follows:
a. cleaning of
The cleanliness of the polyimide surface directly affects the properties of the final composite film. Therefore, the polyimide film was first cleaned using a large amount of absolute ethanol and acetone solution before the reaction started.
b. Hydrolysis reaction
100ml of KOH solution was prepared, and the concentration was set at 4 mol/L. In order to obtain sufficient dissolution of the KOH solid in solution, the prepared KOH solution is typically left to stand overnight for the next day of use. And (3) immersing the cleaned film into the prepared potassium hydroxide solution to perform hydrolysis reaction, and taking out after 3 hours. In order to prevent the unreacted hydroxyl from generating chemical reaction with other treatment liquids in subsequent experiments, after the surface modification is completed, the surface of the film is washed by using a large amount of deionized water and ultrasonically cleaned so as to clean the solution remained on the surface of the film.
c. Ion exchange
100ml of silver ammonia solution with the concentration of 0.04mol/L is prepared. It should be noted that the silver ammonia solution is needed to be taken and used immediately, so as to prevent the solution from volatilizing after the standing time is too long and influence the experimental effect. And (3) putting the film cleaned before into the prepared silver ammonia solution for ion exchange reaction, wherein the process lasts for 2 hours, so that potassium ions and silver ammonia complex ions on the surface of the film are fully replaced. Similarly, in order to prevent the silver salt solution from remaining and affecting the subsequent experimental process, after the reaction is completed, the film is taken out to be cleaned and naturally dried at normal temperature.
d. Reduction reaction
1000ml of hydrogen peroxide solution with the concentration of 0.01mol/L is prepared. And immersing the dried film into the prepared hydrogen peroxide solution for rapid reduction operation, and obtaining the metal layer with a smooth surface after 30 seconds.
In order to prove that the silver layer prepared by the normal-temperature wet method is uniform, the thickness of the silver layer is measured at different positions of the silver layer, and the test result is shown in fig. 6. As can be seen from FIG. 6, the thicknesses of the five tests were 7.803 μm, 7.787 μm, 7.811 μm, 7.796 μm and 7.801 μm, respectively. This demonstrates that the silver layer obtained by the reaction is substantially uniform, meeting the requirements for the manufacture of flexible devices. The prepared PI/Ag composite film has the effects of smooth and compact surface and uniform section thickness. These results all meet the basic fabrication requirements for circuits.
The chemical reaction equations in steps b, c and d correspond to the three chemical reaction equations in fig. 4, respectively.
According to the result of computer simulation, when the requirement is met, a computer model can be instantiated, and the steps are as follows:
1. mask layer printing
The required pattern was drawn using Visio software. The polyimide film after natural drying was spread and smoothly stuck on a4 paper, and the mask layer was transferred to the surface of the film by a general and office laser printer. During the pasting process, it is necessary to ensure that the film is completely attached to the A4 paper, otherwise the mask transferring effect is affected.
2. Chemical reduction
The hydrogen peroxide is used as a clean reagent and is environment-friendly. The metal ions are quickly reduced by using 0.01mol of hydrogen peroxide, and the process can be finished in only 30 seconds. Due to the shielding of the mask layer, the silver ions on the surface of the area which is not masked are only reduced into silver by hydrogen peroxide.
3. Masking layer processing
The reduction reaction only reduces silver ions into silver atoms, and the mask layer is not affected, namely after the reduction reaction is finished, the mask layer on the surface of the PI/Ag composite film needs to be subjected to subsequent treatment. The mask pattern is cleaned herein by using an acetone solution.
Through the process, the graphical PI/Ag composite film can be finally realized, namely the required flexible microwave filter is formed.
As can be seen from the above-mentioned manufacturing process, in the manufacturing process of the present invention, the following factors need to be studied in the chemical process:
(I) the effect of KOH solution treatment time on resistivity;
(II)Ag(NH3)2the effect of OH solution treatment time on resistivity;
(III)H2O2effect of solution treatment time on resistivity.
Here, the resistivity refers to the resistivity of the flexible microwave filter.
The above three influencing factors exist in sequence in steps (1) (2) (4) in fig. 3.
In the conventional research method, the influence of each factor needs to be repeated for a plurality of times, a plurality of samples are prepared to test the resistivity of each sample, and then the influence of the change of each factor on the resistivity is obtained. For example, in a conventional research method, in order to obtain the effect of the KOH solution processing time on the resistivity, 0.5 hour, 1 hour, 1.5 hours, 2 hours, 2.5 hours, 3 hours, 3.5 hours, and 4 hours may be respectively used to process samples with the KOH solution, so as to obtain 8 samples processed with the KOH solution, and the resistivity of the 8 samples is tested, so as to analyze the effect of the KOH solution processing time on the resistivity. For Ag (NH)3)2Effect of OH solution treatment time on resistivity, H2O2The effect of solution treatment time on resistivity was the same as for the study method.
Obviously, such a method requires a lot of samples to be prepared and a lot of tests to be performed with different processing times in order to obtain a relatively accurate curve, and the whole process is cumbersome, time-consuming, and error-prone.
In order to solve the technical problem, the invention provides a method for quickly optimizing a manufacturing process of a flexible microwave filter. The specific embodiments are illustrated below:
method for fast study of the effect of KOH solution treatment time on resistivity:
as shown in fig. 5, the container 3 containing the chemical solution is fixedly placed on the frame 1, the frame 1 is provided with an upper fixing mechanism 7, the upper fixing mechanism 7 fixes the container 3 by using bolts 5 and nuts 6, and the bottom of the container 3 is supported by a bottom transverse plate 4. The KOH solution 10 is contained in the container, the bottom of the container 3 is provided with a discharge pipeline 8, the discharge pipeline 8 is provided with a dripping device 9, the dripping device 9 can drip the KOH solution 10 at a preset constant speed, the dripping device 9 is similar to a medical infusion apparatus, and the difference is that the material is alkali-resistant and corrosive. A waste liquid receiver, not shown, is arranged directly below the dripping device 9.
A polyimide film 12 is placed in the container 3, the length of the polyimide film 12 being greater than the depth of the container 3.
While the polyimide film 12 was placed in the container 3 with sagging, the switch of the dripping device 9 was immediately turned on to drip the KOH solution at a predetermined constant speed, and the timer 11 was used to start timing.
The container is a container which always keeps constant horizontal sectional area at different heights, such as a cylindrical container or a square cylindrical container. In such a container 3, when the dripping device 9 drips the KOH solution at a constant speed, the height of the liquid level 2 of the KOH solution in the container 3 is also lowered at a constant speed, and as a result, the action time of the KOH solution 10 on the polyimide film 12 at different heights is linear with the corresponding heights.
For example, below the liquid level, the polyimide film is 1cm from the initial liquid level and immersed in the KOH solution for 5min, and then the polyimide film is 2cm from the initial liquid level and immersed in the KOH solution for 10min, which are recurrently repeated, with the polyimide film being 3cm from the initial liquid level and immersed in the KOH solution for 15min, … ….
Further, it can be concluded that, in such a technical solution of the present invention, since the liquid level of the KOH solution in the container is decreased at a constant rate, different heights of the polyimide film from the initial liquid level linearly represent the KOH solution processing time, and finally the resistivity of the polyimide film at different heights is measured, so as to obtain the effect of the KOH solution processing time on the resistivity.
Preferably, the polyimide film is tightly fixed on the corrosion-resistant elongated plate without wrinkles, and the polyimide film and the corrosion-resistant elongated plate are placed in the container together, so that the time of the action of the KOH solution on different heights of the polyimide film has an accurate linear relation.
When the solution 10 in the container 3 is completely dripped, the timer 11 is stopped to count time, and the time of the whole reaction process is obtained.
Similarly, Ag (NH) was studied3)2In the treatment of OH solutionInfluence of the spacing on the resistivity, H2O2The effect of solution treatment time on resistivity, and so on. Except that Ag (NH) was studied3)2When the OH solution treatment time affects the resistivity, the materials of the container, the dripping device and the strip-shaped plate are selected not to be Ag (NH)3)2Material of OH solution reaction; study H2O2When the solution treatment time affects the resistivity, the container, the dripping device and the strip-shaped plate are made of materials different from H2O2The material of the solution reaction.
The KOH solution in the vessel was exchanged for Ag (NH) at different experimental stages3)2OH solution, H2O2And (3) solution. Before replacement, the container is cleaned. Three sets of identical test devices can also be prepared, and KOH solution and Ag (NH) can be respectively put into the containers of the three sets of test devices3)2OH solution, H2O2The solution, polyimide film, was transferred between three containers.
Claims (5)
1. A method for rapidly manufacturing a flexible filter, wherein a flexible substrate is a polyimide film, and the manufacturing method comprises the following steps:
(1) adopting a computer to carry out simulation design on the flexible microwave filter to obtain theoretical structure size parameters of the flexible microwave filter;
(2) and (2) manufacturing the flexible microwave filter with the structural design completed in the step (1) by adopting a normal-temperature wet process, wherein the polyimide film of the flexible substrate undergoes the following chemical reactions in sequence:
(3) carrying out electrical performance test and/or mechanical performance test on the flexible band-pass filter obtained in the step (2), if the test result deviates from the expected value, adjusting parameters, returning to the step (1) and/or the step (2), and remanufacturing the flexible microwave filter; and (3) if the test result meets the expected value, fixing the parameters in the steps (1) and (2) and carrying out mass production on the flexible microwave filter.
2. The method of claim 1, wherein: the step (2) is specifically described as follows:
(A) using KOH solution to carry out surface modification on the polyimide film;
(B) using Ag (NH)3)2The OH solution realizes ion exchange on the surface of the polyimide film obtained in the step (A);
(C) printing a pattern of a required flexible microwave filter on the surface of the polyimide obtained in the step (B) by ink jet;
(D) by H2O2Carrying out reduction treatment on the surface of the polyimide obtained in the step (C);
(E) cleaning the polyimide film obtained in the step (D);
finally obtaining the high-conductivity and high-reflectivity patterned polyimide/Ag composite film.
3. The method of claim 1, wherein: the mechanical performance test in the step (3) includes but is not limited to: and carrying out performance tests on the flexible microwave filter in straight, bent, folded, bent and curled states.
4. The method of claim 2, wherein: the chemical process in the method has the following three influencing factors:
(I) the effect of KOH solution treatment time on resistivity;
(II)Ag(NH3)2the effect of OH solution treatment time on resistivity;
(III)H2O2the effect of solution treatment time on resistivity;
the resistivity refers to the resistivity of the metal layer of the flexible microwave filter.
5. The method of claim 4, wherein: in the step (3), the parameters in the adjusting step (2) are specifically: the three influencing factors are quickly obtained through experiments.
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| CA2352567A1 (en) * | 2001-07-06 | 2003-01-06 | Mohamed Latreche | Translucent material displaying ultra-low transport of gases and vapors, and method for its production |
| CN106544655A (en) * | 2016-10-13 | 2017-03-29 | 上海交通大学 | A kind of preparation method of polyimide surface patterned conductive Ag films |
| CN107452685A (en) * | 2016-03-16 | 2017-12-08 | 阿尔莫 | Print the manufacture method of photovoltaic module and related photovoltaic module |
| CN110854488A (en) * | 2019-11-25 | 2020-02-28 | 天津大学 | Band-pass filter based on flexible substrate and manufacturing method |
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| CN101838399A (en) * | 2010-05-28 | 2010-09-22 | 北京化工大学 | Preparation method of polyimide/silver composite film having conduction and reflection characteristics |
| CN107238648A (en) * | 2017-06-13 | 2017-10-10 | 复旦大学 | The method of low temperature preparation two-dimension flexible ion sensing fet |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2352567A1 (en) * | 2001-07-06 | 2003-01-06 | Mohamed Latreche | Translucent material displaying ultra-low transport of gases and vapors, and method for its production |
| CN107452685A (en) * | 2016-03-16 | 2017-12-08 | 阿尔莫 | Print the manufacture method of photovoltaic module and related photovoltaic module |
| CN106544655A (en) * | 2016-10-13 | 2017-03-29 | 上海交通大学 | A kind of preparation method of polyimide surface patterned conductive Ag films |
| CN110854488A (en) * | 2019-11-25 | 2020-02-28 | 天津大学 | Band-pass filter based on flexible substrate and manufacturing method |
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