CN104977338A - Method for processing microelectrode on PDMS substrate based on inkjet printing technology - Google Patents
Method for processing microelectrode on PDMS substrate based on inkjet printing technology Download PDFInfo
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Abstract
The invention relates to a method for processing a microelectrode on a PDMS substrate based on an inkjet printing technology. The method comprises: preparing a PDMS substrate, wherein a PDMS monomer and a curing agent are uniformly mixed according to a mass ratio of 10:1, gas bubbles are removed, the PDMS mixed with the curing agent is poured onto the surface of a polished silicon wafer, and the obtained material is placed into a constant temperature oven for 2 h to cure; increasing adhesion of the PDMS on the metal electrode; and carrying out splitting and re-combination on the effective pixel part in the original electrode pattern by using a digital image treatment method, and then carrying out spray printing in a one-by-one manner according to the effective pixel in the new pattern. According to the present invention, the problem of poor electrode continuity caused by the surface tension of the liquid droplet is overcome, the hydrophobic property of the PDMS surface is improved, the processing efficiency is improved, and the poor adhesion of the silver electrode on the PDMS surface is solved; and the method has characteristics of high efficiency, convenience and high automation degree, and the processed electrode has characteristics of good PDMS surface adhesion and high quality.
Description
Technical field
The present invention relates to one and process microelectrode on PDMS.Particularly relate to a kind of jet printing method of Pixel-level and utilize chemical coupling agent MPTMS to improve its surface hydrophobicity characteristic and the adhering method of processing microelectrode in PDMS substrate based on inkjet technology with silver electrode to surperficial modification of PDMS.
Background technology
Micro-fluidic chip based on PDMS (dimethyl silicone polymer) has been widely used in the fields such as biomacromolecule detection, electrochemical sensing, Medical Instruments manufacture and wearable device.PDMS is as a kind of flexible material, and its nontoxic, transparent, easy processing and bio-compatibility well all become the preferred material manufacturing integrated upper sensor-based system.But the biology sensor of integrated microelectrode formation functionalization remains a challenge of scientific circles in microfluidic channel, because process the technical barrier that microelectrode is a whole academia of puzzlement on PDMS always.As a kind of biomaterial, the poor adhesion of PDMS and metal, is unfavorable for that metal microelectrode adheres to, and this seriously constrains it in micro-fluidic and application that is electrochemical sensing field.
The method of processing microelectrode at present on PDMS mainly contains chemical reduction method, evaporation or sputtering method, silk screen print method and pattern transfer method etc.But chemical reduction method needs for processing microtubule road in advance containing the solution of metal cation, wayward to the concentration of chemical solution, and the continuity of electrode and poorly conductive; And evaporation or sputtering method are only for naive model, complex model needs mask, and needs huge vacuum installations; The microelectrode thickness that silk screen print method processes comparatively large (5-10um), makes, sealing is poor between layers with during other PDMS layer bonding, usually to cause the fluid sample in microtubule road to leak; Pattern transfer method is a kind of common method, which solves the problem of microelectrode in PDMS surface attachment, but needs electrode to process on other substrates by additive method, so complex process, especially, time larger for electrode area, its long processing time, efficiency is low.Inkjet technology makes on PDMS, process microelectrode as a kind of process technology of rising gradually in recent years becomes possibility.Inkjet technology achieves only at appointed area machined electrode, and without the need to mask, and thickness of electrode is less than 100nm, meets the bonding requirement of micro-fluidic chip.Its automaticity is high, and process is efficient, save time, and is a kind of Perfected process processing microelectrode on PDMS.
The drop spacing that Fig. 1 a, Fig. 1 b are arranged when illustrating system spray printing, and the actual diameter depending on drop in different base of this spacing, in order to form the silver electrode layer that continuity is better, edge is more neat, drop spacing is preferably arranged to the half of liquid-drop diameter, and such adjacent drops can overlap to form the higher electrode layer of quality.
As shown in Fig. 2 a, Fig. 2 b, PDMS surface is extremely hydrophobic, cause liquid-drop diameter less, cannot spread out in substrate, be unfavorable for the evaporation of drop solvent like this, because the operating rate of sprayed printed system and drop spacing (from Fig. 2 a, Fig. 2 b, less liquid-drop diameter needs to arrange less drop spacing) are directly proportional, so the hydrophobic property on PDMS surface causes process consuming time longer.
As shown in Figure 3, the problem shown in Fig. 2 a, Fig. 2 b to result between adjacent moistening drop because surface tension is attracted each other, is shifted and defines larger circular drop equally, former spray printing region is occurred blank, is unfavorable for that the good electrode of continuity is formed like this.
So need to improve the hydrophobic property on PDMS surface and overcome attracting each other between adjacent drops, displacement problem.
Summary of the invention
Technical matters to be solved by this invention is, provides a kind of process simple, efficient, can realize the method for processing microelectrode in PDMS substrate based on inkjet technology that is higher in PDMS upper surface crudy, the good silver electrode of adhesiveness
The technical solution adopted in the present invention is: a kind of method of processing microelectrode in PDMS substrate based on inkjet technology, comprises the steps:
1) be first the preparation of PDMS substrate, PDMS monomer is mixed according to mass ratio 10:1 with hardening agent, removing bubble, is evenly poured over the silicon chip surface of polishing, then places in constant temperature oven and be cured for 2 hours by the PDMS being mixed with hardening agent;
2) increase PDMS to the adhesiveness of metal electrode, comprising:
(1) PDMS after solidification peeled off from silicon chip surface and cut into the shape of setting, as the substrate of electrode machining;
(2) MPTMS and ethanol are mixed and made into the ethanolic solution of MPTMS with volume ratio 1:200;
(3) PDMS substrate is immersed in the ethanolic solution of MPTMS;
(4) PDMS substrate is taken out after cleaning dries up, to be soaked in the hydrochloric acid solution of 0.1M 0.7 ~ 1.2 hour, by washed with de-ionized water and empty airflow drying after taking-up;
3) utilize the method for Digital Image Processing the valid pixel part in original electrode pattern to be carried out splitting and reconfiguring, then carry out spray printing one by one according to the valid pixel in new figure.
Step 1) described in bubble removing be remove bubble in vacuum tank.
Step 1) described in constant temperature oven be the constant temperature oven of 60 ~ 80 DEG C.
Step 2) in (3) step be PDMS substrate to be immersed in the ethanolic solution of MPTMS 0.6 ~ 1.2 hour.
Step 2) in (4) step in be dry up being immersed in MPTMS ethanolic solution after PDMS substrate is taken out in air stream with ethanol purge.
Step 3) described in the valid pixel part in original electrode pattern is carried out splitting and reconfiguring, be by horizontal and vertical for former graphic file upper respectively with two valid pixels for interval, pixel element in the two directions at a distance of two pixels is taken out, be reassembled into new graphic file, former figure is made to be divided into 9 parts, interval between pixel in so new graphic file just becomes 3 drop spacing, then carries out spray printing one by one successively in order according to the valid pixel in new figure.
Described is undertaken splitting and reconfiguring by the valid pixel part in original electrode pattern, specifically comprises:
(1) the total pixel value of image on horizontal and vertical is determined;
(2), based on these two the total pixel values on horizontal and vertical, circulation obtains the pixel of all two pixels of being separated by horizontal and vertical from being positioned at the pixel of image the first row first row;
(3) all pixels (2) step obtained are the graphic file of white stored in a background colour;
(4) from the pixel of the first row secondary series, according to horizontal and vertical principle of reading in a pixel every two pixels, circulation obtains pixel, then stored in new image file, the like, carry out nine circulations, complete the fractionation of all pixels in original image and reconfigure, obtain nine new graphic files.
When carrying out spray printing in order successively one by one according to the valid pixel in new figure, after numerous droplet dryings of previous spray printing be waited until, then carry out spray printing next time.
The method of processing microelectrode in PDMS substrate based on inkjet technology of the present invention, have employed unique Pixel-level jet printing method, overcome the problem of the electrode continuities difference that drop causes due to capillary effect well, and use MPTMS to carry out chemical modification to PDMS first, not only improve the hydrophobic property on PDMS surface well, improve working (machining) efficiency, and solve the problem of silver electrode in PDMS surface adhesive difference well.Compared in the past in the method for PDMS surface working electrode, the present invention is efficiently simple and direct, and automaticity is high, and the electrode processed is good at PDMS surface adhesion, and quality is high, is applicable to being applied in micro-fluid chip and carries out biomacromolecule detection and electrochemical sensing.There is following features:
1. the processing of the PDMS surface microelectrode in the present invention adopts inkjet technology, and compared with other techniques, process is without the need to additional means, and flow process is simply direct.
2. introduce a kind of jet printing method of Pixel-level in the present invention, effectively overcome the problem of the electrode continuities difference caused because surface tension attracts each other between moistening drop.
3. introduce chemical coupling agent MPTMS in the present invention first to modify PDMS surface, effectively improve the inherent shortcoming of the poor adhesion between PDMS and metal electrode.
4. the MPTMS chemical modification method introduced in the present invention effectively improves the hydrophobic property on PDMS surface simultaneously, and the drop being is larger at PDMS Dispersion on surface area, accelerates the velocity of evaporation of drop solvent, improves electrode machining efficiency.
Accompanying drawing explanation
Fig. 1 a is the relation schematic diagram between the liquid-drop diameter that sprays of sprayed printed system and drop spacing;
Fig. 1 b is the schematic diagram that drop spacing should be set to liquid-drop diameter half for forming continuity good electrode;
Fig. 2 a is the schematic diagram that drop adheres in hydrophobic substrate;
Fig. 2 b be drop at the bottom of hydrophilic group on the schematic diagram that adheres to;
Fig. 3 is that moistening drop causes because surface tension attracts each other occurring blank schematic diagram in the electrode of spray printing;
Fig. 4 is the technological process that the present invention processes microelectrode on PDMS;
Fig. 5 utilizes MPTMS to carry out the schematic flow sheet of chemical modification to PDMS;
Fig. 6 a is the schematic diagram of the pixel of same color in the jet printing method of Pixel-level in the present invention;
Fig. 6 b is the schematic diagram that the jet printing method Central Plains graphic file of Pixel-level in the present invention is divided into 9 parts.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the method for processing microelectrode in PDMS substrate based on inkjet technology of the present invention is described in detail.
The method of processing microelectrode in PDMS substrate based on inkjet technology of the present invention, that what to adopt be model is Dimatix 2831, Fujifilm, Japan's can the ink-jet printer of ejected silver nanoparticles solution, due to nozzle moving left and right and chassis movable on spray printing support bar, the silver nano-grain drop sprayed by nozzle just can process the silver layer model of two-dimensional structure, chassis temperature is 60 DEG C, and after the evaporation of drop solvent, the gathering of silver nano-grain deposition just forms continuous silver layer.Because system carries out spray printing according to the image file designed in advance, so the local depositing silver nano particle only needed, without the need to mask, process is efficiently simple and direct.
The method of processing microelectrode in PDMS substrate based on inkjet technology of the present invention, comprises a kind of spray printing processing procedure of Pixel-level and utilizes chemical coupling agent MPTMS to improve its surface hydrophobicity characteristic and the adhering process with silver electrode to surperficial modification of PDMS.As shown in Figure 4, comprise the steps:
1) be first the preparation of PDMS (dimethyl silicone polymer) substrate, PDMS monomer is mixed according to mass ratio 10:1 with hardening agent, removing bubble, described bubble removing removes bubble in vacuum tank, the PDMS being mixed with hardening agent is evenly poured over the silicon chip surface of polishing, then places 2 hours in constant temperature oven, make it solidification, wherein, described constant temperature oven is the constant temperature oven of 60 ~ 80 DEG C, is PDMS substrate to be immersed in the ethanolic solution of MPTMS 0.6 ~ 1.2 hour;
2) increase PDMS to the adhesiveness of metal electrode, comprising:
(1) PDMS after solidification peeled off from silicon chip surface and cut into the shape of setting, as the substrate of electrode machining;
(2) MPTMS and ethanol are mixed and made into the ethanolic solution of MPTMS with volume ratio 1:200, namely utilize MPTMS to carry out chemical modification to PDMS surface, as the MPTMS of 0.5mL is dissolved in 100mL ethanol;
(3) being immersed in the ethanolic solution of MPTMS by PDMS substrate, is PDMS substrate to be immersed in the ethanolic solution of MPTMS 0.6 ~ 1.2 hour;
(4) after PDMS substrate taking-up cleaning being dried up, be with ethanol purge and dry up in air stream, then 0.7 ~ 1.2 hour is soaked in the hydrochloric acid solution of 0.1M, be hydrolyzed, by washed with de-ionized water and empty airflow drying after taking-up, increase the adhesiveness of PDMS to metal electrode with this, be convenient to manufacture the high electrode of reliability, through the PDMS that modifies using the substrate as machined electrode;
This step 2) hydrophobic property improving PDMS surface is modified to PDMS surface, when making silvering solution drip attachment, diffusional area is comparatively large, is convenient to accelerate drop evaporation rate of solvent, improves working (machining) efficiency.Y
3) Fig. 6 a, shown in Fig. 6 b, the present invention proposes a kind of jet printing method of Pixel-level, because sprayed printed system carries out spray printing according to the pixel in image file and the drop spacing set by software, so in order to overcome the problem attracted each other between adjacent moistening drop, pixel in original image file is separated according to the principle pixel of identical type (in Fig. 6 a) of taking out every two and reconfigures, so, the method of Digital Image Processing is utilized the valid pixel part in original electrode pattern to be carried out splitting and reconfiguring, then spray printing is carried out one by one according to the valid pixel in new figure.Wherein, described is undertaken splitting and reconfiguring by the valid pixel part in original electrode pattern, be by horizontal and vertical for former graphic file upper respectively with two valid pixels for interval, pixel element in the two directions at a distance of two pixels is taken out, be reassembled into new graphic file, former figure is made to be divided into 9 parts, interval between pixel in so new graphic file just becomes 3 drop spacing, can not contact between drop, also the problem attracting displacement would not be designed, then spray printing is carried out one by one successively in order according to the valid pixel in new figure, effectively overcome between adjacent moistening drop and merge the problem of the electrode continuities difference caused because surface tension attracts each other.When carrying out spray printing in order successively one by one according to the valid pixel in new figure, after numerous droplet dryings of previous spray printing will be waited until, carry out spray printing next time again, due to not dry and attracting each other and displacement problem of causing when so just efficiently avoid drop contact.
Described is undertaken splitting and reconfiguring by the valid pixel part in original electrode pattern, specifically comprises:
(1) the total pixel value of image on horizontal and vertical is determined;
(2), based on these two the total pixel values on horizontal and vertical, circulation obtains the pixel of all two pixels of being separated by horizontal and vertical from being positioned at the pixel of image the first row first row;
(3) all pixels (2) step obtained are the graphic file of white stored in a background colour;
(4) from the pixel of the first row secondary series, according to horizontal and vertical principle of reading in a pixel every two pixels, circulation obtains pixel, then stored in new image file, the like, carry out nine circulations, complete the fractionation of all pixels in original image and reconfigure, obtain nine new graphic files.
The method of processing microelectrode in PDMS substrate based on inkjet technology of the present invention, have employed unique Pixel-level jet printing method, overcome the problem of the electrode continuities difference that drop causes due to capillary effect well, and use MPTMS to carry out chemical modification to PDMS first, not only improve the hydrophobic property on PDMS surface well, improve working (machining) efficiency, and solve the problem of silver electrode in PDMS surface adhesive difference well.Compared in the past in the method for PDMS surface working electrode, the present invention is efficiently simple and direct, and automaticity is high, and the electrode processed is good at PDMS surface adhesion, and quality is high, is applicable to being applied in micro-fluid chip and carries out biomacromolecule detection and electrochemical sensing.
The present invention's all combinations that are open and that disclose can produce by using for reference disclosure herein, although combination of the present invention is described by detailed implementation process, but those skilled in the art obviously can be spliced device as herein described or change not departing from content of the present invention, spirit and scope, or increase and decrease some parts, more particularly, all similar replacements and change apparent to those skilled in the art, they are deemed to be included among spirit of the present invention, scope and content.
Claims (8)
1., based on a method of processing microelectrode in PDMS substrate for inkjet technology, it is characterized in that, comprise the steps:
1) be first the preparation of PDMS substrate, PDMS monomer is mixed according to mass ratio 10:1 with hardening agent, removing bubble, is evenly poured over the silicon chip surface of polishing, then places in constant temperature oven and be cured for 2 hours by the PDMS being mixed with hardening agent;
2) increase PDMS to the adhesiveness of metal electrode, comprising:
(1) PDMS after solidification peeled off from silicon chip surface and cut into the shape of setting, as the substrate of electrode machining;
(2) MPTMS and ethanol are mixed and made into the ethanolic solution of MPTMS with volume ratio 1:200;
(3) PDMS substrate is immersed in the ethanolic solution of MPTMS;
(4) PDMS substrate is taken out after cleaning dries up, to be soaked in the hydrochloric acid solution of 0.1M 0.7 ~ 1.2 hour, by washed with de-ionized water and empty airflow drying after taking-up;
3) utilize the method for Digital Image Processing the valid pixel part in original electrode pattern to be carried out splitting and reconfiguring, then carry out spray printing one by one according to the valid pixel in new figure.
2. the method for processing microelectrode in PDMS substrate based on inkjet technology according to claim 1, is characterized in that, step 1) described in bubble removing be remove bubble in vacuum tank.
3. the method for processing microelectrode in PDMS substrate based on inkjet technology according to claim 1, is characterized in that, step 1) described in constant temperature oven be the constant temperature oven of 60 ~ 80 DEG C.
4. the method for processing microelectrode in PDMS substrate based on inkjet technology according to claim 1, is characterized in that, step 2) in (3) step be PDMS substrate to be immersed in the ethanolic solution of MPTMS 0.6 ~ 1.2 hour.
5. the method for processing microelectrode in PDMS substrate based on inkjet technology according to claim 1, it is characterized in that, step 2) in (4) step in be dry up being immersed in MPTMS ethanolic solution after PDMS substrate is taken out in air stream with ethanol purge.
6. the method for processing microelectrode in PDMS substrate based on inkjet technology according to claim 1, it is characterized in that, step 3) described in the valid pixel part in original electrode pattern is carried out splitting and reconfiguring, be by horizontal and vertical for former graphic file upper respectively with two valid pixels for interval, pixel element in the two directions at a distance of two pixels is taken out, be reassembled into new graphic file, former figure is made to be divided into 9 parts, interval between pixel in so new graphic file just becomes 3 drop spacing, then spray printing is carried out one by one successively in order according to the valid pixel in new figure.
7. the method for processing microelectrode in PDMS substrate based on inkjet technology according to claim 6, is characterized in that, described is undertaken splitting and reconfiguring by the valid pixel part in original electrode pattern, specifically comprises:
(1) the total pixel value of image on horizontal and vertical is determined;
(2), based on these two the total pixel values on horizontal and vertical, circulation obtains the pixel of all two pixels of being separated by horizontal and vertical from being positioned at the pixel of image the first row first row;
(3) all pixels (2) step obtained are the graphic file of white stored in a background colour;
(4) from the pixel of the first row secondary series, according to horizontal and vertical principle of reading in a pixel every two pixels, circulation obtains pixel, then stored in new image file, the like, carry out nine circulations, complete the fractionation of all pixels in original image and reconfigure, obtain nine new graphic files.
8. the method for processing microelectrode in PDMS substrate based on inkjet technology according to claim 6, it is characterized in that, when carrying out spray printing in order successively one by one according to the valid pixel in new figure, after will waiting until numerous droplet dryings of previous spray printing, then carry out spray printing next time.
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| CN110248477A (en) * | 2019-06-12 | 2019-09-17 | 西安工程大学 | A kind of manufacturing method of embedded compliant conductive route |
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