CN109330711A - Porous metal capillary liquid-seepage microneedle electrode and preparation method - Google Patents
Porous metal capillary liquid-seepage microneedle electrode and preparation method Download PDFInfo
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- 238000004987 plasma desorption mass spectroscopy Methods 0.000 claims description 20
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 20
- 239000002504 physiological saline solution Substances 0.000 claims description 17
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 15
- 239000010936 titanium Substances 0.000 claims description 15
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
- A61B90/00—Instruments, implements or accessories specially adapted for surgery or diagnosis and not covered by any of the groups A61B1/00 - A61B50/00, e.g. for luxation treatment or for protecting wound edges
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Abstract
The invention discloses a porous metal capillary liquid-permeating microneedle electrode and a preparation method thereof. The porous metal capillary liquid-permeating microneedle electrode comprises a porous microneedle array electrode plate, an insulating shell, an electric signal wire and a capillary liquid-absorbing core ring, wherein a plurality of porous microneedles with channels are arranged on the porous microneedle array electrode plate; a cavity is formed in the insulating shell, an opening is formed in one side of the insulating shell, the porous micro-needle array electrode plate and the opening of the insulating shell are sealed and spliced to form the cavity, and the capillary wick ring is filled in the cavity; the channel is in communication with the cavity. Based on the advantages of the microneedle structure, the invention realizes the direct contact of the sensor and the dermis of the skin by utilizing the adsorbability and the conductivity of the porous channel structure to the solution and the conductivity of the solution, greatly reduces the contact impedance and can acquire the bioelectricity signals with high signal-to-noise ratio.
Description
Technical field
The present invention relates to field of medical device technology, and in particular to a kind of porous metals capillary sepage microneedle electrodes and preparation
Method.
Background technique
With the development of electronic technology with the progress of medical detection technique, human biological electricity, which extracts, to be medical diagnosis on disease and pre-
Anti- offer important evidence, can be used continuously for a long time and the sensor for acquiring high s/n ratio signal receives more and more attention.
Electrode slice is the core component on biopotential sensor, the result of performance direct relation signal acquisition.Currently, city
Common eeg sensor, myoelectric sensor etc. on face, electrode needs that conductive paste is cooperated to use during acquiring electric signal.
First conductive paste is applied on the skin before test, then electrode is placed on conductive paste and is tested, electrode and table in test process
Bark graft touching, cannot directly touch skin corium.The presence of conductive paste and horny layer of epidermis both increases the impedance link of test process,
The electric signal caused is of poor quality, meanwhile, conductive paste be lost or evaporation dry out also result in electric signal signal-to-noise ratio table it is small,
Long-time service can also damage skin.On the other hand, traditional electrode slice surface is more smooth, is easy to generate with skin relatively sliding
It is dynamic, so that the electric signal of acquisition contains a large amount of artefacts.
Summary of the invention
The shortcomings that main object of the present invention is for traditional biological electric transducer use process, proposes a kind of porous metals
Capillary sepage microneedle electrodes and preparation method realize high s/n ratio electrical signal collection, reduce signal artifacts.
In order to achieve the above object, the present invention is realized according to following technical solutions.
A kind of porous metals capillary sepage microneedle electrodes, comprising: the inside of an insulation crust, the insulation crust forms sky
Chamber, and there is an opening in side, electric signal string holes and solution injection orifice are offered on the insulation crust；One porous micropin battle array
The open sealing split of column electrode slice, the porous microneedle array electrode slice and insulation crust, the porous microneedle array electrode
On piece is provided with multiple porous micropins with conduit, the axis parallel of the conduit and micropin, and the conduit through more
Mesoporous metal microneedle array electrode slice is simultaneously connected to cavity；One capillary wick ring, the capillary wick ring filling is in the sky
It is intracavitary, for adsorbing the physiological saline entered by solution injection orifice；One electrical signal line, the electrical signal line are worn from electric signal string holes
Enter and is connect after passing through the capillary wick ring with the porous microneedle array electrode slice.
Further, the porous metals microneedle array electrode slice with a thickness of 1-2mm, be interconnected using with multiple
Micropore and porosity be 30-50% titanium metal material.Titanium can not only be conductive, and has good life with human body
Object compatibility.The micropore for the multiple connections having on microneedle array electrode slice can make liquid medicine or electrolyte pass through
Micropin infiltrates through skin skin corium.
The further microneedle array is rectangular array, and the micropin is cone and micropin base diameter is 200-
500 μm, be highly 400-100 μm, and the spacing between each micropin is 1mm；Described 50-150 μm of conduit diameter.
Further, conduit inner wall has fine fine and soft shape fin structure.The fine fine and soft shape fin structure formed can play tune
The capillary attraction and permeability of conduit are saved, to adjust liquid flowing.
Further, the opening of the insulation crust and the junction of porous microneedle array electrode slice are close by binder
Envelope；The material of the insulation crust is one of silica gel, plastics or a variety of；The binder is epoxy resin or silicone elastomer
Sealant.Insulation crust and porous microneedle array electrode slice are sealed into split by binder, can effectively be prevented showing for leakage
As.
Further, the porosity of the capillary wick ring is 50-70%, and physiology salt is housed in capillary wick ring
Water.The porosity of 50-70% can preferably guarantee liquid electrolyte in the storage adsorbance of capillary wick ring.
Further, the electrical signal line and porous microneedle array electrode slice pass through welded connecting.
The present invention also provides a kind of method for preparing porous metals capillary sepage microneedle electrodes described in any of the above embodiments, packets
Include following steps:
1), take titanium particle, ethyl alcohol, polyvinyl butyral, BBP(Butyl Benzyl Phthalate, dispersing agent by mass fraction
Than mixing for 46:46:1:6.5-7:1-1.5, it is spare to form titanium microparticle suspending liquid by magnetic agitation 0.5-2h；
2), prepare one piece of stainless steel microneedle array template and one piece of uncured PDMS mold, by the micro- of Stainless Molding Board
Needle array surface is pressed on PDMS mold, then carries out vacuum solidification, by microneedle array structure replication to PDMS mold, is removed not
Become rusty steel form, the PDMS mold being cured；
3), the titanium microparticle suspending liquid that step 1) obtains is poured on the PDMS mold being cured, is shaken by ultrasound
It is dynamic that suspension is made to adequately fill up die cavity, then place it in vacuum chamber and stand 10-20min to remove bubble, it air-dries at room temperature
It agglomerates to suspension, takes out suspension agglomeration from PDMS mold after alcohol volatilizees completely；
4), suspension agglomeration is placed in tube furnace, at 1240-1250 DEG C under chemically inert atmosphere
It is sintered 2h, is cooled to room temperature after the completion of sintering with tube furnace, takes out and obtains porous metals microneedle electrodes piece；
5), after the fixed porous microneedle array electrode slice of clamping, conduit, slot are processed downwards on the circular conical surface of each micropin
Road inner wall forms fine fine and soft shape fin structure；
6) electrical signal line, is penetrated and is passed through capillary wick ring from the electric signal string holes for passing through insulation crust, then with it is more
Hole microneedle array electrode slice is welded to connect, then, by the open sealing split of porous microneedle array electrode slice and insulation crust, even
The place of connecing is sealed by binder 5, and inside forms a cavity structure, capillary wick ring filling is fixed in cavity, by physiology
Salt water is injected in capillary wick ring by the solution injection orifice of insulation crust, and porous metals capillary sepage microneedle electrodes are made.
Further, in step (1), the partial size of the metal particle is less than or equal to 10 μm.
Further, in step (4), the chemically inert gas is nitrogen or argon gas.
Compared with prior art, the present invention has the following advantages and effect:
(1) porous metals sepage microneedle electrodes of the invention do not need conductive paste in use, pass through liquid electrolytic
Matter can simplify a large amount of preparations before testing, be also prevented from conductive paste to the damaging action of skin as conductive amplified medium.
(2), porous metals sepage microneedle electrodes of the invention and insulation crust form cavity, and capillary is arranged in cavity
Liquid-sucking core ring, energy efficient absorption physiological saline, cavity are connected to conduit, and liquid electrolyte can directly be arrived at by central channel
The skin corium of skin realizes that electrode is contacted with the direct of skin skin corium, greatly reduction contact impedance, while reducing electrode and skin
Relative sliding between skin reduces signal artifacts, can collect the bioelectrical signals of high s/n ratio.
(3), porous metals capillary sepage microneedle electrodes of the invention are using the porous microneedle configuration for having central channel
With the capillary wick ring of larger porosity, make full use of hole and conduit to the capillary attraction and penetration of physiological saline, dimension
The wetability of micropin is held, while the capillary wick ring of larger porosity can provide physiological saline for the micropin of smaller porosity,
Also it can inhibit and evaporate and overflow in use process.The setting of capillary wick ring and conduit can guarantee physiological saline incessantly
It flows unimpeded, moreover it is possible to control physiological saline velocity of liquid assets, the fine fine and soft shape fin structure of conduit inner wall can play adjusting conduit
Capillary attraction and permeability, thus adjust liquid flowing so that liquid electrolyte flow into skin amount and speed more adduction
Reason, is more applicable for signal acquisition.
(4) traditional electrode is compared, porous metals sepage microneedle electrodes of the invention use microneedle array electrode, can be direct
Arrive at skin skin corium without damage dermal tissue, greatly reduce the electrical impedance of skin-electrode, at the same reduce electrode with
Relative sliding between skin reduces signal artifacts, realizes high-quality signal acquisition.
(5) preparation method of porous metals sepage microneedle electrodes of the invention is simple and efficient, it is easy to accomplish the big rule of low cost
Mould mass production.
Detailed description of the invention
Fig. 1 is a kind of cross-sectional view of porous metals capillary sepage microneedle electrodes of the present invention；
Fig. 2 is the structural schematic diagram of porous microneedle array electrode slice；
Fig. 3 is the scanning electron microscope (SEM) photograph of A in Fig. 2；
Fig. 4 is the structural schematic diagram of insulation crust；
Fig. 5 is the schematic diagram for the PDMS mold that preparation has microneedle array structure in embodiment 1；
Fig. 6 is the schematic diagram of the preliminary forming process of porous metals microneedle electrodes piece in embodiment 1；
Fig. 7 is the porous microneedle array electrode slice structural schematic diagram completed the process in embodiment 1；
Fig. 8 is the scanning electron microscope (SEM) photograph of the fine fine and soft shape fin structure in conduit；
Fig. 9 is the partial enlarged view of B in Fig. 8.
In attached drawing: 1, porous microneedle array electrode slice；2, insulation crust；3, electrical signal line；4, capillary wick ring；5, it glues
Tie agent；7, stainless steel microneedle array template；8, PDMS mold；9, electric signal string holes；10, solution injection orifice；11, suspension knot
Block；12, conduit.
Specific embodiment
The present invention is done below in conjunction with relevant drawings and specific embodiment and is further described in detail, but implementation of the invention
Therefore mode is not limited to the following examples.
Embodiment 1
As shown in figs 1-9, Fig. 1 is a kind of cross-sectional view of porous metals capillary sepage microneedle electrodes of the present invention；Fig. 2 is porous
The structural schematic diagram of microneedle array electrode slice；Fig. 4 is the structural schematic diagram of insulation crust.
As shown in Figure 1 and Figure 4, a kind of porous metals capillary sepage microneedle electrodes, including an insulation crust 2, the insulation
The inside of shell 2 forms cavity, and has an opening in side, offers electric signal string holes 9 and solution on the insulation crust
Injection orifice 10；The open sealing of one porous microneedle array electrode slice 1, the porous microneedle array electrode slice 1 and insulation crust 2 is spelled
It closes, multiple porous micropins with conduit 12, the conduit 12 and micropin is provided on the porous microneedle array electrode slice 1
Axis parallel, and the conduit 12 is connected to through porous metals microneedle array electrode slice 1 and with cavity；One capillary wick ring
4, the capillary wick ring 4 is filled in the cavity, for adsorbing the physiological saline entered by solution injection orifice 10；One electricity
Signal wire 3, the electrical signal line 3 from electric signal string holes 9 penetrate and pass through the capillary wick ring after with the porous micropin
The connection of array electrode piece.
Preferably, as shown in Figures 2 and 3, the porous metals microneedle array electrode slice 1 with a thickness of 2mm, it is more using having
A interconnected micropore and porosity be 30-50% titanium metal material.
Preferably, the microneedle array is rectangular array, preferably quadrate array, is arranged using the structure of 7*7.It is described
Micropin is cone and micropin base diameter is 500 μm, is highly 1000 μm, and the spacing between each micropin is 1mm；The conduit
12 with cavity through porous microneedle array electrode slice 1 and being connected to, described 100 μm of 12 diameter of conduit, and 12 inner wall of conduit have it is fine
Fine and soft shape fin structure, as shown in figure 8, Fig. 8 is the scanning electron microscope (SEM) photograph of the fine fine and soft shape fin structure in conduit, Fig. 9 is B in Fig. 8
Partial enlarged view.As can be seen from the figure the fine fine and soft shape fin structure in conduit.
Preferably, the opening of the insulation crust 2 is formed with porous microneedle array electrode slice 1 by 5 split of binder；Institute
The material for stating insulation crust 2 is plastics；The binder 5 is epoxy resin.Insulation crust 2 should be with porous microneedle array electrode slice
1 is mutually matched, and the cavity shape of formation does not limit, and can be rectangular or round, or is that other shapes are ok, this
It is preferably rectangular in invention.The capillary wick ring 4, which is fixed, to be filled in cavity, the hole of the capillary wick ring 4
Rate is 50-70%, and capillary wick ring 4 is used to fill physiological saline, and physiological saline is injected by solution injection orifice 10.
Preferably, the electrical signal line 3 passes through welded connecting with porous microneedle array electrode slice 1.
Compared to traditional electrode, porous metals capillary sepage microneedle electrodes of the invention, when in use, micropin can be worn
It crosses epidermis and reaches skin corium, the length of micropin is will not to touch the nerve of user by especially considering design, will not
Cause feeling of pain.The porous metals capillary sepage microneedle electrodes, which are connect by electrical signal line 3 with external instrument, obtains electric signal, and
Capillary wick ring 4 can reasonably control circulation and the flow of physiological saline, control stream because of its capillary attraction and penetration
Speed, moreover it is possible to the effective volatilization and spilling for inhibiting liquid in use process.Not by the setting of capillary wick ring 4 and conduit 12
It is only capable of maintaining the wettability of micropin, while physiological saline can also be provided for micropin, physiological saline can pass through porous microneedle array
The hole of electrode slice 1 penetrates into skin, to improve the electric signal of measurement.
The present invention also provides a kind of above-mentioned preparation methods of porous metals capillary sepage microneedle electrodes, include the following steps:
(1), taking partial size is 10 μm of titanium particles, ethyl alcohol, PVB (polyvinyl butyral), BBP (phthalic acid
Butyl benzyl), dispersing agent by 46:46:1:7:1 mass fraction than mixing, magnetic agitation 1h, formed titanium microparticle suspending liquid it is standby
With.
(2), as shown in figure 5, preparing one piece of stainless steel microneedle array template 7 and one piece of uncured PDMS mold 8, micropin
Array is square array, and it is highly 1000 μm that micropin base diameter, which is 500 μm, spacing 1mm, by stainless steel microneedle array
The microneedle array face of template 7 is pressed on PDMS mold 8, then carries out vacuum solidification, by microneedle array structure replication to PDMS mould
On tool 8, Stainless Molding Board is removed, the PDMS mold 8 being cured.
(3), as shown in fig. 6, titanium microparticle suspending liquid prepared by step (1) is poured into cured good PDMS mold
In 8, so that suspension is adequately filled up die cavity by ultrasonic vibration 5min, then places it in vacuum chamber and stand 15min except degassing
Bubble air-dries at room temperature to suspension agglomeration 11, takes suspension agglomeration 11 from PDMS mold 8 after alcohol volatilizees completely
Out.
(4), suspension agglomeration 11 is placed in tube furnace, 1240 DEG C of -1250 DEG C of high temperature under the argon atmosphere of flowing
It is sintered 2h, is cooled to room temperature after the completion of sintering with tube furnace, takes out the porous metals microneedle electrodes piece 1 of completion.As shown in Figure 7.
(5), after the fixed porous microneedle array electrode slice 1 of clamping, using 100 μm of diameter of micro- milling cutters each micropin circle
Conduit 12 is processed on the conical surface downwards, so that 12 inner wall of conduit processed forms fine fine and soft shape fin structure, such as Fig. 8-9 institute
Show.
(6) the electric signal string holes 9 of the self-insulating shell 2 of electrical signal line 3 is penetrated and passes through the capillary wick ring 4, so
Afterwards with porous microneedle array electrode slice 1 by being welded to connect, then by the opening of porous microneedle array electrode slice 1 and insulation crust 2
Split is sealed, junction is sealed by binder 5, and in the cavities, physiological saline is led to for the fixed filling of the capillary wick ring 4
The solution injection orifice 10 for crossing insulation crust 2 injects in capillary wick ring 4, and porous metals capillary sepage microneedle electrodes are made.
Dispersing agent described above is preferably polyethylene glycol or methyl styrene.
Compared with prior art, porous metals sepage microneedle electrodes production method of the invention is simple, from Fig. 2 and Fig. 3
As can be seen that micropin also has many interconnected micropores in obtained porous metals microneedle electrodes piece other than conduit 12,
The micropore of formation has adsorptivity to solution, and the capillary wick ring 4 of larger porosity can mention for the micropin of smaller porosity
For physiological saline, it also can inhibit and evaporate and overflow in use process.Electric conductivity can be enhanced in physiological saline, improves and extracts letter
Number ability, reduce physiological signal noise so that signal-to-noise ratio is improved.
Embodiment 2
The porous metals capillary sepage microneedle electrodes of the present embodiment are same as Example 1, the difference is that, it is described porous
Metal micro-needle array electrode piece with a thickness of 1.5mm.Micropin base diameter is 300 μm, is highly 500 μm, spacing 1mm, slot
100 μm of 12 diameter of road.The material of insulation crust 2 is silica gel, and binder 5 is silicone elastomer sealant.
The preparation method of the porous metals capillary sepage microneedle electrodes is similar to Example 1, the difference is that the titanium
It is 5 μm that particle, which selects diameter, and the titanium particle, ethyl alcohol, PVB, BBP, dispersing agent are divided by the quality of 46:46:1:6.5:1.5
Number is than mixing.And it is sintered under the atmosphere of nitrogen in step (4).
Specific embodiments of the present invention are only to say bright examples made by the present invention to be clear, and it is real to the present invention for being not
Apply the restriction of mode.For the skilled worker in corresponding field, similar change can also be made on the basis of the above description
Dynamic, variation within the scope of the claims also can be achieved, and can not and be not necessarily to be exhaustive all embodiments herein.It is all
Any modifications, equivalent replacements, and improvements etc. made within the spirit and principles in the present invention should be included in right of the present invention and want
Within the protection scope asked.
Claims (10)
1. a kind of porous metals capillary sepage microneedle electrodes, which is characterized in that including,
One insulation crust, the inside of the insulation crust forms cavity, and has an opening in side, opens on the insulation crust
Equipped with electric signal string holes and solution injection orifice；
The open sealing split of one porous microneedle array electrode slice, the porous microneedle array electrode slice and insulation crust, it is described
It is provided with multiple porous micropins with conduit on porous microneedle array electrode slice, the axis parallel of the conduit and micropin,
And the conduit is connected to through porous metals microneedle array electrode slice and with cavity；
One capillary wick ring, the capillary wick ring filling are entered for adsorbing by solution injection orifice in the cavity
Physiological saline；
One electrical signal line, the electrical signal line penetrated from electric signal string holes and pass through after the capillary wick ring with it is described porous
The connection of microneedle array electrode slice.
2. a kind of porous capillary metal sepage microneedle electrodes according to claim 1, which is characterized in that the porous metals
Microneedle array electrode slice with a thickness of 1-2mm, use with multiple interconnected micropores and porosity for 30-50%'s
Titanium metal material.
3. a kind of porous metals capillary sepage microneedle electrodes according to claim 1, which is characterized in that the microneedle array
For rectangular array, it is highly 400-1000 μm that the micropin, which is cone, and micropin base diameter is 200-500 μm, each micropin
Between spacing be 1mm；Described 50-150 μm of conduit diameter.
4. a kind of porous metals capillary sepage microneedle electrodes according to claim 1, which is characterized in that the conduit inner wall
There is fine fine and soft shape fin structure.
5. a kind of porous metals capillary sepage microneedle electrodes according to claim 1, it is characterised in that: the insulation crust
Opening pass through first binding agent seal with the junction of porous microneedle array electrode slice；The material of the insulation crust is silica gel, modeling
One of material is a variety of；The binder is epoxy resin or silicone elastomer sealant.
6. a kind of porous metals capillary sepage microneedle electrodes according to claim 1, which is characterized in that the capillary wick
The porosity of core ring is 50-70%.
7. a kind of porous metals capillary sepage microneedle electrodes according to claim 1, which is characterized in that the electrical signal line
Pass through welded connecting with porous microneedle array electrode slice.
8. a kind of described in any item preparation methods of porous metals capillary sepage microneedle electrodes of claim 1~7, feature exist
In including the following steps:
1) titanium particle, ethyl alcohol, polyvinyl butyral, BBP(Butyl Benzyl Phthalate, the dispersing agent, is taken to be by mass fraction ratio
46:46:1:6.5-7:1-1.5 it is spare to form titanium microparticle suspending liquid by mixing, magnetic agitation 0.5-2h；
2), prepare one piece of stainless steel microneedle array template and one piece of uncured PDMS mold, by the micropin battle array of Stainless Molding Board
Column face is pressed on PDMS mold, then carries out vacuum solidification, by microneedle array structure replication to PDMS mold, removes stainless steel
Template, the PDMS mold being cured；
3), the titanium microparticle suspending liquid that step 1) obtains is poured on the PDMS mold being cured, is made by ultrasonic vibration
Suspension adequately fills up die cavity, then places it in vacuum chamber and stand 10-20min to remove bubble, is air-dried at room temperature to outstanding
Supernatant liquid agglomeration takes out suspension agglomeration after alcohol volatilizees completely from PDMS mold；
4), suspension agglomeration is placed in tube furnace, in 1240-1250 under the chemically inert atmosphere of flowing
DEG C it is sintered 2h, is cooled to room temperature after the completion of sintering with tube furnace, taken out and obtain porous metals microneedle electrodes piece；
5), after the fixed porous microneedle array electrode slice of clamping, conduit is processed downwards on the circular conical surface of each micropin, in conduit
Wall forms fine fine and soft shape fin structure；
6) electrical signal line, is penetrated and is passed through capillary wick ring from the electric signal string holes for passing through insulation crust, then with it is porous micro-
Needle-array electrode piece is welded to connect, then, by the open sealing split of porous microneedle array electrode slice and insulation crust, junction
It is sealed by binder 5, inside forms a cavity structure, capillary wick ring filling is fixed in cavity, by physiological saline
It is injected in capillary wick ring by the solution injection orifice of insulation crust, porous metals capillary sepage microneedle electrodes is made.
9. a kind of preparation method of porous metals capillary sepage microneedle electrodes according to claim 8, which is characterized in that step
It is rapid 1) in, the partial size of the metal particle is less than or equal to 10 μm.
10. a kind of preparation method of porous metals capillary sepage microneedle electrodes according to claim 8, which is characterized in that
In step 4), the chemically inert gas nitrogen or argon gas.
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