CN108034972A - A kind of silicon based electrode surface modifying method based on porous gold-Pt nanoparticle - Google Patents
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Abstract
The invention discloses a kind of silicon based electrode surface modifying method based on porous golden Pt nanoparticle, this method carries out surface preparation to silicon substrate microelectrode first, then pretreated silicon substrate microelectrode is immersed in gold chloride, chloroplatinic acid and copper sulphate mixed solution, deposits one layer of three metal alloy nanoparticle of golden platinoid on the site of silicon substrate microelectrode using the method for electro-deposition；Finally the silicon substrate microelectrode that golden three metal alloy nanoparticle of platinoid is modified is immersed in copper etching liquid, the copper component in alloy nanoparticle is fallen by electrochemistry selective etch, finally obtains the nano-particle modified silicon substrate microelectrode of porous plation.This method device therefor is cheap, and operating procedure is simple, strong applicability, high treating effect, reliable and stable.Various silicon substrate microelectrode surfaces are can be widely applied to be modified.The interface impedance of silicon substrate microelectrode site can be greatly reduced, improve its electroneurographic signal in body acquisition performance and electro photoluminescence performance.
Description
Technical field
The invention belongs to silicon substrate microelectrode process for modifying surface field, and in particular to one kind is received based on porous gold-platinum alloy
The silicon substrate microelectrode surface modifying method of rice grain.
Background technology
Somatic nerves electrical signal collection for neuroscientist study nervous system basic principle provide it is a kind of strong
Instrument, and lesions located in deep brain shows big advantage and potentiality in the neural class diseases such as treatment Parkinson.Whether it is refreshing
Collection through electric signal still rolls into a ball brain core and carries out electro photoluminescence, and micro- brain electrode is often a part mostly important among these, and
The surface characteristic of micro- brain electrode has been largely fixed its electro photoluminescence performance and electroneurographic signal acquisition performance.Due to micro electronmechanical
System (Micro-electro-mechanical systems, abbreviation MEMS) technology can with explication electrode size, shape,
The batch that multiple record site/stimulation sites prepared on single silicon substrate microelectrode bar and can realize microelectrode can be given birth to
Production, therefore, various MEMS silicon substrates microelectrodes were developed and were applied to neuroscience field in recent years.
For MEMS silicon substrate microelectrodes, multiple electro photoluminescence/electrical signal collections are often integrated on single microelectrode bar
Site, and the smaller damage to reduce in implantation process to brain tissue of overall dimensions of micro-electrode chip, and reduce microelectrode
One of size is inevitably the result is that electrode site interface impedance can significantly increase.The increase of interface impedance often exists
Higher thermal noise is introduced in electroneurographic signal gatherer process, for faint electroneurographic signal, this can undoubtedly reduce letter
Number collection quality.In addition, the increase of electrode site impedance is unfavorable for the injection of electric charge during electro photoluminescence, micro- brain electrode is reduced
Electro photoluminescence performance.Therefore research carries out MEMS silicon substrates microelectrode surface modification to improve its performance, has higher reality
Application value.
Currently used silicon substrate microelectrode surface modification technology mainly has physics and chemical vapour deposition technique, plasma etching
Method, self-assembled monolayer embrane method and sol-gel process, these techniques can substantially meet the demand of silicon substrate microelectrode surface modification,
But the problems such as these techniques are expensive there are equipment, and processing step is complicated, and processing time is long.In recent years, electrochemical deposition method
Since equipment is cheap, becomes silicon to preparing the advantages that environmental requirement is relatively low, technique is simple, convenient and efficient and sedimentary morphology controllable
Base microelectrode surface is modified widely used method.Relevant researcher uses electrochemical deposition method, in silicon substrate microelectrode
Surface deposition platinum black (M á rton G, Bakos I, Fekete Z, et al.Durability of high surface area
platinum deposits on microelectrode arrays for acute neural recordings[J]
.Journal of Materials Science:Materials in Medicine, 2014,25 (3)：931-940), aoxidize
Iridium (Kang X, Liu J, Tian H, et al.Optimization and electrochemical
characterization of RF-sputtered iridium oxide microelectrodes for electrical
stimulation[J].Journal of Micromechanics&Microengineering,2014,24(2):153-
163), gold nano grain (Zhang H, Shih J, Zhu J, et al.Layered nanocomposites from gold
Nanoparticles for neural prosthetic devices [J] .Nano Letters, 2012,12 (7)：3391-
3398) come to carry out surface modification to microelectrode.But there are surface modification effect is general, machine for these microelectrode surface modifying materials
The shortcomings of tool stability is poor.
The data-searching for making to carry out according to applicant, at present, does not relate in existing microelectrode process for modifying surface patent
And the silicon substrate microelectrode surface modifying method based on porous gold-platinum alloy nano particle.
The content of the invention
In view of the above-mentioned drawbacks of the prior art or deficiency, it is an object of the present invention to propose it is a kind of based on porous gold-
The silicon substrate microelectrode surface modifying method of platinum alloy nano particle, the silicon substrate microelectrode prepared using this method, can be greatly reduced
Microelectrode site interface impedance, improves its neural telecommunications collection/electro photoluminescence performance.
In order to realize above-mentioned task, the present invention uses following technical solution：
A kind of silicon substrate microelectrode surface modifying method based on porous gold-platinum alloy nano particle, it is characterised in that include
Following steps：
Step 1, silicon substrate microelectrode is respectively cleaned by ultrasonic 5 minutes with ethanol solution, salpeter solution and ultra-pure water successively, ultrasound
Silicon substrate microelectrode after cleaning is placed to be spontaneously dried in atmosphere；
Step 2：Pretreated silicon substrate microelectrode is immersed in gold chloride, chloroplatinic acid and copper sulphate mixed solution；Adopt
With three-electrode system, the electrode site above silicon substrate microelectrode to be finished is working electrode, and large area platinum electrode is to electricity
Pole, Ag/AgCl electrodes are the deposition voltage of reference electrode, then application -0.2V or -0.3V, sedimentation time 500s-600s,
So as to obtain the silicon substrate microelectrode of gold-three metal alloy nanoparticle of platinum-copper modification；
Step 3：The silicon substrate microelectrode of gold-three metal alloy nanoparticle of platinum-copper modification is immersed in copper etching liquid, is passed through
Electrochemistry selective etch falls the copper component in alloy nanoparticle, obtains the nano-particle modified silicon substrate of porous gold-platinum alloy
Microelectrode.
According to the present invention, the ethanol solution described in step 1 is with volume ratio 1 according to absolute ethyl alcohol and ultra-pure water:1 prepares
Form；Salpeter solution described in step 1 is with volume ratio 1 according to pure salpeter solution and ultra-pure water:1 is formulated.
Further, the gold chloride described in step 2, chloroplatinic acid and copper sulphate mixed solution use the sulfuric acid of 0.5mol/L
Solution is formulated, and the total concentration of gold chloride, chloroplatinic acid and copper-bath is 1-2mmol/L, gold chloride, chloroplatinic acid and sulfuric acid
The concentration ratio of copper is 2:2:1 or 1:1:1.
Copper etching liquid described in step 3 is the salpeter solution that concentration is 50%-70%, the temperature of etching liquid keep 60 DEG C-
Between 80 DEG C, when etch period is 0.5-1 small.
The silicon substrate microelectrode surface modifying method based on porous gold-platinum alloy nano particle of the present invention, passes through electrochemistry
Sedimentation and chemical etching method are nano-particle modified in silicon substrate microelectrode site by porous gold-platinum alloy, device therefor price
Cheaply, operating procedure is simple, strong applicability, high treating effect, reliable and stable, can be widely used for all kinds silicon substrate microelectrode
Surface is modified.
The interface resistance of the nano-particle modified silicon substrate microelectrode of porous gold-platinum alloy that applicant obtains according to the above method
Resist and carry out experimental evaluation in somatic nerves electrical signal collection performance, the results showed that, with unmodified microelectrode site, gold nano
The modified microelectrode site of grain is compared, its microelectrode site interface impedance is greatly reduced, and the acquisition performance of electroneurographic signal is believed
Number signal-to-noise ratio be substantially improved.
Brief description of the drawings
Fig. 1 is the nano-particle modified site (Fig. 1 C) of the obtained porous gold-platinum alloy of embodiment 1, and as control
Untreated microelectrode site (Figure 1A), gold nano particle modification site (Figure 1B) scanning electron microscope diagram piece；
Fig. 2 is the nano-particle modified site of the obtained porous gold-platinum alloy of embodiment 1, and is not located as what is compareed
Manage microelectrode site, gold nano particle modification site interface impedance curve；
Fig. 3 is the nano-particle modified site (Fig. 3 B) of the obtained porous gold-platinum alloy of embodiment 1, and as control
Gold nano particle modification the electroneurographic signal that is collected in rat brain of site (Fig. 3 A)；
Below in conjunction with drawings and examples, the present invention is described in further detail.
Embodiment
Applicants have found that porous gold-platinum alloy nano particle has the cooperative effect of two kinds of monometallic nano particles,
Compared with corresponding monometallic nano particle (gold or Pt nanoparticle), there is the surface area of bigger, faster electron transmission speed
Numerous advantages such as rate, the electro catalytic activity of stronger mechanical stability and higher.In addition, porous nanometer material has larger table
Area, can greatly increase electrode-electric solution liquid contact area and have good charge storage, therefore, apply for person
By the use of porous gold-platinum alloy nano particle as silicon substrate microelectrode surface modified new-material, and further experimental study is carried out, obtained
A kind of silicon substrate microelectrode surface modifying method based on porous gold-platinum alloy nano particle is arrived.
Silicon substrate microelectrode employed in following embodiments, the microelectrode site above it are circular carat (measure of the purity of gold) point, diameter
20 microns.
Embodiment 1：
Step 1：Surface preparation is carried out to silicon substrate microelectrode：
Successively with ethanol solution (absolute ethyl alcohol and the ultrapure water volume ratio 1 that concentration is 50%:1), concentration is 50% nitre
Acid solution (pure salpeter solution and ultrapure water volume ratio 1:1) silicon substrate microelectrode is respectively cleaned by ultrasonic 5 minutes with ultra-pure water, and will be clear
Silicon substrate microelectrode after washing is placed to be spontaneously dried in atmosphere；
Step 2：Pretreated silicon substrate microelectrode is immersed in gold chloride, chloroplatinic acid and copper sulphate mixed solution, is mixed
Close solution to be formulated using the sulfuric acid solution of 0.5mol/L, the total concentration of gold chloride, chloroplatinic acid and copper-bath is
1mmol/L, the concentration ratio of gold chloride, chloroplatinic acid and copper sulphate is 2:2:1；Using three-electrode system, the micro- electricity of silicon substrate to be finished
Electrode site extremely above is working electrode, and large area platinum electrode is that Ag/AgCl electrodes are reference electrode, then to electrode
The deposition voltage of application -0.2V, sedimentation time 600s, so as to obtain the silicon of gold-three metal alloy nanoparticle of platinum-copper modification
Base microelectrode；
Step 3：The silicon substrate microelectrode of gold-three metal alloy nanoparticle of platinum-copper modification of gained is immersed copper etching liquid
In (concentration be 60% salpeter solution) 1 it is small when, the temperature of etching liquid is maintained at 60 DEG C, falls to close by electrochemistry selective etch
Copper component in gold nano grain, finally obtains the nano-particle modified silicon substrate microelectrode of porous gold-platinum alloy.
Embodiment 2：
Step 1：Surface preparation is carried out to silicon substrate microelectrode：
It is successively 50% ethanol solution (absolute ethyl alcohol and ultrapure water volume ratio 1 with concentration:1), concentration is molten for 50% nitric acid
Liquid (pure salpeter solution and ultrapure water volume ratio 1:1) silicon substrate microelectrode is respectively cleaned by ultrasonic 5 minutes with ultra-pure water, and by after cleaning
Silicon substrate microelectrode place spontaneously dry in atmosphere；
Step 2：Pretreated silicon substrate microelectrode is immersed in gold chloride, chloroplatinic acid and copper sulphate mixed solution, is mixed
Close solution to be formulated using the sulfuric acid solution of 0.5mol/L, the total concentration of gold chloride, chloroplatinic acid and copper-bath is
1mmol/L, the concentration ratio of gold chloride, chloroplatinic acid and copper sulphate is 1:1:1；Using three-electrode system, the micro- electricity of silicon substrate to be finished
Electrode site extremely above is working electrode, and large area platinum electrode is that Ag/AgCl electrodes are reference electrode, then to electrode
The deposition voltage of application -0.2V, sedimentation time 600s, so as to obtain the silicon of gold-three metal alloy nanoparticle of platinum-copper modification
Base microelectrode；
Step 3：The silicon substrate microelectrode of gold-three metal alloy nanoparticle of platinum-copper modification of gained is immersed copper etching liquid
In (concentration be 60% salpeter solution) 0.5 it is small when, the temperature of etching liquid is maintained at 80 DEG C, is fallen by electrochemistry selective etch
Copper component in alloy nanoparticle, finally obtains the nano-particle modified silicon substrate microelectrode of porous gold-platinum alloy.
Embodiment 3：
Step 1：Surface preparation is carried out to silicon substrate microelectrode：
Successively with ethanol solution (absolute ethyl alcohol and the ultrapure water volume ratio 1 that concentration is 50%:1), concentration is 50% nitre
Acid solution (pure salpeter solution and ultrapure water volume ratio 1:1) silicon substrate microelectrode is respectively cleaned by ultrasonic 5 minutes with ultra-pure water, and will be clear
Silicon substrate microelectrode after washing is placed to be spontaneously dried in atmosphere；
Step 2：Pretreated silicon substrate microelectrode is immersed in gold chloride, chloroplatinic acid and copper sulphate mixed solution, is mixed
Close solution to be formulated using the sulfuric acid solution of 0.5mol/L, the total concentration of gold chloride, chloroplatinic acid and copper-bath is
2mmol/L, the concentration ratio of gold chloride, chloroplatinic acid and copper sulphate is 2:2:1；Using three-electrode system, the micro- electricity of silicon substrate to be finished
Electrode site extremely above is working electrode, and large area platinum electrode is that Ag/AgCl electrodes are reference electrode, then to electrode
The deposition voltage of application -0.2V, sedimentation time 600s, so as to obtain the silicon of gold-three metal alloy nanoparticle of platinum-copper modification
Base microelectrode；
Step 3：The silicon substrate microelectrode of gold-three metal alloy nanoparticle of platinum-copper modification of gained is immersed copper etching liquid
In (concentration be 60% salpeter solution) 1 it is small when, the temperature of etching liquid is maintained at 60 DEG C, falls to close by electrochemistry selective etch
Copper component in gold nano grain, finally obtains the nano-particle modified silicon substrate microelectrode of porous gold-platinum alloy.
Reference examples：The preparation of the microelectrode site of gold nano particle modification:
Step 1：Surface preparation is carried out to silicon substrate microelectrode, i.e., successively with ethanol solution (the anhydrous second that concentration is 50%
Alcohol and ultrapure water volume ratio 1:1) salpeter solution (pure salpeter solution and the ultrapure water volume ratio 1 that, concentration is 50%:1) it is and ultrapure
Water is respectively cleaned by ultrasonic 5 minutes silicon substrate microelectrode, and the silicon substrate microelectrode after cleaning is placed and is spontaneously dried in atmosphere；
Step 2：Pretreated silicon substrate microelectrode is immersed in the chlorauric acid solution of the sulfuric acid solution preparation of 0.5mol/L
In, the concentration of chlorauric acid solution is 1-2mmol/L；Using three-electrode system, the electrode position above silicon substrate microelectrode to be finished
Point be working electrode, and for large area platinum electrode for electrode, Ag/AgCl electrodes are reference electrode, then application -0.2V or -
The deposition voltage of 0.3V, sedimentation time 500s-600s, so as to obtain the silicon substrate microelectrode of gold nano particle modification；
Morphology characterization and performance test
1st, the nano-particle modified microelectrode site of porous gold-platinum alloy for obtaining embodiment 1, gold prepared by reference examples
Nano-particle modified microelectrode site and unmodified microelectrode site are scanned electron microscope experiment, obtained knot
Fruit is as shown in Figure 1.It can be seen in fig. 1 that unmodified naked gold electrode site surface is smooth；Gold nano is deposited in the above
After particle (Figure 1B), it can be seen that many nano particles in irregular shape, are densely distributed in gold electrode site surface；And
The electron micrograph of Fig. 1 C shows that prepared gold-Pt nanoparticle diameter is about 200nm, has the shape of cauliflower-shaped
Shape, is uniformly densely distributed in the surface in gold electrode site.(figure is can see from the electron microscope picture of amplification factor higher
The embedded figure of 1C), prepared gold-Pt nanoparticle has very coarse surface, and has many differences on nano particle
The hole of size, this leads mainly due to the copper component in gold-platinum-copper alloy nano particle is fallen by electrochemistry selective etch
Cause.Such nanostructured will greatly reduce the impedance of microelectrode site, increase the surface roughness in site, improve electricity
Sub- transfer rate and the electroneurographic signal collection/electro photoluminescence performance for strengthening microelectrode.
2nd, the nano-particle modified microelectrode site of porous gold-platinum alloy for obtaining embodiment 1, prepares in reference examples
The microelectrode site of gold nano particle modification and unmodified microelectrode site carry out testing impedance experiment, and obtained result is such as
Shown in Fig. 2.Fig. 2 is average impedance change curve of three kinds of microelectrode sites in 1kHz-100kHz frequency ranges.It can see
Go out, with the increase of frequency, the trend of monotone decreasing occurs in the impedance of three kinds of microelectrode sites；Unmodified microelectrode site
The interface impedance of maximum, and the microelectrode site that porous gold-platinum alloy is nano-particle modified are shown in whole frequency range
Impedance in whole frequency range is almost minimum.This explanation, relative to gold nano grain, porous gold-platinum alloy nano particle
The interface impedance of microelectrode site can substantially be reduced.
3rd, a main function of silicon substrate microelectrode is the collection realized in somatic nerves electric signal.In order to verify according to this
The microelectrode that inventive method was modified can be significantly improved in somatic nerves electrical signal collection performance, embodiment 1 is obtained porous
The nano-particle modified site of gold-platinum alloy, and carried out as the site of the gold nano particle modification of control in rat brain
Electroneurographic signal collection experiment, the results are shown in Figure 3.Fig. 3 A and 3B are respectively the site of gold nano particle modification, porous gold-platinum
The typical spike action potential signals sequence that the site of alloy nanoparticle modification collects.As can be seen that two kinds of microelectrode positions
The amplitude of action potential that point collects is not much different, but what the nano-particle modified site of porous gold-platinum alloy collected
Spike signals, its ambient noise are smaller.Gathered for the spike action potential signals of two kinds of microelectrode sites of quantitative contrast
Quality, average amplitude, the average signal ratio (SNR) of the spike action potential signals collected to two kinds of microelectrode sites carry out
Statistical analysis.The result shows that although being averaged detected by the nano-particle modified microelectrode site of porous gold-platinum alloy
Between the average spike amplitudes (281.2 ± 39.7) in the site of spike amplitudes (273.7 ± 25.2) and gold nano particle modification
And no difference of science of statistics (P ＞ 0.05), but the former average SNR reaches 4.8 ± 0.3, the average SNR of the latter for 3.4 ±
0.4, the former is statistically apparently higher than the latter, this is mainly due to the nano-particle modified microelectrode of porous gold-platinum alloy
Being greatly reduced for ambient noise is surveyed in site in physical examination.
It should be appreciated that the description of above-described embodiment is only to explain the present invention, it is the common skill for ease of the technical field
Art personnel are understood that and use, and the objects, technical solutions and advantages of the present invention are more clearly understood, and the present invention is not restricted to these
Embodiment, person skilled in the art's obtained technical inspiration according to the present invention, it is clear that can be readily to these realities
Apply example and make various additions or replacement, and the General Principle of this explanation is applied in other embodiment without carrying out creativeness
Work.Therefore, those skilled in the art are not departing from addition that scope made or replacement is regarded as the present invention's
Within protection domain.
Claims (4)
1. a kind of silicon based electrode surface modifying method based on porous gold-Pt nanoparticle, it is characterised in that include following step
Suddenly：
Step 1, silicon substrate microelectrode is respectively cleaned by ultrasonic 5 minutes with ethanol solution, salpeter solution and ultra-pure water successively, be cleaned by ultrasonic
Silicon substrate microelectrode afterwards is placed and spontaneously dried in atmosphere；
Step 2：Pretreated silicon substrate microelectrode is immersed in gold chloride, chloroplatinic acid and copper sulphate mixed solution；Using three
Electrode system, the electrode site above silicon substrate microelectrode to be finished are working electrode, large area platinum electrode be to electrode,
Ag/AgCl electrodes are the deposition voltage of reference electrode, then application -0.2V or -0.3V, sedimentation time 500s-600s, so that
Obtain the silicon substrate microelectrode of gold-three metal alloy nanoparticle of platinum-copper modification；
Step 3：The silicon substrate microelectrode of gold-three metal alloy nanoparticle of platinum-copper modification is immersed in copper etching liquid, passes through electrification
Selective etch falls the copper component in alloy nanoparticle, obtains the nano-particle modified micro- electricity of silicon substrate of porous gold-platinum alloy
Pole.
2. the method as described in claim 1, it is characterised in that the ethanol solution described in step 1 be according to absolute ethyl alcohol with
Ultra-pure water is with volume ratio 1:1 is formulated；Salpeter solution described in step 1 is with volume according to pure salpeter solution and ultra-pure water
Than 1:1 is formulated.
3. the method as described in claim 1, it is characterised in that gold chloride, chloroplatinic acid and copper sulphate mixing described in step 2
Solution is formulated using the sulfuric acid solution of 0.5mol/L, and the total concentration of gold chloride, chloroplatinic acid and copper-bath is 1-
2mmol/L, the concentration ratio of gold chloride, chloroplatinic acid and copper sulphate is 2:2:1 or 1:1:1.
4. the method as described in claim 1, it is characterised in that the copper etching liquid described in step 3 is that concentration is 50%-70%
Salpeter solution, between 60 DEG C -80 DEG C of the temperature holding of etching liquid, when etch period is 0.5-1 small.
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Cited By (3)
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| CN108802140A (en) * | 2018-08-13 | 2018-11-13 | 广州钰芯传感科技有限公司 | A kind of interdigital electrode and its preparation method and application of porous gold modification |
| CN111326754B (en) * | 2020-03-10 | 2021-05-14 | 中南林业科技大学 | Preparation method of fusiform platinum nanoparticles |
| CN117059713A (en) * | 2023-10-11 | 2023-11-14 | 深圳市领耀东方科技股份有限公司 | Preparation method of high-brightness LED chip based on micro-nano processing technology |
-
2017
- 2017-10-10 CN CN201710936101.3A patent/CN108034972A/en active Pending
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| CAIXIA XU ET. AL.: "Dealloying to nanoporous Au/Pt alloys and their structure sensitive electrocatalytic properties", 《PHYSICAL CHEMISTRY CHEMICAL PHYSICS》 * |
| ZONGYA ZHAO ET. AL.: "In Vivo Neural Recording and Electrochemical Performance of Microelectrode Arrays Modified by Rough-Surfaced AuPt Alloy Nanoparticles with Nanoporosity", 《SENSORS》 * |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108802140A (en) * | 2018-08-13 | 2018-11-13 | 广州钰芯传感科技有限公司 | A kind of interdigital electrode and its preparation method and application of porous gold modification |
| CN111326754B (en) * | 2020-03-10 | 2021-05-14 | 中南林业科技大学 | Preparation method of fusiform platinum nanoparticles |
| CN117059713A (en) * | 2023-10-11 | 2023-11-14 | 深圳市领耀东方科技股份有限公司 | Preparation method of high-brightness LED chip based on micro-nano processing technology |
| CN117059713B (en) * | 2023-10-11 | 2024-02-02 | 深圳市领耀东方科技股份有限公司 | Preparation method of high-brightness LED chip based on micro-nano processing technology |
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Application publication date: 20180515 |