CN102279220A - Method for manufacturing chip, gas sensor assembly and method for plating carbon nano tube on chip - Google Patents
Method for manufacturing chip, gas sensor assembly and method for plating carbon nano tube on chip Download PDFInfo
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- CN102279220A CN102279220A CN2011100586480A CN201110058648A CN102279220A CN 102279220 A CN102279220 A CN 102279220A CN 2011100586480 A CN2011100586480 A CN 2011100586480A CN 201110058648 A CN201110058648 A CN 201110058648A CN 102279220 A CN102279220 A CN 102279220A
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Abstract
The invention provides a method for manufacturing a chip. The chip is applicable to a gas sensor; and the method comprises the following steps of: 102, preparing electrodes of the chip on a substrate; 104, preparing connection lines between the electrodes on the substrate; and 106, plating carbon nano tubes onto the electrodes. By adopting the technical scheme of the invention, the chip provided with the carbon nano tube on the electrode can be manufactured, and the carbon nano tube guarantees detection of the gas sensor on gas to be rapid and sensitive. The invention also provides a gas sensor assembly and a method for plating the carbon nano tubes on the chip. According to the invention, fast and sensitivity of the chip of the gas sensor on gas detection are improved by virtue of the carbon nano tubes on the electrodes.
Description
Technical field
The present invention relates to receive the Mechatronic Systems technical field, in particular to a kind of make the method for chip, a kind of gas sensor device and a kind of on chip the method for plating carbon nano-tube.
Background technology
Breathing is human basic biological phenomena, by to breathing the physical features (as behavioral characteristics such as expiration amount, respiratory rates) had and the check and analysis of chemical feature (as the branch subconstiuent in the expiratory air), can obtain the important information of relevant human physiology, pathology, psychologic status, universal day by day along with the residential care notion makes miniaturization, low cost, portable medical diagnostic equipment progressively come into family.Simultaneously, also constantly towards the development of residential care medical Instrument field, these fields also require the MEMS senser element to develop to miniaturization, low cost and high reliability direction to MEMS (receive Mechatronic Systems) sensor, to cooperate this type of application.
Traditional respiration transducer product all is the attached of other sensor specials, main adopts pressure sensor spare, the change of shape of chest, belly, perhaps near the variation of temperature temperature sensor monitors muzzle when draught head that real-time monitoring respiratory air flow causes or breathing.From practical application, these sensors have brought great inconvenience all for monitored person, and the comfort level that influence is used is difficult to portable use.And also there is the price height in more existing products on the market, and sensitivity is low, and system responses is slow, can not fast detecting number of chemical gas ingredients etc. fatal shortcoming.
Therefore, need a kind of new mode, can be delicately, the breathing gas at the user detects apace, and can accomplish portablely, do not influence the comfortable of user simultaneously.
Summary of the invention
Technical matters to be solved by this invention is, a kind of new mode is provided, can be delicately, the breathing gas at the user detects apace, and can accomplish portablely, do not influence the comfortable of user simultaneously.
In view of this, the invention provides a kind of method of making chip, chip is used for gas sensor, comprising: step 102, the electrode of making chip in substrate; Step 104 is made interelectrode line in substrate; Step 106 plates carbon nano-tube on electrode.By the technical program, can produce the chip that has carbon nano-tube on the electrode, guaranteed that by carbon nano-tube gas sensor detects rapidly and sensitively to gas.
In technique scheme, preferably, step 102 comprises: select the substrate as chip of silicon chip, piezoid or glass sheet, and dry; Sputter Cr/Cu Seed Layer in substrate; To carrying out whirl coating, photoetching on the suprabasil Cr/Cu; Suprabasil Cr/Cu is carried out etching, to form electrode.
In technique scheme, preferably, step 104 comprises: carry out whirl coating, photoetching in substrate; Sputter Cr/Cu Seed Layer in substrate; Substrate is removed photoresist, to form line.
In technique scheme, preferably, step 106 comprises: carry out whirl coating, photoetching in substrate, with the protection line, discharge electrode; Electronickelling on electrode; On the nickel of electrode, plate carbon nano-tube.
The present invention also provides a kind of gas sensor device, comprises signal generator, sensor chip, current/voltage converter, bandpass filter, AC/DC converter, A/D converter, Programmable Logic Controller, wherein,
Signal generator is for sensor chip provides the sine wave AC signal;
Sensor is coated with carbon nano-tube on the electrode of the chip of sensor, receives the sine wave AC signal of automatic signal generator, and gas is produced induction, forms current signal;
Current/voltage converter receives the current signal from sensor, and induction current is carried out current/voltage-converted and difference amplification, forms ac voltage signal;
Bandpass filter receives the ac voltage signal from the current/voltage sensor, and ac voltage signal is carried out Filtering Processing;
The AC/DC converter receives the ac voltage signal from bandpass filter, and converts d. c. voltage signal to;
A/D converter receives the d. c. voltage signal from the AC/DC converter, is digital signal with voltage signal by analog signal conversion;
Programmable Logic Controller receives the digital signal from A/D converter, and digital signal is carried out analyzing and processing, and the output result data.By this technical scheme, gas sensor device is detected gas rapidly and sensitively, and gas is analyzed.
In technique scheme, preferably, signal generator is the oscillator of being made up of operational amplifier and RC Wien bridge circuit.
In technique scheme, preferably, current/voltage converter is the negative-feedback circuit of being made up of operational amplifier and feedback resistance in parallel.
In technique scheme, preferably, bandpass filter is the second-order bandpass filter that RC feedback network and operational amplifier are formed.
In technique scheme, preferably, the AC/DC converter is a linear detection circuit.
In technique scheme, preferably, also comprise: display module receives the result data from Programmable Logic Controller, and the mode of result data with waveform is shown; Memory module receives from the result data of Programmable Logic Controller and stores; Abnormal module receives the result data from Programmable Logic Controller, and judges according to result data whether gas exists unusually.
The present invention also provides a kind of method of plating carbon nano-tube on chip, and chip is used for gas sensor, comprising: step 302 is dispersed in even carbon nanotube in the acetone soln; Step 304 is carried out sonicated to the acetone soln that contains carbon nano-tube; Step 306 by electrophoresis, is plated to the carbon nano-tube in the acetone soln on the electrode of chip.By this technical scheme, can guarantee the susceptibility of chip with on the electrode of even carbon nanotube attached to chip to gas.
By above technical scheme, can realize a kind of method of making method, the gas sensor device of chip and on chip, plating carbon nano-tube, by the carbon nano-tube on the electrode, strengthen of speed and the sensitivity of the chip of gas sensor to gas detection.
Description of drawings
Fig. 1 is the process flow diagram of the method for manufacturing chip according to an embodiment of the invention;
Fig. 2 is the block diagram of gas sensor device according to an embodiment of the invention;
Fig. 3 is the process flow diagram that plates the method for carbon nano-tube on chip according to an embodiment of the invention;
Fig. 4 A to Fig. 4 E, Fig. 5 A to Fig. 5 D and Fig. 6 A to 6D all are synoptic diagram of the method for manufacturing chip according to an embodiment of the invention;
Fig. 7 is chip according to an embodiment of the invention induction synoptic diagram to gas when being used for gas sensor;
Fig. 8 is the principle schematic of chip detection gas according to an embodiment of the invention;
Fig. 9 is the block diagram of the device of gas sensor according to an embodiment of the invention;
Figure 10 is the circuit diagram of gas sensor according to an embodiment of the invention;
Figure 11 is the synoptic diagram of the electrode gap that produces of the method for manufacturing chip according to an embodiment of the invention;
Figure 12 is the comparison synoptic diagram of breathing response curve of the respiration transducer device of gas sensor device according to an embodiment of the invention and prior art;
Figure 13 is the waveform synoptic diagram that gas sensor device response according to an embodiment of the invention is breathed;
Figure 14 A to 14F is respectively the waveform synoptic diagram that the response of gas sensor device according to an embodiment of the invention under different temperatures breathed;
Figure 15 is the performance comparison synoptic diagram of gas sensor according to an embodiment of the invention and Honeywell sensor.
Embodiment
In order more to be expressly understood above-mentioned purpose of the present invention, feature and advantage, the present invention is further described in detail below in conjunction with the drawings and specific embodiments.
Set forth a lot of details in the following description so that fully understand the present invention, still, the present invention can also adopt other to be different from other modes described here and implement, and therefore, the present invention is not limited to the restriction of following public specific embodiment.
Fig. 1 is the process flow diagram of the method for manufacturing chip according to an embodiment of the invention.
As shown in Figure 1, the invention provides a kind of method of making chip, chip is used for gas sensor, comprising: step 102, the electrode of making chip in substrate; Step 104 is made interelectrode line in substrate; Step 106 plates carbon nano-tube on electrode.By the technical program, can produce the chip that has carbon nano-tube on the electrode, guaranteed that by carbon nano-tube gas sensor detects rapidly and sensitively to gas.
In technique scheme, step 102 comprises: select the substrate as chip of silicon chip, piezoid or glass sheet, and dry; Sputter Cr/Cu Seed Layer in substrate; To carrying out whirl coating, photoetching on the suprabasil Cr/Cu; Observe the development situation of substrate; According to the development situation, suprabasil Cr/Cu is carried out etching, to form electrode.
In technique scheme, step 104 comprises: carry out whirl coating, photoetching in substrate; Sputter Cr/Cu Seed Layer in substrate; Substrate is removed photoresist, to form line.
In technique scheme, step 106 comprises: carry out whirl coating, photoetching in substrate, with the protection line, discharge electrode; Electronickelling on electrode; On the nickel of electrode, plate carbon nano-tube.
Fig. 2 is the block diagram of gas sensor device according to an embodiment of the invention.
As shown in Figure 2, the present invention also provides a kind of gas sensor device 200, comprise signal generator 202, sensor 204, current/voltage converter 206, bandpass filter 208, AC/DC converter 210, A/D converter 212, Programmable Logic Controller 214, wherein
Signal generator 202 is for sensor 204 provides the sine wave AC signal;
Sensor 204 is coated with carbon nano-tube on the electrode of the chip of sensor 204, receives the sine wave AC signal of automatic signal generator 202, and gas is produced induction, forms current signal;
Current/voltage converter 206 receives the current signal from sensor 204, and induction current is carried out current/voltage-converted and difference amplification, forms ac voltage signal;
Bandpass filter 208 receives the ac voltage signal from current/voltage sensor 206, and ac voltage signal is carried out Filtering Processing;
AC/DC converter 210 receives the ac voltage signal from bandpass filter 208, and converts d. c. voltage signal to;
A/D converter 212 receives the d. c. voltage signal from AC/DC converter 210, is digital signal with voltage signal by analog signal conversion;
Programmable Logic Controller 214 receives the digital signal from A/D converter 212, and digital signal is carried out analyzing and processing, and the output result data.By this technical scheme, gas sensor device is detected gas rapidly and sensitively, and gas is analyzed.
In technique scheme, preferably, signal generator 202 is the oscillator of being made up of operational amplifier and RC Wien bridge circuit.
In technique scheme, preferably, current/voltage converter 206 is the negative-feedback circuit of being made up of operational amplifier and feedback resistance in parallel.
In technique scheme, preferably, bandpass filter 208 is the second-order bandpass filter that RC feedback network and operational amplifier are formed.
In technique scheme, preferably, AC/DC converter 210 is a linear detection circuit.
In technique scheme, preferably, also comprise: display module receives the result data from Programmable Logic Controller, and the mode of result data with waveform is shown; Memory module receives from the result data of Programmable Logic Controller and stores; Abnormal module receives the result data from Programmable Logic Controller, and judges according to result data whether gas exists unusually.
Fig. 3 is the process flow diagram that plates the method for carbon nano-tube on chip according to an embodiment of the invention.
As shown in Figure 3, the present invention also provides a kind of method of plating carbon nano-tube on chip, and chip is used for gas sensor, comprising: step 302 is dispersed in even carbon nanotube in the acetone soln; Step 304 is carried out sonicated to the acetone soln that contains carbon nano-tube; Step 306 by electrophoresis, is plated to the carbon nano-tube in the acetone soln on the electrode of chip.By this technical scheme, can guarantee the susceptibility of chip with on the electrode of even carbon nanotube attached to chip to gas.
Fig. 4 A to Fig. 4 E, Fig. 5 A to Fig. 5 D and Fig. 6 A to 6D all are synoptic diagram of the method for manufacturing chip according to an embodiment of the invention.
The manufacturing of sensor chip may further comprise the steps:
1. preparation electrode pattern
1) shown in Fig. 4 A, the baking sheet is the surface of substrate 402 with dry silicon chip, piezoid or glass sheet;
2) shown in Fig. 4 B, sputter Cr/Cu 404 Seed Layer;
3) shown in Fig. 4 C, whirl coating 406 wherein needs:
Preceding baking is to remove surface moisture; The little lines of photoetching sun plate need " overexposure " (Cr plate, positive plate) when exposing; Develop; Steps such as back baking.
4) shown in Fig. 4 D, observe the situation of development part 408;
5) shown in Fig. 4 E, wet etching is carved copper and is carved chromium, reserves Cr/Cu chip structure figure 410, forms electrode pattern.
2. make and electroplate with each interelectrode line
1) shown in Fig. 5 A, whirl coating 502, photoetching;
2) shown in Fig. 5 B, develop normal exposure, the effect of observation development part 504;
3) shown in Fig. 5 C, sputter Cr/Cu Seed Layer (also can use the Ti/Cu Seed Layer instead);
4) shown in Fig. 5 D, carry out lift-off, and immersion in acetone (whether decision ultrasonic according to circumstances).
3. swimming plating
1) as shown in Figure 6A, whirl coating 602 covers the line zone
2) shown in Fig. 6 B, photoetching is developed, and observes the effect of development part 604, discharges the electrode part, protection line part;
3) electronickelling 606;
4) whirl coating protection, fast baking;
5) back of the body is cut hemisection;
6) electroplate carbon nano-tube;
4. nitrogen dries up, test.
Wherein, the operating process of electronickelling:
1) nickel plating solution heats on magnetic stirring apparatus, stirs;
2) stop during nickel plating stirring, constant temperature carries out, and the electronickelling plate connects+utmost point, and device connects-utmost point;
3) power supply is selected constant current mode, Control current density;＜=2～3mA/cm2
4) control electrode area.Method:
Electroplate the process of carbon nano-tube:
1) acetone soln cleans beaker;
2) measure acetone, MWNT, Mg (NO3) 26H2O is an amount of, obtains acetone soln;
3) preservative film covers beaker and carries out ultrasonicly, takes out after every ultrasonic a period of time and leaves standstill cooling, prevents that temperature is higher;
4) power supply is selected constant voltage mode, slow then boosted voltage value, the relation of Control work voltage and electrode separation, and control electrophoresis time.
We have made the chip of gas sensor by above method.The characteristic of this sensor is: by adding local high electric field, make gas ionization to be measured, the detection to gas is carried out in the generation discharge.Different gas, its voltage breakdown difference, and also a kind of gas is under same voltage, and its gas concentration also will have different discharge currents.Utilize this specific character, the ionization type gas sensor can be discerned the kind and the concentration of gas.Now the gas that can discern has following several:
1.CH
4(methane)
(2.He helium)
3.H
2(hydrogen)
(4.Ar argon gas)
(5.CO carbon monoxide)
(6.Air air)
7.N
2(nitrogen)
8.O
2(oxygen)
The chip of this gas sensor to the induction curve of above all gases as shown in Figure 7.
The ionization mechanism of this gas sensor is: electronics begins to quicken under electric field action, electric field energy is converted into electronic kinetic energy, and electronics collides with neutral ion in motion process, in this process, if the energy that neutral particle absorbs is greater than its ionization energy, ionization process produces, and causes new electronics to generate, more electronics will cause more substantial ionization process, increase as the avalanche type effect.The avalanche effect model is shown in Fig. 8 A to 8C.
Fig. 9 is the block diagram of the device of gas sensor according to an embodiment of the invention.
As shown in Figure 9, the structure of gas sensor comprises: compositions such as signal generator 902, sensor (having carbon nano-tube on the electrode) 904, current/voltage converter 906, bandpass filter 908, AC/DC converter 910, A/D converter (A/D) 912, FPGA programmable logic device 914, LCD LCD MODULE 916, SD card memory circuit 918, adnormal respiration warning circuit 920.
Its principle of work is, the sine wave AC signal that signal generator 202 sends is supplied with carbon nano-tube respiration transducer 904, the current signal that respiration transducer 904 changes with the power output of breathing, this signal converts ac voltage signal to through current/voltage converter 906, through bandpass filter 908 the operational amplifier spurious signal is filtered, through AC/DC converter 910 ac voltage signal is converted to d. c. voltage signal then, through A/D converter 912 analog signal conversion is become digital signal again, carry out data processing by FPGA programmable logic device 914, by SD card memory circuit 918 storage data, demonstrate the breath signal of measurement simultaneously by LCD LCD MODULE 916, when the breathing appearance is unusual, report to the police by warning circuit 920.
Figure 10 is the circuit diagram of gas sensor according to an embodiment of the invention.
As shown in figure 10, the circuit of gas sensor is as follows in the present embodiment: as the signal generator 1002 of alternating-current voltage source, the oscillator of forming by amplifier and RC Wien bridge circuit that adopts, it produces fixed ampllitude, frequency stabilization sine wave signal, adopt the negative feedback network of resistance and diode composition for fixed ampllitude, utilize diode forward resistance with the principle that the rising of voltage reduces, depth of feedback is promptly gained change, thereby reach the purpose of fixed ampllitude.The negative-feedback circuit in parallel that current/voltage converter 1004 is made up of operational amplifier and feedback resistance, its input, output impedance are all very low, and output voltage is controlled by input current fully.Bandpass filter 1006 is the degenerative second-order bandpass filters of multichannel, and it is made up of R.C feedback network and operational amplifier.AC/DC converter 1008 is linear detection circuits, its input ac voltage signal, output be absolute average.It is made up of two stage amplifer, and prime is full-wave rectification, and the back level is a low-pass filtering.And the A/D converter (not shown) can adopt serial chip ADS7816..
Figure 11 is the synoptic diagram of the electrode gap that produces of the method for manufacturing chip according to an embodiment of the invention.
Chip electrode gap location SEM (scanning electron microscope) photo for sensor has covered the moderate multi-wall carbon nano-tube film of one deck concentration on the show electrode among the figure, the tip of a lot of carbon nano-tube is arranged on electrode sidewall.
Test result shows that carbon nano-tube film has greatly strengthened the susceptibility of sensor to breathing gas, and simultaneously sensor sheet has revealed high sensitivity and to the high noise immunity of temperature drift and air draught.The longitudinal axis is response current the voltage signal that through peripheral system circuit amplification obtain of sensor to human body respiration in the test result, corresponding to the respiratory intensity of respiratory wave.The sensor current response signal through the gain that peripheral circuit is converted into voltage signal is.The transverse axis coordinate is the time, the frequency characteristic that can obtain breathing by test result.
Figure 12 is the comparison synoptic diagram of breathing response curve of the respiration transducer device of gas sensor device according to an embodiment of the invention and prior art.Have carbon nano-tube on the electrode according to the gas of technical solution of the present invention (at breathing) sensor device chip, and do not have carbon nano-tube on the electrode of the gas sensor device chip of prior art (being the simple metal electrode).As shown in Figure 6, simple metal electrode sensor output signal is difficult to be detected, and carbon nano tube sensor has shown good susceptibility.
Figure 13 is the waveform synoptic diagram that gas sensor device response according to an embodiment of the invention is breathed.
As shown in figure 13, this gas sensor device can be differentiated 100 times/minute breathing, breathe far above the normal human 16～20 times/minute.With flowmeter breathing gas is carried out the demarcation of flow simultaneously, this sensor can be differentiated the respiratory wave of 0.5slpm flow as can be known.
Figure 14 A to 14F is respectively the waveform synoptic diagram that the response of gas sensor device according to an embodiment of the invention under different temperatures breathed.
Shown in Figure 14 A to 14F, be respectively the breathing response test result that gas sensor device carries out under different temperature, be specially 35,40,45,50, under 6 condition of different temperatures of 55,60 degree, the breathing Response Table of gas sensor device has revealed good stability.Simultaneously, be the response of test gas sensor device under extraneous air-flow effect, pressurized air is acted on the sensor chip of gas sensor device with the form of pulse gas, can find that signal can not recognize that almost this gas sensor device has shown good antijamming capability.
Figure 15 is the performance comparison synoptic diagram of gas sensor according to an embodiment of the invention and Honeywell sensor.
As shown in figure 15, be the performance synoptic diagram relatively of gas sensor in the present embodiment and Honeywell sensor (MFM), as seen, the performance of the gas sensor in the present embodiment is obviously more excellent.
In sum, can realize a kind of method of making method, the gas sensor device of chip and on chip, plating carbon nano-tube,, strengthen of speed and the sensitivity of the chip of gas sensor gas detection by the carbon nano-tube on the electrode.
The above is the preferred embodiments of the present invention only, is not limited to the present invention, and for a person skilled in the art, the present invention can have various changes and variation.For example, though the present invention has mentioned respiration transducer, should be appreciated that the present invention can be used in the occasion that any needs carry out gas sensing.Therefore, within the spirit and principles in the present invention all, any modification of being done, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. method of making chip, described chip is used for gas sensor, it is characterized in that, comprising:
Step 102, the electrode of the described chip of making in substrate;
Step 104 is made described interelectrode line in described substrate;
Step 106 plates carbon nano-tube on described electrode.
2. method according to claim 1 is characterized in that, described step 102 comprises:
Select the substrate of silicon chip, piezoid or glass sheet, and dry as described chip;
Sputter Cr/Cu Seed Layer in described substrate;
To carrying out whirl coating, photoetching on the described suprabasil Cr/Cu;
Described suprabasil Cr/Cu is carried out etching, to form described electrode.
3. method according to claim 1 is characterized in that, described step 104 comprises:
In described substrate, carry out whirl coating, photoetching;
Sputter Cr/Cu Seed Layer in described substrate;
Described substrate is removed photoresist, to form described line.
4. method according to claim 1 is characterized in that, described step 106 comprises:
In described substrate, carry out whirl coating, photoetching,, discharge described electrode to protect described line;
Electronickelling on described electrode;
On the nickel of described electrode, plate carbon nano-tube.
5. a gas sensor device is characterized in that, comprises signal generator, sensor chip, current/voltage converter, bandpass filter, AC/DC converter, A/D converter, Programmable Logic Controller, wherein,
Described signal generator is for described sensor chip provides the sine wave AC signal;
Described sensor is coated with carbon nano-tube on the electrode of the chip of described sensor, receives the described sine wave AC signal from described signal generator, and gas is produced induction, forms current signal;
Described current/voltage converter receives the described current signal from described sensor, and described induction current is carried out current/voltage-converted and difference amplification, forms ac voltage signal;
Described bandpass filter receives the described ac voltage signal from described current/voltage sensor, and described ac voltage signal is carried out Filtering Processing;
Described AC/DC converter receives the described ac voltage signal from described bandpass filter, and converts d. c. voltage signal to;
Described A/D converter receives the described d. c. voltage signal from described AC/DC converter, is digital signal with described voltage signal by analog signal conversion;
Described Programmable Logic Controller receives the described digital signal from described A/D converter, and described digital signal is carried out analyzing and processing, and the output result data.
6. gas sensor device according to claim 5 is characterized in that, described signal generator is the oscillator of being made up of operational amplifier and RC Wien bridge circuit.
7. gas sensor device according to claim 5 is characterized in that, described current/voltage converter is the negative-feedback circuit of being made up of operational amplifier and feedback resistance in parallel.
8. gas sensor device according to claim 5 is characterized in that, described AC/DC converter is a linear detection circuit.
9. according to each described gas sensor device in the claim 5 to 8, it is characterized in that, also comprise:
Display module receives the described result data from described Programmable Logic Controller, and the mode of described result data with waveform shown;
Memory module receives from the described result data of described Programmable Logic Controller and stores;
Abnormal module receives the described result data from described Programmable Logic Controller, and judges according to described result data whether gas exists unusually.
One kind on chip the plating carbon nano-tube method, described chip is used for gas sensor, it is characterized in that, comprising:
Step 302 is dispersed in even carbon nanotube in the acetone soln;
Step 304 is carried out sonicated to the described acetone soln that contains described carbon nano-tube;
Step 306 by electrophoresis, is plated to the described carbon nano-tube in the described acetone soln on the electrode of described chip.
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| CN109336047A (en) * | 2018-10-08 | 2019-02-15 | 东北大学 | A kind of multilayered structure ion source chip and mass spectral analysis sampling system based on MEMS technology |
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| CN103529105A (en) * | 2013-11-06 | 2014-01-22 | 惠州市富济电子材料有限公司 | Tube-type oxygen sensor testing electrodes and protective layers |
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Application publication date: 20111214 |