CN112798649B - Method for preparing noble metal quantum dot modified multilayer nano composite film gas sensor - Google Patents

Method for preparing noble metal quantum dot modified multilayer nano composite film gas sensor Download PDF

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CN112798649B
CN112798649B CN202011565905.5A CN202011565905A CN112798649B CN 112798649 B CN112798649 B CN 112798649B CN 202011565905 A CN202011565905 A CN 202011565905A CN 112798649 B CN112798649 B CN 112798649B
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drying
noble metal
wafer substrate
quantum dot
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CN112798649A (en
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王海容
田鑫
王久洪
曹慧通
李剑
金成�
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Shenzhen Tianditong Electronics Co ltd
Xian Jiaotong University
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Xian Jiaotong University
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Abstract

The invention discloses a preparation method of a noble metal quantum dot modified multilayer nano composite film gas sensor, which adopts a double-sided oxidation and silicon nitride wafer as a substrate, adopts a noble metal quantum dot modified multilayer nano composite film as a gas sensitive material, is deposited on the silicon wafer substrate by a sputtering method, and is overlapped with a test electrode at the center above the front side of a silicon nitride layer, and the test electrode with a comb tooth-inserted tooth composite structure is arranged above the sensitive material; the heating wire is in a scissor shape and surrounds two layers on the periphery of the testing electrode, the leading-out end of the comb tooth-gear shaping composite testing electrode is arranged at the scissor opening of the heating wire, and the heating wire and the testing electrode are respectively connected with a pair of symmetrically distributed lead discs. The invention adopts the sputtering method to prepare the multilayer nano composite film and the quantum dots, and the sensor has simple structure, easy packaging, miniaturized structure and low power consumption; the gas-sensitive film has high consistency, and can detect target gas with extremely low concentration; the preparation process is streamlined, has high sensitivity and meets the production requirement of the wafer-level gas sensor.

Description

Method for preparing noble metal quantum dot modified multilayer nano composite film gas sensor
Technical Field
The invention relates to a Micro-Electro-mechanical System (MEMS) processing technology, in particular to a preparation method of a gas sensor based on a noble metal quantum dot modified multilayer nano composite film.
Background
Atmospheric pollution has become a common problem facing human beings, and there is an urgent need to maintain the cleanliness of the atmospheric environment on which we live by monitoring the air pollution condition and adopting measures to improve the air quality. The gas sensor is widely used for detecting gases such as air pollution, flammability, explosiveness, toxicity and harm as the most direct means for detecting the gases. With the development of scientific technology, the film type metal oxide gas sensor based on the MEMS technology becomes the mainstream gas sensor at present because of its good sensitivity, selectivity, stability and consistency. However, in some special occasions, the detection limit of the target gas needs to be extremely high, and a single gas-sensitive film often cannot meet the detection requirement, so that the structure of the gas-sensitive film needs to be researched to improve the detection limit. The existing research shows that the gas-sensitive effect can be greatly increased by a heterostructure formed by a noble metal quantum dot prepared by a hydrothermal method and a composite film, but the consistency of the sensor cannot be ensured, and the cost is high
The development of the MEMS technology pushes the traditional gas sensor to be miniaturized, the miniaturized gas sensor based on the MEMS technology not only ensures the consistency of a gas sensitive film, but also greatly reduces the price of the gas sensor, and the miniaturized gas sensor becomes the development trend of the gas sensor in the future. Therefore, research needs to be carried out on the noble metal quantum dots and the composite film to prepare the gas sensor based on the MEMS technology, which has high sensitivity, high consistency and low price.
Disclosure of Invention
In order to solve the defects in the prior art, the invention aims to provide a gas sensor based on a noble metal quantum dot modified multilayer nano composite film and a preparation method thereof, the invention solves the problem that the high sensitivity of the gas sensor and the MEMS process cannot be obtained at the same time, and the prepared sensor has simple structure and is easy to package; the structure is miniaturized, and the power consumption is low; the preparation process is streamlined, has high sensitivity, meets the wafer-level production requirement and greatly reduces the cost; the multilayer nano composite film and the quantum dots are prepared by a sputtering method, and the gas-sensitive film formed by the multilayer nano composite film and the quantum dots has high consistency. Extremely low concentrations of the target gas can be detected.
The invention is realized by the following technical scheme.
The invention discloses a preparation method of a noble metal quantum dot modified multilayer nano composite film gas sensor, which comprises the following steps:
1) selecting a silicon wafer substrate subjected to double-sided thermal oxidation and nitridation treatment;
2) uniformly coating photoresist on the selected silicon wafer substrate at low speed and high speed respectively;
3) drying the silicon wafer coated with the photoresist, and exposing to obtain a sensitive material pattern;
4) developing the silicon wafer etched with the sensitive material pattern by using an alkaline solution, drying after drying by blowing with nitrogen;
5) carrying out front sputtering SnO on the silicon chip obtained in the step 4) in sequence2、TiO2To obtain SnO2-TiO2Nano composite film, TiO on last layer2Sputtering a layer of noble metal quantum dots;
6) sequentially putting the silicon wafer obtained in the step 5) into acetone and absolute ethyl alcohol to be respectively soaked and ultrasonically stripped, then washing with deionized water, drying with nitrogen at high temperature, and annealing;
7) uniformly coating photoresist on the front side of the silicon wafer obtained in the step 6) by adopting the method in the step 2);
8) drying the silicon wafer obtained in the step 7), and then carrying out exposure to obtain the designed graphs of the heating wire and the lead wire disc thereof;
9) developing the silicon wafer obtained in the step 8) by using a NaOH solution, and then drying;
10) evaporating Cr and Au on the front surface of the silicon wafer obtained in the step 9) by using an electron beam;
11) sequentially putting the silicon chip obtained in the step 10) into acetone and absolute ethyl alcohol to respectively soak and ultrasonically strip, then washing with deionized water, drying with nitrogen and drying at high temperature;
12) uniformly coating photoresist on the front side of the silicon wafer obtained in the step 11) by adopting the method in the step 2), drying the silicon wafer coated with the photoresist, and then carrying out full exposure;
13) scribing, developing, washing away photoresist by using NaOH solution, and drying to obtain the noble metal quantum dot modified multilayer nano composite film-based gas sensor.
With respect to the above technical solutions, the present invention has a further preferable solution:
preferably, in the step 1), the selected silicon wafer is an N-type doped silicon wafer; and uniformly coating the selected silicon wafer substrate with photoresist at low speed of 500r/min and 6s and at high speed of 1500r/min and 40s respectively.
Preferably, in the steps 3), 8) and 12), the drying temperature is 80-100 ℃, the drying time is 5-10 min, and the exposure time is 7-9 s.
Preferably, in the steps 4), 9) and 13), the concentration of the alkaline solution is 5 per mill of NaOH, 5 per mill of KOH solution or 2.38% of TMAH solution, the developing time is 17s-25s, and the drying is carried out at the temperature of 100-120 ℃ for 10min-20 min.
Preferably, in the step 5), the selected SnO2Target and TiO2The purity is 99.99 percent, SnO2The layer thickness is 60nm-80nm, TiO2The thickness of the layer is 20nm-30nm, and the thickness of the noble metal quantum dot layer is 3nm-8 nm.
Preferably, in the step 5), SnO2The layers are sputtered by radio frequency: the power is 100W-150W, the sputtering time is 20min-30min, the argon flow is 20-30sccm, and the rotating speed of the silicon wafer substrate is 15-25 r/min;
TiO2the layers are sputtered by direct current: the sputtering current is 0.4-0.6A, the sputtering time is 10min-20min, the argon flow is 20-30sccm, and the rotating speed of the silicon wafer substrate is 15-25 r/min.
Preferably, in the step 5), the noble metal quantum dots are used for obtaining SnO2-TiO2Continuously sputtering Pt, Au, Ag or Pd by direct current in the same chamber on the basis of the nano composite film, wherein the sputtering current is 0.25-0.4A, the sputtering time is 8-20 s, the argon flow is 20-30sccm, and the rotating speed of a silicon wafer substrate is 50-60 r/min; the working pressure in the cavity is 3X10-3—1X10-3Pa。
Preferably, in the steps 6) and 11), the silicon wafer is sequentially soaked in acetone for 10-15min, ultrasonic treatment is carried out for 30-40s, and circulation is carried out for 2-4 times; then soaking in absolute ethyl alcohol for 10-30s, drying at 100-120 ℃ for 10-20 min, and annealing at 500-600 ℃ for 3-4 h.
Preferably, in the step 10), the thickness of the Cr layer is 50-100nm, and the thickness of the Au layer is 250-300 nm.
The invention further provides a noble metal quantum dot modified multilayer nano composite film gas sensor prepared by the method, which comprises a silicon wafer, silicon oxide, silicon nitride, a heating wire, a sensitive material, a test electrode, a heating wire lead disc and a test electrode lead disc; silicon oxide is arranged on the upper surface and the lower surface of the silicon chip, silicon nitride is arranged on the outer layer of the silicon oxide, and a heating wire, a sensitive material, a test electrode, a heating wire lead disc and a test electrode lead disc are arranged on one silicon nitride surface;
the testing electrode and the sensitive material are arranged above the front surface of the silicon nitride layer in a central lamination mode; the test electrode with the comb tooth-gear shaping composite structure is arranged above the sensitive material; the heating wires are in a scissor shape and surround the periphery of the test electrode for two layers; the leading-out end of the comb tooth-gear shaping composite testing electrode is arranged at the scissor opening of the heating wire; the heating wire and the testing electrode are respectively connected with a pair of symmetrically distributed lead discs.
Preferably, the test electrodes with the comb tooth-gear shaping composite structure are a pair, the comb teeth are inserted into each other to form gear shaping, and the leading-out ends of the test electrodes are led out from the diagonal line of the comb tooth structure and connected with the test electrode lead disc.
Preferably, the heating wire lead disc and the test electrode lead disc are symmetrically distributed along the right angle line of the sensitive material.
Due to the adoption of the technical scheme, the invention has the following beneficial effects:
1. based on MEMS technology, the structure is miniaturized, compared with the traditional ceramic tube type gas sensor, the size is reduced, and the power consumption is reduced.
2. The multilayer nano composite film modified by the noble metal quantum dots has a multilayer heterostructure, and the catalytic action of noble metals is added, so that the sensitivity is greatly improved, and target gas with extremely low concentration can be detected.
3. The multilayer nano composite film modified by the noble metal quantum dots with high sensitivity is combined with the MEMS technology, the preparation process is streamlined, the high sensitivity is realized, the wafer-level production requirement is met, and the cost is greatly reduced.
4. The sputtering method is adopted to carry out uniform mechanical film coating on the whole wafer, the film forming consistency is good, and the high consistency of a plurality of wafer-level gas sensors is ensured.
The sensitivity (S ═ R) of the gas sensor of the noble metal quantum dot modified multilayer nano composite film prepared by the methoda/Rg) Not less than 5.67, which is much higher than the sensitivity of the existing gas sensor.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the principles of the invention:
FIG. 1 is a cross-sectional view of a noble metal quantum dot-based multilayer nanocomposite film-modified gas sensor according to the present invention;
FIG. 2 is a plan view of a heater wire, a heater wire lead plate, a test electrode lead plate, and a sensitive material of the noble metal quantum dot-modified multilayer nanocomposite film-based gas sensor according to the present invention;
FIG. 3 is a flow chart of the present invention for preparing a gas sensor based on noble metal quantum dot modified multilayer nanocomposite film;
4(a) -4 (k) are flow charts of the manufacturing process of the gas sensor based on noble metal quantum dot modified multilayer nanocomposite film according to the present invention;
in the figure: 1. silicon; 2. silicon oxide; 3. silicon nitride; 4. heating wires; 5. a sensitive material; 6. a test electrode; 7. a heating wire lead disc; 8. the electrode lead pads are tested.
Detailed Description
The present invention will now be described in detail with reference to the drawings and specific embodiments, wherein the exemplary embodiments and descriptions of the present invention are provided to explain the present invention without limiting the invention thereto.
As shown in FIG. 1 and FIG. 2, the present invention is based on the quantum dot modification of noble metalsA gas sensor decorated with a multilayer nano composite film comprises a silicon chip 1 (figure 4(a)), silicon oxide 2, silicon nitride 3, a heating wire 4, a sensitive material 5, a test electrode 6, a heating wire lead disk 7 and a test electrode lead disk 8; silicon oxide 2 is arranged on the upper surface and the lower surface of a silicon wafer 1 (figure 4(b)), the outer layer of the silicon oxide 2 is silicon nitride 3, and a heating wire 4, a sensitive material 5, a test electrode 6, a heating wire lead disc 7 and a test electrode lead disc 8 are arranged on one silicon nitride 3 surface; the test electrode 6 and the sensitive material 5 are arranged above the front surface of the silicon nitride layer 3 in a central lamination mode; the test electrode 6 with the comb tooth-gear shaping composite structure is arranged above the sensitive material 5; the heating wire 4 is in a scissor shape and surrounds two layers on the periphery of the test electrode 6; the leading-out end of the comb tooth-gear shaping composite testing electrode 6 is arranged at the shearing edge of the heating wire 4; the heating wire 4 and the test electrode 6 are respectively connected with a pair of symmetrically distributed heating wire lead discs 7 and test electrode lead discs 8; cr and Au are used as the materials of the heating wire, the test electrode, the heating wire lead disc and the test electrode lead disc. Multilayer SnO with sensitive material modified by noble metal quantum dots2/TiO2A nanocomposite film.
As shown in fig. 2, a pair of test electrodes 6 with a comb-tooth and gear shaping composite structure are provided, the comb teeth are inserted into each other to form gear shaping, and the leading-out end of the test electrode 6 is led out from the diagonal line of the comb-tooth structure and connected with a test electrode lead disc 7; the heating wire 4 is in a scissor-shaped structure, is arranged above the silicon wafer substrate, and surrounds two layers on the periphery of the test electrode 6; the heating wire lead disc 7 and the test electrode lead disc 8 are stacked and distributed along the right angle line of the sensitive material 5.
The following provides a method for preparing a noble metal quantum dot-modified multilayer nanocomposite film-based gas sensor according to the present invention, as shown in fig. 3, comprising the following steps:
1) selecting a silicon wafer substrate subjected to double-sided thermal oxidation and nitridation treatment, as shown in fig. 4 (c); the selected silicon wafer is an N-type doped silicon wafer;
2) uniformly coating EPG535 photoresist on the selected silicon chip substrate at low speed of 500r/min and 6s and at high speed of 1500r/min and 40s, respectively, as shown in figure 4 (d);
3) drying the silicon wafer coated with the photoresist at 80-100 ℃ for 5-10 min, and exposing for 7-9 s to obtain a sensitive material pattern;
4) developing the silicon wafer etched with the sensitive material pattern for 17s-25s by using an alkaline solution, drying at 100-120 ℃ for 10min-20min after drying by nitrogen; the concentration of the alkaline solution is 5 per mill NaOH, (5 per mill) KOH solution or (2.38%) TMAH solution, as shown in figure 4 (e);
5) carrying out front sputtering SnO on the silicon chip obtained in the step 4) in sequence2、TiO2To obtain SnO2-TiO2Multilayer nanocomposite film, TiO on last layer2A layer of noble metal quantum dots is sputtered on the surface, as shown in fig. 4 (f).
Selected SnO2Target and TiO2The purity is 99.99 percent, SnO2The layer thickness is 60nm-80nm, TiO2The thickness of the layer is 20nm-30nm, and the thickness of the noble metal quantum dot layer is 3-8 nm;
SnO2the layers are sputtered by radio frequency: the power is 100W-150W, the sputtering time is 20min-30min, the argon flow is 20-30sccm, and the rotating speed of the silicon wafer substrate is 15-25 r/min.
TiO2The layers are sputtered by direct current: the sputtering current is 0.4-0.6A, the sputtering time is 10min-20min, the argon flow is 20-30sccm, and the rotating speed of the silicon wafer substrate is 15-25 r/min.
Obtaining SnO from noble metal quantum dots2-TiO2Continuously sputtering Pt, Au, Ag or Pd by direct current in the same chamber on the basis of the nano composite film, wherein the sputtering current is 0.25-0.4A, the sputtering time is 8-20 s, the argon flow is 20-30sccm, and the rotating speed of a silicon wafer substrate is 50-60 r/min; the working pressure in the cavity is 3X10-3—1X10-3Pa。
6) Sequentially putting the silicon chip obtained in the step 5) into acetone for soaking for 10-15min, performing ultrasonic treatment for 30-40s, and circulating for 2-4 times; stripping, soaking in anhydrous ethanol for 10-30s, washing with deionized water, blowing with nitrogen, drying at 100-120 deg.C for 10-20 min, and annealing at 600 deg.C for 3-4h, as shown in FIG. 4 (g);
7) uniformly coating photoresist on the front side of the silicon wafer obtained in the step 6) by adopting the method in the step 2), and obtaining a graph in fig. 4 (h);
8) drying the silicon wafer obtained in the step 7) at 80-100 ℃ for 5-10 min, and then exposing for 7-9 s to obtain the designed patterns of the heating wire and the lead plate thereof;
9) developing the silicon wafer obtained in the step 8) by using an alkaline solution for 17s-25s, drying the silicon wafer at 100-120 ℃ for 10min-20min after drying by using nitrogen, and obtaining a graph (i) in fig. 4;
10) evaporating Cr and Au on the front surface of the silicon wafer obtained in the step 9) by using an electron beam; the thickness of the Cr layer is 50-100nm, the thickness of the Au layer is 250-300 nm, see FIG. 4 (j);
11) sequentially putting the silicon chip obtained in the step 10) into acetone for soaking for 10-15min, performing ultrasonic treatment for 30-40s, and circulating for 2-4 times; stripping, soaking in anhydrous ethanol for 10-30s, washing with deionized water, blowing with nitrogen, drying at 100-120 deg.C for 10-20 min, and annealing at 600 deg.C for 3-4h, as shown in FIG. 4 (k);
12) uniformly coating photoresist on the front side of the silicon wafer obtained in the step 11) by adopting the method in the step 2), drying the silicon wafer coated with the photoresist at 80-100 ℃ for 5-10 min, and then carrying out full exposure for 7-9 s;
13) scribing the sheet in the step 12), developing for 17s-25s, washing away photoresist by using an alkaline solution, drying for 10min-20min at 100-120 ℃ after drying by nitrogen, and obtaining the gas sensor based on the noble metal quantum dot modified multilayer nano composite film.
The process of the invention is further illustrated by the following examples.
Example 1
1) Selecting a silicon wafer with N type doping, crystal orientation of 100, resistance of 1-5ohm.cm and thickness of 400um, then carrying out double-sided thermal oxidation to form an oxide layer with thickness of 500nm, and depositing Si by double-sided LPCVD3N4The thickness of the formed desalination layer is 150 nm;
2) uniformly coating EPG535 type photoresist on a silicon wafer substrate with a double-sided oxide layer and a fading layer at low speed of 500r/min and 6s and at high speed of 1500r/min and 40s respectively;
3) baking the silicon wafer evenly coated with the photoresist for 5min at 95 ℃, and then exposing the photoresist for 7s by using a designed sensitive material mask to obtain a designed sensitive material graph;
4) placing the exposed silicon wafer in 5 per mill NaOH solution for developing for 20s, drying by blowing with nitrogen and drying at 110 ℃ for 10 min;
5) putting the silicon slice obtained in the step 4) into a sputtering machine for front sputtering SnO2、TiO2Six times in total to obtain the nano composite film SnO2-TiO2-SnO2-TiO2-SnO2-TiO2Six layers in total, the SnO2 layer adopts radio frequency sputtering, the power is 100W, the sputtering time is 25min, the argon flow is 20sccm, the rotating speed of the silicon wafer substrate is 20r/min, and the SnO is obtained2The monolayer thickness is 70 nm; TiO 22The layer is sputtered by direct current with sputtering current of 0.5A for 15min, argon flow of 20sccm, and silicon wafer substrate rotation speed of 10r/min to obtain TiO2The monolayer thickness is 25.5 nm; TiO in the last layer2A layer of Pt quantum dots is sputtered by direct current, the sputtering current is 0.3A, the sputtering time is 10s, the argon flow is 20sccm, and the rotating speed of the silicon wafer substrate is 50 r/min; the thickness of the noble metal quantum dot layer is 8 nm; the working pressure in the cavity is 1X10-3Pa；
6) Sequentially putting the silicon chip obtained in the step 5) into acetone for soaking for 12min, performing ultrasonic treatment for 30s, and circulating for 3 times; stripping, then soaking in absolute ethyl alcohol for 30s, washing with deionized water, drying with nitrogen, drying at a high temperature of 110 ℃ for 10min, and annealing at a temperature of 500 ℃ for 3 h;
7) uniformly coating photoresist on the front side of the silicon wafer obtained in the step 6) by adopting the method in the step 2);
8) baking the silicon wafer obtained in the step 7) at 95 ℃ for 5min, and then exposing the photoresist for 7s by using a designed mask plate with heating wires, test electrodes and the like to obtain a designed graph with the heating wires, the test electrodes and the like;
9) placing the exposed silicon wafer in 5 per mill NaOH solution for developing for 20s, drying by blowing with nitrogen and drying at 110 ℃ for 10 min;
10) performing electron beam evaporation on the front surface of the silicon wafer obtained in the step 9) to form Cr and Au, wherein the thickness of the Cr layer is 50nm, and the thickness of the Au layer is 250 nm;
11) sequentially putting the silicon chip obtained in the step 10) into acetone for soaking for 10min, performing ultrasonic treatment for 40s, and circulating for 4 times; stripping, then soaking in absolute ethyl alcohol for 10s, washing with deionized water, drying with nitrogen, drying at high temperature of 100 ℃ for 15min, and annealing at 550 ℃ for 4 h;
12) uniformly coating photoresist on the front side of the silicon wafer obtained in the step 11) by adopting the method in the step 2), drying the silicon wafer coated with the photoresist for 5min at 95 ℃, and then carrying out full exposure for 9 s;
13) scribing the film in the step 12), developing for 20s, washing away photoresist by using 5 per mill NaOH solution, and drying at 110 ℃ for 10min to obtain the noble metal quantum dot modified multilayer nano composite film-based gas sensor.
When the chip is placed in 50ppm ethanol gas to be detected, voltage is applied to two ends of the heating wire, the heating wire instantly generates 240 ℃ high temperature, the sensitive material and the gas to be detected react at the high temperature to change the conductivity of the gas-sensitive film, and the sensitivity of the gas sensor of the noble metal quantum dot modified multilayer nano composite film is detected by the testing electrode to be 23.46.
Example 2
1) Selecting a silicon wafer with N type doping, crystal orientation of 100, resistance of 1-5ohm.cm and thickness of 400um, then carrying out double-sided thermal oxidation to form an oxide layer with thickness of 500nm, and depositing Si by double-sided LPCVD3N4The thickness of the formed desalination layer is 150 nm;
2) uniformly coating EPG535 type photoresist on a silicon wafer substrate with a double-sided oxide layer and a fading layer at low speed of 500r/min and 6s and at high speed of 1500r/min and 40s respectively;
3) baking the silicon wafer evenly coated with the photoresist for 8min at 80 ℃, and then exposing the photoresist for 9s by using a designed sensitive material mask to obtain a designed sensitive material graph;
4) placing the exposed silicon wafer in 5% KOH solution for developing for 17s, drying by blowing with nitrogen, and drying at 120 ℃ for 15 min;
5) putting the silicon slice obtained in the step 4) into a sputtering machine for front sputtering SnO2、TiO2Six times in total to obtain the nano composite film SnO2-TiO2-SnO2-TiO2-SnO2-TiO2Six layers in total, SnO2The layer adopts radio frequency sputtering, the power is 150W, the sputtering time is 20min, the argon flow is 20sccm, the rotating speed of the silicon wafer substrate is 15r/min, and SnO is obtained2Single layer thickness of 70nm；TiO2The layer is sputtered by direct current with sputtering current of 0.6A for 10min, argon flow of 20sccm, and silicon wafer substrate rotation speed of 15r/min to obtain TiO2The monolayer thickness is 25.5 nm; TiO in the last layer2A layer of Pt quantum dots is sputtered by direct current, the sputtering current is 0.4A, the sputtering time is 15s, the argon flow is 30sccm, and the rotating speed of the silicon wafer substrate is 60 r/min; the thickness of the noble metal quantum dot layer is 3 nm; the working pressure in the cavity is 3X10-3Pa；
6) Sequentially putting the silicon chip obtained in the step 5) into acetone for soaking for 10min, performing ultrasonic treatment for 40s, and circulating for 4 times; stripping, then soaking in absolute ethyl alcohol for 20s, washing with deionized water, drying with nitrogen, drying at high temperature of 100 ℃ for 15min, and annealing at 550 ℃ for 3 h;
7) uniformly coating photoresist on the front side of the silicon wafer obtained in the step 6) by adopting the method in the step 2);
8) baking the silicon wafer obtained in the step 7) at 100 ℃ for 8min, and then exposing the photoresist for 8s by using a designed mask plate with heating wires, test electrodes and the like to obtain a designed graph with the heating wires, the test electrodes and the like;
9) placing the exposed silicon wafer in 5 per mill KOH solution for developing for 25s, drying by blowing with nitrogen and then drying at 100 ℃ for 10 min;
10) performing electron beam evaporation on the front surface of the silicon wafer obtained in the step 9) to form Cr and Au, wherein the thickness of the Cr layer is 100nm, and the thickness of the Au layer is 280 nm;
11) sequentially putting the silicon chip obtained in the step 10) into acetone for soaking for 12min, performing ultrasonic treatment for 30s, and circulating for 3 times; stripping, then soaking in absolute ethyl alcohol for 20s, washing with deionized water, drying with nitrogen, drying at a high temperature of 110 ℃ for 10min, and annealing at a temperature of 500 ℃ for 3 h;
12) uniformly coating photoresist on the front side of the silicon wafer obtained in the step 11) by adopting the method in the step 2), drying the silicon wafer coated with the photoresist for 10min at 100 ℃, and then carrying out full exposure for 7 s;
13) scribing the film in the step 12), developing for 17s, washing away photoresist by using 5 per mill NaOH solution, and drying at 100 ℃ for 20min to obtain the noble metal quantum dot modified multilayer nano composite film-based gas sensor.
When the chip is placed in 50ppm ethanol gas to be detected, voltage is applied to two ends of the heating wire, the heating wire instantly generates 240 ℃ high temperature, the sensitive material and the gas to be detected react at the high temperature to change the conductivity of the gas-sensitive film, and the sensitivity of the gas sensor of the noble metal quantum dot modified multilayer nano composite film is detected by the testing electrode to be 13.98.
Example 3
1) Selecting a silicon wafer with N type doping, crystal orientation of 100, resistance of 1-5ohm.cm and thickness of 400um, then carrying out double-sided thermal oxidation to form an oxide layer with thickness of 500nm, and depositing Si by double-sided LPCVD3N4The thickness of the formed desalination layer is 150 nm;
2) uniformly coating EPG535 type photoresist on a silicon wafer substrate with a double-sided oxide layer and a fading layer at low speed of 500r/min and 6s and at high speed of 1500r/min and 40s respectively;
3) baking the silicon wafer with the photoresist uniformly at 100 ℃ for 10min, and then exposing the photoresist for 8s by using a designed sensitive material mask to obtain a designed sensitive material graph;
4) placing the exposed silicon wafer in a 2.38% TMAH solution for developing for 20s, drying the silicon wafer by nitrogen for drying for 20min at 100 ℃;
5) putting the silicon slice obtained in the step 4) into a sputtering machine for front sputtering SnO2、TiO2Six times in total to obtain the nano composite film SnO2-TiO2-SnO2-TiO2-SnO2-TiO2Six layers in total, wherein the SnO2 layer is sputtered by radio frequency, the power is 130W, the sputtering time is 30min, the argon flow is 30sccm, the rotating speed of a silicon wafer substrate is 25r/min, and the SnO is obtained2The single-layer thickness is 80 nm; TiO 22The layer is sputtered by direct current with sputtering current of 0.4A for 20min, argon flow of 30sccm, and silicon wafer substrate rotation speed of 25r/min to obtain TiO2The monolayer thickness is 20 nm; TiO in the last layer2A layer of Pt quantum dots is sputtered by direct current, the sputtering current is 0.25A, the sputtering time is 20s, the argon flow is 25sccm, and the rotating speed of the silicon wafer substrate is 55 r/min; the thickness of the noble metal quantum dot layer is 5 nm; the working pressure in the cavity is 2X10-3Pa；
6) Sequentially putting the silicon chip obtained in the step 5) into acetone for soaking for 15min, performing ultrasonic treatment for 30s, and circulating for 2 times; stripping, then soaking in absolute ethyl alcohol for 10s, washing with deionized water, drying with nitrogen, drying at high temperature of 120 ℃ for 20min, and annealing at 600 ℃ for 4 h;
7) uniformly coating photoresist on the front side of the silicon wafer obtained in the step 6) by adopting the method in the step 2);
8) baking the silicon wafer obtained in the step 7) at 80 ℃ for 10min, and then exposing the photoresist for 9s by using a designed mask plate with heating wires, test electrodes and the like to obtain a designed graph with the heating wires, the test electrodes and the like;
9) placing the exposed silicon wafer in 5 per mill NaOH solution for developing for 17s, drying by blowing with nitrogen, and drying at 120 ℃ for 20 min;
10) performing electron beam evaporation on the front surface of the silicon wafer obtained in the step 9) to form Cr and Au, wherein the thickness of the Cr layer is 70nm, and the thickness of the Au layer is 300 nm;
11) sequentially putting the silicon chip obtained in the step 10) into acetone for soaking for 15min, performing ultrasonic treatment for 30s, and circulating for 2 times; stripping, then soaking in absolute ethyl alcohol for 30s, washing with deionized water, drying with nitrogen, drying at high temperature of 120 ℃ for 20min, and annealing at 600 ℃ for 3 h;
12) uniformly coating photoresist on the front side of the silicon wafer obtained in the step 11) by adopting the method in the step 2), drying the silicon wafer coated with the photoresist for 9min at 80 ℃, and then carrying out full exposure for 8 s;
13) scribing the film in the step 12), developing for 25s, washing away photoresist by using 5 per mill NaOH solution, and drying at 120 ℃ for 15min to obtain the noble metal quantum dot modified multilayer nanocomposite film-based gas sensor.
When the chip is placed in 50ppm ethanol gas to be detected, voltage is applied to two ends of the heating wire, the heating wire instantly generates 240 ℃ high temperature, the sensitive material and the gas to be detected react at the high temperature to change the conductivity of the gas-sensitive film, and the sensitivity of the gas sensor of the noble metal quantum dot modified multilayer nano composite film is detected by the testing electrode to be 11.94.
Example 4
1) Selecting N type doping, crystal orientation 100 and resistance 1-5ohm.cm, the thickness is 400um, then the double-sided thermal oxidation is carried out, the thickness of the formed oxide layer is 500nm, and Si is deposited by double-sided LPCVD3N4The thickness of the formed desalination layer is 150 nm;
2) uniformly coating EPG535 type photoresist on a silicon wafer substrate with a double-sided oxide layer and a fading layer at low speed of 500r/min and 6s and at high speed of 1500r/min and 40s respectively;
3) baking the silicon wafer evenly coated with the photoresist for 5min at 100 ℃, and then exposing the photoresist for 8s by using a designed sensitive material mask to obtain a designed sensitive material graph;
4) placing the exposed silicon wafer in 5 per mill NaOH solution for developing for 20s, drying by nitrogen and drying at 100 ℃ for 20 min;
5) putting the silicon slice obtained in the step 4) into a sputtering machine for front sputtering SnO2、TiO2Six times in total to obtain the nano composite film SnO2-TiO2-SnO2-TiO2-SnO2-TiO2Six layers in total, the SnO2 layer adopts radio frequency sputtering, the power is 120W, the sputtering time is 30min, the argon flow is 20sccm, the rotating speed of the silicon wafer substrate is 20r/min, and the SnO is obtained2The monolayer thickness is 70 nm; TiO 22The layer is sputtered by direct current with sputtering current of 0.5A for 25min, argon flow of 20sccm, and silicon wafer substrate rotation speed of 10r/min to obtain TiO2The single-layer thickness is 30 nm; TiO in the last layer2A layer of Pt quantum dots is sputtered by direct current, the sputtering current is 0.4A, the sputtering time is 15s, the argon flow is 30sccm, and the rotating speed of the silicon wafer substrate is 50 r/min; the working pressure in the cavity is 3X10-3Pa；
6) Sequentially putting the silicon chip obtained in the step 5) into acetone for soaking for 15min, performing ultrasonic treatment for 30s, and circulating for 3 times; stripping, then soaking in absolute ethyl alcohol for 20s, washing with deionized water, drying with nitrogen, drying at high temperature of 120 ℃ for 15min, and annealing at 600 ℃ for 3 h;
7) uniformly coating photoresist on the front side of the silicon wafer obtained in the step 6) by adopting the method in the step 2);
8) baking the silicon wafer obtained in the step 7) at 90 ℃ for 5min, and then exposing the photoresist for 8s by using a designed mask plate with heating wires, test electrodes and the like to obtain a designed graph with the heating wires, the test electrodes and the like;
9) placing the exposed silicon wafer in 5 per mill NaOH solution for developing for 18s, drying by blowing with nitrogen, and drying at 110 ℃ for 15 min;
10) performing electron beam evaporation on the front surface of the silicon wafer obtained in the step 9) to form Cr and Au, wherein the thickness of the Cr layer is 70nm, and the thickness of the Au layer is 290 nm;
11) sequentially putting the silicon chip obtained in the step 10) into acetone for soaking for 15min, performing ultrasonic treatment for 40s, and circulating for 3 times; stripping, then soaking in absolute ethyl alcohol for 20s, washing with deionized water, drying with nitrogen, drying at high temperature of 110 ℃ for 20min, and annealing at 600 ℃ for 3 h;
12) uniformly coating photoresist on the front side of the silicon wafer obtained in the step 11) by adopting the method in the step 2), drying the silicon wafer coated with the photoresist for 10min at 90 ℃, and then carrying out full exposure for 9 s;
13) scribing the film in the step 12), developing for 25s, washing away photoresist by using 5 per mill NaOH solution, and drying at 120 ℃ for 10min to obtain the noble metal quantum dot modified multilayer nano composite film-based gas sensor.
When the chip is placed in 50ppm ethanol gas to be detected, voltage is applied to two ends of the heating wire, the heating wire instantly generates 240 ℃ high temperature, the sensitive material and the gas to be detected react at the high temperature to change the conductivity of the gas-sensitive film, and the sensitivity of the gas sensor of the noble metal quantum dot modified multilayer nano composite film is detected by the testing electrode to be 5.67.
The noble metal quantum dot modified multilayer nano composite film gas sensor prepared by the method has the advantages of simple structure, local high temperature and easy packaging, and the structure is miniaturized, the size is reduced, and the power consumption is reduced based on the MEMS technology; the multilayer nano composite film modified based on the quantum dots greatly improves the gas-sensitive performance of the gas sensor, and can detect target gas with extremely low concentration; the high-sensitivity gas-sensitive film is combined with the MEMS technology, the preparation process is streamlined, high-sensitivity and wafer-level production are realized, and the cost is greatly reduced; the multilayer nano composite film and the quantum dots are prepared by a sputtering method, and the gas-sensitive film formed by the multilayer nano composite film and the quantum dots has high consistency. The preparation method can be used for preparing the gas sensor of the multilayer nano composite film modified by the noble metal quantum dots in large batch in industrial production.
The present invention is not limited to the above-mentioned embodiments, and based on the technical solutions disclosed in the present invention, those skilled in the art can make some substitutions and modifications to some technical features without creative efforts according to the disclosed technical contents, and these substitutions and modifications are all within the protection scope of the present invention.

Claims (8)

1. A preparation method of a noble metal quantum dot modified multilayer nano composite film gas sensor is characterized by comprising the following steps:
1) selecting a silicon wafer substrate subjected to double-sided thermal oxidation and nitridation treatment;
2) uniformly coating photoresist on the selected silicon wafer substrate at low speed and high speed respectively;
3) drying the silicon wafer substrate coated with the photoresist, and exposing to obtain a sensitive material pattern;
4) developing the silicon wafer substrate etched with the sensitive material pattern by using an alkaline solution, drying after drying by blowing with nitrogen;
5) carrying out front sputtering SnO on the silicon chip substrate obtained in the step 4) in sequence2、TiO2To obtain SnO2-TiO2Nano composite film, TiO on last layer2Sputtering a layer of noble metal quantum dots;
SnO2the layers are sputtered by radio frequency: the power is 100W-150W, the sputtering time is 20min-30min, the argon flow is 20-30sccm, and the rotating speed of the silicon wafer substrate is 15-25 r/min;
TiO2the layers are sputtered by direct current: sputtering current of 0.4-0.6A, sputtering time of 10-20 min, argon flow of 20-30sccm, and silicon wafer substrate rotation speed of 15-25 r/min;
obtaining SnO from noble metal quantum dots2-TiO2Sputtering Pt, Au, Ag or Pd continuously in the same chamber by direct current on the basis of the nano composite film, wherein the sputtering current is 0.25-0.4A, the sputtering time is 8-20 s, the argon flow is 20-30sccm, and the silicon waferThe rotating speed of the substrate is 50-60 r/min; working pressure in chamber 3X10-3—1Ⅹ10-3Pa；
6) Sequentially placing the silicon wafer substrate obtained in the step 5) into acetone and absolute ethyl alcohol to be respectively soaked and ultrasonically stripped, then washing with deionized water, drying with nitrogen, drying at high temperature, and annealing;
7) uniformly coating photoresist on the front side of the silicon wafer substrate obtained in the step 6) by adopting the method in the step 2);
8) drying the silicon wafer substrate obtained in the step 7) at 95 ℃ for 5min, and then exposing the photoresist for 7s by using a designed mask plate with a heating wire, a test electrode, a heating wire lead disc and a test electrode lead disc to obtain a designed pattern with the heating wire, the test electrode, the heating wire lead disc and the test electrode lead disc;
9) developing the silicon wafer substrate obtained in the step 8) by using a NaOH solution, and then drying;
10) evaporating Cr and Au on the front surface of the silicon wafer substrate obtained in the step 9) by using an electron beam;
11) sequentially placing the silicon wafer substrate obtained in the step 10) into acetone and absolute ethyl alcohol to be respectively soaked and ultrasonically stripped, then washing with deionized water, drying with nitrogen and drying at high temperature;
12) uniformly coating photoresist on the front side of the silicon wafer substrate obtained in the step 11) by adopting the method in the step 2), drying the silicon wafer substrate coated with the photoresist, and then carrying out full exposure;
13) scribing the silicon wafer substrate obtained in the step 12), developing, washing away photoresist by using NaOH solution, and drying to obtain the noble metal quantum dot modified multilayer nano composite film as the gas sensor of the sensitive material.
2. The method for preparing a noble metal quantum dot modified multilayer nanocomposite film gas sensor according to claim 1, wherein in the step 1), the selected silicon wafer substrate is an N-type doped silicon wafer; uniformly coating the silicon wafer substrate selected in the step 2) with photoresist at low speed of 500r/min and 6s and at high speed of 1500r/min and 40s respectively.
3. The method for preparing a noble metal quantum dot modified multilayer nanocomposite film gas sensor according to claim 1, wherein in the steps 3) and 12), the drying temperature is 80 ℃ to 100 ℃, the drying time is 5min to 10min, and the exposure time is 7s to 9 s.
4. The method for preparing a noble metal quantum dot modified multilayer nanocomposite film gas sensor according to claim 1, wherein in the step 4), the concentration of the alkaline solution is 5% o NaOH, 5% o KOH solution or 2.38% TMAH solution, the developing time is 17s-25s, and the sensor is dried at 100 ℃ -120 ℃ for 10min-20 min.
5. The method for preparing a noble metal quantum dot modified multilayer nanocomposite film gas sensor as claimed in claim 1, wherein in the step 5), the selected SnO2Target and TiO2The purity is 99.99 percent, SnO2The layer thickness is 60nm-80nm, TiO2The thickness of the layer is 20nm-30nm, and the thickness of the noble metal quantum dot layer is 3nm-8 nm.
6. The method for preparing the noble metal quantum dot modified multilayer nanocomposite film gas sensor according to claim 1, wherein in the steps 6) and 11), the silicon wafer substrate is sequentially soaked in acetone for 10-15min, subjected to ultrasonic treatment for 30-40s, and circulated for 2-4 times; then soaking in absolute ethyl alcohol for 10-30s, drying at 100-120 ℃ for 10-20 min, and annealing at 500-600 ℃ for 3-4 h.
7. The method for preparing a noble metal quantum dot modified multilayer nanocomposite film gas sensor according to claim 1, wherein in the step 10), the thickness of the Cr layer is 50-100nm, and the thickness of the Au layer is 250-300 nm.
8. A noble metal quantum dot modified multilayer nanocomposite thin film gas sensor prepared by the method of any one of claims 1 to 7, comprising a silicon wafer substrate, silicon oxide, silicon nitride, a heater wire, a sensitive material, a test electrode, a heater wire lead pad and a test electrode lead pad; silicon oxide is arranged on the lower surface of the silicon wafer substrate, silicon nitride is arranged on the outer layer of the silicon oxide, and a heating wire, a sensitive material, a test electrode, a heating wire lead disc and a test electrode lead disc are arranged on one silicon nitride surface;
the testing electrode and the sensitive material are arranged above the front surface of the silicon nitride layer in a central lamination mode; the test electrode with the comb tooth-gear shaping composite structure is arranged above the sensitive material; the heating wires are in a scissor shape and surround the periphery of the test electrode for two layers; the leading-out end of the comb tooth-gear shaping composite testing electrode is arranged at the scissor opening of the heating wire; the heating wire and the test electrode are respectively connected with a pair of symmetrically distributed lead discs;
the sensitive material is multilayer SnO modified by noble metal quantum dots2-TiO2A nanocomposite film.
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