CN109613085A - One kind being based on the gas sensitization chip array and preparation method thereof of [111] monocrystalline silicon - Google Patents
One kind being based on the gas sensitization chip array and preparation method thereof of [111] monocrystalline silicon Download PDFInfo
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- CN109613085A CN109613085A CN201811517619.4A CN201811517619A CN109613085A CN 109613085 A CN109613085 A CN 109613085A CN 201811517619 A CN201811517619 A CN 201811517619A CN 109613085 A CN109613085 A CN 109613085A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
Abstract
One kind being based on the gas sensitization chip array and preparation method thereof of [111] monocrystalline silicon, is related to gas sensor technical field.The present invention is to solve the problems, such as that the processing technology of the micro- heating plate of existing gas sensor is complicated.It is square wave-shaped configuration that the present invention, which heats electrode, Sensitive membrane electrode is pectinate texture, a pair of of Sensitive membrane electrode is located at the two sides of heating electrode, and heat the tooth for having a Sensitive membrane electrode between two adjacent square waves of electrode, the upper surface of heating electrode and two Sensitive membrane electrodes is covered with gas sensitization film, [111] monocrystal silicon substrate upper surface is provided with heat-insulation chamber, supporting layer is covered on [111] monocrystal silicon substrate upper surface, the etch pit of multiple rectangular array arrangements is provided on supporting layer, a gas sensitization chip is respectively and fixedly provided between two adjacent etch pits of every a line, the length direction of the extraction electrode of gas sensitization chip is in the same direction with [211] crystal orientation of [111] monocrystal silicon substrate.
Description
Technical field
The invention belongs to gas sensor technical fields.
Background technique
Conductor oxidate gas sensor is due to having many advantages, such as that making simple, at low cost, high sensitivity has obtained extensively
General application, but its poor selectivity, which also limits it, further to be developed.In order to improve conductor oxidate gas sensing
The selectivity of device, numerous researchers are also dedicated to exploitation gas sensor battle array in addition to conducting a research in terms of gas sensitive material
Column, by improving selectivity based on the mode identification method of sensor array.Such as: Publication No. CN104931540A, title
For a kind of gas sensor array and preparation method thereof " Chinese invention patent, disclose using single semi-conductive metal oxide
The gas sensor array of object nano material building, to improve the selectivity of gas sensor.But above-mentioned patent uses still
It is so the heater-type gas sensor based on traditional ceramic tube, can there is that volume is larger, the larger problem of power consumption.
With the fast development of microelectromechanical systems (MEMS) technology, make small in size, low-power consumption, it is easy of integration,
The MEMS micro-hotplate gas sensor of mass becomes numerous researcher's focus of attention.There is researcher to pass through silicon single-sided process work
Skill carries out corrosion from (100) silicon wafer is just faced to obtain hanging micro- heating board structure.But due to the spy of (100) crystal face
Point, needing to corrode deeper depth to silicon can discharge completely the silicon below micro-hotplate.Such as: Publication No.
CN105928567B, the China of entitled " a kind of the silicon substrate gas sensitization chip of integrated Temperature Humidity Sensor and preparation method thereof "
Patent of invention discloses and multiple gas sensor units, temperature sensitive unit and wet sensitive unit is integrated in (100) by the two-sided processing technology of silicon
On monocrystalline silicon piece, and the heat-insulated through-hole of two-stage is used, has many advantages, such as that multifunctional measuring, selectivity are good, low in energy consumption.But it relates to
And the two-sided processing technology of silicon, manufacture craft are complex.
In addition, there are also some domestic and foreign scholars to use surface micromachined technique, by making sacrificial layer, gas is passed
The problem of micro- heating plate of sensor is discharged, this kind of method equally exists complex manufacturing technology, and need special equipment (such as
CO 2 supercritical drying instrument) guarantee the reliability of technique.
In conclusion in the research of conductor oxidate gas sensor, when being processed to the micro- heating plate of gas sensor,
Technique is complex.
Summary of the invention
The present invention is now to provide one to solve the problems, such as that the processing technology of the micro- heating plate of existing gas sensor is complicated
Kind is based on the gas sensitization chip array and preparation method thereof of [111] monocrystalline silicon.
One kind being based on the gas sensitization chip array of [111] monocrystalline silicon, comprising: multiple gas sensitization chips, [111] monocrystalline
Silicon base 1 and supporting layer 2, the gas sensitization chip include: heating electrode 3, a pair of of Sensitive membrane electrode 4 and gas sensitive membrane 7；
Heating electrode 3 is square wave-shaped configuration, and Sensitive membrane electrode 4 is pectinate texture, and a pair of of Sensitive membrane electrode 4, which is located at, to be added
The two sides of thermode 3 and the tooth for having a Sensitive membrane electrode 4 between two adjacent square waves of electrode 3 is heated, heats electrode 3
It is covered with gas sensitization film 7 with the upper surface of a pair of of Sensitive membrane electrode 4, the both ends of each heating electrode 3 are respectively connected with extraction electricity
The first and last end of pole 5, a pair of of Sensitive membrane electrode 4 is oppositely arranged, and the end of a pair of of Sensitive membrane electrode 4 is respectively connected with extraction electrode 5, often
The end of a extraction electrode 5 is respectively connected with an electrode pad 6,
[111] 1 upper surface of monocrystal silicon substrate is provided with heat-insulation chamber 9, and supporting layer 2 is covered on table in [111] monocrystal silicon substrate 1
Face is provided with the etch pit 8 of multiple rectangular arrays arrangements on supporting layer 2, and each etch pit 8 is connected to heat-insulation chamber 9, the square
The row of shape array is set along [110] the crystal orientation setting of [111] monocrystal silicon substrate 1, [211] crystal orientation of column edge [111] monocrystal silicon substrate 1
It sets, is respectively and fixedly provided with a gas sensitization chip, the extraction electrode 5 of gas sensitization chip between two adjacent etch pits of every a line
Length direction it is in the same direction with [211] crystal orientation of [111] monocrystal silicon substrate 1.
Above-mentioned rectangular array is the rectangular array of M × N, and wherein the value range of M and N is 1~20.
Specifically, the material of supporting layer 2 be silicon nitride, supporting layer 2 with a thickness of 1 μm~10 μm.
Specifically, the material of heating electrode 3 and a pair of of Sensitive membrane electrode 4 is Pt, Au, W or Ag.
Specifically, the material of gas sensitization film 7 includes at least SnO2、WO3、In2O3Or one of ZnO.
Specifically, the depth of heat-insulation chamber 9 is 10 μm~300 μm.
The production method of above-mentioned gas sensitive chip array, comprising the following steps:
Step 1: using PECVD in 1 upper surface depositing support layer 2 of [111] monocrystal silicon substrate,
Step 2: 400 angstroms of Cr and 4000 angstrom of Pt laminated film is made in 2 upper surface of supporting layer, utilizes dry etching
It carves and removes extra metal, retain and obtain heating electrode 3, a pair of of Sensitive membrane electrode 4, extraction electrode 5 and electrode pad 6,
Step 3: firstly, etching the profile of etch pit 8 on supporting layer 2 using photoetching, then, dry etching is utilized
It carves except silicon nitride extra in profile, finally, being carved in [111] monocrystal silicon substrate 1 using inductively coupled plasma etching method
Area of insulation out is lost, which is overlapped with etch pit 8,
Step 4: using concentration be 15% tetramethyl ammonium hydroxide solution, under 85 DEG C of environmental condition, to [111]
The adjacent area of insulation part of monocrystal silicon substrate 1 is corroded, so that all area of insulation are connected to form heat-insulation chamber 9,
Step 5: it in heating electrode 3 and 4 surface coating gas sensitive membrane 7 of Sensitive membrane electrode, and is heated in Muffle furnace
Temperature fall after 400 DEG C and heat preservation 2 hours, obtains gas sensitization chip array.
The invention proposes a kind of gas sensitization chip arrays and preparation method thereof for being based on [111] monocrystalline silicon, with tradition
Array and production method, which are compared, to be had the advantages that
1, gas sensor array is made using silicon single-sided process, manufacture craft is simple；
2, corrosion is carried out to [111] monocrystalline silicon surface and makes micro- heating plate, the depth of heat-insulation chamber can be by etch pit
Etching depth flexibly controlled；
3, the gas sensitization chip array of hanging bridge structure can be effectively reduced biosensor power consumption, and power consumption is traditional heater-type knot
10% or less structure.
Detailed description of the invention
Fig. 1 is the array schematic diagram containing 3 gas sensitization chips；
Fig. 2 is the sectional view along A-A of Fig. 1；
The structural schematic diagram of micro-hotplate when Fig. 3 is non-blanketing gas sensitive membrane；
The structural schematic diagram of gas sensitization chip when Fig. 4 is non-blanketing gas sensitive membrane；
Fig. 5 is structural schematic diagram of multiple gas sensitization chip arrays in [111] monocrystal silicon substrate, lateral arrows in figure
It indicates
[110] crystal orientation, longitudinal arrow indicate [211] crystal orientation.
Specific embodiment
Specific embodiment 1: one kind described in present embodiment is based on the gas sensitization chip array of [111] monocrystalline silicon,
It include: 3 gas sensitization chips, [111] monocrystal silicon substrate 1 and supporting layer 2,
Each gas sensitization chip includes: heating electrode 3, a pair of of Sensitive membrane electrode 4 and gas sensitive membrane 7；
Referring to shown in Fig. 3, heating electrode 3 is square wave-shaped configuration, and Sensitive membrane electrode 4 is pectinate texture, a pair of of sensitive membrane electricity
Pole 4 is located at the two sides of heating electrode 3 and each tooth of Sensitive membrane electrode 4 is respectively positioned on two adjacent square waves of heating electrode 3
Between, heating electrode 3 and a pair of of Sensitive membrane electrode 4 collectively form micro-hotplate.The upper surface of micro-hotplate is covered with gas sensitization film
7。
As shown in figure 4, the both ends of heating electrode 3 are respectively connected with extraction electrode 5, the first and last end of a pair of of Sensitive membrane electrode 4 is anti-
To setting, the end of a pair of of Sensitive membrane electrode 4 is also respectively connected with extraction electrode 5, it may be assumed that there are four extraction electrode 5, each extractions altogether
The end of electrode 5 is respectively connected with an electrode pad 6.
[111] 1 upper surface of monocrystal silicon substrate is provided with heat-insulation chamber 9, and supporting layer 2 is covered on table in [111] monocrystal silicon substrate 1
Face is provided with multiple etch pits 8 on supporting layer 2, and each etch pit 8 is connected to heat-insulation chamber 9, and multiple etch pits 8 are in the square of M × N
The arrangement of shape array format, wherein the value range of M and N is 1~20 (as shown in Figure 5), and the row of the rectangular array is along [111]
[110] the crystal orientation setting of monocrystal silicon substrate 1, column are arranged along [211] crystal orientation of [111] monocrystal silicon substrate 1.
Specifically, as depicted in figs. 1 and 2, the number of etch pit is 4, in the form of a line eight arranges in present embodiment
Arrangement.A gas sensitization chip, the extraction electricity of gas sensitization chip are respectively and fixedly provided between two adjacent etch pits of every a line
The length direction of pole 5 is in the same direction with [211] crystal orientation of [111] monocrystal silicon substrate 1.
Specifically, the material of above-mentioned supporting layer 2 be silicon nitride, supporting layer 2 with a thickness of 1 μm~10 μm.
Specifically, the material of above-mentioned heating electrode 3 and a pair of of Sensitive membrane electrode 4 is Pt, Au, W or Ag.
Specifically, the material of above-mentioned gas sensitive membrane 7 includes at least SnO2、WO3、In2O3Or one of ZnO.
Specifically, the depth of above-mentioned heat-insulation chamber 9 is 10 μm~300 μm.
Specific embodiment 2: the production method of gas sensitization chip array described in specific embodiment one, is adopted first
[111] monocrystal silicon substrate 1 is cleaned with standard cleaning liquid, then starts following making step:
Step 1: using PECVD, (Plasma Enhanced Chemical Vapor Deposition, plasma increase
The vapour deposition process of extensive chemical) silicon nitride medium layer of the method in 1 upper surface of [111] monocrystal silicon substrate, 2 μ m-thicks of deposition, the dielectric layer
As supporting layer 2；
Step 2: 400 angstroms of Cr and 4000 angstrom of Pt laminated film is made in 2 upper surface of supporting layer, utilizes dry etching
It carves and removes extra metal, retain and obtain heating electrode 3, a pair of of Sensitive membrane electrode 4, extraction electrode 5 and electrode pad 6,
Step 3: firstly, etching the profile of etch pit 8 on supporting layer 2 using photoetching, then, dry etching is utilized
It carves except silicon nitride extra in profile, finally, using ICP method (inductively coupled plasma etching method) in [111] monocrystalline silicon substrate
Area of insulation is etched on bottom 1, which is overlapped with etch pit 8,
Step 4: using concentration be 15% tetramethyl ammonium hydroxide solution, under 85 DEG C of environmental condition, to [111]
The adjacent area of insulation part of monocrystal silicon substrate 1 is corroded, so that all area of insulation are connected to form heat-insulation chamber 9,
Step 5: it in heating electrode 3 and 4 surface coating gas sensitive membrane 7 of Sensitive membrane electrode, and is heated in Muffle furnace
Temperature fall after 400 DEG C and heat preservation 2 hours, obtains gas sensitization chip array.
Claims (9)
1. the gas sensitization chip array that one kind is based on [111] monocrystalline silicon characterized by comprising multiple gas sensitization chips,
[111] monocrystal silicon substrate (1) and supporting layer (2), the gas sensitization chip include: heating electrode (3), a pair of of Sensitive membrane electrode
(4) and gas sensitive membrane (7)；
Heating electrode (3) is square wave-shaped configuration, and Sensitive membrane electrode (4) is pectinate texture, and a pair of of Sensitive membrane electrode (4) is located at
It heats the two sides of electrode (3) and heats the tooth for having a Sensitive membrane electrode (4) between two adjacent square waves of electrode (3), add
The upper surface of thermode (3) and a pair of of Sensitive membrane electrode (4) is covered with gas sensitization film (7), the both ends of each heating electrode (3)
It is respectively connected with extraction electrode (5), the first and last end of a pair of of Sensitive membrane electrode (4) is oppositely arranged, the end of a pair of of Sensitive membrane electrode (4)
It being respectively connected with extraction electrode (5), the end of each extraction electrode (5) is respectively connected with an electrode pad (6),
[111] monocrystal silicon substrate (1) upper surface is provided with heat-insulation chamber (9), and supporting layer (2) is covered in [111] monocrystal silicon substrate (1)
Surface, is provided with the etch pit (8) of multiple rectangular arrays arrangements on supporting layer (2), each etch pit (8) with heat-insulation chamber (9)
Connection, [110] crystal orientation of the row of the rectangular array along [111] monocrystal silicon substrate (1) is arranged, column are along [111] monocrystal silicon substrate
(1) [211] crystal orientation is arranged, and is respectively and fixedly provided with a gas sensitization chip between two adjacent etch pits of every a line, gas is quick
The length direction of the extraction electrode (5) of sense chip is in the same direction with [211] crystal orientation of [111] monocrystal silicon substrate (1).
2. a kind of gas sensitization chip array for being based on [111] monocrystalline silicon according to claim 1, which is characterized in that square
Shape array is the rectangular array of M × N, and wherein the value range of M and N is 1~20.
3. a kind of gas sensitization chip array for being based on [111] monocrystalline silicon according to claim 1 or 2, which is characterized in that
The material of supporting layer (2) be silicon nitride, supporting layer (2) with a thickness of 1 μm~10 μm.
4. a kind of gas sensitization chip array for being based on [111] monocrystalline silicon according to claim 1 or 2, which is characterized in that
The material for heating electrode (3) and a pair of of Sensitive membrane electrode (4) is Pt, Au, W or Ag.
5. a kind of gas sensitization chip array for being based on [111] monocrystalline silicon according to claim 1 or 2, which is characterized in that
The material of gas sensitization film (7) includes at least SnO2、WO3、In2O3Or one of ZnO.
6. a kind of gas sensitization chip array for being based on [111] monocrystalline silicon according to claim 1 or 2, which is characterized in that
The depth of heat-insulation chamber (9) is 10 μm~300 μm.
7. the production method of gas sensitization chip array of any of claims 1 or 2, which comprises the following steps:
Step 1: using PECVD in [111] monocrystal silicon substrate (1) upper surface depositing support layer (2),
Step 2: 400 angstroms of Cr and 4000 angstrom of Pt laminated film is made in supporting layer (2) upper surface, is carved using dry etching
Except extra metal, retains and obtains heating electrode (3), a pair of of Sensitive membrane electrode (4), extraction electrode (5) and electrode pad (6),
Step 3: firstly, the profile of etch pit (8) is etched on supporting layer (2) using photoetching,
Then, it is carved using dry etching except silicon nitride extra in profile,
It, should be every finally, etch area of insulation in [111] monocrystal silicon substrate (1) using inductively coupled plasma etching method
Thermal region is overlapped with etch pit (8),
Step 4: using concentration be 15% tetramethyl ammonium hydroxide solution, under 85 DEG C of environmental condition, to [111] monocrystalline
The adjacent area of insulation part of silicon base (1) is corroded, so that all area of insulation are connected to form heat-insulation chamber (9),
Step 5: it in heating electrode (3) and Sensitive membrane electrode (4) surface coating gas sensitive membrane (7), and is heated in Muffle furnace
To 400 DEG C and keep the temperature 2 hours after Temperature fall, obtain gas sensitization chip array.
8. production method according to claim 7, which is characterized in that in step 1, supporting layer (2) is the nitridation of 2 μ m-thicks
Silicon dielectric layer.
9. production method according to claim 7 or 8, which is characterized in that before step 1, use standard cleaning first
Liquid cleans [111] monocrystal silicon substrate (1).
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113514498A (en) * | 2020-04-10 | 2021-10-19 | 中国石油化工股份有限公司 | Common-chip heating array type gas detection microchip and preparation method thereof |
| CN114965625A (en) * | 2022-05-24 | 2022-08-30 | 广东芯阅科技有限公司 | Electrochemical sensitive chip based on suspension working electrode and processing method |
| CN115535959A (en) * | 2022-11-23 | 2022-12-30 | 山东大学 | Wet etching auxiliary femtosecond laser processing method for monocrystalline silicon microstructure array |
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