CN105987935B - MEMS gas sensor and preparation method thereof - Google Patents
MEMS gas sensor and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to gas detection technology fields, provide MEMS gas sensor and preparation method thereof, and MEMS gas sensor includes monocrystalline substrate；Upper silicon nitride layer and upper silicon oxide layer, are stacked and placed on the monocrystalline substrate upper surface from the bottom to top；Lower silicon nitride layer is placed in the monocrystalline substrate lower surface；Electrode is heated, is placed on the upper silicon oxide layer；Insulating layer is placed on the heating electrode；Measuring electrode is placed on the insulating layer；Gas sensitization layer is placed in the measuring electrode, and is electrically connected with the measuring electrode；Heat-insulation chamber is located at below the upper silicon nitride layer, the lower silicon nitride layer and the monocrystalline substrate corruption is carved and formed.In the present invention, gas sensor precision itself is high, light-weight, size is small, it is low in energy consumption, efficiency is high, it is at low cost, can produce in enormous quantities.
Description
Technical field
The present invention relates to gas detection technology fields, are to be related to a kind of MEMS gas sensor and its system more specifically
Make method.
Background technique
MEMS (Micro-Electro-Mechanical System, MEMS) gas sensor is based on micro- electricity
Sub- technology and the gas sensor of micro-processing technology manufacture.The principle of gas sensor is using made of metal-oxide film
Impedance device, at a certain temperature, gas molecule cause the variation of resistivity in surface and reactive metal oxide, thus real
Now to the detection of gas.
Although with the development of MEMS technology, the production technology successive optimization of gas sensor, current gas sensing
Device mass production, high-precision, it is integrated and in terms of there are still improved spaces.
Summary of the invention
The purpose of the present invention is to provide a kind of MEMS gas sensors and preparation method thereof, it is intended to solve in the prior art
The gas sensor problem unexcellent in mass production, high-precision, integrated and low-power consumption.
In order to solve the above technical problems, the technical scheme is that provide a kind of MEMS gas sensor, including,
Monocrystalline substrate；
Upper silicon nitride layer and upper silicon oxide layer, are stacked and placed on the monocrystalline substrate upper surface from the bottom to top；
Lower silicon nitride layer is placed in the monocrystalline substrate lower surface；
Electrode is heated, is placed on the upper silicon oxide layer；
Insulating layer is placed on the heating electrode, and insulating layer is equipped with connecting hole；
Measuring electrode is placed on the insulating layer, and is connected to by the connecting hole with the heating electrode；
Gas sensitization layer is placed in the measuring electrode, and is electrically connected with the measuring electrode；
Heat-insulation chamber, is located at below the upper silicon nitride layer, and the lower silicon nitride layer and the monocrystalline substrate corruption are carved shape
At.
Specifically, the heating electrode is formed for polysilicon ion, and doped with phosphorus, and concentration ratio shared by phosphorus is 1%
~3%.
Specifically, the gas sensitization layer material is stannic oxide or tungstic acid.
The present invention also provides a kind of production methods of MEMS gas sensor, comprise the following steps that:
S1: preparation monocrystalline substrate, and silicon nitride is deposited respectively in the upper surface of the monocrystalline substrate and lower surface
Layer and lower silicon nitride layer；
S2: upper silicon oxide layer is deposited in the upper silicon nitride layer；
S3: in preparation heating electrode on the upper silicon oxide layer；
S4: in preparing insulating layer on the heating electrode, and in connecting hole is arranged on the insulating layer；
Measuring electrode is prepared on S5: Yu Suoshu insulating layer, the measuring electrode is in the connection hole and heating electricity
Pole conducting；
Gas sensitization layer is prepared in S6: Yu Suoshu measuring electrode；
S7: product bottom in S6 step is corroded, and forms the heat-insulation chamber being located at below the upper silicon nitride layer；
S8: the product after etching in S7 step is made annealing treatment, and is cooled into the MEMS gas sensor.
Specifically, the heating electrode in the S3 step is formed for polysilicon ion, and doped with phosphorus, and concentration shared by phosphorus
Ratio is 1%~3%.
Specifically, in the S5 step, measuring electrode using evaporation or sputtered film depositing system deposition 100nm~
The gold or platinum of 1000nm and formed.
Specifically, in the S6 step, the gas sensitization layer material is tungstic acid or stannic oxide.
Specifically, it in the S7 step, is performed etching using potassium hydroxide or tetramethyl ammonium hydroxide solution.
Specifically, in the S8 step, annealing temperature rises to 600 DEG C~800 by 100 DEG C~150 DEG C in annealing
DEG C when keep two hours, and in air keep 600 DEG C~800 DEG C two hours.
In the present invention, gas sensor made by the above method is had the advantages that
One, it can in high volume manufacture parallel, can reach system-level integrated, encapsulation integrated level height, it can be compatible with chip technology；
Two, gas sensor precision itself is high, light-weight, size is small, low in energy consumption, efficiency is high, at low cost, being capable of high-volume
Production.
Three, it is able to achieve to CO, NO2, the detection of the multiple gases such as CH4.
Detailed description of the invention
Fig. 1 is the schematic diagram of manufacturing method of MEMS gas sensor provided in an embodiment of the present invention；
10- monocrystalline substrate；The upper silicon nitride layer of 11a-；Silicon nitride layer under 11b-；
The upper silicon oxide layer of 12a-；13- heats electrode；14- insulating layer；
15- measuring electrode；16- gas sensitization layer；17- heat-insulation chamber.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.
It should be noted that it can be directly another when element is referred to as " being fixed on " or " being set to " another element
On one element or it may be simultaneously present centering elements.When an element referred to as " is connected to " another element, it can be with
It is directly to another element or may be simultaneously present centering elements.
It should also be noted that, the positional terms such as left and right, upper and lower in the present embodiment, be only each other relative concept or
It is reference with the normal operating condition of product, and should not be regarded as restrictive.
Fig. 1 G is the longitudinal sectional view of MEMS gas sensor provided by the invention.It includes monocrystalline substrate 10, under
The supreme upper silicon nitride layer 11a for being deposited on 10 upper surface of monocrystalline substrate and upper silicon oxide layer 12a；It is deposited on monocrystalline substrate 10
The lower silicon nitride layer 11b of lower surface；It is placed in the heating electrode 13 of silicon oxide layer 12a；The insulating layer being placed on heating electrode 13
14；The measuring electrode 15 being placed on insulating layer 14, measuring electrode 15 and heating electrode 13 are in conducting shape；It is placed in measuring electrode 15
Gas sensitization layer 16, gas sensitization layer 16 and be electrically connected with measuring electrode 15；Heat-insulation chamber below upper silicon nitride layer 11a
17, heat-insulation chamber 17 penetrates monocrystalline substrate 10, lower silicon nitride layer 11b.
Wherein, heating electrode 13 is formed for polysilicon ion, and doped with phosphorus, and concentration ratio shared by phosphorus be 1% to
3%.It should be noted that the heating electrode 13 is to generate joule's heat energy by Injection Current.
Wherein, gas sensitization layer 16 includes stannic oxide, tungstic acid.
Referring to Fig.1, the present invention also provides the production methods of above-mentioned MEMS gas sensor comprising following technique step
It is rapid:
Such as Figure 1A, S1: preparation monocrystalline substrate 10, and deposited respectively in the upper surface of monocrystalline substrate 10 and lower surface
Silicon nitride layer 11a and lower silicon nitride layer 11b；
In the implementation case: monocrystalline substrate 10 chooses 6 inches of n-type silicon chips of twin polishing, and material parameter is that<100>are brilliant
To 0.05 μm of finish <, flatness≤± 2 μm are not damaged, and with a thickness of 500 ± 10 μm, resistivity is 1~5 Ω cm.Silicon wafer
After cleaning up, using LPCVD (Low Pressure Chemical Vapor Deposition, low-pressure chemical vapor deposition
Area method) in silicon wafer upper surface and lower surface the low stress nitride silicon layer of 100nm-600nm is deposited respectively.Meanwhile upper silicon nitride layer
11a and lower silicon nitride layer 11b play a protective role to monocrystalline substrate 10 in postorder wet-etching technology as barrier layer.
Such as Figure 1B, S2: in the upper silicon oxide layer 12a of deposition on upper silicon nitride layer 11a；
In this step, using LPCVD method in upper silicon nitride layer 11a deposition silicon oxide layer 12a.Since the present invention is implemented
In example, the entire device of gas sensor needs to carry out wet etching, uses again after depositing low stress SiNx in S1 step
LPCVD deposits low stress silica, in this way, entire device membrane stress is lower than 200Mpa, structural stability is more preferable.Meanwhile oxygen
SiClx and the thermal conductivity of silicon nitride can not show a candle to silicon therefore can play the role of preventing heat loss again.
Such as Fig. 1 C, S3: in preparation heating electrode 13 on upper silicon oxide layer 12a；
In this step, equally using LPCVD method in the polysilicon ion for depositing 8k on upper silicon oxide layer 12a, meanwhile, from
The phosphorus that sub- implantation concentration ratio is 1% to 3% enhances electric conductivity.This is because polycrystalline silicon is different from metal, it is removed
It is conductive by also to come by hole outside free electron, when polysilicon contains the impurity of denier, so that it may make its conductance
Rate varies widely, and can effectively reduce resistivity, therefore adulterates phosphorus, and conductivity can be improved.And when phosphorus concentration be 1% to
When 3%, resistivity≤800 Ω cm, conductive effect is best.Then pass through positive photoresist whirl coating, after front baking photoetching development, dry technique afterwards
After carry out reactive ion etching, remove heating electrode 13 described in gum forming after etching figure polysilicon ion layer.Gas passes
When sense device working, polysilicon heating electrode 13 can not only provide optimal operating temperature to gas sensor and reach best work
Make state, and the gas molecule being adsorbed in sensitive membrane can be made to obtain enough energy desorptions.
Such as Fig. 1 D, insulating layer 14 is prepared on S4: Yu Jiare electrode 13；
In this step, using PECVD (Plasma Enhanced Chemical Vapor Deposition, plasma
Body enhances chemical vapour deposition technique) silica of one layer 1.5 μm of deposition on Yu Jiare electrode 13, silica has preferable
Insulation performance is placed on heating electrode 13 as insulating layer 14.Sharp whirl coating after deposit simultaneously, develops after front baking photoetching, RIE etc.
Ion etching silicon dioxide layer, and in forming connecting hole 141 in silicon dioxide layer, heating electrode 13 is deposited at connecting hole 141,
Purpose provides electric current heating to heating electrode 13 by connecting hole 141 convenient for measuring electrode 15.
Such as Fig. 1 E, S5: in the measuring electrode 15 for being prepared on insulating layer 14 with heating the insulation of electrode 13；
In this step, in the manner of sputtering or the mode of thermal evaporation on insulating layer 14 deposit 100nm~
The gold or platinum of 1000nm.Measuring electrode is the flexibility because the density of gold or platinum is relatively high using gold or platinum
Very well, it will not be cut through when making punching lead and influence other film layers.Specifically, it prior to positive glue on insulating layer 14, uses
Negative version photomask carries out stripping technology, first whirl coating, dries after carrying out after lithographic after front baking, front gluing protects gold electrode, applies
It should be avoided during glue and aeration protecting effect occur, and dried under 80 DEG C~100 DEG C high temperature, when shortening solidification
Between.Herein, it selects metallic gold to do measuring electrode 15, is that can accurately measure gas sensitization layer 16 because golden antioxygenic property is preferable
Resistance change rate.
Such as Fig. 1 F, S6: in preparing gas sensitization layer 16 in measuring electrode 15；
In this step, gas sensitization layer material is the metal oxides such as stannic oxide or tungstic acid, and is added simultaneously
There is noble metal, noble metal can be Pt, Pd etc. with catalytic action, and the effect that noble metal is added is to reduce stannic oxide or three
The barrier potential of a semiconductor of tungsten oxide promotes the selectivity of gas sensor.When specific operation, by stannic oxide, tungstic acid and expensive
Intermetallic composite coating is taken shape in measuring electrode 15 at target by way of vapor deposition.The admixture mass ratio of noble metal is 1%-5%,
Improve air-sensitive sensibility.When gas sensitization layer is with a thickness of 5um-8um, susceptibility highest.
It should be noted that Pt, Pd are good oxidation catalysts, if the amount of addition is excessive, can make tested flammable
Significant combustion reaction occurs on it for gas, and gas sensing layer temperature is sharply increased, performance is caused to deteriorate, therefore under normal conditions
The doping of the noble metals such as Pt, Pd is preferred with being no more than 5%.
Such as Fig. 1 G, S7: product bottom in S6 step being corroded, is formed heat-insulated below upper silicon nitride layer 11a
Chamber 17；
In this step, one layer of protective glue of product upper surface spin coating in S6 step, not for protective gas sensitive layer 16
By alkali corrosion.The positive photoresist on the back side of product in S6 step, after front baking makes the window development of silica wet etching by lithography
It is 20% with concentration after baking, the KOH solution that 80 degrees Celsius of temperature carries out silicon etching, the nitrogen until etching into upper layer LPCVD deposition
Until this layer of SiClx.Barrier layer is discharged with oxonium ion after wet process body silicon etching.It should be noted that above-mentioned KOH solution can also be with
It is substituted using tetramethyl ammonium hydroxide solution.Both solution can etch the structure of inclined ladder shape, and technique low cost, be suitble to
It in concentration is 20%~30% in KOH or tetramethyl ammonium hydroxide solution in mass production, silicon wafer when 80 DEG C of temperature
When etch rate is about 1 μm/min, etching effect is best.
S8: the product after etching in S7 step is made annealing treatment, and is cooled into the MEMS gas sensor.
It should be noted that further including being cut to product in above-mentioned S7, being cut into multiple before being made annealing treatment
The step of gas sensor semi-finished product.Herein, preferential using laser cutting, will not polluted gas sensitive layer 16, and cut place is flat
It is whole, it is high-efficient.
In S8 step, each gas sensor semi-finished product of well cutting are subjected to annealing process, annealing is by 100 DEG C
~150 DEG C are kept for two hours when rising to 600 DEG C~800 DEG C, and keep 600 DEG C~800 DEG C in air two hours, finally
Natural cooling obtains poroid sensitive thin film on gas sensitization layer 16.
The corresponding table of the bulk resistor Standard resistance range of 1 tin dioxide thin film of table or WO 3 film and annealing
Without annealing process in current production technology, by can be clearly seen that in table 1, when without annealing process
When, the bulk resistor Standard resistance range of tin dioxide thin film or WO 3 film is smaller, and in fixed range 3k Ω~
7kΩ；And when being made annealing treatment, with the raising of annealing temperature, the bulk resistor resistance value model of tin dioxide thin film or tungstic acid
It encloses and is gradually increased, when reaching 700 DEG C, the bulk resistor Standard resistance range of tin dioxide thin film or tungstic acid is 5k Ω~20k Ω.And
And when annealing temperature is 400 DEG C, 500 DEG C, 600 DEG C, 700 DEG C, the respective linearity of gas sensor is relatively good, with moving back
The raising of fiery temperature, tin dioxide thin film or WO 3 film for the fuel gas such as hydrogen, methane sensitivity significantly
It improves.
To sum up, above-mentioned gas sensor made by the above method, has the advantages that
One, it can in high volume manufacture parallel, can reach system-level integrated, encapsulation integrated level height, it can be compatible with chip technology；
Two, gas sensor precision itself is high, light-weight, size is small, low in energy consumption, efficiency is high, at low cost.
Three, it is able to achieve to CO, NO2, the detection of the multiple gases such as CH4.
The above is merely preferred embodiments of the present invention, be not intended to limit the invention, it is all in spirit of the invention and
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within principle.
Claims (8)
1. a kind of MEMS gas sensor, which is characterized in that including,
Monocrystalline substrate；
Upper silicon nitride layer and upper silicon oxide layer, are stacked and placed on the monocrystalline substrate upper surface from the bottom to top；
Lower silicon nitride layer is placed in the monocrystalline substrate lower surface；
Electrode is heated, is placed on the upper silicon oxide layer；
Insulating layer is placed on the heating electrode, and insulating layer is equipped with connecting hole；
Measuring electrode is placed on the insulating layer, and is connected to by the connecting hole with the heating electrode；
Gas sensitization layer is placed in the measuring electrode, and is electrically connected with the measuring electrode；
Heat-insulation chamber is located at below the upper silicon nitride layer, the lower silicon nitride layer and the monocrystalline substrate corruption is carved and formed；
There are two the heating electrode, each heating electrode extends to the monocrystalline silicon from right above the heat-insulation chamber
The surface of substrate, two heating electrodes are put using the center of the heat-insulation chamber as symmetrical centre and being spaced apart from each other；
The insulating layer extends to oxide layer right above the heat-insulation chamber across in two heating electrode surfaces
Surface；
The gas sensitization layer is across right above two heating electrodes；
Wherein, adding in the gas sensitization layer has noble metal, and the admixture mass ratio of the noble metal is 1 ~ 5%；
The heating electrode is formed for polysilicon ion, and doped with phosphorus, and concentration ratio shared by phosphorus is 1% to 3%.
2. MEMS gas sensor as described in claim 1, which is characterized in that the gas sensitization layer material is stannic oxide
Or tungstic acid.
3. the production method of MEMS gas sensor as described in claim 1, which is characterized in that comprise the following steps that:
S1: preparation monocrystalline substrate, and in the upper surface of the monocrystalline substrate and lower surface deposit respectively silicon nitride layer and
Lower silicon nitride layer；
S2: upper silicon oxide layer is deposited in the upper silicon nitride layer；
S3: in preparation heating electrode on the upper silicon oxide layer；
S4: in preparing insulating layer on the heating electrode, and in connecting hole is arranged on the insulating layer；
Measuring electrode is prepared on S5: Yu Suoshu insulating layer, the measuring electrode is led in the connection hole and the heating electrode
It is logical；
Gas sensitization layer is prepared in S6: Yu Suoshu measuring electrode；
S7: product bottom in S6 step is corroded, and forms the heat-insulation chamber being located at below the upper silicon nitride layer；
S8: the product after etching in S7 step is made annealing treatment, and is cooled into the MEMS gas sensor.
4. the production method of MEMS gas sensor as claimed in claim 3, which is characterized in that the heating in the S3 step
Electrode is formed for polysilicon ion, and doped with phosphorus, and concentration ratio shared by phosphorus is 1% ~ 3%.
5. the production method of MEMS gas sensor as claimed in claim 3, which is characterized in that in the S5 step, measurement
Electrode is formed using the gold or platinum of evaporation or sputtered film depositing system deposition 100nm ~ 1000nm.
6. the production method of MEMS gas sensor as claimed in claim 3, which is characterized in that described in the S6 step
Gas sensitization layer material is tungstic acid or stannic oxide.
7. the production method of MEMS gas sensor as claimed in claim 3, which is characterized in that in the S7 step, use
Potassium hydroxide or tetramethyl ammonium hydroxide solution perform etching.
8. the production method of MEMS gas sensor as claimed in claim 3, which is characterized in that in the S8 step, annealing
It is kept for two hours when annealing temperature rises to 600 DEG C ~ 800 DEG C by 100 DEG C ~ 150 DEG C in processing, and keeps 600 in air
DEG C ~ 800 DEG C two hours.
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| EP3542152B1 (en) * | 2016-11-21 | 2020-04-29 | Unilever N.V. | A gas sensor for detecting a gas component |
| CN106770499B (en) * | 2017-01-13 | 2021-05-18 | 京东方科技集团股份有限公司 | Carbon monoxide sensor, manufacturing method and control method thereof and smart television |
| DE102017210585B3 (en) * | 2017-06-23 | 2018-09-27 | Robert Bosch Gmbh | Bondpad layer system, gas sensor and method for producing a gas sensor |
| CN108275649B (en) * | 2018-03-16 | 2023-06-23 | 苏州芯镁信电子科技有限公司 | MEMS combustible gas sensor and processing method thereof |
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| CN110577187B (en) * | 2018-06-07 | 2023-01-24 | 上海新微技术研发中心有限公司 | Electric heating thin film layer structure and preparation method |
| CN109613085A (en) * | 2018-12-12 | 2019-04-12 | 中国电子科技集团公司第四十九研究所 | One kind being based on the gas sensitization chip array and preparation method thereof of [111] monocrystalline silicon |
| CN110031512B (en) * | 2019-04-28 | 2021-09-07 | 湖州师范学院 | Single particle sensitive gas sensor and preparation method and application thereof |
| 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 |
| CN111610233A (en) * | 2020-06-16 | 2020-09-01 | 黑龙江省网络空间研究中心 | Preparation method of MEMS catalytic combustion type gas sensor |
| CN113049645A (en) * | 2021-03-15 | 2021-06-29 | 吉林大学 | Based on two-dimentional stratiform SnS2NO of nanoflower semiconductor material2Gas sensor and preparation method thereof |
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