CN105987935A - Mems gas sensor and manufacturing method thereof - Google Patents
Mems gas sensor and manufacturing method thereof Download PDFInfo
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Abstract
The invention relates to the technical field of gas detection, and provides an MEMS gas sensor and a manufacturing method thereof. The MEMS gas sensor comprises: a monocrystalline silicon substrate; an upper silicon nitride layer and an upper silicon oxide layer which are superposed on the upper surface of the monocrystalline silicon substrate from bottom to top; a lower silicon nitride layer placed on the lower surface of the monocrystalline silicon substrate; a heating electrode placed on the silicon oxide layer; an insulating layer placed on the heating electrode; a measurement electrode placed on the insulating layer; a gas-sensitive layer placed on the measurement electrode and electrically connected with the measurement electrode; and a heat insulation chamber positioned under the upper silicon nitride layer and formed by etching the lower silicon nitride layer and the monocrystalline silicon substrate. The gas sensor has the advantages of high precision, light weight, small dimension, low power dissipation, high usefulness, low cost, and realization of large-batch production.
Description
Technical field
The present invention relates to gas detection technology field, more specifically, relate to a kind of MEMS gas sensor and preparation method thereof.
Background technology
MEMS (Micro-Electro-Mechanical System, MEMS) gas sensor is the gas sensor manufactured based on microelectric technique and micro-processing technology.The principle of gas sensor is the impedance device utilizing metal-oxide film to make, and at a certain temperature, gas molecule causes the change of resistivity at surface and reactive metal oxide, thus realizes the detection to gas.
Although along with the development of MEMS technology, the production technology successive optimization of gas sensor, but at present gas sensor mass production, in high precision, the aspect such as integrated and low-power consumption still suffer from the space improved.
Summary of the invention
It is an object of the invention to provide a kind of MEMS gas sensor and preparation method thereof, it is intended to solve gas sensor in prior art mass production, in high precision, the problem that integrated and low-power consumption is the most excellent.
For solving above-mentioned technical problem, the technical scheme is that a kind of MEMS gas sensor of offer, including,
Monocrystalline substrate；
Upper silicon nitride layer and upper silicon oxide layer, be stacked and placed on described monocrystalline substrate upper surface from the bottom to top；
Lower silicon nitride layer, is placed in described monocrystalline substrate lower surface；
Add thermode, be placed on described upper silicon oxide layer；
Insulating barrier, be placed in described in add on thermode, insulating barrier is provided with connecting hole；
Measure electrode, be placed on described insulating barrier, and connected with the described thermode that adds by described connecting hole；
Gas sensitization layer, is placed on described measurement electrode, and electrically connects with described measurement electrode；
Heat-insulation chamber, is positioned at below described upper silicon nitride layer, described lower silicon nitride layer and described monocrystalline substrate corruption is carved and is formed.
Specifically, described in add thermode be that polysilicon ion is formed, and doped with phosphorus, and concentration ratio shared by phosphorus is 1%～3%.
Specifically, described gas sensitization layer material is tin ash or Tungstic anhydride..
Present invention also offers the manufacture method of a kind of MEMS gas sensor, comprise the following steps that:
S1: preparation monocrystalline substrate, and deposit upper silicon nitride layer and lower silicon nitride layer respectively in upper surface and the lower surface of described monocrystalline substrate；
S2: in the upper silicon oxide layer of described upper silicon nitride layer deposition；
S3: preparation adds thermode on described upper silicon oxide layer；
S4: prepare insulating barrier on thermode in described adding, and connecting hole is set on described insulating barrier；
S5: electrode is measured in preparation on described insulating barrier, described measurement electrode is in described connection hole and described heating electrode conduction；
S6: prepare gas sensitization layer on described measurement electrode；
S7: will corrode bottom product in S6 step, is formed and is positioned at the heat-insulation chamber below described upper silicon nitride layer；
S8: the product after etching in S7 step is made annealing treatment, and is cooled into described MEMS gas sensor.
Specifically, the thermode that adds in described S3 step is that polysilicon ion is formed, and doped with phosphorus, and concentration ratio shared by phosphorus is 1%～3%.
Specifically, in described S5 step, measure electrode and use evaporation or the gold of sputtered film depositing system deposition 100nm～1000nm or platinum to be formed.
Specifically, in described S6 step, described gas sensitization layer material is Tungstic anhydride. or tin ash.
Specifically, in described S7 step, potassium hydroxide or tetramethyl ammonium hydroxide solution is used to perform etching.
Specifically, in described S8 step, in annealing, annealing temperature keeps two hours when being risen to 600 DEG C～800 DEG C by 100 DEG C～150 DEG C, and keep in atmosphere 600 DEG C～800 DEG C two hours.
In the present invention, the gas sensor using said method to make, have the advantages that
One, high-volume can manufacture parallel, can reach system-level integrated, encapsulation integrated level is high, can be compatible with chip technology；
Two, the precision of gas sensor own is high, lightweight, size is little, low in energy consumption, usefulness is high, low cost, it is possible to produce in enormous quantities.
Three, can realize CO, the detection of the multiple gases such as NO2, CH4.
Accompanying drawing explanation
Fig. 1 is the manufacture method schematic diagram of the MEMS gas sensor that the embodiment of the present invention provides；
10-monocrystalline substrate；The upper silicon nitride layer of 11a-；Silicon nitride layer under 11b-；
The upper silicon oxide layer of 12a-；13-adds thermode；14-insulating barrier；
15-measures electrode；16-gas sensitization layer；17-heat-insulation chamber.
Detailed description of the invention
In order to make the purpose of the present invention, technical scheme and advantage clearer, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not intended to limit the present invention.
It should be noted that be referred to as " being fixed on " or " being arranged at " another element when element, it can be directly on another element or may be simultaneously present centering elements.When an element is referred to as " being connected to " another element, and it can be directly to another element or may be simultaneously present centering elements.
Also, it should be noted the orientation term such as left and right, upper and lower in the present embodiment, it is only relative concept or with the normal operating condition of product as reference each other, and should not be regarded as restrictive.
Fig. 1 G, for the longitudinal sectional view of the MEMS gas sensor that the present invention provides.It includes monocrystalline substrate 10, is deposited on the upper silicon nitride layer 11a and upper silicon oxide layer 12a of monocrystalline substrate 10 upper surface from the bottom to top；It is deposited on the lower silicon nitride layer 11b of monocrystalline substrate 10 lower surface；Be placed in silicon oxide layer 12a adds thermode 13；It is placed in the insulating barrier 14 added on thermode 13；The measurement electrode 15 being placed on insulating barrier 14, measures electrode 15 and adds thermode 13 in conducting shape；It is placed in the gas sensitization layer 16 measured on electrode 15, gas sensitization layer 16 and electrically connecting with measuring electrode 15；Being positioned at the heat-insulation chamber 17 below silicon nitride layer 11a, monocrystalline substrate 10, lower silicon nitride layer 11b are penetrated by heat-insulation chamber 17.
Wherein, add thermode 13 and formed for polysilicon ion, and doped with phosphorus, and concentration ratio shared by phosphorus is 1% to 3%.It should be noted that this adds thermode 13 is to produce joule's heat energy by injection current.
Wherein, gas sensitization layer 16 includes tin ash, Tungstic anhydride..
With reference to Fig. 1, present invention also offers the manufacture method of above-mentioned MEMS gas sensor, it comprises the following steps that:
Such as Figure 1A, S1: preparation monocrystalline substrate 10, and deposit upper silicon nitride layer 11a and lower silicon nitride layer 11b respectively in upper surface and the lower surface of monocrystalline substrate 10；
In the implementation case: monocrystalline substrate 10 chooses 6 inches of n-type silicon chip of twin polishing, material parameter is<100>crystal orientation, fineness ＜ 0.05 μm, flatness≤± 2 μm, not damaged, and thickness is 500 ± 10 μm, and resistivity is 1～5 Ω cm.After Wafer Cleaning is clean, LPCVD (Low Pressure Chemical Vapor Deposition, low-pressure chemical vapour deposition technique) is used to deposit the low stress nitride silicon layer of 100nm-600nm respectively in silicon chip upper surface and lower surface.Meanwhile, monocrystalline substrate 10, as barrier layer, is played a protective role in postorder wet-etching technology by upper silicon nitride layer 11a and lower silicon nitride layer 11b.
Such as Figure 1B, S2: deposit upper silicon oxide layer 12a on upper silicon nitride layer 11a；
In this step, LPCVD method silicon oxide layer 12a in upper silicon nitride layer 11a deposition is used.Owing to, in the embodiment of the present invention, the whole device of gas sensor needs to carry out wet etching, using LPCVD to deposit low stress silicon oxide in S1 step after depositing low stress SiNx again, so, whole device membrane stress is less than 200Mpa, and structural stability is more preferable.Meanwhile, the heat conductivity of silicon oxide and silicon nitride can not show a candle to silicon therefore can play again the effect preventing heat to scatter and disappear.
Such as Fig. 1 C, S3: on upper silicon oxide layer 12a, preparation adds thermode 13；
In this step, the same polysilicon ion using LPCVD method to deposit 8k on upper silicon oxide layer 12a, meanwhile, ion implantation concentration ratio is that the phosphorus of 1% to 3% is to strengthen electric conductivity.This is because polycrystalline silicon is different from metal, it is in addition to free electron to be relied on, and hole to be relied on is conducted electricity, when polysilicon contains the impurity of denier, so that it may make its electrical conductivity vary widely, resistivity can be effectively reduced, therefore Doping Phosphorus, conductivity can be improved.And when the concentration of phosphorus is 1% to 3%, resistivity≤800 Ω cm, conductive effect is optimal.It is then passed through positive glue whirl coating, after front baking photoetching development, after after bake technique, carries out reactive ion etching, go after polysilicon ion layer is etched figure to add thermode 13 described in gum forming.During gas sensor work, polysilicon adds thermode 13 can not only provide optimal operating temperature to reach optimum Working to gas sensor, and absorption gas molecule in sensitive membrane can be made to obtain enough energy desorptions.
Such as Fig. 1 D, S4: prepare insulating barrier 14 on thermode 13 in adding；
In this step, use PECVD (Plasma Enhanced Chemical Vapor Deposition, plasma enhanced chemical vapor deposition method) in adding the silicon dioxide depositing one layer of 1.5 μm on thermode 13, silicon dioxide has preferable insulating properties, is placed in as insulating barrier 14 and adds on thermode 13.Profit whirl coating the most after deposit, develop after front baking photoetching, RIE plasma etching silicon dioxide layer, and on silicon dioxide layer, form connecting hole 141, adding thermode 13 and be deposited at connecting hole 141, purpose is easy to measure electrode 15 provides electric current to heat by connecting hole 141 to adding thermode 13.
Such as Fig. 1 E, S5: the measurement electrode 15 prepared on insulating barrier 14 with add thermode 13 insulation；
In this step, the mode of sputtering or the mode of thermal evaporation is used to deposit gold or the platinum of 100nm～1000nm on insulating barrier 14.The density that measurement electrode use gold or platinum are because gold or platinum is higher, and pliability is fine, doing the when that punching going between and will not cut through and affect other film layer.Specifically; prior to positive-glue removing on insulating barrier 14; stripping technology is carried out with cloudy version photomask; first whirl coating; carry out after bake, front gluing protection gold electrode after front baking after lithographic, aeration protected effect during gluing, should be avoided the occurrence of; and dry under 80 DEG C～100 DEG C of high temperature, shorten hardening time.Herein, select Aurum metallicum to do measurement electrode 15, be because gold antioxygenic property preferable, can accurately measure the resistance change rate of gas sensitization layer 16.
Such as Fig. 1 F, S6: prepare gas sensitization layer 16 in measuring on electrode 15；
In this step, gas sensitization layer material is the metal-oxide such as tin ash or Tungstic anhydride., and simultaneously added with noble metal, noble metal can be Pt, the Pd etc. with catalytic action, the effect adding noble metal is, reduce tin ash or the barrier potential of a semiconductor of Tungstic anhydride., promote the selectivity of gas sensor.During concrete operations, tin ash, Tungstic anhydride. and noble metal are processed into target, take shape in by the way of evaporation on measurement electrode 15.The admixture mass ratio of noble metal is 1%-5%, improves air-sensitive sensitivity.When the thickness of gas sensitization layer is 5um-8um when, sensitivity is the highest.
It should be noted that, Pt, Pd are good oxidation catalysts, if the amount added is too much, can make tested fuel gas that significant combustion reaction occurs thereon, gas sensing layer temperature is made significantly to raise, cause performance degradation, therefore the doping of the noble metal such as Pt, Pd is to be preferred less than 5% under normal circumstances.
Such as Fig. 1 G, S7: will S6 step be corroded bottom product, formed and be positioned at the heat-insulation chamber 17 below silicon nitride layer 11a；
In this step, product upper surface spin coating one layer protection glue in S6 step, for protective gas sensitive layer 16 not by alkali corrosion.Positive glue on the back side of product in S6 step, after front baking makes the window development after bake of silicon dioxide wet etching by lithography, is 20% by concentration, and the KOH solution that temperature is 80 degrees Celsius carries out silicon etching, until etching into this layer of silicon nitride of upper strata LPCVD deposition.Barrier layer is discharged with oxonium ion after wet method body silicon etching.It should be noted that above-mentioned KOH solution can also use tetramethyl ammonium hydroxide solution to substitute.Both solution can etch the structure of inclined ladder shape, and technique cost is low, it is suitable for producing in a large number, is 20%～30% at KOH or tetramethyl ammonium hydroxide solution in concentration, when the when of temperature 80 DEG C, the etch rate of silicon chip 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 described MEMS gas sensor.
It should be noted that before making annealing treatment, also include product in above-mentioned S7 is cut, cut into the step of multiple gas sensor semi-finished product.Herein, preferentially use cut, will not dusty gas sensitive layer 16, and cut place is smooth, and efficiency is high.
In S8 step, each gas sensor semi-finished product of well cutting are carried out annealing process, annealing keeps two hours when being and risen to 600 DEG C～800 DEG C by 100 DEG C～150 DEG C, and in atmosphere keep 600 DEG C～800 DEG C two hours, last natural cooling, gas sensitization layer 16 i.e. obtains poroid sensitive thin film.
The bulk resistor Standard resistance range of table 1 tin dioxide thin film or WO 3 film and the corresponding table of annealing
All not having annealing process in current production technology, be can be clearly seen that by table 1, when not carrying out annealing process when, the bulk resistor Standard resistance range of tin dioxide thin film or WO 3 film is less, and 3k Ω～7k Ω in fixed range；And when making annealing treatment, along with the bulk resistor Standard resistance range of the rising of annealing temperature, tin dioxide thin film or Tungstic anhydride. is gradually increased, when reaching 700 DEG C, the bulk resistor Standard resistance range of tin dioxide thin film or Tungstic anhydride. is 5k Ω～20k Ω.And when annealing temperature be 400 DEG C, 500 DEG C, 600 DEG C, 700 DEG C time, the respective linearity of gas sensor is relatively good, along with the raising of annealing temperature, tin dioxide thin film or WO 3 film increase substantially for the sensitivity of the fuel gas such as hydrogen, methane.
To sum up, the above-mentioned gas sensor using said method to make, have the advantages that
One, high-volume can manufacture parallel, can reach system-level integrated, encapsulation integrated level is high, can be compatible with chip technology；
Two, the precision of gas sensor own is high, lightweight, size is little, low in energy consumption, usefulness is high, low cost.
Three, can realize CO, the detection of the multiple gases such as NO2, CH4.
These are only presently preferred embodiments of the present invention, not in order to limit the present invention, all any amendment, equivalent and improvement etc. made within the spirit and principles in the present invention, should be included within the scope of the present invention.
Claims (9)
1. a MEMS gas sensor, it is characterised in that include,
Monocrystalline substrate；
Upper silicon nitride layer and upper silicon oxide layer, be stacked and placed on described monocrystalline substrate upper surface from the bottom to top；
Lower silicon nitride layer, is placed in described monocrystalline substrate lower surface；
Add thermode, be placed on described upper silicon oxide layer；
Insulating barrier, be placed in described in add on thermode, insulating barrier is provided with connecting hole；
Measure electrode, be placed on described insulating barrier, and connected with the described thermode that adds by described connecting hole；
Gas sensitization layer, is placed on described measurement electrode, and electrically connects with described measurement electrode；
Heat-insulation chamber, is positioned at below described upper silicon nitride layer, by described lower silicon nitride layer and described monocrystalline substrate
Rotten quarter is formed.
2. MEMS gas sensor as claimed in claim 1, it is characterised in that described in add thermode and be
Polysilicon ion is formed, and doped with phosphorus, and concentration ratio shared by phosphorus is 1% to 3%.
3. MEMS gas sensor as claimed in claim 1, it is characterised in that described gas sensitization layer
Material is tin ash or Tungstic anhydride..
4. the manufacture method of MEMS gas sensor as claimed in claim 1, it is characterised in that include
Following processing step:
S1: preparation monocrystalline substrate, and deposit respectively in upper surface and the lower surface of described monocrystalline substrate
Silicon nitride layer and lower silicon nitride layer；
S2: in the upper silicon oxide layer of described upper silicon nitride layer deposition；
S3: preparation adds thermode on described upper silicon oxide layer；
S4: prepare insulating barrier on thermode in described adding, and connecting hole is set on described insulating barrier；
S5: on described insulating barrier preparation measure electrode, described measurement electrode in described connection hole with described
Heating electrode conduction；
S6: prepare gas sensitization layer on described measurement electrode；
S7: will corrode bottom product in S6 step, forms be positioned at below described upper silicon nitride layer heat insulation
Chamber；
S8: the product after etching in S7 step is made annealing treatment, and is cooled into described MEMS gas
Body sensor.
5. the manufacture method of MEMS gas sensor as claimed in claim 4, it is characterised in that described
The thermode that adds in S3 step is that polysilicon ion is formed, and doped with phosphorus, and concentration ratio shared by phosphorus is
1%～3%.
6. the manufacture method of MEMS gas sensor as claimed in claim 4, it is characterised in that described
In S5 step, measure electrode use evaporation or sputtered film depositing system deposition 100nm～1000nm gold or
Platinum and formed.
7. the manufacture method of MEMS gas sensor as claimed in claim 4, it is characterised in that described
In S6 step, described gas sensitization layer material is Tungstic anhydride. or tin ash.
8. the manufacture method of MEMS gas sensor as claimed in claim 4, it is characterised in that described
In S7 step, potassium hydroxide or tetramethyl ammonium hydroxide solution is used to perform etching.
9. the manufacture method of MEMS gas sensor as claimed in claim 4, it is characterised in that described
In S8 step, in annealing, annealing temperature keeps when being risen to 600 DEG C～800 DEG C by 100 DEG C～150 DEG C
Two hours, and in atmosphere keep 600 DEG C～800 DEG C two hours.
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