CN103675028B - Semiconductor gas sensor and preparation method thereof - Google Patents
Semiconductor gas sensor and preparation method thereof Download PDFInfo
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Abstract
Present invention is disclosed a kind of semiconductor gas sensor and preparation method thereof, wherein this semiconductor gas sensor comprises: substrate, and described substrate has surface; Be arranged on the heating electrode on described surface; Be positioned at the signal sensing electrode of the thermal field that described heating electrode is formed, described signal sensing electrode comprises conductive electrode and is electrically connected the gas sensitive of described conductive electrode; Wherein, insulating medium layer is provided with between described heating electrode and described signal sensing electrode.Semiconductor gas sensor provided by the invention prepares insulating medium layer by adopting the mode of ink jet printing, can greatly reduce the production cost of sensor, and the resolution of ink jet printing is high, can the accurate pattern that designs of positioning printing, technological process is simple.
Description
Technical Field
The invention belongs to the technical field of electronic device manufacturing, and particularly relates to a semiconductor gas sensor and a preparation method of the semiconductor gas sensor.
Background
With the development of society and the advancement of science and technology, the scale of industrial production is gradually enlarged, but accidents caused by the accidents are also continuous, such as flammable, explosive, toxic and harmful gases generated in petrochemical industry and coal mine industry, once the gases exceed standards and leak, the health of production personnel and residents living around can be seriously affected, and casualties and property loss can be caused if the gases cause explosion. In addition, with the improvement of living standard of people and the transformation of decoration requirements of people on home environment, the problem of indoor air quality is increasingly outstanding, and malignant cases caused by toxic standard exceeding after decoration are reported more often. In order to ensure safety and prevent diseases, various detection methods and detection instruments have been developed, and among them, gas sensors have been widely used in the production and living fields of various industries.
Gas sensors are mainly classified into electrochemical type, semiconductor type, thermal conduction type, optical type, and the like. Among them, the semiconductor sensor is receiving more and more attention because of its high detection sensitivity, short response recovery time, small element size, long life and low price. In particular, with the development of micro-machining technology in recent years, the semiconductor gas sensor is developed toward integration and intellectualization by means of microelectronic process. Because the metal oxide semiconductor used as the gas sensitive material shows better sensitive characteristics when being heated to a higher temperature, a heating electrode of the gas sensitive material must be prepared first and then a signal sensing electrode must be prepared when the semiconductor gas sensor is prepared.
At present, a semiconductor gas sensor prepared by a microelectronic process generally has two structures, wherein a heating electrode and a signal sensing electrode are arranged on two sides of a substrate in the first structure, and the heating electrode is used for heating the signal sensing electrode through the substrate, so that the required power consumption is large; in the structure, the heating electrode and the signal sensing electrode are arranged on the same side of the substrate, and the heating electrode and the signal sensing electrode are separated by using an insulating medium layer on the same side, the insulating medium layer is prepared by adopting a physical vapor deposition mode, expensive physical vapor deposition equipment is required, a complex etching process is required to be mastered, and the production cost of the sensor is increased.
Disclosure of Invention
It is an object of the present invention to provide a semiconductor gas sensor which is inexpensive to produce.
The invention also aims to provide a preparation method of the semiconductor gas sensor.
To achieve one of the above objects, the present invention provides a semiconductor gas sensor comprising:
a substrate having a surface;
a heating electrode disposed on the surface;
the signal sensing electrode is positioned in a thermal field formed by the heating electrode and comprises a conductive electrode and a gas-sensitive material electrically connected with the conductive electrode, and the gas-sensitive material is positioned on the conductive electrode; wherein,
an insulating medium layer is arranged between the heating electrode and the signal sensing electrode.
As a further improvement of the invention, the material of the insulating medium layer is selected from one or more of aluminum oxide, silicon dioxide and hafnium dioxide.
As a further improvement of the invention, adhesive layers are respectively arranged among the substrate, the heating electrode and the signal sensing electrode.
As a further improvement of the invention, the bonding layer is a Ti metal film, a Cr metal film or a Ti/Cr alloy film.
As a further improvement of the invention, the substrate is selected from one of a silicon wafer with oxidized surface, a glass sheet, a quartz sheet, an alumina ceramic sheet, an aluminum nitride ceramic sheet, a zirconia ceramic sheet and a polyimide film, and the thickness of the substrate is 100-1000 um.
In a further improvement of the present invention, the material of the heating electrode is one selected from gold, silver, platinum, copper, tungsten, platinum-gold alloy, silver-palladium alloy, nickel-chromium alloy, molybdenum-manganese alloy, titanium nitride, and ruthenium oxide, and the material of the conductive electrode is one selected from gold, silver, platinum, copper, and tungsten.
As a further improvement of the invention, the heating electrode is in a square wave shape, or a sawtooth wave shape, or a triangular wave shape, or a sine wave shape, or a snake shape.
As a further improvement of the invention, the insulating medium layer is prepared by means of ink jet printing.
In order to achieve another object of the present invention, the present invention provides a method for manufacturing a semiconductor gas sensor, the method comprising the steps of:
s1, manufacturing a heating electrode on the substrate;
s2, ink-jet printing a layer of precursor ink of the insulating medium layer on the substrate;
s3, annealing the substrate processed in the step S2 to obtain an insulating medium layer formed on the substrate;
and S4, manufacturing a conductive electrode on the insulating medium layer, and depositing a gas-sensitive material on the conductive electrode to obtain the semiconductor gas sensor.
As a further improvement of the invention, the annealing temperature in the step S3 is 500-1000 ℃, and the time of the annealing treatment is 10 min-24 h.
As a further improvement of the invention, the thickness of the insulating dielectric layer formed in the step S3 is 200 nm-2 um.
Compared with the prior art, the semiconductor gas sensor provided by the invention has the advantages that the insulating medium layer is prepared by adopting an ink jet printing mode, the production cost of the sensor can be greatly reduced, the ink jet printing resolution is high, the designed patterns can be accurately positioned and printed, and the process flow is simple.
Drawings
FIG. 1 is a schematic structural diagram of one embodiment of a semiconductor gas sensor of the present invention;
FIG. 2 is a schematic structural view of the semiconductor gas sensor shown in FIG. 1 without signal sensing electrodes;
FIG. 3 is a schematic diagram of a structure of a semiconductor gas sensor shown in FIG. 1, in which a heater electrode is formed on a substrate;
FIG. 4 is a schematic structural view of a semiconductor gas sensor according to still another embodiment of the present invention;
FIG. 5 is a schematic structural view of a semiconductor gas sensor according to still another embodiment of the present invention;
FIG. 6 is a schematic structural view of a semiconductor gas sensor according to still another embodiment of the present invention;
FIG. 7 is a schematic structural view of a semiconductor gas sensor according to still another embodiment of the present invention;
FIG. 8 is a schematic view of the shape of a sawtooth waveform heating electrode;
FIG. 9 is a schematic view of the shape of a triangular wave-shaped heating electrode;
FIGS. 10 and 11 are schematic views of the shape of a sine wave heating electrode;
FIG. 12 is a flow chart of a method of manufacturing the semiconductor gas sensor of the present invention.
Detailed Description
The present invention will be described in detail below with reference to specific embodiments shown in the drawings. These embodiments are not intended to limit the present invention, and structural, methodological, or functional changes made by those skilled in the art according to these embodiments are included in the scope of the present invention.
Referring to fig. 1 to 3, describing an embodiment of the semiconductor gas sensor of the present invention, the semiconductor gas sensor 100 includes a substrate 10, a signal sensing electrode 30, a heating electrode 20, and an insulating dielectric layer 40.
The substrate 10 has a surface 11, the surface 11 being relatively defined for subsequent circuit layout, a heating electrode 20 being fabricated on the surface 11, a signal sensing electrode 30 being located in a thermal field formed by the heating electrode 20, and an insulating dielectric layer 40 being disposed between the heating electrode 20 and the signal sensing electrode 30 to insulate the heating electrode 20 and the signal sensing electrode 30 from each other.
The substrate 10 can be one selected from a silicon wafer, a glass sheet, a quartz sheet, an alumina ceramic sheet, an aluminum nitride ceramic sheet, a zirconia ceramic sheet and a polyimide film with oxidized surfaces, and the thickness of the substrate 10 is 100 um-1000 um. The material of the heating electrode 20 is selected from one of gold, silver, platinum, copper, tungsten, platinum-gold alloy, silver-palladium alloy, nickel-chromium alloy, molybdenum-manganese alloy, titanium nitride, and ruthenium oxide.
The signal sensing electrode 30 includes two conductive electrodes 31 and a gas sensitive material (not shown) electrically connected to the two conductive electrodes. The conductive electrode 31 may be made of one of metals, such as Pt, Au, Ag, Cu, Al, Ni, and W, and at least two signal sensing electrodes 30 are included in one semiconductor gas sensor 100, and more signal sensing electrodes may be provided depending on the kind of sensor.
The gas-sensitive material is a key component of a semiconductor gas sensor, for example, a semiconductor gas sensor is provided, wherein the selected gas-sensitive material is a nano metal oxide functionalized carbon nanotube material, the nano metal oxide functionalized carbon nanotube material comprises a carbon nanotube and nickel oxide, and the mass ratio of the carbon nanotube to the nickel oxide is 1: 0.1-1: 30. Further preferably, the mass ratio of the carbon nanotubes to the nickel oxide is 1:1 to 1:20, or even more preferably 1:1.7 to 1: 18. The carbon nanotube has hydroxyl bond on its surface to adsorb nickel oxide and to maintain the nickel oxide.
The microcosmic carbon nanotubes in the provided nano metal oxide functionalized carbon nanotube material are overlapped randomly, more gaps exist between the microcosmic carbon nanotubes, the nickel oxide is adsorbed on the surface of the functional layer, and the nickel oxide can be adsorbed in the gaps in the whole carbon nanotube material area, so that gas to be detected can flow between the gaps formed by overlapping the carbon nanotubes, and the detection effect of the sensor is better.
The material of the insulating medium layer is selected from one or more of aluminum oxide, silicon dioxide and hafnium dioxide. The thickness of the insulating medium layer is thinner than that of the substrate, so that the requirement for the heating efficiency of the heating electrode is not high, and the insulating effect is good. The insulating medium layer is manufactured in an ink jet printing mode, the ink jet printing resolution is high, the accuracy can reach several micrometers, designed patterns can be printed in an accurate positioning mode, the process flow is simple, the operation is convenient, and the cost is low.
In order to improve the bonding strength between the substrate 10, the heating electrode 20, and the signal sensing electrode 30, an adhesive layer (not shown) is disposed therebetween. The bonding layer may be a Ti metal film, or a Cr metal film, or a Ti/Cr alloy film.
The heating electrode 20 is disposed around the signal sensing electrode 30 to provide a uniform thermal field. The "surrounding" may be closed or non-closed, and the surrounding heating electrodes 20 may provide a uniform thermal field to generate a better heating effect for the signal sensing electrodes. Also, due to the presence of the insulating dielectric layer 40, the heating electrode 20 and the signal sensing electrode 30 may have a staggered portion with each other.
Referring to fig. 4, in one embodiment of the semiconductor gas sensor 100, it should be noted that the insulating dielectric layer 40 between the heater electrode 20 and the signal sensing electrode 30 is omitted here for clarity of illustration of a preferred embodiment. The heating electrode 20 includes a main heating part 21 and a sub-heating part 22 connected to the main heating part 21, the main heating part 21 includes a first main heating section 211 and a second main heating section 212 symmetrically disposed, and the signal sensing electrode 30 is located between the first main heating section 211 and the second main heating section 212. The main heating part 21 is positioned closer to the signal sensing electrode 30 than the sub-heating part 22, and it should be understood that the terms "main heating part 21" and "sub-heating part 22" are merely defined for convenience of description, and do not represent fundamental differences in manufacturing processes or structures. Also, although the signal sensing electrode 30 is shown between the first main heating section 211 and the second main heating section 212, there may be substantially an interleaving between the signal sensing electrode 30 and the heating electrode due to the presence of the insulating medium layer.
In the main heating part 21, the temperature difference of the thermal field generated by the first main heating section 211 and the second main heating section 212 is less than 100 ℃, and further, the temperature difference of the thermal field is controlled to be less than 50 ℃ to ensure the sensitivity and reliability of the semiconductor gas sensor to the detection of the target gas. Of course, in the most desirable alternative embodiment, the first main heating section 211 and the second main heating section 212 have equal resistance values to ensure that the temperature of the thermal field generated by the first main heating section 211 and the second main heating section 212 is the same.
The distance between the first main heating section 211 and the adjacent conductive electrode 31 is equal to the distance between the second main heating section 212 and the adjacent conductive electrode 31 to ensure uniform heating of the conductive electrode, the secondary heating section 22 includes a first secondary heating section 221 and a second secondary heating section 222 connected to the first main heating section 211 and the second main heating section 212, respectively, and the resistance values of the first secondary heating section 221 and the second secondary heating section 222 are also preferably equal.
The first heating stage 221 and the second heating stage 222 form an identical pattern in a plan view, and more preferably, the first heating stage 221 and the second heating stage 222 are symmetrically disposed with respect to each other.
While various specific heater electrode shapes can be designed to satisfy the above limitations of all or part of the features of the heater electrode 20, it is preferred to select specific embodiments for exemplary illustration, and the insulating medium layer in these embodiments is omitted, and the heater electrode and the signal sensing electrode in these embodiments may have a staggered portion due to the insulating medium layer 40, and are not limited to the embodiments shown in the drawings.
Referring to the embodiment of fig. 4, the main heating portion 21 has a flat-bottomed U-shape and surrounds the signal sensing electrode 30, and the entire heating electrode 20 has a square waveform, and the entire heating electrode is arranged in mirror symmetry along the signal sensing electrode 31. The line width of the heating electrode 20 is 10um ~200um, and the interval of each part in the heating electrode 20 changes between 10um ~100 um.
Referring to the embodiment of fig. 5, unlike fig. 4, in the present embodiment, the first and second sub-heating sections 221a and 222a on both sides of the main heating section 21a are provided with a more square wave-shaped extension to provide a more powerful heating effect and a more uniform thermal field. The line width of the heating electrode 20a is 10um ~200um, and the interval of each part in the heating electrode changes between 10um ~100 um.
Referring to the embodiment of fig. 6, the main heating part 21b is in a coupled U-shape, the sub-heating part 22b is coupled to the main heating part 21b, and the lengths of the heating electrodes 20b on both sides of the signal sensing electrode 30b are substantially equal to provide a uniform thermal field. The line width of the heating electrode 20b is 10 um-200 um, and the distance between each part in the heating electrode 20b is changed between 10 um-100 um.
Referring to the embodiment of FIG. 7, the heater electrode 20c has a serpentine shape as a whole, and the lengths of the heater electrodes on both sides of the signal sensing electrode 30c are substantially equal to provide a uniform thermal field. The line width of the heating electrode 20c is 10 um-200 um, and the distance between each part in the heating electrode 20c is changed between 10 um-100 um.
The heating electrode may have a sawtooth waveform as shown in fig. 8, a triangular waveform as shown in fig. 9, or a sinusoidal waveform as shown in fig. 10 and 11.
With reference to fig. 1, in the present embodiment, the heating electrode 20 has a constant width, and since the thicknesses of the heating electrodes 20 to be manufactured are equal, the heating electrode 20 provides a uniform amount of heat generation in each portion within the effective heat generation region.
Referring to fig. 12, a method of fabricating a semiconductor gas sensor according to an embodiment of the present invention is provided below. In this embodiment, the method comprises the steps of:
s1, manufacturing a heating electrode on the substrate.
The heating electrode can be prepared by physical vapor deposition or printing, and the shape of the heating electrode can be a square sheet or a serpentine shape.
And S2, ink-jet printing a layer of precursor ink of the insulating medium layer on the substrate.
The precursor ink is one or a combination of more of alumina ink, silicon dioxide ink and hafnium dioxide ink.
And S3, annealing the substrate processed in the step S2 to obtain an insulating medium layer formed on the substrate.
The annealing temperature is 500-1000 ℃, the annealing time is 10 min-24 h, and the finally formed insulating medium layer is controlled to be 200 nm-2 um.
And S4, manufacturing a conductive electrode on the insulating medium layer, and depositing a gas-sensitive material on the conductive electrode to obtain the semiconductor gas sensor.
Some embodiments of fabricating the semiconductor gas sensor of the present invention are described below.
Example 1
Spin-coating a layer of photoresist on a soda-lime glass substrate, transferring a snakelike heating electrode pattern onto glass after exposure and development, sputtering a layer of nickel-chromium alloy with the thickness of 500nm by using a magnetron sputtering method to form a heating electrode, printing an alumina insulating medium layer with the thickness of 200nm on the soda-lime glass substrate on which the heating electrode is formed by sputtering by using an ink-jet printer, annealing at the temperature of 500 ℃ for 10 hours, finally sputtering a layer of gold on the insulating medium layer by using the magnetron sputtering method to serve as a conductive electrode, and depositing a gas-sensitive material on the conductive electrode to obtain the semiconductor gas sensor chip.
Example 2
Spin-coating a layer of photoresist on an alumina ceramic substrate, transferring a serpentine heating electrode pattern onto glass after exposure and development, sputtering a layer of silver palladium alloy with the thickness of 800nm by a magnetron sputtering method to form a heating electrode, printing a layer of silicon oxide insulating medium with the thickness of 800nm on the alumina ceramic substrate on which the heating electrode is sputtered by an ink-jet printer, annealing at 1000 ℃ for 10min, sputtering a layer of gold on the insulating medium layer by the magnetron sputtering method to serve as a conductive electrode, and depositing a gas-sensitive material on the conductive electrode to obtain the semiconductor gas sensor chip.
Example 3
Printing a silver-palladium alloy serpentine heating electrode with the thickness of 5 microns on an alumina ceramic substrate by a screen printing method, printing an alumina insulating medium layer with the thickness of 1 micron on the substrate on which the heating electrode is formed by an ink-jet printer, annealing at 1000 ℃ for 5 hours, sputtering a platinum layer on the insulating medium layer by a magnetron sputtering method to be used as a conductive electrode, and depositing a gas-sensitive material on the conductive electrode to obtain the semiconductor gas sensor chip.
Example 4
Printing a layer of ruthenium dioxide square heating electrode with the thickness of 2um on a quartz glass substrate by a screen printing method, printing a layer of hafnium oxide insulating medium layer with the thickness of 2um on the substrate on which the heating electrode is formed by an ink-jet printer, annealing at 700 ℃ for 10 hours, finally sputtering a layer of silver on the insulating medium layer by a magnetron sputtering method to be used as a conductive electrode, and depositing a gas-sensitive material on the conductive electrode to obtain the semiconductor gas sensor chip.
Example 5
Printing a silver palladium square heating electrode with the thickness of 10 microns on an aluminum nitride ceramic substrate by a screen printing method, printing an alumina insulating medium layer with the thickness of 800nm on the substrate on which the heating electrode is formed by an ink-jet printer, annealing at 700 ℃ for 24 hours, finally printing a silver layer on the insulating medium layer by the screen printing method to be used as a conductive electrode, and depositing a gas-sensitive material on the conductive electrode to obtain the semiconductor gas sensor chip.
Example 6
Spin-coating a layer of photoresist on a hafnium oxide ceramic substrate, transferring a snakelike heating electrode pattern to the hafnium oxide ceramic substrate after exposure and development, sputtering a layer of gold with the thickness of 800nm by using a magnetron sputtering method to serve as a heating electrode, printing a layer of hafnium oxide insulating medium with the thickness of 500nm on the substrate on which the heating electrode is formed by sputtering by using an ink-jet printer, annealing at the temperature of 800 ℃ for 1 hour, finally printing a layer of gold by using a screen printing method to serve as a conductive electrode, and depositing a gas-sensitive material on the conductive electrode to obtain the semiconductor gas sensor chip.
The invention has the following beneficial effects through the above embodiment: the semiconductor gas sensor provided by the invention has the advantages that the insulating medium layer is prepared by adopting an ink jet printing mode, the production cost of the sensor can be greatly reduced, the ink jet printing resolution is high, the designed patterns can be accurately positioned and printed, and the process flow is simple.
It should be understood that although the present description refers to embodiments, not every embodiment contains only a single technical solution, and such description is for clarity only, and those skilled in the art should make the description as a whole, and the technical solutions in the embodiments can also be combined appropriately to form other embodiments understood by those skilled in the art.
The above-listed detailed description is only a specific description of a possible embodiment of the present invention, and they are not intended to limit the scope of the present invention, and equivalent embodiments or modifications made without departing from the technical spirit of the present invention should be included in the scope of the present invention.
Claims (10)
1. A semiconductor gas sensor, comprising:
a substrate having a surface;
a heating electrode disposed on the surface;
the signal sensing electrode is positioned in a thermal field formed by the heating electrode and comprises a conductive electrode and a gas-sensitive material electrically connected with the conductive electrode, and the gas-sensitive material is positioned on the conductive electrode; wherein,
an insulating medium layer is arranged between the heating electrode and the signal sensing electrode.
2. The semiconductor gas sensor according to claim 1, wherein the insulating dielectric layer is made of one or more materials selected from the group consisting of alumina, silica, and hafnia.
3. The semiconductor gas sensor according to claim 1, wherein adhesive layers are provided between the substrate, the heating electrode, and the signal sensing electrode, respectively.
4. The semiconductor gas sensor according to claim 3, wherein the bonding layer is a Ti metal thin film, or a Cr metal thin film, or a Ti/Cr alloy thin film.
5. The semiconductor gas sensor according to claim 1, wherein the substrate is one selected from a silicon wafer, a glass wafer, a quartz wafer, an alumina ceramic wafer, an aluminum nitride ceramic wafer, a zirconia ceramic wafer, and a polyimide film, and the thickness of the substrate is 100 to 1000 um.
6. The semiconductor gas sensor according to claim 1, wherein the material of the heater electrode is one selected from gold, silver, platinum, copper, tungsten, platinum-gold alloy, silver-palladium alloy, nickel-chromium alloy, molybdenum-manganese alloy, titanium nitride, and ruthenium oxide, and the material of the conductive electrode is one selected from gold, silver, platinum, copper, and tungsten.
7. The semiconductor gas sensor according to claim 1, wherein the heating electrode has a square wave, or a sawtooth wave, or a triangular wave, or a sine wave, or a serpentine shape.
8. The semiconductor gas sensor according to claim 1, wherein the insulating medium layer is formed by means of ink-jet printing.
9. A method of manufacturing a semiconductor gas sensor, the method comprising the steps of:
s1, manufacturing a heating electrode on the substrate;
s2, ink-jet printing a layer of precursor ink of the insulating medium layer on the substrate;
s3, annealing the substrate processed in the step S2 to obtain an insulating medium layer formed on the substrate;
and S4, manufacturing a conductive electrode on the insulating medium layer, and depositing a gas-sensitive material on the conductive electrode to obtain the semiconductor gas sensor.
10. The method of claim 9, wherein the annealing temperature in step S3 is 500 ℃ to 1000 ℃, the annealing time is 10min to 24h, and the thickness of the formed insulating dielectric layer is 200nm to 2 um.
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