CN114107924B - Heat-sensitive film for uncooled infrared micro-measurement bolometer - Google Patents
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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Abstract
The invention relates to the technical field of uncooled infrared detection, and discloses a thermosensitive film for an uncooled infrared microbolometer, which is characterized by comprising Sn x Zn 1‑x O material, wherein the value range of x is 0.15-0.35; at 25 ℃, the sheet resistance of the thermosensitive film is 1-200 KΩ/≡and the temperature coefficient of resistance is-1.8 to-3.8%/K; doping Sn into ZnO to obtain Sn x Zn 1‑x Compared with the non-doped Sn, the O thermosensitive film can obtain higher temperature coefficient of resistance under the condition of lower sheet resistance; the thermosensitive film has good long-term stability of electrical property, simple and feasible preparation process and suitability for large-scale production.
Description
Technical Field
The invention relates to the technical field of uncooled infrared detection, in particular to a thermosensitive film for an uncooled infrared micro-bolometer.
Background
Infrared imaging is a technique for performing thermal imaging, detecting and identifying a target using naturally radiated infrared rays of a detection object. The key components of the infrared imaging technology are infrared detectors, the infrared detectors are divided into two major types, namely photon detectors and heat detectors, although the sensitivity, response speed, detection distance and other performances of the photon detectors such as dysprosium-cadmium-mercury (HgCdTe) detectors (working in the wave band of 8-14 mu m) and indium antimonide (InSb) detectors (working in the wave band of 3-5 mu m) are relatively high, liquid nitrogen is required to be used for cooling (about 80K), and almost all infrared imaging is required to use a mechanical scanning device, so that the whole infrared imaging system is complex in structure and high in cost, and large-scale popularization and application cannot be realized. Under the promotion of large-scale and ultra-large-scale integrated circuit technology, infrared detectors have rapidly developed from a unit type to a focal plane array (Focal Plane Array-FPA). Compared with the refrigeration type infrared detector, the uncooled infrared detector has the main advantages of low cost, small volume, light weight, low power consumption, wide response wave band and mass production, and has wide application in military fields such as night vision, accurate guidance, infrared tracking and the like and civil fields such as fire protection, public security, medical treatment, industrial control and the like.
The most important product of the prior uncooled thermal imaging technology is a micro-bolometer array, and the micro-bolometer detects and images the change of the sensitive film resistance along with the temperature as the change of voltage or current signals. The specific process is as follows: the target radiates a certain amount of infrared rays outwards at a certain temperature, the microbolometer generates heat after absorbing infrared radiation, the temperature of the microbolometer is changed, the thermosensitive film converts the change into resistance change, the resistance change is transmitted to a reading circuit through an electrical channel in a microbridge, the change of the resistance value is detected, and the detection of the target is completed. In this process, a thermosensitive film, one of the key components of a microbolometer, needs to meet three most important requirements: (1) suitable resistance, compatible with readout circuitry; (2) The temperature coefficient of resistance is high, preferably greater than 2%/K (absolute value); and (3) the process repeatability is good, and the electrical performance is stable for a long time.
There are many kinds of heat-sensitive materials currently available for microbolometers, such as metallic titanium, metallic platinum, vanadium oxide, silicon germanium alloy, amorphous silicon, superconducting oxides, giant magnetoresistance materials, etc. Among them, the most used is the vanadium oxide and amorphous silicon because of their proper resistance and high temperature coefficient of resistance. However, these two materials still have drawbacks, such as the vanadium dioxide in the vanadium oxide compound has a metal-insulator phase transition around 68 ℃, which can lead to thermal hysteresis loops, thereby affecting the stability and reliability of the device; in addition, the vanadium oxide meeting the thermosensitive requirement of the microbolometer is relatively complex in process because of more valence states of vanadium elements. For amorphous silicon materials, the resistance is large in the application, which results in 1 +.fThe noise is large, thereby affecting the detection rate of the device.
In the patent of the invention with the authority of the person entitled CN 109988997B and the name of thermosensitive film and the preparation method and application thereof, a thermosensitive film used in an uncooled infrared microbolometer is disclosed, which is made of ZnOx material, wherein the value range of x is 0.7-0.95; at 25 ℃, the sheet resistance of the thermosensitive film is 5-500 KΩ/≡and the temperature coefficient of resistance is-1.5 to-3.5%/K. However, since the film is found to have a relatively high resistance when the TCR is satisfactory when used in a detector, there is a certain difference from the ideal. The device is required to have a larger temperature coefficient of resistance under a proper sheet resistance, and if the sheet resistance is too large, the device is incompatible with a read circuit, and the reliability of the device is affected. Therefore, in the field of uncooled infrared detection, the exploration and process improvement of the thermosensitive film are still hot spots and difficulties in current research. Researchers are still constantly exploring new heat sensitive materials, and at the same time, new processes are being studied to improve the performance of existing heat sensitive materials.
Disclosure of Invention
The invention aims to: aiming at the problems existing in the prior art, the invention provides a thermosensitive film for a non-refrigeration infrared microbolometer, which is prepared by doping Sn into ZnO x Zn 1-x Compared with the non-doped Sn, the O thermosensitive film can obtain higher temperature coefficient of resistance under the condition of lower sheet resistance; the thermosensitive film has good long-term stability of electrical property, simple and feasible preparation process and suitability for large-scale production.
The technical scheme is as follows: the invention provides a thermosensitive film for an uncooled infrared microbolometer, which consists of Sn x Zn 1-x O material, wherein the value range of x is 0.15-0.35; at 25 ℃, the sheet resistance of the thermosensitive film is 1-200 KΩ/≡and the temperature coefficient of resistance is-1.8 to-3.8%/K; the preparation method comprises the following steps: s1: placing the dry and clean substrate into a DC reaction magnetron sputtering furnace, and vacuumizing to 1×10 -4 Pa, heating the substrate to 100-300 ℃; s2: using a baffle plate to block the substrate, and pre-sputtering a metal zinc target and a tin target; s3: removing the baffle plate, controlling the sputtering power of the zinc target to be 80-120W, controlling the sputtering power of the tin target to be 10-20W, and depositing Sn with the thickness of 50-350 nm on the substrate by reactive sputtering x Zn 1-x An O film; the flow rate ratio of oxygen to argon during sputtering is 10-30%; s4: simultaneously closing the oxygen flow, the argon flow and the sputtering current; s5: after the DC reaction magnetron sputtering furnace is stabilized, the background vacuum is up to 1.0 multiplied by 10 -4 ~1.5×10 -4 After Pa, for the Sn x Zn 1-x Annealing the O film; s6: through the process ofAnnealing to obtain Sn x Zn 1-x And (3) cooling the O film to room temperature in high vacuum or oxygen atmosphere to obtain the thermosensitive film, and taking out for later use.
Preferably, after S6, a passivation film of an insulating material is further deposited on the thermosensitive film. Because of Sn x Zn 1-x The O film material has strong activity and is extremely easy to be oxidized by air, so that the stability and reliability of the resistance and the temperature coefficient of resistance of the material are reduced. To isolate Sn x Zn 1-x O film material and air react with each other, and the invention also discloses Sn x Zn 1-x And depositing a passivation film on the O film material. Because the passivation film and Sn located thereunder x Zn 1-x Since the O thin film is parallel to the readout circuit, the passivation film is required to have good insulation so as not to generate additional resistance.
Preferably, the thickness of the passivation film is 10-50 nm. The passivation film with the thickness within the range can effectively isolate the interaction between the air and the thermosensitive layer and prevent the thermosensitive layer from being oxidized. Preferably, the insulating material is SiC, si 3 N 4 、SiO 2 TiN or TiO 2 . According to the effect of the passivation film, to prevent the passivation film from being mixed with Sn x Zn 1-x Since the oxide film material is required to have a weak oxidizing ability due to the interaction of the O film material, it is preferable to use insulating materials such as SiC and Si having a weak oxidizing ability 3 N 4 、SiO 2 TiN or TiO 2 。
Preferably, in the step S2, the flow rate of argon is 50-100 sccm, the sputtering current is 0.1-0.6A, and the pre-sputtering time is 10-20 min.
Preferably, in the step S3, the working pressure during sputtering is 1-2.5 Pa, the sputtering temperature is 100-300 ℃, the sputtering current is 0.1-0.6A, and the sputtering time is 10-50 min.
Preferably, in the step S5, the annealing atmosphere in the annealing treatment is 1.0X10% under vacuum -4 ~1.5×10 -4 And under Pa or oxygen atmosphere, the annealing temperature is 200-400 ℃ and the heat preservation time is 20-60 min, wherein the temperature is 0.1-1.5 Pa.
Preferably, in said S6The high vacuum is 1.0X10 -4 ~1.5×10 -4 Pa, the oxygen atmosphere is 0.1-1.5 Pa.
The beneficial effects are that: in the invention, the thermosensitive film adopts Sn x Zn 1-x The resistance of the thermosensitive film is 1 to 200KΩ/≡, the resistance is proper, the thermosensitive film can be well compatible with a reading circuit, the Temperature Coefficient of Resistance (TCR) is higher, and the voltage response rate of the device can be improved between-1.8 and-3.8%/K, so that the detection rate of the device is improved. The thermosensitive film has no phase change in the application range of the device, and the resistance is easy to control, so that the defects in the prior art can be overcome, the long-term stability of the electrical property is good, the preparation process is simple and easy to implement, and the thermosensitive film is suitable for large-scale production.
The most important point is that the Sn doping can effectively reduce the sheet resistance of the film without reducing or increasing the temperature coefficient of the film resistance relative to the ZnO film material, and the film has long-term stable electrical property, the sheet resistance is comparable with the temperature coefficient of the resistance and vanadium oxide, and the invention of the material opens up a new path for researching the heat-sensitive material for the uncooled infrared device.
Sn x Zn 1-x The preparation method of the O film material is to combine direct current magnetron reactive sputtering with in-situ annealing, and Sn is controlled by adjusting parameters such as sputtering power, sputtering pressure, oxygen-argon ratio, sputtering temperature, sputtering current, sputtering time, annealing atmosphere, annealing pressure, annealing temperature, annealing time and the like in the sputtering process x Zn 1-x Oxygen vacancy concentration in the O thin film material to achieve effective control of Sn x Zn 1-x The purpose of the resistance and the temperature coefficient of resistance of the O film material.
Drawings
FIG. 1 is a side view of a thermosensitive film in the present invention;
fig. 2 is a sheet resistance-temperature curve of the thermosensitive film obtained in embodiment 2.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings.
Embodiment 1:
sequentially placing K9 glass substrate into acetone, alcohol and deionized water solution, ultrasonically cleaning, blow-drying with nitrogen, placing the substrate into a DC reaction magnetron sputtering furnace, and vacuumizing to 1×10 -4 Pa. During this period, the substrate was warmed to 200 ℃. The substrate was blocked by using a baffle plate, and the metallic zinc target and the tin target were simultaneously pre-sputtered for 10 minutes with a sputtering current of 0.4A at an argon flow rate of 100 sccm. After pre-sputtering, maintaining the argon flow of 100 sccm and the sputtering current of the zinc target unchanged, reducing the sputtering current of the tin target to 0.1A, adding oxygen with the flow of 10sccm, operating the pressure of 1.5 Pa, removing the baffle, sputtering on the substrate for 20 min, and maintaining the substrate holder to rotate at a constant speed in the sputtering process. And after the sputtering is finished, simultaneously closing the oxygen flow, the argon flow and the sputtering current. After the sputtering furnace is stable, the background vacuum reaches 1 multiplied by 10 -4 After Pa, the substrate is heated to 300 ℃, oxygen is added to keep the pressure of the chamber at 1.5 Pa, the film is annealed for 20 min by oxygen, then the film is naturally cooled, and the sample can be taken out after the temperature is reduced to normal room temperature. Obtaining Sn with the thickness of about 120 nm, the sheet resistance of 5K omega/≡and the resistance temperature coefficient of-1.8%/K at 25 DEG C 0.15 Zn 0.85 And (3) an O film. Finally, depositing TO with the thickness of 20nm on the prepared film 2 And a passivation layer made of materials.
Fig. 1 is a side view of a thermosensitive film covered with a passivation film according to the present invention.
Fig. 2 shows the resistance-temperature curve of the thermosensitive film (sample R1 in the figure, where the curves at the time of temperature increase and temperature decrease overlap) obtained in the present embodiment. Therefore, the resistance changes exponentially with temperature, and no thermal hysteresis loop is found in the heating and cooling processes.
Embodiment 2:
sequentially placing K9 glass substrate into acetone, alcohol and deionized water solution, ultrasonically cleaning, blow-drying with nitrogen, placing the substrate into a DC reaction magnetron sputtering furnace, and vacuumizing to 1×10 -4 Pa. During this period, the substrate was warmed to 200 ℃. The substrate was blocked by using a baffle plate, and the metallic zinc target and the tin target were simultaneously pre-sputtered for 10 minutes with a sputtering current of 0.4A at an argon flow rate of 100 sccm. After pre-sputtering, the sputtering current of the zinc target is kept unchanged while the argon flow is 100 sccmThe sputtering current of the tin target is reduced to 0.15A, the oxygen adding flow is 10sccm, the working pressure is 1.5 and Pa, the baffle plate is removed, the sputtering is carried out on the substrate for 20 min, and the substrate holder is kept to rotate at a constant speed in the sputtering process. And after the sputtering is finished, simultaneously closing the oxygen flow, the argon flow and the sputtering current. After the sputtering furnace is stable, the background vacuum reaches 1.5 multiplied by 10 -4 After Pa, the substrate is heated to 300 ℃, oxygen is added to keep the pressure of the chamber at 1.5 Pa, the film is annealed for 20 min by oxygen, then the film is naturally cooled, and the sample can be taken out after the temperature is reduced to normal room temperature. Obtaining Sn with the thickness of about 115 nm, the sheet resistance of 90KΩ/≡at 25 ℃ and the temperature coefficient of resistance of-2.3%/K 0.2 Zn 0.8 And (3) an O film. Finally, TO with the thickness of 20nm is deposited on the prepared film 2 And a passivation layer made of materials.
Fig. 2 shows the sheet resistance-temperature curve (sample R2 in the figure, where the curves at the time of temperature increase and temperature decrease overlap) of the thermosensitive film obtained in the present embodiment. Therefore, the resistance changes exponentially with temperature, and no thermal hysteresis loop is found in the heating and cooling processes.
Embodiment 3:
sequentially placing K9 glass substrate into acetone, alcohol and deionized water solution, ultrasonically cleaning, blow-drying with nitrogen, placing the substrate into a DC reaction magnetron sputtering furnace, and vacuumizing to 1×10 -4 Pa. During this period, the substrate was warmed to 200 ℃. The substrate was blocked by using a baffle plate, and the metallic zinc target and the tin target were simultaneously pre-sputtered for 10 minutes with a sputtering current of 0.4A at an argon flow rate of 100 sccm. After pre-sputtering, maintaining the argon flow of 100 sccm and the sputtering current of the zinc target unchanged, reducing the sputtering current of the tin target to 0.2A, adding oxygen with the flow of 10sccm, the working pressure of 1.5 Pa, removing the baffle plate, sputtering on the substrate for 20 min, and maintaining the substrate holder to rotate at a constant speed in the sputtering process. And after the sputtering is finished, simultaneously closing the oxygen flow, the argon flow and the sputtering current. After the sputtering furnace is stable, the background vacuum reaches 1.5 multiplied by 10 -4 After Pa, the substrate is heated to 300 ℃, oxygen is added to keep the pressure of the chamber at 1.5 Pa, the film is annealed for 20 min by oxygen, then the film is naturally cooled, and the sample can be taken out after the temperature is reduced to normal room temperature. The obtained product has a thickness of about 118 and nm, a sheet resistance of K Ω/≡and a resistance temperature at 25deg.CSn with a degree coefficient of-3.8%/K 0.25 Zn 0.75 And (3) an O film. Finally, TO with the thickness of 20nm is deposited on the prepared film 2 And a passivation layer made of materials.
Fig. 2 shows the sheet resistance-temperature curve (sample R2 in the figure, where the curves at the time of temperature increase and temperature decrease overlap) of the thermosensitive film obtained in the present embodiment. Therefore, the resistance changes exponentially with temperature, and no thermal hysteresis loop is found in the heating and cooling processes.
The foregoing embodiments are merely illustrative of the technical concept and features of the present invention, and are intended to enable those skilled in the art to understand the present invention and to implement the same, not to limit the scope of the present invention. All equivalent changes or modifications made according to the spirit of the present invention should be included in the scope of the present invention.
Claims (8)
1. A thermosensitive film for uncooled infrared microbolometer is characterized by comprising Sn x Zn 1-x O material, wherein the value range of x is 0.15-0.35; at 25 ℃, the sheet resistance of the thermosensitive film is 1-200 KΩ/≡and the temperature coefficient of resistance is-1.8 to-3.8%/K; the preparation method comprises the following steps:
s1: placing the dry and clean substrate into a DC reaction magnetron sputtering furnace, and vacuumizing to 1×10 -4 Pa, heating the substrate to 100-300 ℃;
s2: using a baffle plate to block the substrate, and pre-sputtering a metal zinc target and a tin target;
s3: removing the baffle plate, controlling the sputtering power of the zinc target to be 80-120W, controlling the sputtering power of the tin target to be 10-30W, and depositing Sn with the thickness of 50-350 nm on the substrate by reactive sputtering x Zn 1-x An O film; the flow rate ratio of oxygen to argon during sputtering is 10-30%;
s4: simultaneously closing the oxygen flow, the argon flow and the sputtering current;
s5: after the DC reaction magnetron sputtering furnace is stabilized, the background vacuum is up to 1.0 multiplied by 10 -4 ~1.5×10 -4 After Pa, for the Sn x Zn 1-x O film feedingCarrying out annealing treatment;
s6: annealing to obtain Sn x Zn 1-x And (3) cooling the O film to room temperature in high vacuum or oxygen atmosphere to obtain the thermosensitive film, and taking out for later use.
2. The uncooled infrared microbolometer thermosensitive film according to claim 1, wherein a passivation film of insulating material is further deposited on the thermosensitive film after S6.
3. The thermosensitive film for uncooled infrared microbolometer according to claim 2, wherein the passivation film has a thickness of 10 to 50 nm.
4. The uncooled infrared microbolometer thermosensitive film of claim 2, wherein the insulating material is SiC, si 3 N 4 、SiO 2 TiN or TiO 2 A dielectric film.
5. The uncooled infrared microbolometer thermosensitive film according to any one of claims 1 to 4, wherein in S2, the flow rate of argon gas is 50 to 100 sccm, the sputtering current is 0.1 to 0.6A, and the pre-sputtering time is 10 to 20 min.
6. The uncooled infrared microbolometer thermosensitive film according to any one of claims 1 to 4, wherein in S3, the working pressure at the time of sputtering is 1.0 to 2.5 Pa, the sputtering temperature is 100 to 300 ℃, the sputtering current is 0.1 to 0.6A, and the sputtering time is 10 to 50 min.
7. The uncooled infrared microbolometer thermosensitive film according to any one of claims 1 to 4, wherein in S5, the annealing atmosphere at the time of annealing treatment is 1.0×10 under vacuum -4 ~1.5×10 -4 And under Pa or oxygen atmosphere, the annealing temperature is 200-400 ℃ and the heat preservation time is 20-60 min, wherein the temperature is 0.1-1.5 Pa.
8. The uncooled infrared microbolometer thermosensitive film of claim 7, wherein in S6, the high vacuum is 1.0 x 10 -4 ~1.5×10 -4 Pa, the oxygen atmosphere is 0.1-1.5 Pa.
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| CN114107924A (en) | 2022-03-01 |
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Application publication date: 20220301 Assignee: Huai'an Anming Technology Co.,Ltd. Assignor: HUAIYIN INSTITUTE OF TECHNOLOGY Contract record no.: X2023980037658 Denomination of invention: A Thermosensitive Thin Film for Uncooled Infrared Microbolometer Granted publication date: 20230620 License type: Common License Record date: 20230707 |