CN101774530B - Microbolometer and preparation method thereof - Google Patents
Microbolometer and preparation method thereof Download PDFInfo
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- CN101774530B CN101774530B CN2010101049411A CN201010104941A CN101774530B CN 101774530 B CN101774530 B CN 101774530B CN 2010101049411 A CN2010101049411 A CN 2010101049411A CN 201010104941 A CN201010104941 A CN 201010104941A CN 101774530 B CN101774530 B CN 101774530B
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Abstract
The invention relates to a microbolometer, which comprises a microbridge structure, wherein a thermosensitive resistance material and an infrared absorption material layer in the microbridge structure are of a carbon nanometer tube-amorphous silicon composite film, the carbon nano tube-amorphous silicon composite film is formed by compounding an one-dimension carbon nano-tube and a two-dimensional amorphous silicon film, and the microbridge structure is of a three-layer sandwich structure; the most bottom layer is of a amorphous silicon nitride film which is used as a supporting and insulation material of the microbridge; the intermediate layer is of one layer or multiple layers of carbon nano-tube-amorphous composite film, the stress is opposite to the nature of the bottom layer silicon nitride film, and the carbon nano-tube-amorphous composite film is used as the thermosensitive layer and the infrared absorption layer of the microbolometer; and the surface layer is of an amorphous silicon nitride film, the stress of the amorphous silicon nitride film is opposite to the nature of the intermediate carbon nano-tube-amorphous composite film, and the amorphous silicon nitride film is used as a passivation layer of the inforared sensing film and a control layer of the stress. The microbolometer and the preparation method can overcome the weaknesses of the prior art, improves the working performance of the part, reduces the cost of the raw material and are applicable to the industrialized mass production.
Description
Technical field
The present invention relates to the uncooled ir technical field of detection, be specifically related to a kind of micro-metering bolometer and preparation method thereof.
Background technology
Infrared Detectors is converted into the detectable signal of telecommunication to sightless infrared emanation, realizes the observation of affairs to external world.Infrared Detectors is divided into two types of quantum detector and thermal detectors.Thermal detector is claimed the non-refrigeration type Infrared Detectors again, can at room temperature work, and has advantages such as the high and price of good stability, integrated level is low, has wide practical use in field such as military, commercial and civilian.Non-refrigerated infrared detector mainly comprises three types of pyroelectricity, thermocouple, thermistors etc.; Wherein, Based on micro-metering bolometer (Microbolometer) focus planardetector of thermistor, be the very swift and violent a kind of non-refrigerated infrared detector of developed recently (referring to Leonard P.Chen, " Advanced FPAs for Multiple Applications " Proc.SPIE; 4721,1-15 (2002) document).The infrared detective process of micro-metering bolometer is mainly accomplished through the micro-bridge structure that suspends, so the suspension microbridge is to influence the key factor that device is made success or failure and performance height.Micro-metering bolometer has special requirement to constructing the thermistor material of the thin-film material of its suspension microbridge, especially core, is embodied in: associated materials should have suitable electricity, optics, reach mechanical property etc.
There is multiple material can be used as the thermistor material of micro-metering bolometer.Wherein, vanadium oxide film has very good electricity and optical property, and the integrated level of material preparation is high, is the most frequently used high-performance non-refrigerated infrared detector thermistor material.The U.S. Pat P 6489613 that the people such as the Mori Toru of NEC Corporation that authorized on December 3rd, 2002 declare; A kind of preparation method who is used for the vanadium oxide film of micro-metering bolometer has just been described; This invention utilizes collosol and gel (Sol-gel) technology; Mix specific metal impurities, make the electric property of vanadium oxide meet the requirement of device.Document H.Jerominek, F.Picard, et al., " Micromachined, uncooled, VO
2-based, IR bolometer arrays ", Proc.SPIE, 2746,60-71 (1996) has then described a kind of micro-metering bolometer micro-bridge structure based on vanadium oxide thermistor film.Yet, because the electronic structure of vanadium atom is 3d
34s
2, 4s wherein and 3d track all can lose part or all of electronics, so the vanadium oxide film of conventional method preparation contains the shortcoming that itself can't overcome: i.e. the valence state of V element complicacy, film chemical stability of structure difference etc. in the vanadium oxide film.For example; When adopting magnetron sputtering to prepare vanadium oxide film; V element wherein generally comprises 0 ,+2 ,+3 ,+4 ,+multiple valence states such as 5 (referring to Xiaomei.Wang, Xiangdong.Xu, et al.; " Controlling the growth of VOxfilms for various optoelectronic applications "; Proceedings of the 2009 16th IEEEInternational Symposium on the Physical and Failure Analysis of Integrated Circuits, IPFA, p 572-576 (2009) document).Because the composition of V element is complicated, preparation technology's minor variations all can produce bigger influence to the chemical composition of vanadium oxide film, thereby makes the performance generation significant changes such as electricity, optics, mechanics of film, and then has influence on the performance of device.So based on the major defect of the micro-metering bolometer of vanadium oxide film be: preparation technology's difficulty of vanadium oxide film is big, the repeatability of product and poor stability etc.
Amorphous silicon membrane is the thermistor material that another kind is usually used in micro-metering bolometer, has higher temperature-coefficient of electrical resistance (TCR).The U.S. Pat P 6777681B1 that the people such as Raytheon company's T homas R.Schimert that authorize in the U.S. Pat P 5288649 that the Wiiliam F.Keenan of Texas Instruments company that authorized on February 22nd, 1994 declares and on August 17th, 2004 declare has described two kinds of non-refrigerated infrared detectors based on the non-crystalline silicon thermistor thin film respectively.Yet, because the resistance of intrinsic amorphous silicon film is big, noise is high.So, of these two patents, need mode through mixing, for example phosphorus doping or boron doping etc., the resistance of reduction amorphous silicon membrane reaches the requirement of micro-metering bolometer.In order to improve carrier density effectively, the electronic structure and the Si atom that mix foreign atom have bigger difference, possibly be (doping of P type) atoms of electron rich (doping of N type) or short of electricity.In addition, the doping process also needs certain high temperature to handle, to disperse foreign atom, to form homogeneous film.But; These impurity add and high-temperature process tends to the chemical constitution of amorphous silicon film is produced bigger influence; For example have influence on Si in the amorphous silicon film dangling bonds, Si-Si key and H element content and become key mode etc., thereby have influence on the physical property of amorphous silicon film.So traditional doping process all has negative effect to the chemical constitution and the physical property of amorphous silicon film.
On the other hand, CNT is a kind of very important monodimension nanometer material.From 1991, and since the Ijima of the Japan discovery CNT (referring to Sumio Iijima, " Helical microtubules of graphiticcarbon "; Nature; 354,56, (1991) document); Increasing research shows that this special monodimension nanometer material has physics and the chemical property and the wide application prospect of many uniquenesses.At first, CNT has very excellent chemical stability, in vacuum condition; CNT is under 1200 ℃ high temperature; It is stable that its chemical constitution can also keep, and in atmospheric environment, CNT also is being chemically stable below 650 ℃; Obviously, the chemical stability of CNT is higher than vanadium oxide and amorphous silicon membrane far away.In addition, CNT also has good electricity and optical property, and for example, the temperature-coefficient of electrical resistance of bibliographical information CNT (TCR) can reach 0.3～2.5%/K, and under the specified conditions, its absorption coefficient of light can reach 10
4～5Cm
-1(referring to M.E.Itkis, F.Borondics, A.Yu.R.C.Haddon; " Bolometric InfraredPhotoresponse of Suspended Single-Walled Carbon Nanotube Films "; Science, 312,413-416 (2006) document).So CNT is a kind of thermistor material with potential using value, can overcome the shortcoming of traditional thermal film chemical poor stabilities such as vanadium oxide, non-crystalline silicon.
At present, people have carried out multiple trial in the carbon nano tube device application.The European patent EP 1944589A1 that the people such as the Barrettt E.Cole of Honeywell company that authorized on July 16th, 2008 declare has just described a kind of sensor based on CNT.The carbon nano-tube bundle that this invention is upwards erect through catalyst inducement, growth; Improve the absorbent properties of material to infrared light; Thereby system temperature under the infrared light radiation effects is risen, and corresponding platinum (Pt) sensor of temperature variations below CNT measured.In this invention, the CNT of setting mainly plays a part infrared absorbing material.
The Chinese patent ZL 02114434.6 that the people such as Liu Junhua that authorized on January 26th, 2005 declare; A kind of carbon nano tube film micromechanical infrared detector has then been described; This invention also is to utilize the absorbing material of CNT as infra-red radiation; The warpage through measuring the micromechanical resonator cause thus or the situation of change of its natural mode shape realize the detection to the radiation light intensity.The Chinese patent ZL 200320109976.X that the people such as Liu Junhua that authorized on May 4th, 2005 declare; A kind of carbon nano-tube film pressure drag heat-sensitive type Infrared Detectors has been described; This invention utilizes CNT as infrared Absorption and thermo-sensitive material equally, when micromechanics receives light radiation, the drift of warpage or resonant frequency will occur; Thereby the pressure drag factor of the CNT that is bonded on the micromechanics is changed; Utilize the piezoresistive effect of CNT, the drift through CNT change in resistance frequency comes sense temperature to distribute and then the measuring radiation light intensity, and this invention has solved problems such as pyroelectric detector sensitivity is low, cost height.Regrettably, CNT, especially accumbency are at the CNT of substrate surface; Its INFRARED ABSORPTION performance not undesirable in fact (referring to Z.Wu, Z.Chen, et al.; " Transparent, Conductive Carbon Nanotube Films ", Science; 305,1273-1276 (2004) .), the deficiency of this respect will badly influence the performance of related device.
Research recently shows, builds carbon nano-tube film in the structure that suspends, and can improve the light sensitive characteristic of CNT significantly; Under given conditions, can satisfy infrared acquisition requirement (referring to M.E.Itkis, F.Borondics; A.Yu.R.C.Haddon, " Bolometric Infrared Photoresponse of SuspendedSingle-Walled Carbon Nanotube Films ", Science; 312,413-416 (2006) document).Yet; There is a significantly deficiency in this structure based on simple CNT, that is: because the pi-electron of CNT has stronger electric conductivity, when directly adopting simple carbon nano-tube film as thermo-sensitive material; The resistance of film is less; So, must be under the cryogenic conditions of liquid helium, just can detect the faint variation of the CNT resistance that infra-red radiation causes.This explanation can not be satisfied the requirement of non-refrigerated infrared detector merely based on the micro-bridge structure of CNT.Traditionally, the method that improves CNT resistance is, is dispersed in CNT in the middle of some high molecular systems; Like Merlon or polystyrene etc.; Formation CNT-macromolecule laminated film (referring to A.E.Aliev, " Bolometric detector on the basis of single-wall carbonnanotube/polymer composite ", Infrared Physics & Technology; 51,541-545 (2008) document).Though this CNT-macromolecule laminated film can satisfy the requirement of micro-metering bolometer electric property,, still there is the another one weak point in it, that is: at 1～10 mu m waveband; CNT is to the absorbability of infrared light more weak (absorption coefficient is little), absorptivity only be about 10% (referring to Z.Wu, Z.Chen; Et al., " Transparent, Conductive Carbon Nanotube Films "; Science, 305,1273-1276 (2004) .).Common high molecular materials helps little to the optical property of CNT.So, common CNT and high molecular composite, inaccessible Infrared Detectors is to the infrared Absorption performance demands.
In a word, the electric conductivity of amorphous silicon membrane and chemical stability exist obviously not enough, need to improve.The part and CNT comes with some shortcomings at aspects such as electricity and optical properties equally; So also suitable simple CNT or the common CNT-macromolecule laminated film of adopting is as infrared Absorption and thermistor material, directly be applied in the non-refrigerated infrared detector.
Summary of the invention
Problem to be solved by this invention is: how a kind of micro-metering bolometer and preparation method thereof is provided; This micro-metering bolometer and preparation method thereof can overcome existing defective in the prior art; Improved working performance of devices, reduced cost of material, suitable large-scale industrialized production.
Technical problem proposed by the invention is to solve like this: a kind of micro-metering bolometer is provided; Comprise micro-bridge structure; It is characterized in that; Thermistor material in this micro-bridge structure and infrared absorbing material layer are the carbon nano-tube-amorphous composite membrane, and this carbon nano-tube-amorphous composite membrane is to be composited by one dimension CNT and bidimensional amorphous silicon membrane.
According to micro-metering bolometer provided by the present invention, it is characterized in that said micro-bridge structure is the three-layer sandwich structure: the bottom is one deck amorphous silicon nitride films, as the support and the insulating materials of microbridge; The intermediate layer is one deck or multilayer carbon nanotube-non-crystalline silicon composite membrane, and the incompatibility of its stress and underlying silicon nitride film is as the thermally sensitive layer and the infrared Absorption layer of micro-metering bolometer; The top layer is one deck amorphous silicon nitride films, and the incompatibility of its stress and middle carbon nanotube-non-crystalline silicon composite membrane is as the passivation layer of infrared-sensitive film and the regulation and control layer of stress.
The preparation method of above-mentioned carbon nano-tube-amorphous composite membrane is characterized in that, may further comprise the steps:
1. clean substrate, use N
2After air-blowing is done, subsequent use;
2. be placed on the good CNT of prepared beforehand in the middle of the beaker, mix with organic solvent, ultrasonic dispersion then, is transferred to the surface of the substrate after the cleaning to dispersion liquid, makes solvent evaporates, forms netted, interconnected carbon nano-tube film;
3. put into the substrate that 2. obtains in steps the reactor of vacuum pumping, use SiH
4As reacting gas, utilize reactor growth one deck amorphous silicon film, the non-crystalline silicon of being grown is dispersed in the middle of the gap of surface and tube and tube of CNT, and annealing forms the carbon nano-tube-amorphous structure of composite membrane;
4. after being cooled to room temperature, from reactor, take out;
5. as required, repeat CNT dispersion, amorphous silicon deposition and annealing steps successively, form carbon nano-tube-amorphous MULTILAYER COMPOSITE membrane structure.
Preparation method according to carbon nano-tube-amorphous composite membrane provided by the present invention; It is characterized in that; Step 2. in; Process for dispersing is wherein a kind of of spin coating (Spin Coating) or electrophoresis, printing transplanting etc., and when adopting the method for spin coating (Spin coating), used dispersion liquid is ethanol or isopropyl alcohol or other organic solvent.
Preparation method according to carbon nano-tube-amorphous composite membrane provided by the present invention; It is characterized in that; Step 2. in resulting CNT accumbency on the surface of substrate, be netted interconnect architecture; CNT is single wall or multi-walled carbon nano-tubes, and the diameter of CNT is 1～50nm, and the best is 2nm, 5nm, 10nm, 15nm, 20nm, 25nm, 30nm etc.; The length of CNT is 50～30000nm, and the best is 500nm, 800nm, 1000nm, 1200nm, 1500nm etc.
The preparation method of above-mentioned carbon nano-tube-amorphous composite membrane is characterized in that, may further comprise the steps:
1. clean substrate, use N
2After air-blowing is done, subsequent use;
2. utilize a kind of in chemical gas-phase deposition system or arc discharge system or the laser deposition system reactor, induce through metallic catalyst, directly reaction grows into netted, interconnected carbon nano-tube film on the surface of clean substrate;
3. put into the substrate that 2. obtains in steps the reactor of vacuum pumping, use SiH
4As reacting gas, utilize reactor growth one deck amorphous silicon film, the non-crystalline silicon of being grown is dispersed in the middle of the gap of surface and tube and tube of CNT, and annealing forms the carbon nano-tube-amorphous structure of composite membrane;
4. after being cooled to room temperature, from reactor, take out;
5. as required, repeat carbon nano tube growth, amorphous silicon deposition and annealing steps successively, form carbon nano-tube-amorphous MULTILAYER COMPOSITE membrane structure.
Preparation method according to carbon nano-tube-amorphous composite membrane provided by the present invention is characterized in that, step 2. in, when adopting chemical gas-phase deposition system, adopt methane (CH as the reactor of the one dimension CNT in the middle of the growing mixed film of reaction
4) or ethene (C
2H
4), acetylene (C
2H
2) and benzene (C
6H
6) wait one or more organic mixtures in the organic matter as reacting gas; The mixture that adopts one or more metals in the transition metal such as Fe, Co and Ni simultaneously is as catalyst; The induced carbon nanotube is grown directly upon the surface of substrate; The growth temperature of CNT is 300～1100 ℃, and the best is 450 ℃, 500 ℃, 550 ℃, 600 ℃, 650 ℃, 700 ℃ etc.
Preparation method according to carbon nano-tube-amorphous composite membrane provided by the present invention; It is characterized in that; Step 2. in resulting CNT accumbency on the surface of substrate, be netted interconnect architecture; CNT is single wall or multi-walled carbon nano-tubes, and the diameter of CNT is 1～50nm, and the best is 2nm, 5nm, 10nm, 15nm, 20nm, 25nm, 30nm etc.; The length of CNT is 50～30000nm, and the best is 500nm, 800nm, 1000nm, 1200nm, 1500nm etc.
A kind of preparation method of micro-metering bolometer is characterized in that, may further comprise the steps:
1. clean the monocrystalline silicon piece substrate that contains integrated circuit (ROIC), utilize reactor deposition one deck amorphous silica film as passivation layer; The thickness of silica coating is 300～1500nm, and the best is 600nm, 700nm, 800nm, 900nm, 1000nm etc.;
2. on the surface of silicon dioxide passivation layer, utilize reactor to deposit the metallic aluminium that a layer thickness is 100～1000nm, the best is 150nm, 200nm, 250nm, 300nm, 350nm, 400nm, 450nm, 500nm etc., as the reflecting layer of microbridge;
3. carve the pier pattern of microactuator suspension bridge in the surface light of above-mentioned metallic aluminium, this metal aluminium lamination of etching to following silicon dioxide passivation layer forms microbridge bridge pier hole and metallic aluminium isolated island;
4. on the surface of above-mentioned metallic aluminium isolated island, spin coating one layer thickness is the photosensitive polyimide film of 1～4 μ m, and the best is 1.5 μ m, 2 μ m, 2.5 μ m etc.;
5. Kapton is carried out photoetching treatment, form the bridge pier hole of Kapton isolated island and suspension microbridge, carry out imidization then and handle;
6. on the surface in Kapton isolated island and bridge pier hole, utilize reactor deposition one deck amorphous silicon nitride film, thickness is 10～1500nm, as the support and the insulating materials of microbridge; Then, after cleaning dries up, clean substrate, it is subsequent use to dry up the back; Be placed on the good CNT of prepared beforehand in the middle of the beaker, mix ultrasonic dispersion with organic solvent; Then, transfer to the surface of the substrate after the cleaning to dispersion liquid, make solvent evaporates; Form netted, interconnected carbon nano-tube film, put into the reactor of vacuum pumping to the substrate that obtains, use SiH
4As reacting gas, utilize reactor growth one deck amorphous silicon film, the non-crystalline silicon of being grown is dispersed in the middle of the gap of surface and tube and tube of CNT; Annealing forms the carbon nano-tube-amorphous structure of composite membrane, be cooled to room temperature after; From reactor, take out; As required, repeat CNT dispersion, amorphous silicon deposition and annealing steps successively, form carbon nano-tube-amorphous MULTILAYER COMPOSITE membrane structure.
7. utilize reactor to deposit the metal that a layer thickness is 10～500nm, graphical, as the electrode of device;
8. last; Utilize reactor; On the surface of metal electrode and carbon nano-tube-amorphous composite membrane, deposition covers one deck amorphous silicon nitride film, and thickness is 10～1500nm; Carbon nano-tube-amorphous composite membrane in the middle of its stress and the microbridge opposite is as the passivation layer of electrode and photaesthesia film and the regulation and control layer of stresses of parts;
9. the surface light at above-mentioned laminated film carves microactuator suspension bridge construction figure, and this THIN COMPOSITE rete of etching forms bridge floor, bridge leg and the pier pattern of suspension microbridge to polyimide layer;
10. adopt oxygen plasma to remove the Kapton of bridge floor and bridge leg figure bottom, form cavity, constitute micro-metering bolometer.
A kind of preparation method of micro-metering bolometer is characterized in that, may further comprise the steps:
1. clean the monocrystalline silicon piece substrate that contains integrated circuit (ROIC), utilize reactor deposition one deck amorphous silica film as passivation layer; The thickness of silica coating is 300～1500nm, and the best is 600nm, 700nm, 800nm, 900nm, 1000nm etc.;
2. on the surface of silicon dioxide passivation layer, utilize reactor to deposit the metallic aluminium that a layer thickness is 100～1000nm, the best is 150nm, 200nm, 250nm, 300nm, 350nm, 400nm, 450nm, 500nm etc., as the reflecting layer of microbridge;
3. carve the pier pattern of microactuator suspension bridge in the surface light of above-mentioned metallic aluminium, this metal aluminium lamination of etching to following silicon dioxide passivation layer forms microbridge bridge pier hole and metallic aluminium isolated island;
4. on the surface of above-mentioned metallic aluminium isolated island, spin coating one layer thickness is the photosensitive polyimide film of 1～4 μ m, and the best is 1.5 μ m, 2 μ m, 2.5 μ m etc.;
5. Kapton is carried out photoetching treatment, form the bridge pier hole of Kapton isolated island and suspension microbridge, carry out imidization then and handle;
6. on the surface in Kapton isolated island and bridge pier hole, utilize reactor deposition one deck amorphous silicon nitride film, thickness is 10～1500nm, as the support and the insulating materials of microbridge, then, cleans and uses N
2After air-blowing is done; Utilize a kind of in chemical gas-phase deposition system or arc discharge system or the laser deposition system reactor; Induce through metallic catalyst; Direct reaction grows into netted, interconnected carbon nano-tube film on the surface of clean substrate, puts into the reactor of vacuum pumping to the substrate that obtains, and uses SiH
4As reacting gas, utilize reactor growth one deck amorphous silicon film, the non-crystalline silicon of being grown is dispersed in the middle of the gap of surface and tube and tube of CNT; Annealing forms the carbon nano-tube-amorphous structure of composite membrane, be cooled to room temperature after; From reactor, take out; As required, repeat carbon nano tube growth, amorphous silicon deposition and annealing steps successively, form carbon nano-tube-amorphous MULTILAYER COMPOSITE membrane structure;
7. utilize reactor to deposit the metal that a layer thickness is 10～500nm, graphical, as the electrode of device;
8. last; Utilize reactor; On the surface of metal electrode and carbon nano-tube-amorphous composite membrane, deposition covers one deck amorphous silicon nitride film, and thickness is 10～1500nm; Carbon nano-tube-amorphous composite membrane in the middle of its stress and the microbridge opposite is as the passivation layer of electrode and photaesthesia film and the regulation and control layer of stresses of parts;
9. the surface light at above-mentioned laminated film carves microactuator suspension bridge construction figure, and this THIN COMPOSITE rete of etching forms bridge floor, bridge leg and the pier pattern of suspension microbridge to polyimide layer;
10. adopt oxygen plasma to remove the Kapton of bridge floor and bridge leg figure bottom, form cavity, constitute micro-metering bolometer.
Preparation method according to micro-metering bolometer provided by the present invention; It is characterized in that, the bottom of micro-metering bolometer microbridge, and the reactor of top layer silicon nitride film be wherein a kind of such as plasma enhanced chemical vapor deposition (PECVD) system or low-pressure chemical vapor deposition (LPCVD) system, high vacuum chemical vapour deposition (UHVCVD) system, electron beam evaporation system, laser deposition system, magnetic control sputtering system.The bottom of said micro-metering bolometer microbridge, and the thickness of top layer silicon nitride film be 10～1500nm, the best is 50nm, 100nm, 150nm, 200nm, 250nm, 300nm, 350nm, 400nm, 450nm, 500nm etc.The intermediate layer of said micro-metering bolometer microbridge is the carbon nano-tube-amorphous composite membrane; The thickness of one deck carbon nano-tube-amorphous composite membrane is 10～1500nm; The best is 50nm, 100nm, 150nm, 200nm, 250nm, 300nm, 350nm, 400nm, 450nm, 500nm etc., and the electrode of said micro-metering bolometer is wherein a kind of of metallic aluminium or titanium alloy, nichrome etc.When adopting metallic aluminium as the electrode of micro-metering bolometer, the thickness of electrode is 10～500nm, and the best is 50nm, 100nm, 150nm, 200nm, 250nm, 300nm, 350nm, 400nm etc.
The present invention considers the specific (special) requirements of micro-metering bolometer micro-bridge structure; To existing thermistor thin films such as vanadium oxide, non-crystalline silicon are in the deficiency of aspects such as material property and preparation method in the device, the present invention proposes a kind of method that adopts the composite of one dimension CNT and bidimensional amorphous silicon film as the thermistor material and the infrared absorbing material of micro-metering bolometer simultaneously.Utilize CNT excellent chemical stability and electric conductivity on the one hand; Utilize in the CNT Si atom in the C atom and non-crystalline silicon to have the characteristics of identical electronic structure (C and Si are congeners) simultaneously; Improve the low shortcoming with poor chemical stability of traditional non-crystalline silicon thermistor thin film electric conductivity effectively, the negative effect of having avoided traditional doping process that amorphous silicon film is produced simultaneously.On the other hand, utilize non-crystalline silicon high resistance, with and good infrared Absorption performance, remedy the deficiency of CNT at aspects such as electricity and optical properties, improve the combination property of device.In addition; The present invention proposes to adopt material character close but silicon nitride film and carbon nano-tube-amorphous composite membrane that stress is opposite are formed a kind of three-layer sandwich structure; Be used to make up the micro-bridge structure of micro-metering bolometer; Can improve the membrane stress gradient of originally precipitous and monotone variation, reduce the residual stress of microbridge effectively, preferably performances such as the mechanics of control device and optics.On this basis, through regulating the ratio of CNT and non-crystalline silicon, can also be more prone to, trim membrane stress more exactly, satisfy the special requirement of micro-bridge structure.Utilize the sensitive material of the micro-metering bolometer that this composite by special monodimension nanometer material and bidimensional film makes, improved working performance of devices, reduced the raw material manufacturing cost, suitable large-scale industrialized production.
Description of drawings
Fig. 1 is the plane of carbon nano-tube-amorphous structure of composite membrane of the present invention;
Fig. 2 is the sectional view of the carbon nano-tube-amorphous structure of composite membrane of individual layer of the present invention;
Fig. 3 is the sectional view of the carbon nano-tube-amorphous structure of composite membrane of multilayer of the present invention;
Fig. 4 is the sectional view of underlying silicon nitride film of the present invention, intermediate layer carbon nano-tube-amorphous composite membrane, top layer silicon nitride film three-layer sandwich structure;
Fig. 5 is the sectional view based on the micro-bridge structure of the micro-metering bolometer of carbon nano-tube-amorphous composite membrane that the present invention proposes;
Fig. 6 is the plane based on the micro-bridge structure of the micro-metering bolometer of carbon nano-tube-amorphous composite membrane that the present invention proposes;
Fig. 7 is the stereogram based on the micro-bridge structure of the micro-metering bolometer of carbon nano-tube-amorphous composite membrane that the present invention proposes.
Wherein, 1, silicon substrate, 2, silicon dioxide passivation layer, 3, metallic aluminium reflecting layer; 4, Kapton, 5, composite three-layer sandwich structure, 6, metal electrode, 7, the suspension microbridge; 8, micro-metering bolometer, 510, the underlying silicon nitride film, 520, the carbon nano-tube-amorphous composite membrane, 521, the CNT in the middle of the carbon nano-tube-amorphous composite membrane; 522, the non-crystalline silicon in the middle of the carbon nano-tube-amorphous composite membrane, 530, the top layer silicon nitride film, 710, the microbridge bridge floor; 720, microbridge bridge leg, 730, the microbridge bridge pier, 740, optical resonator.
The specific embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is further described:
I. the preparation method of one dimension CNT and bidimensional amorphous silicon film composite
Guiding theory of the present invention is in the carbon nano-tube-amorphous structure of composite membrane; Utilize CNT and non-crystalline silicon superior electrical and optical property separately; Prepare the better laminated film of combination property (as shown in Figure 1); As the infrared Absorption and the thermistor material (shown in Fig. 5 and 6) of micro-metering bolometer, improve device performance.Preparation carbon nano-tube-amorphous composite membrane embodiment of the present invention is following: 1. select the substrate 1 of silicon wafer as film growth for use; Earlier with Piranha solution-treated and washed with de-ionized water; Soak with rare hydrofluoric acid solution then; After drying up with nitrogen, put into plasma and strengthen (PECVD) system, vacuumize; 2. on the surface of silicon substrate 1, use SiH
4And NH
3As reacting gas, utilizing PECVD is the amorphous silicon nitride underlying membrane 510 of 10～1500nm at 300 ℃ of layer thicknesses of growing down; 3. on the surface of silicon nitride underlying membrane 510, at first be placed on the good CNT of prepared beforehand in the middle of the beaker, mix ultrasonic dispersion with organic solvent; Then, transfer to the surface of clean substrate to dispersion liquid, make solvent evaporates, form netted, interconnected carbon nano-tube film 521; 4. the substrate 1 that is dispersed with CNT 521 to the surface is put into the reactor of vacuum pumping, uses SiH
4As reacting gas, utilize PECVD 200 ℃ down growth one layer thicknesses be the amorphous silicon film 522 of 10～1500nm, non-crystalline silicon 522 covers in the middle of the gap of surface and tube and tube of CNT 521, annealing forms carbon nano-tube-amorphous composite membrane 520; 5. as required, can repeat steps such as CNT 521 dispersions, non-crystalline silicon 522 depositions and annealing successively, form carbon nano-tube-amorphous MULTILAYER COMPOSITE membrane structure 520; 6. on the surface of carbon nano-tube-amorphous composite membrane 520, use SiH
4And NH
3As reacting gas, utilize PECVD 300 ℃ down growth one layer thicknesses be the amorphous silicon nitride top layer film 530 of 10～1500nm, as the passivation layer of carbon nano-tube-amorphous composite membrane 520, and stress regulation and control layer; 7. after sample is cooled to room temperature, take out sample from the PECVD system.In the middle of carbon nano-tube-amorphous composite membrane 520, the introducing of CNT 521, electric property and steady chemical structure property that makes non-crystalline silicon 522 etc. effectively improved, and meets the requirement of non-refrigerated infrared detector.
The concrete technology of above-mentioned preparation embodiment comprises: the preparation of (1) film growth substrate: select for use 4 inches Si (100) silicon chip as growth for Thin Film substrate 1; Before the experiment; Earlier with the Piranha solution (concentrated sulfuric acid: hydrogen peroxide=7: 3 (volume ratio)) handled 10 minutes down in 80 ℃; Rinsing well with deionized water, is to soak 90 seconds under the room temperature in 1.5: 10 hydrofluoric acid (HF) solution in concentration then, dries up silicon chip with high pure nitrogen at last; Transfer to immediately in the prechamber of PECVD system, vacuumize; (2) growth of silicon nitride underlying membrane 510: when the pressure of prechamber reaches 4 * 10
-2Behind the Torr, pass to main vacuum chamber to Si (100) substrate 1, substrate is heated to 300 ℃, behind the temperature stabilization, opens radio-frequency power supply, feeds silane (SiH
4) and ammonia (NH
3) reaction gas, the representative condition of deposition underlying silicon nitride film is: rf frequency is 13.56MHz; Power is 600W; NH
3/ SiH
4Flow-rate ratio is 200/250sccm; Underlayer temperature is 300 ℃; The about 0.8nm/s of sedimentation rate, sedimentation time are 240 seconds; The pressure of main vacuum chamber is 0.6Torr in the deposition; The thickness of silicon nitride underlying membrane is 200nm; (3) dispersion of CNT 521: be placed on the good CNT of prepared beforehand in the middle of the beaker, mix ultrasonic dispersion with alcohol solvent mutually; Then,, transfer to the surface of clean substrate to dispersion liquid, make the alcohol solvent volatilization, form netted, interconnected carbon nano-tube film 521 through spin coating (Spin Coating) method; (4) deposition of non-crystalline silicon 522: use SiH
4As reacting gas, as carrier gas, utilizing PECVD is the amorphous silicon film 522 of 10～1500nm at 200 ℃ of layer thicknesses of growing down with argon gas (Ar).The representative condition of deposition of amorphous silicon is: rf frequency is 13.56MHz; Power is 600W; SiH
4/ Ar flow-rate ratio is 100/400sccm; Underlayer temperature is 200 ℃; The about 1.5nm/s of sedimentation rate; Deposition growing 65 seconds; The pressure of main vacuum chamber is 0.6Torr in the deposition; The thickness of amorphous silicon film is about 100nm; Annealing in process forms carbon nano-tube-amorphous composite membrane 520; (5) as required, can repeat steps such as CNT 521 dispersions, non-crystalline silicon 522 depositions and annealing successively, form carbon nano-tube-amorphous MULTILAYER COMPOSITE membrane structure 520; (6) growth of silicon nitride top layer film 530:, use SiH on the surface of carbon nano-tube-amorphous composite membrane 520
4And NH
3As reacting gas, utilizing PECVD is the amorphous silicon nitride top layer film 530 of 10～1500nm at 300 ℃ of layer thicknesses of growing down, the incompatibility of the stress of top layer film 530 and carbon nano-tube-amorphous composite membrane; The representative condition of PECVD deposited top layer silicon nitride film is: rf frequency is 13.56MHz; Power is 600W; NH
3/ SiH
4Flow-rate ratio is 200/250sccm; Underlayer temperature is 300 ℃; The about 0.8nm/s of sedimentation rate, sedimentation time are 240 seconds; The pressure of main vacuum chamber is 0.6Torr in the deposition; The thickness of silicon nitride underlying membrane is 200nm; (7) after (6) step; Sample is cool to room temperature in main vacuum chamber; Then, from vacuum chamber, take out sample, be the three-layer sandwich structure 5 that contains the carbon nano-tube-amorphous composite membrane that the present invention proposes; Wherein carbon nano-tube-amorphous composite membrane 520 is in the intermediate layer, and 530 and following 510 respectively is one deck amorphous silicon nitride film above it.
Silicon chip of the present invention 1 cleans not to be only limited to and adopts Piranha and hydrofluoric acid solution, also comprises the cleaning that other solution that employing is known in the industry and method are carried out.The film growth substrate does not receive special restriction yet, except Si (100) silicon chip, also comprises the monocrystalline silicon piece of other crystal orientation and size or the substrate of other material (different according to the substrate kind, as to adopt suitable cleaning).CNT 521 does not receive special restriction yet, except through spin coating technique, is dispersed in the good CNT of prepared beforehand outside the substrate surface, and the CNT in the middle of the composite can also utilize chemical gas-phase deposition system, adopts methane (CH
4) or ethene (C
2H
4), acetylene (C
2H
2), benzene (C
6H
6) wait a kind of or several kinds of organic mixtures in the organic matter as reacting gas; The mixture that adopts a kind of or several kinds of metals in the transition metal such as Fe, Co, Ni simultaneously is as catalyst; In growth temperature is under 300～1100 ℃, and the induced carbon nanotube is grown directly upon the surface of substrate.In addition, the method for the CNT in the middle of the growing mixed material does not receive special restriction yet, except chemical gas-phase deposition system, can adopt other method as required, for example vacuum arc system, laser deposition system etc.
Among the present invention following 510 of the carbon nano-tube-amorphous composite membrane and above 530 one decks, promptly lowermost layer in the middle of the three-layer sandwich structure and top layer are not only limited to silicon nitride (SiN
x) film, can also be silica (SiO
x) or silicon oxynitride (SiN
xO
y) wherein a kind of such as film or their composite membrane.
The preparation method of film such as silicon nitride 510 and 530, non-crystalline silicon 522 is not only limited to the PECVD technology among the present invention, also comprises films such as the silicon nitride that utilizes other method preparation that low pressure or rpcvd (LPCVD, RPCVD), high vacuum chemical vapour deposition (UHVCVD), electron beam evaporation (EBE), ald (ALD), magnetron sputtering (MS) etc. are known in the industry, non-crystalline silicon.
II. based on the preparation method of the micro-metering bolometer of one dimension CNT and bidimensional non-crystalline silicon composite
Employing one dimension CNT that the foregoing description provided and bidimensional non-crystalline silicon composite are as the structural material of micro-metering bolometer; Can control the electricity and the optical property of material better; The changes in material properties of avoiding microbridge sensitive material altered chemical structure to cause, the combination property of raising device.Making of the present invention is following based on the micro-metering bolometer embodiment of carbon nano-tube-amorphous composite membrane: 1. select for use the silicon wafer that contains integrated circuit (ROIC) as substrate 1; After the cleaning back dries up with nitrogen; Put into plasma and strengthen (PECVD) system; The deposited amorphous silicon dioxide film is as passivation layer 2, and the thickness of silicon dioxide passivation layer is 300～1500nm; 2. on the surface of silicon dioxide passivation layer, utilize magnetic control sputtering system, deposit the metallic aluminium that a layer thickness is 100～1000nm, as the reflecting layer 3 of microbridge 7; 3. carve bridge pier 730 figures of microactuator suspension bridge 7 in the surface light of metallic aluminium 3, this metal aluminium lamination 3 of etching forms microbridge bridge pier hole and metallic aluminium isolated island to following silicon dioxide passivation layer 2; 4. on the surface of above-mentioned metallic aluminium 3, spin coating one layer thickness is the photosensitive polyimide film 4 of 1～4 μ m; 5. Kapton 4 is carried out photoetching treatment, form the bridge pier hole of Kapton isolated island and suspension microbridge, carry out imidization then and handle; 6. on the surface in Kapton isolated island and bridge pier hole, utilize PECVD under 300 ℃, deposit thickness is the amorphous silicon nitride 510 of 10～1500nm, as the support and the insulating materials of suspension microbridge 7; Then, I embodiment provides the preparation method of carbon nano-tube-amorphous composite membrane 520 according to the present invention, and elder generation is at the surperficial dispersing Nano carbon tubes 521 of silicon nitride film 510; Then; Utilize reactor, deposited amorphous silicon fiml 522, annealing; Forming thickness is the carbon nano-tube-amorphous laminated film 520 of 10～1500nm, as the light absorption and the heat-sensitive material of micro-metering bolometer; 7. follow, utilize reactor to deposit the metallic aluminium that a layer thickness is 10～500nm, graphical, as the electrode 6 of device; 8. last; Utilize reactor, on the surface of metal electrode 6 and carbon nano-tube-amorphous composite membrane 520, deposition covers one deck amorphous silicon nitride film 530; Thickness is 10～1500nm, as electrode 6 and the passivation layer of photaesthesia film 520 and the regulation and control layer of microbridge 7 stress; 9. carve the structure graph of microactuator suspension bridge 7 in the surface light of silicon nitride passivation 530; Etching carbon nano-tube-amorphous composite membrane 520 and underlying silicon nitride film 510 to polyimide layer 4, bridge floor 710, bridge leg 720 and bridge pier 730 figures of formation suspension microbridge 7; 10. adopt oxygen plasma to remove the Kapton 4 of bridge floor 710 and bridge leg 720 figures bottom, form cavity 740, as the optical resonator of device.Prepare micro-metering bolometer 8 thus based on carbon nano-tube-amorphous composite membrane 520.
The present invention propose based on the micro-metering bolometer structure of carbon nano-tube-amorphous composite membrane such as Fig. 5, Fig. 6 and shown in Figure 7.
Summary is got up, and the present invention forms composite through adding the one dimension CNT in the bidimensional amorphous silicon membrane, make amorphous silicon membrane electric property, reach chemical stability etc. and effectively improved, meet the needs of non-refrigerated infrared detector.With traditional independent employing individual layer amorphous silicon membrane or adopt CNT to compare separately as the device architecture of infrared-sensitive material; The present invention adopts the micro-metering bolometer based on the carbon nano-tube-amorphous composite membrane to have following advantage: (1) utilizes performances such as the good separately electricity of one dimension CNT and bidimensional non-crystalline silicon, optics; Obtain the better carbon nano-tube-amorphous composite film material of combination property, satisfy the specific (special) requirements of non-refrigerated infrared detector; (2) the quantitative adjusting of the content ratio through CNT, non-crystalline silicon can be more prone to, the membrane stress of trim more exactly, to satisfy the special requirement of micro-metering bolometer micro-bridge structure; (3) structure of composite membrane can also obviously improve its electric property under the prerequisite that keeps the good optical property of non-crystalline silicon, avoids the negative effect of traditional doping process to the non-crystalline silicon chemical constitution simultaneously, and this is the advantage that simple amorphous silicon film can't possess.So, adopt the present invention to adopt one dimension CNT and bidimensional amorphous silicon film composite as the INFRARED ABSORPTION and the thermistor material of micro-metering bolometer microbridge, can overcome existing defective in the prior art, reduce technology difficulty, improve device performance.
Claims (3)
1. micro-metering bolometer; Comprise micro-bridge structure; It is characterized in that thermistor material in this micro-bridge structure and infrared absorbing material layer are the carbon nano-tube-amorphous composite membrane, this carbon nano-tube-amorphous composite membrane is to be composited by one dimension CNT and bidimensional amorphous silicon membrane; Said micro-bridge structure is the three-layer sandwich structure: the bottom is one deck amorphous silicon nitride films, as the support and the insulating materials of microbridge; The intermediate layer is one deck or multilayer carbon nanotube-non-crystalline silicon composite membrane, and the incompatibility of its stress and underlying silicon nitride film is as the thermally sensitive layer and the infrared Absorption layer of micro-metering bolometer; The top layer is one deck amorphous silicon nitride films, and the incompatibility of its stress and middle carbon nanotube-non-crystalline silicon composite membrane is as the passivation layer of infrared-sensitive film and the regulation and control layer of stress.
2. the preparation method of a micro-metering bolometer is characterized in that, may further comprise the steps:
1. clean the monocrystalline silicon piece substrate that contains integrated circuit, utilize reactor deposition one deck amorphous silica film as passivation layer;
2. on the surface of silicon dioxide passivation layer, utilize reactor to deposit the metallic aluminium that a layer thickness is 100～1000nm, as the reflecting layer of microbridge;
3. carve the pier pattern of microactuator suspension bridge in the surface light of above-mentioned metallic aluminium, this metal aluminium lamination of etching to following silicon dioxide passivation layer forms microbridge bridge pier hole and metallic aluminium isolated island;
4. on the surface of above-mentioned metallic aluminium isolated island, spin coating one layer thickness is the photosensitive polyimide film of 1～4 μ m;
5. Kapton is carried out photoetching treatment, form the bridge pier hole of Kapton isolated island and suspension microbridge, carry out imidization then and handle;
6. on the surface in Kapton isolated island and bridge pier hole, utilize reactor deposition one deck amorphous silicon nitride film, thickness is 10～1500nm, as the support and the insulating materials of microbridge; Then, after cleaning dries up, clean substrate, it is subsequent use to dry up the back; Be placed on the good CNT of prepared beforehand in the middle of the beaker, mix with organic solvent, ultrasonic dispersion, then; Transfer to the surface of the substrate after the cleaning to dispersion liquid, make solvent evaporates, form netted, interconnected carbon nano-tube film, put into the substrate that obtains the reactor of vacuum pumping; As reacting gas, utilize reactor growth one deck amorphous silicon film with SiH4, the non-crystalline silicon of being grown is dispersed in the middle of the gap of surface and tube and tube of CNT, annealing; Form the carbon nano-tube-amorphous structure of composite membrane, be cooled to room temperature after, from reactor, take out; As required, repeat CNT dispersion, amorphous silicon deposition and annealing steps successively, form carbon nano-tube-amorphous MULTILAYER COMPOSITE membrane structure;
7. utilize reactor to deposit the metal that a layer thickness is 10～500nm, graphical, as the electrode of device;
8. last; Utilize reactor; On the surface of metal electrode and carbon nano-tube-amorphous composite membrane, deposition covers one deck amorphous silicon nitride film, and thickness is 10～1500nm; Carbon nano-tube-amorphous composite membrane in the middle of its stress and the microbridge opposite is as the passivation layer of electrode and photaesthesia film and the regulation and control layer of stresses of parts;
9. the surface light at above-mentioned laminated film carves microactuator suspension bridge construction figure, and this THIN COMPOSITE rete of etching forms bridge floor, bridge leg and the pier pattern of suspension microbridge to polyimide layer;
10. adopt oxygen plasma to remove the Kapton of bridge floor and bridge leg figure bottom, form cavity, constitute micro-metering bolometer.
3. the preparation method of a micro-metering bolometer is characterized in that, may further comprise the steps:
1. clean the monocrystalline silicon piece substrate that contains integrated circuit, utilize reactor deposition one deck amorphous silica film as passivation layer;
2. on the surface of silicon dioxide passivation layer, utilize reactor to deposit the metallic aluminium that a layer thickness is 100～1000nm, as the reflecting layer of microbridge;
3. carve the pier pattern of microactuator suspension bridge in the surface light of above-mentioned metallic aluminium, this metal aluminium lamination of etching to following silicon dioxide passivation layer forms microbridge bridge pier hole and metallic aluminium isolated island;
4. on the surface of above-mentioned metallic aluminium isolated island, spin coating one layer thickness is the photosensitive polyimide film of 1～4 μ m;
5. Kapton is carried out photoetching treatment, form the bridge pier hole of Kapton isolated island and suspension microbridge, carry out imidization then and handle;
6. on the surface in Kapton isolated island and bridge pier hole, utilize reactor deposition one deck amorphous silicon nitride film, thickness is 10～1500nm; Support and insulating materials as microbridge; Then, clean dry up after, utilize a kind of in chemical gas-phase deposition system or arc discharge system or the laser deposition system reactor; Induce through metallic catalyst; Direct reaction grows into netted, interconnected carbon nano-tube film on the surface of clean substrate, puts into the reactor of vacuum pumping to the substrate that obtains, and uses SiH
4As reacting gas, utilize reactor growth one deck amorphous silicon film, the non-crystalline silicon of being grown is dispersed in the middle of the gap of surface and tube and tube of CNT; Annealing forms the carbon nano-tube-amorphous structure of composite membrane, be cooled to room temperature after; From reactor, take out; As required, repeat carbon nano tube growth, amorphous silicon deposition and annealing steps successively, form carbon nano-tube-amorphous MULTILAYER COMPOSITE membrane structure;
7. utilize reactor to deposit the metal that a layer thickness is 10～500nm, graphical, as the electrode of device;
8. last; Utilize reactor; On the surface of metal electrode and carbon nano-tube-amorphous composite membrane, deposition covers one deck amorphous silicon nitride film, and thickness is 10～1500nm; Carbon nano-tube-amorphous composite membrane in the middle of its stress and the microbridge opposite is as the passivation layer of electrode and photaesthesia film and the regulation and control layer of stresses of parts;
9. the surface light at above-mentioned laminated film carves microactuator suspension bridge construction figure, and this THIN COMPOSITE rete of etching forms bridge floor, bridge leg and the pier pattern of suspension microbridge to polyimide layer;
10. adopt oxygen plasma to remove the Kapton of bridge floor and bridge leg figure bottom, form cavity, constitute micro-metering bolometer.
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