CN101820016A - Method for preparing titanium dioxide ultraviolet photoelectric detector - Google Patents
Method for preparing titanium dioxide ultraviolet photoelectric detector Download PDFInfo
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- CN101820016A CN101820016A CN201010150438A CN201010150438A CN101820016A CN 101820016 A CN101820016 A CN 101820016A CN 201010150438 A CN201010150438 A CN 201010150438A CN 201010150438 A CN201010150438 A CN 201010150438A CN 101820016 A CN101820016 A CN 101820016A
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Abstract
The invention discloses a method for preparing a titanium dioxide ultraviolet photoelectric detector, relates to a semiconductor photoelectric detection device, and provides a titanium dioxide ultraviolet photoelectric detector with low dark current and a preparation method thereof. The detector has a metal-semiconductor-metal structure, and comprises an insulating substrate, a polycrystal TiO2 film deposited on the insulating substrate by using magnetron sputtering technology and an interdigital metal electrode prepared on the TiO2 film by using magnetron sputtering or electron beam evaporation technology from the bottom to the top. The high-quality polycrystal TiO2 film is deposited by adopting optimized sputtering process parameters, and the deposited film has ideal chemical proportion and high compactness and crystallinity. The MSM structural ultraviolet detector prepared by using the film as a matrix has the advantages of high response degree, low dark current, high ultraviolet visible suppression ratio and the like. The preparation method has simple process and low cost; if the detector is manufactured on a Si-based substrate, the method can be compatible with the mature Si process; and the method is favorable for photoelectric integration and easy for industrialization.
Description
Technical field
The present invention relates to a kind of semiconductor photo detector spare, especially relate to a kind of polycrystalline TiO with the magnetron sputtering technique deposition
2Film is MSM (metal-semiconductor-metal) structure UV photodetector of matrix and preparation method thereof.
Background technology
The ultraviolet detection technology has become the another important detecting technique that countries in the world are paid close attention to after infrared and laser acquisition technology, has broad application prospects at scientific research, military affairs, civilian and many industrial circles.Present widely used UV photodetector mainly is silica-based ultraviolet light fulgurite and photomultiplier, its technical matters maturation, highly sensitive, but because the restriction of its material itself, have that resistance to elevated temperatures is poor, high-pressure work is fragile and need add shortcoming such as filter plate during use.Semiconductor material with wide forbidden band as SiC, GaN, ZnO and diamond film, has that band gap is wide, critical breakdown electric field is high and characteristics such as thermal conductivity height, utilizes appearance of its preparation UV photodetector part to promote the development of ultraviolet detection technology.Yet the preparation cost height of these materials, technology difficulty is bigger, and is comparatively harsh to the requirement of equipment and processing conditions, also is difficult to be popularized in the ultraviolet detector field rapidly.
TiO
2Be a kind of semiconductor material with wide forbidden band, anatase structured TiO
2, its energy gap is 3.2eV, visible light is absorbed hardly, and have very high absorptivity in ultraviolet portion.In addition, TiO
2Have high dielectric constant and refractive index and outstanding physics and chemical stability.Yet, TiO
2Natural is weak n section bar material, and its p type mixes very difficult, adds the thick TiO of preparation high-quality
2The difficulty of film is bigger, and the detector of pn junction type development at present is also very difficult, so TiO
2The research of base ultraviolet light electric explorer mainly concentrates in the preparation of Schottky junction structure and MSM structure.The TiO that has reported
2The base ultraviolet light electric explorer mainly is the TiO that adopts the sol-gel process growth
2Film is the MSM structure ultraviolet light detector of matrix.(Applied Physics Letters, 94,123502 (2009)) such as Hailin Xue etc. (Applied Physics Letters, 90,201118 (2007)) and Xiangzi Kong have been reported and have been utilized sol-gel process growth TiO
2The ultraviolet light detector of film preparation MSM structure.This detector has high responsiveness owing to having very high photoconductive gain.Yet because the film of sol-gel process growth has many holes that are difficult to avoid, the stoichiometric proportion mismatch is serious, the oxygen room is obvious, finally cause the detector dark current that is prepared into bigger, the UV, visible light rejection ratio can't improve, simultaneously owing to the photoconductive phenomenon that continues, degradation time response of detector.Therefore, how to obtain not have hole, density height, degree of crystallinity height, the TiO of desirable stoicheiometry
2Film becomes and improves TiO
2The key of base ultraviolet light electric explorer combination property.
Magnetron sputtering technique can be at growing film under the high-speed low temperature, and sputtering parameter is controlled easily, good process repeatability, and stability is high, is fit to extensive growth.The film of deposition have very high density, and the adhesive force between substrate is big, when adopting highly purified TiO
2During target, can obtain the TiO of desirable stoicheiometry
2Film.Adopt the TiO of magnetron sputtering technique deposition
2Film is developed MSM structure UV photodetector, the responsiveness height of device, dark current is little, UV, visible light rejection ratio height, it is simple, stable to have preparation technology simultaneously, cheap, compatible and be easy to advantage such as industrialization with silicon planner technology, therefore have broad application prospects in the ultraviolet detector field.
Summary of the invention
The objective of the invention is at existing TiO
2Deficiencies such as the ultraviolet light detector dark current is big, the UV, visible light rejection ratio is less provide a kind of and have that responsiveness height, dark current are little, the titanium dioxide ultraviolet photoelectric detector of UV, visible light rejection ratio advantages of higher.
Another object of the present invention is to provide a kind of technology comparatively simple, stable,, be easy to the preparation method of the titanium dioxide ultraviolet photoelectric detector of integrated and industrialization with the silicon planner technology compatibility.
Titanium dioxide ultraviolet photoelectric detector of the present invention is provided with dielectric substrate and TiO from top to bottom successively
2Polycrystal film is at TiO
2Polycrystal film is provided with interdigital metal electrode, described TiO
2The thickness of polycrystal film is 0.15～0.25 μ m, and crystallite dimension is greater than 50nm, and it is 1.95～2.05 that the oxygen titanium atom is counted ratio; The thickness of interdigital metal electrode is 0.1～0.3 μ m, and finger beam is 2～20 μ m, and spacing is 2～20 μ m, refers to that length is 300 μ m, and photosensitive area is 200 μ m * 300 μ m; Interdigital metal electrode is the high metals of work function such as Au, Pt and Ni; Dielectric substrate is selected from quartz glass, sapphire, growth silicon chip of silica or silicon nitride dielectric layer etc.
The preparation method of titanium dioxide ultraviolet photoelectric detector of the present invention may further comprise the steps:
1) with after the dielectric substrate cleaning, dries up dry for standby;
2) depositing Ti O on dielectric substrate
2Film;
3) with TiO
2Film thermal annealing, annealing finish to take out after the back sample naturally cools to room temperature with stove;
4) TiO behind thermal annealing
2The interdigital metal electrode figure of photoetching on the film;
5) deposition of interdigital metal electrode and peeling off
Adopt dc magnetron sputtering method sputter layer of metal on the good interdigital electrode figure of photoetching, the sample of the intact metal of sputter is immersed in the acetone sonicated, stripping photoresist and cover metal on it, dry up after the rinsing, promptly obtain titanium dioxide ultraviolet photoelectric detector.
In step 1), described with the dielectric substrate cleaning, preferably place the ultrasonic cleaning respectively of toluene, acetone, ethanol and deionized water successively; Describedly dry up available nitrogen and dry up, the temperature of described oven dry can be 100～120 ℃.
In step 2) in, described on dielectric substrate depositing Ti O
2Film can adopt rf magnetron sputtering (RF magnetronsputtering) method, and its concrete grammar is:
Open the magnetic control sputtering system growth room, load onto TiO
2Ceramic target is placed under the ceramic target dielectric substrate is parallel, closes the vacuum growth room; Forvacuum is arrived pressure less than 10
-4Pa feeds the sputter gas argon gas, makes growth room's air pressure remain 0.5～1.0Pa; Open radio frequency source, the adjusting radio-frequency power is 150～250W, begins the TiO that grows
2Film, growth time are 1～3h, and the film thickness of growth is 0.15～0.25 μ m.
In step 3), described thermal annealing can be with TiO
2Film is put into Muffle furnace and carry out thermal annealing under air ambient or aerating oxygen, and annealing temperature remains on 300～700 ℃, and annealing time is 1～3h.
In step 4), described TiO behind thermal annealing
2The interdigital metal electrode figure of photoetching can adopt standard photolithography process on the film, and concrete steps are as follows:
(1) gluing: with polycrystalline TiO
2Film sample places on the sol evenning machine sucker, first spin coating one deck tackifier, rotating speed 2500～3500rpm, even glue 15～25s, the even glue spin coating one deck reversal photoresist AZ5214E again that finishes, rotating speed 2500～3500rpm, even glue 35～45s;
(2) preceding baking: in 95 ℃ baking oven, toast 9～11min;
(3) exposure: earlier with mask exposure once, the time for exposure is 10.6s, then in 90 ℃ baking oven, toast 12～14min after, remove mask and expose again once, the time for exposure is 12s;
(4) develop: the 45～55s that develops in photoresist developing liquid, expose the TiO that needs metal electrode in the sputter after the development
2Film surface obtains needed photoresist interdigital structure.
In step 5), described employing magnetically controlled DC sputtering technology is the sputter layer of metal on the good interdigital electrode figure of photoetching, is less than 10 at base vacuum pressure
-4Under the Pa condition, feed the sputter gas argon gas, sputter growth room pressure is maintained at about 0.8Pa, and sputtering power is 60～80W, and sputtering time is 2～5min.The thickness of interdigital metal electrode is 0.1～0.3 μ m, and finger beam is 2～20 μ m, and spacing is 2～20 μ m; Sample with the intact metal of sputter is immersed in the acetone again, and sonicated 5～10min can fall photoresist and the metal-stripping that covers on it, then successively in ethanol and rinsed with deionized water, with nitrogen sample is dried up at last again.
The present invention makes metal-TiO with device
2-metal flat structure, this device have two schottky junctions of series connection back-to-back, and there always have a schottky junction to be in during work to be partially anti-.In order to improve the anti-height of Schottky barrier partially as far as possible, reduce the device dark electric current, adopt the high metal material of work function during design, as Au, Pt and Ni etc.
Adopting quartz glass of the present invention, sapphire, and growth the insulating material such as silicon chip of silica or silicon nitride dielectric layer are arranged is substrate, with the high-quality TiO of magnetron sputtering growth
2Film is that matrix prepares the new ultra-violet photodetector, makes the device dark electric current be reduced to 10 under the 5V bias voltage
-11The A order of magnitude, the UV, visible light rejection ratio brings up to 10
3More than the order of magnitude.The technology that the present invention simultaneously adopts is simple, stable, with the silicon planner technology compatibility, is easy to integrated and industrialization, for the further research of large tracts of land, array ultraviolet light detector and ultraviolet imagery system is laid a good foundation, therefore has important application value.
TiO of the present invention
2Base MSM structure UV photodetector, TiO
2The deposition process of semiconductive thin film and thermal annealing process have extremely important influence to the performance of device.TiO
2Membrane deposition method is rf magnetron sputtering (RF magnetronsputtering) technology, adopts highly purified TiO
2Ceramic target by optimizing the sputter growth parameter(s), obtains the TiO of even compact, desirable stoicheiometry at last
2Film.For obtaining the film of high-crystallinity, with TiO
2Film (in air or aerating oxygen) under aerobic environment carries out thermal anneal process, crackle occurs for avoiding film, and intensification and rate of temperature fall before and after the annealing are very important.
Description of drawings
Fig. 1 is the structural representation of the prepared titanium dioxide ultraviolet photoelectric detector of the present invention.In Fig. 1,1 expression quartz glass, sapphire, and growth has the dielectric substrate such as silicon chip of silica or silicon nitride dielectric layer; 2 expressions utilize the TiO of magnetron sputtering technique growth
2Polycrystal film; The high interdigital metal electrodes of work function such as 3 expression Au, Pt and Ni.
Fig. 2 is the dark current and the photocurrent characteristics curve of the prepared titanium dioxide ultraviolet photoelectric detector of the present invention.In Fig. 2, abscissa is voltage Voltage (V), and ordinate is electric current Current (A); ■ is a dark current, ● be photoelectric current; Interdigital electrode finger beam 3 μ m, spacing 3 μ m, the dark current of device are 10 under the 5V bias voltage
-11The A magnitude.
Fig. 3 is the prepared spectral response characteristic curve of titanium dioxide ultraviolet photoelectric detector under the 10V bias voltage of the present invention.In Fig. 3, abscissa is wavelength Wavelength (nm), and ordinate is optical responsivity Photoresponse (A/W); Interdigital electrode finger beam 3 μ m, spacing 3 μ m, detector is very low in the visible light wave range responsiveness greater than 380nm, has significant photoresponse at the ultraviolet band of 240～360nm, and UV, visible light rejection ratio (310nm place/400nm place) is greater than 3 orders of magnitude.
Embodiment
The high performance Ti O of the present invention's preparation
2Base MSM structure UV photodetector, the high metals of work function such as the optional Au of interdigital electrode material, Pt and Ni; The optional quartz glass of dielectric substrate, sapphire, and growth has the silicon chip of silica or silicon nitride dielectric layer.If on silicon chip substrate, make, can with the Si process compatible of maturation, it is integrated to help photoelectricity, is easy to industrialization.Below be substrate with the quartz glass, be the preparation implementation process that metal electrode illustrates detector of the present invention with Au.
Below provide concrete steps:
(1) processing of substrate
Dielectric substrate is selected quartz glass (thickness 0.5mm, diameter 1inch), and substrate is placed toluene, acetone, ethanol and deionized water ultrasonic cleaning 10min respectively successively, dries up with high pure nitrogen, then dry for standby in 110 ℃ baking oven.
(2) TiO
2Depositing of thin film
1. adopt radiofrequency magnetron sputtering technology depositing Ti O on quartz substrate
2Film.Open the magnetic control sputtering system power supply, the growth room is opened in the inflation of vacuum growth room, loads onto high-purity Ti O
2Ceramic target (diameter is 101mm, and purity is 99.99%) is with the parallel TiO that is placed on of quartz substrate
2Sample stage under the ceramic target, target and sample stage vertical range are 8cm, airtight growth room.
2. open mechanical pump forvacuum to pressure less than 5Pa, then open molecular pump, pumping high vacuum to pressure is 6 * 10
-4Pa opens air valve, slowly feeds the sputter gas high-purity argon gas, keeps growth room's pressure to be about 0.8Pa.
3. open radio frequency source, preheating 5min, the adjusting radio-frequency power is 200W, beginning sputter growth TiO
2Film, growth room's temperature are normal temperature, and growth time is 130min, and the film thickness of growth is about 0.18 μ m.
(3) TiO
2The heat treatment of film
With TiO
2Film is put into Muffle furnace and carry out thermal annealing under air ambient, and the cycle annealing temperature and time is set 600 ℃ and 2h respectively.The annealing beginning, sample slowly heats up with body of heater in Muffle furnace, and heating rate is 5 ℃/min; Annealing finishes, and sample takes out after naturally cooling to room temperature with stove.
(4) photoetching of interdigital metal electrode figure
Adopt the AZ5214E reversal photoresist at polycrystalline TiO
2The film surface interdigital metal electrode figure of standard photolithography process photoetching.
The photoetching concrete steps are as follows:
1. gluing: open the sol evenning machine power supply, ventilation is with polycrystalline TiO
2Film sample is adsorbed on the sol evenning machine sucker, first spin coating one deck tackifier, and rotating speed is 3000rpm, even glue 20s; And then spin coating one deck reversal photoresist AZ5214E, rotating speed is 3000rpm, even glue 40s.
2. preceding baking: will spare the sample that glue finishes and put into baking oven, and vacuumize, and under 95 ℃ of temperature, toast 10min;
3. exposure: load onto mask, expose once, the time for exposure is 10.6s; Toast 13min once more in 90 ℃ baking oven after, remove mask and expose once again, the time for exposure is 12.0s.
4. develop: in photoresist developing liquid, behind the development 50s, promptly obtain needed photoresist interdigital structure with rinsed with deionized water.
(5) deposition of interdigital Au electrode and peeling off
As interdigital metal electrode, utilize magnetically controlled DC sputtering technology sputtering sedimentation Au film on the good interdigital figure of photoetching with Au.To sputtering system growth room pumping high vacuum to pressure is 8 * 10
-4Pa feeds the sputter gas argon gas, and sputter growth room pressure remains 0.8Pa, and sputtering power is set at 70W, and sputtering time is 220s.The thickness that obtains the Au interdigital electrode at last is 0.25 μ m, and finger beam is two kinds of 2 μ m and 3 μ m, and spacing is four kinds of 3 μ m, 4 μ m, 6 μ m and 10 μ m.
Place acetone ultrasonic in the sample of Au film in the sputter, ultrasonic time is 10min, photoresist and the Au that covers on it can be peeled off, and is remaining unstripped as also having, and dips in acetone with cotton swab and cleans gently and get final product.To peel off the sample rinsing in ethanol and deionized water successively of success at last, dry up with high pure nitrogen again, promptly obtain the device of preparation that this patent is invented.
Claims (8)
1. a titanium dioxide ultraviolet photoelectric detector is characterized in that being provided with successively from top to bottom dielectric substrate and TiO
2Polycrystal film is at TiO
2Polycrystal film is provided with interdigital metal electrode, described TiO
2The thickness of polycrystal film is 0.15～0.25 μ m, and crystallite dimension is greater than 50nm, and it is 1.95～2.05 that the oxygen titanium atom is counted ratio; The thickness of interdigital metal electrode is 0.1～0.3 μ m, and finger beam is 2～20 μ m, and spacing is 2～20 μ m, refers to that length is 300 μ m, and photosensitive area is 200 μ m * 300 μ m; Interdigital metal electrode is selected from Au, Pt or Ni; Dielectric substrate is selected from the silicon chip that quartz glass, sapphire, growth have silica or silicon nitride dielectric layer.
2. the preparation method of titanium dioxide ultraviolet photoelectric detector as claimed in claim 1 is characterized in that may further comprise the steps:
1) with after the dielectric substrate cleaning, dries up dry for standby;
2) depositing Ti O on dielectric substrate
2Film;
3) with TiO
2Film thermal annealing, annealing finish to take out after the back sample naturally cools to room temperature with stove;
4) TiO behind thermal annealing
2The interdigital metal electrode figure of photoetching on the film;
5) deposition of interdigital metal electrode and peeling off
Adopt dc magnetron sputtering method sputter layer of metal on the good interdigital electrode figure of photoetching, the sample of the intact metal of sputter is immersed in the acetone sonicated, stripping photoresist and cover metal on it, dry up after the rinsing, promptly obtain titanium dioxide ultraviolet photoelectric detector.
3. the preparation method of titanium dioxide ultraviolet photoelectric detector as claimed in claim 2 is characterized in that in step 1), and is described with the dielectric substrate cleaning, is to place the ultrasonic cleaning respectively of toluene, acetone, ethanol and deionized water successively.
4. the preparation method of titanium dioxide ultraviolet photoelectric detector as claimed in claim 2 is characterized in that in step 1), and described drying up is to dry up with nitrogen, and the temperature of described oven dry is 100～120 ℃.
5. the preparation method of titanium dioxide ultraviolet photoelectric detector as claimed in claim 2 is characterized in that in step 2) in, described on dielectric substrate depositing Ti O
2Film is to adopt radio frequency magnetron sputtering method, and its concrete grammar is:
Open the magnetic control sputtering system growth room, load onto TiO
2Ceramic target is placed under the ceramic target dielectric substrate is parallel, closes the vacuum growth room; Forvacuum is arrived pressure less than 10
-4Pa feeds the sputter gas argon gas, makes growth room's air pressure remain 0.5～1.0Pa; Open radio frequency source, the adjusting radio-frequency power is 150～250W, begins the TiO that grows
2Film, growth time are 1～3h, and the film thickness of growth is 0.15～0.25 μ m.
6. the preparation method of titanium dioxide ultraviolet photoelectric detector as claimed in claim 2 is characterized in that in step 3), and described thermal annealing is with TiO
2Film is put into Muffle furnace and carry out thermal annealing under air ambient or aerating oxygen, and annealing temperature remains on 300～700 ℃, and annealing time is 1～3h.
7. the preparation method of titanium dioxide ultraviolet photoelectric detector as claimed in claim 2 is characterized in that in step 4), described TiO behind thermal annealing
2The interdigital metal electrode figure of photoetching on the film is to adopt standard photolithography process, and concrete steps are as follows:
(1) gluing: with polycrystalline TiO
2Film sample places on the sol evenning machine sucker, first spin coating one deck tackifier, rotating speed 2500～3500rpm, even glue 15～25s, the even glue spin coating one deck reversal photoresist AZ5214E again that finishes, rotating speed 2500～3500rpm, even glue 35～45s;
(2) preceding baking: in 95 ℃ baking oven, toast 9～11min;
(3) exposure: earlier with mask exposure once, the time for exposure is 10.6s, then in 90 ℃ baking oven, toast 12～14min after, remove mask and expose again once, the time for exposure is 12s;
(4) develop: the 45～55s that develops in photoresist developing liquid, expose the TiO that needs metal electrode in the sputter after the development
2Film surface obtains needed photoresist interdigital structure.
8. the preparation method of titanium dioxide ultraviolet photoelectric detector as claimed in claim 2 is characterized in that in step 5), and described employing magnetically controlled DC sputtering technology is the sputter layer of metal on the good interdigital electrode figure of photoetching, is less than 10 at base vacuum pressure
-4Under the Pa condition, feed the sputter gas argon gas, sputter growth room pressure is maintained at about 0.8Pa, and sputtering power is 60～80W, and sputtering time is 2～5min.The thickness of interdigital metal electrode is 0.1～0.3 μ m, and finger beam is 2～20 μ m, and spacing is 2～20 μ m; Sample with the intact metal of sputter is immersed in the acetone again, and sonicated 5～10min falls photoresist and the metal-stripping that covers on it, then successively in ethanol and rinsed with deionized water, with nitrogen sample is dried up at last again.
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