CN101030533A - Production of ZnO metal Schottky-based contact and its use in ultraviolet detector - Google Patents
Production of ZnO metal Schottky-based contact and its use in ultraviolet detector Download PDFInfo
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Abstract
The invention is concerned with a method to form Schottky contacts by in-situ producing metal thin film electrode on ZnO crystal thin film surface with MBE low temperature growth method, especially a method to use ultra-high vacuum in-situ depositing metal conduct thin film. Use ultra-high vacuum sample-feeding system and send ZnO crystal thin film sample produced in MBE growth room to electrode evaporation room during ultra-high vacuum. The sample table can cool and maintain the ZnO thin film sample under the room temperature(<=20 degree), then the deposition of metal thin film can be carried by MBE method with low temperature. The ZnO surface with continuous and equably deposit metal conductive film can be prepared and can be used to produce and research the metal-semiconductor Schottky contacts and other devices, especially ZnO base ultraviolet detector with high photo-electricity responsivity with good schottky junction fromed by silver and n tape of ZnO.
Description
Technical field
The present invention relates to a kind of method in the metal Schottky-based contact of ZnO monocrystal thin films surface preparation, especially in ultra-high vacuum environment, thereby utilize molecular beam epitaxy technique in-situ low-temperature depositing metal films preparation Schottky contacts on the ZnO clean surface, and the method for further making ultraviolet detector.
Background technology
As the semi-conductive key foundation material of the third generation, ZnO has very superior photoelectric properties, its room temperature energy gap is that 3.37eV, free exciton binding energy are 60meV, become another important semiconductor material with wide forbidden band after GaN (the free exciton binding energy is 25meV), very wide application prospect has been arranged in low threshold value, high efficiency short-wavelength light field of electronic devices.Two potential zno-based ultraviolet detector and zno-based short wavelength laser diodes (LED) of being applied as that present ZnO is expected in the world most.
Because ZnO has good photoconductive property, is fit to very much be produced on " sun blindness " medium ultraviolet detector that has important value on the national defence high-tech.The medium ultraviolet detector is not disturbed by sunlight, civilian and military on great application value is all arranged, as ozone detector, flame sensor, contamination monitor, secure communication, guided missile plumage smoke detector and Air Vehicle Detection device etc.Particularly in this military high-tech sector of electrooptical countermeasures, ultraviolet countermeasure has occupied more and more important position with the anti-technology of opposition, and exploitation can be operated under the higher temperature, more efficient and more reliable medium ultraviolet detector has very important effect to improving ultraviolet alarm technique level.Energy gap is that the intrinsic ZnO of 3.37eV is after mixing, as mix Mg and form the ZnMgO alloy, its energy gap can broaden with the increase of Mg content, thereby makes that investigative range can be to medium ultraviolet and even the expansion of deep ultraviolet direction, and this militarily has extremely important using value.The Y.Lu of calendar year 2001 U.S. Rutgers University leader's seminar is developed into that optical responsivity is that 1.5A/W, leakage current are the ZnO Schottky ultraviolet detector (its combination property is above the GaN ultraviolet detector) that is respectively 1nA, rising and fall time 12ns and 50ns under 5 volts bias voltages, this group is developing the shorter ZnMgO medium ultraviolet detector of cut-off wavelength at present, is used for surveying 0.2～0.3 micron medium ultraviolet light wave of " day blind area ".
It is Schottky type and back-to-back Schottky that the Schottky barrier that utilizes the metal-semiconductor contact to form is surveyed ultraviolet light, i.e. MSM (metal-semiconductor-metal) type detector its working principles.The key for preparing this detector will deposit the metal that one deck can form Schottky barrier with this semiconductor at semiconductor surface exactly, makes contact have rectification characteristic.This layer metal will have good electrical conductivity, can be used as electrode and use, otherwise its photoelectric characteristic can't be detected by the external world; In addition, should keep smooth precipitous interface between the metal-semiconductor contact, no interdiffusion phenomenon can avoid tunnelling current to cause the device performance variation like this.
This shows, in development process based on the medium ultraviolet detector of novel Zn O alloy firm, the technology of preparing of surface metal electrode is a key link of influence even decision device performance, and the preparation technology of stable Schottky contacts will be that the ZnO material is realized the basis that the ultraviolet detection device is used.Yet up to the present, metal/ZnO interface that a lot of groups obtain often presents very strong unsteadiness, and the repeatability of experimental result is lower.On the one hand relevant, then relevant on the other hand with factors such as the counterdiffusion of contingent interface or film surface damage in the electrode production process with the unsteadiness of ZnO polar surfaces.
The ZnO of wurtzite structure does not have the plane of symmetry in [0001] direction, and be a polar material: the Zn of four-coordination and O atom have very strong ionic bond characteristic, thereby present very strong spontaneous polarization electric field on [0001] direction, forms two kinds of polar surfaces of Zn, O.In exposing Atmospheric processes, polar surfaces is more vulnerable to pollution, easier changing than apolar surfaces, therefore, the metallic film interface that obtains and even inevitable not ideal enough of on this surface, growing with the contact performance of ZnO, so the in-situ deposition of metal film electrode on the ZnO clean surface has crucial meaning for the influence of research and control metal/ZnO interface and even contact performance, be that the ZnO device is marched toward one step of key of practicability.
Electrode preparation method commonly used at present has magnetron sputtering, thermal evaporation, electron beam evaporation etc., still, and the shortcoming that traditional deposit metal films technology all has some to be difficult to overcome.As magnetically controlled sputter method, its plated film principle is to utilize gas ion through quickening back bombardment metal target surface, and atom that sputters or elementide are deposited on material surface and form film.This method makes the single crystalline substrate surface sustain damage easily, produces a large amount of defectives, is unfavorable for obtaining good metal-semiconductor contact.In addition, the magnetron sputtering embrane method is to carry out electro-deposition under air pressure is about the rough vacuum of 1Pa magnitude, and substrate surface has suffered pollution to a certain degree, can't protect the clean surface of ZnO sample, the electro-deposition of more impossible realization original position.The limitation of thermal evaporation is: 1. the refractory metal steam forces down, and is difficult to make film; 2. some element easily and heater strip formation alloy; 3. be difficult to obtain the uniform alloy film of composition.In addition, because its deposition velocity is very fast, metal electrode is the polycrystalline phase, does not utilize to form excellent contact character.And electron-beam vapor deposition method is because cost is higher, for deposition fusing point lower metal, as gold, silver etc., generally all will not adopt.
Schottky metal electrode commonly used has silver, gold, platinum, nickel etc.Wherein, gold, silver and n type ZnO can form the higher Schottky contacts of potential barrier, have good rectification characteristic, and better heat stability, and this is having important role aspect preparation of photodetector.
Molecular beam epitaxy (MBE) technology is a kind of thin-film material growing technology that is proposed and grown up by people such as Zhuo Yihe in 1971 by the people such as J.R.Arthur of U.S.'s Bell Laboratory in nineteen sixty-eight.It refers at ultra-high vacuum system (＜10
-7Torr, ultimate vacuum can reach 10
-11Torr) in, the heating electron gun makes molecule or atom with certain heat energy be ejected into the adjustable single crystalline substrate surface of temperature, by molecule, atom the substrate surface migration and and the surface react and reach epitaxially grown purpose.Adopted the MBE method to carry out the preparation of the metal Schottky-based contact in ZnO clean surface among the present invention, this method has its irreplaceable advantage:
1) have the ultra high vacuum growing environment, the purity of metal material is high especially.And can link to each other with the sample grown chamber, atmosphere needn't be exposed after sample grown finishes and just electrode evaporation chamber can be directly imported into, can guarantee that like this sample can be maintained in the clean condition before evaporation, avoid the single crystal samples surface to be subjected to contaminating impurity, be fit to the in-situ deposition of metal electrode under the ultra high vacuum;
2) deposition velocity of metal evaporation sources can accurately be controlled and be adjusted by the diffusion furnace temperature, can grow that nanoscale is thick, the semi-transparent metals film of even composition;
3) growth temperature is controlled, can avoid the issue of inter-diffusion of growth course median surface atom, obtains smooth precipitous interface, is fit to growing metal-semiconductor Schottky contacts system material, can also avoid the elevated temperature heat generation of defects;
4) can not cause any damage in the growth course, help forming good metal-semiconductor contact, and under optimized conditions, can obtain the metallic film of monocrystalline, help the improvement of electric property the surface
5) with respect to electron beam evaporation methods, cost is lower.
Therefore, in order to obtain high-quality metal-semiconductor Schottky contacts, advance " sun blindness " medium ultraviolet detector to move towards practical, we have invented the MBE low-temperature epitaxy method of the metal Schottky-based contact of in-situ deposition on the ZnO clean surface, and have further made high performance MSM ultraviolet detector.
Summary of the invention
Primary and foremost purpose of the present invention is to provide a kind of and new prepares the method for metal Schottky-based contact by the MBE low-temperature epitaxy on ZnO cleaning monocrystal thin films surface; Further aim of the present invention is to provide a kind of method of making ultraviolet detector; promptly underlayer temperature control at low temperatures (≤20 ℃) carry out the molecular beam epitaxy deposition of ultra high vacuum conductive metal film; acquisition has the high-quality continuous film of stable Schottky contacts characteristic; on above-mentioned metallic film, utilize magnetron sputtering method deposited gold film protective layer then; by ultraviolet photolithographic technology, and utilize reactive ion etching technology to make the Schottky ultraviolet detector.Utilize this method to obtain to have the zno-based MSM ultraviolet detector of superior photoelectric properties.
Method at ZnO monocrystal thin films surface deposition conductive metal film provided by the invention is achieved by the following technical solution:
1) the single crystal ZnO film with the growth of MBE chamber passes the electrode deposition system that the importing of sample system is attached thereto by ultra high vacuum, and this system possesses the ultra high vacuum background gas pressure equally, and its sample stage also has refrigerating function simultaneously;
2) under the ultra high vacuum background, be cooled to the ZnO film sample below the room temperature and keep;
3) reached under the condition of low temperature at sample, come depositing metal films by the temperature of control metal diffusing stove.
Further, temperature step 2) is-150 ℃-20 ℃.
Further, the thickness of metallic film described in the step 3) is 20nm～80nm.
Further, metallic film described in the step 3) is the high silver of work function or platinum or thin nickel metal film.
Further, metallic film described in the step 3) is the high gold thin film of work function.
Further, if described metallic film is silver or platinum or thin nickel metal film, then on above-mentioned existing step basis, increase: step 4): utilize the thick golden protective layer of known magnetron sputtering method deposition 20～50nm on the surface of the prepared metallic film of step 3); Step 5): utilize known ultraviolet photolithographic technology and produce the metal electrode of interdigitated,, thereby prepare the Schottky ultraviolet detector again at surface of metal electrode welding electrode lead-in wire in conjunction with known reactive ion etching technology.
If described metallic film is a gold thin film, then only increase: step 5): utilize known ultraviolet photolithographic technology and produce the metal electrode of interdigitated in conjunction with known reactive ion etching technology, go between at the surface of metal electrode welding electrode again, thereby prepare the Schottky ultraviolet detector.
The MBE method of above-mentioned ZnO monocrystal thin films deposit metal electrodes and the difference of existing deposition process mainly contain 2 points:
1) at low temperatures metallic film is deposited.
When temperature is no more than 20 ℃, situation when the activity of atom and energy all are not so good as high temperature, be difficult for taking place metallic atom and ZnO surface atom and intercourse (being counterdiffusion) or phenomenons such as chemical reaction, formation alloy take place, therefore can obtain precipitous metal/semiconductor interface.In addition, we find because the big mismatch and the key mismatch problem of metal/semiconductor system be higher than under the condition of room temperature, when the enterprising row metal epitaxial growth of ZnO, tend to occur film discontinuous/problem of fracture.This is because in the big mismatch system epitaxial process, for the stability of guarantee system, surface energy must be minimum.When growth temperature was higher, foreign atom can obtain enough energy and fully move, finds the minimum nucleating center of energy to become the key growth on the surface, and therefore surface energy is minimized; Not and not matching owing to metallic bond and covalent bond, cause combination between the external metallic atom be better than far away they with the Semiconductor substrate atom between combine, metallic atom tends to mutual Cheng Jian, polymerization so that grow up, in ensuing growth course, the atom that arrives semiconductor surface is always sought existing elementide, cause original cluster long more big more, become isolated one by one island, form discontinuous metal film the most at last.And we adopt the purpose of low-temperature epitaxy be exactly by reduce metallic atom at the transfer ability on ZnO surface, reduce its migration length, make it can't obtain enough energy and go to seek the minimum position of energy, therefore can only be attached to the ZnO surface location that arrives at first, with surface atom Cheng Jian, thereby reach continuously and the purpose of deposition equably, so both can solve the continuous metal film in the epitaxially grown difficulty in ZnO surface, can obtain smooth precipitous interface according to the result of anticipation again, for the improvement significantly of device performance provides governed foundation.
2) under the ultra high vacuum background, utilize the MBE method to carry out the in-situ deposition of metal electrode.
The ZnO monocrystal thin films sample that the MBE growth room is prepared directly is sent to the MBE deposition (as shown in Figure 1) that the electrode deposited chamber carries out the low temperature metal membrane through ultra-high vacuum environment (sample distributor chamber), at first, avoided the absorption and the pollution of impurity in the atmosphere, protected stable polar surfaces of ZnO and electronic state thereof, prevented the influence of some X factors (as surface conductance etc.) its surface; Secondly, adopted the MBE method to carry out the preparation of the metal Schottky-based contact in ZnO clean surface, with respect to electro-deposition method commonly used, as magnetron sputtering method, this method can not cause any damage to the surface, helps forming good metal-semiconductor Schottky contacts.Therefore help to obtain interface electronic structure and the contact performance that abundant information is analyzed understanding metal/ZnO by the present invention, for final stable, the practical metal/ZnO Schottky contacts that obtains solves crucial technical barrier.On the high-test metal electrode for preparing, utilize magnetron sputtering method deposited gold film protective layer, by ultraviolet photolithographic technology, and utilize reactive ion etching technology to make interdigited electrode.The zno-based MSM ultraviolet detector that utilizes this method to make to have superior photoelectric properties.
Description of drawings
Fig. 1 is the present invention's device therefor structural representation when ultra high vacuum MBE low temperature depositing conductive metal film;
Fig. 2 is embodiment of the invention SEM scintigram (a) at n type ZnO monocrystal thin films surface MBE method plated metal silver in the time of 20 ℃, and the pattern contrast (b) during deposition during with 60 ℃;
Fig. 3 is the structural representation (a) of the ultraviolet detector of embodiment of the invention made, and makes flow chart (b);
The MSM type ultraviolet detector I-V resonse characteristic figure (a) that Fig. 4 prepares behind depositing silver on the n type ZnO monocrystal thin films sample for the embodiment of the invention, and with the contrast (b) of the device of magnetically controlled sputter method deposition silverskin made.
Embodiment
The present invention is described in detail below in conjunction with embodiment and accompanying drawing.
As shown in Figure 1, low temperature depositing metal silverskin and prepare the method for MSM type ultraviolet detector on n type ZnO clean surface:
1) the n type ZnO monocrystal thin films with the growth of MBE chamber passes sample system iontophoresis electrode deposition system by ultra high vacuum, and the sample stage of this system has refrigerating function;
2) under the ultra high vacuum background, this sample is cooled to (≤20 ℃) below the room temperature and keeps with liquid nitrogen; To the cooling of substrate, be to realize in this step by long-time method of leading to liquid nitrogen in the cold-trap that surrounds sample stage;
3) reached under the condition of low temperature at sample, heated silver-colored diffusion furnace, made the line of silver reach 8 * 10
-5About Pa, deposit thickness is about the metal silverskin of 50nm;
4) on above-mentioned metal silverskin, utilize the thick golden protective layer of known magnetron sputtering method deposition 20～50nm;
5) utilize known ultraviolet photolithographic technology and produce the metal electrode of interdigitated,, thereby prepare the Schottky ultraviolet detector again at surface of metal electrode welding electrode lead-in wire in conjunction with known reactive ion etching technology.
So-called known ultraviolet photolithographic technology and reactive ion etching technology are specially: the positive glue that at first is covered with a layer thickness on the above-mentioned golden film surface for preparing and is 1 micron, and utilize the ultraviolet photolithographic fabrication techniques to go out the interdigitated pattern, and then utilize reactive ion etching technology to produce the silver/gold electrode of interdigitated.Utilize supersonic welding connection technology or other suitable welding means welding electrodes lead-in wire at surface of metal electrode more at last, thereby prepare antetype device.
Metallic film in the present embodiment is a silverskin, also can adopt platinum film or nickel film or golden film certainly, and its preparation method is identical.
When metallic film is silverskin or platinum film or nickel film, because therefore these three kinds of easy oxidations of metal need deposit one deck gold film on its surface again as diaphragm; And when metallic film directly adopts golden film, then need not be again at its surface deposition one deck gold film.
At the above-mentioned metallic film of deposition, and during follow-up golden diaphragm, guarantee metallic film effectively cover ZnO film, guarantee semi-transparent, and guarantee can suitably adjust the thickness of metallic film and golden protective film under the situation of reliable carrying.
Usually the total thickness at metallic film and golden diaphragm is no more than under the situation of 100nm, can guarantee the semi-transparent characteristic of film.
Utilize scanning electron microscopy at first to characterize the continuity and the uniformity of the n type ZnO film sample surfaces metal silverskin of the present invention's preparation, shown in Fig. 2 a.(Fig. 2 b) compares with the sample for preparing under the higher condition of growth temperature, can see, the method for the low temperature deposit metal silverskin that we invented has solved the continuous metal film really in the epitaxially grown difficulty in ZnO surface.
Though conventional magnetically controlled sputter method also can prepare continuous conductive metal film, but its operation principle has determined that depositing metallic films will inevitably have certain damage to substrate surface in this way, and this damage appears undoubtedly in the performance test of device the influence that metal-semiconductor contacts.For advantage of the present invention is described, we at first utilize magnetron sputtering method at n type ZnO film surface deposition silverskin, making flow process according to device architecture and Fig. 3 b of Fig. 3 a, we have prepared MSM type ultraviolet detector antetype device, and its current-voltage (I-V) resonse characteristic is shown in Fig. 4 b.As seen from the figure, during 2V photoelectric current only than high 2 orders of magnitude of dark current.By contrast, the photoelectric characteristic of the MSM type ultraviolet detector that the Ag/ZnO Schottky contacts knot that utilizes the present invention to prepare is developed has obtained significantly improving, shown in Fig. 4 a, its dark current is the nA order of magnitude (analog value that obtains than magnetron sputtering method hangs down 1 order of magnitude at least).When bias voltage was 2V, photoelectric current was than high 4 orders of magnitude of dark current.Test result shows, we have guaranteed that sample can be maintained in the clean condition by the ultra high vacuum low temperature MBE depositing silver membrane technology of invention before evaporation, avoided sample surfaces to be subjected to contaminating impurity, also solved the problem such as counterdiffusion, elevated temperature heat defective, particle bombardment damage of growth course median surface atom in addition, finally improved the various aspects of performance of device, laid a solid foundation for it moves towards practicability.
Claims (7)
1. method at ZnO monocrystal thin films surface deposition conductive metal film, its concrete steps are as follows:
1) the single crystal ZnO film with the growth of MBE chamber passes the electrode deposition system that the importing of sample system is attached thereto by ultra high vacuum, and this system possesses the ultra high vacuum background gas pressure equally, and its sample stage also has refrigerating function simultaneously;
2) under the ultra high vacuum background, be cooled to the ZnO film sample below the room temperature and keep;
3) reached under the condition of low temperature at sample, come depositing metal films by the temperature of control metal diffusing stove.
2. according to claim 1 in the method for ZnO monocrystal thin films surface deposition conductive metal film, it is characterized in that described step 2) described in temperature be-150 ℃-20 ℃.
3. according to claim 1 in the method for ZnO monocrystal thin films surface deposition conductive metal film, it is characterized in that the thickness of metallic film described in the described step 3) is 20nm～80nm.
4. according to claim 1 in the method for ZnO monocrystal thin films surface deposition conductive metal film, it is characterized in that the described metallic film in the described step 3) is the high silver of work function or platinum or thin nickel metal film.
5. according to claim 1 in the method for ZnO monocrystal thin films surface deposition conductive metal film, it is characterized in that the described metallic film in the described step 3) is the high gold thin film of work function.
6. method for preparing the Schottky ultraviolet detector that is based upon on the arbitrary described method of the claim 1-4 basis, it is characterized in that, on above-mentioned existing step basis, increase: step 4): utilize the thick golden protective layer of known magnetron sputtering method deposition 20～50nm on the surface of the prepared metallic film of step 3); Step 5): utilize known ultraviolet photolithographic technology and produce the metal electrode of interdigitated,, thereby prepare the Schottky ultraviolet detector again at surface of metal electrode welding electrode lead-in wire in conjunction with known reactive ion etching technology.
7. method for preparing the Schottky ultraviolet detector that is based upon on the described method of claim 5 basis, it is characterized in that, on above-mentioned existing step basis, increase: step 5): utilize known ultraviolet photolithographic technology and produce the metal electrode of interdigitated in conjunction with known reactive ion etching technology, go between at the surface of metal electrode welding electrode again, thereby prepare the Schottky ultraviolet detector.
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| CN102332474A (en) * | 2011-10-18 | 2012-01-25 | 北京工业大学 | InGaZnO (indium-gallium-zinc-oxide) Schottky diode device and manufacturing method thereof |
| CN102694067A (en) * | 2012-05-23 | 2012-09-26 | 中国科学院苏州纳米技术与纳米仿生研究所 | Method for preparing voltage modulation ultraviolet bicolor photoelectric response detector |
| CN103147069A (en) * | 2011-12-07 | 2013-06-12 | 周义才 | Manufacturing method for metalorganic epitaxial thin film |
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| AU2002312293A1 (en) * | 2002-01-04 | 2003-07-30 | Rutgers, The State University Of New Jersey | SCHOTTKY DIODE WITH SILVER LAYER CONTACTING THE ZnO AND MgxZn1-xO FILMS |
| JP2006073726A (en) * | 2004-09-01 | 2006-03-16 | Shin Etsu Handotai Co Ltd | Manufacturing method of compound semiconductor element |
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| CN102332474A (en) * | 2011-10-18 | 2012-01-25 | 北京工业大学 | InGaZnO (indium-gallium-zinc-oxide) Schottky diode device and manufacturing method thereof |
| CN103147069A (en) * | 2011-12-07 | 2013-06-12 | 周义才 | Manufacturing method for metalorganic epitaxial thin film |
| CN102694067A (en) * | 2012-05-23 | 2012-09-26 | 中国科学院苏州纳米技术与纳米仿生研究所 | Method for preparing voltage modulation ultraviolet bicolor photoelectric response detector |
| CN102694067B (en) * | 2012-05-23 | 2016-04-27 | 中国科学院苏州纳米技术与纳米仿生研究所 | The preparation method of the detector of the ultraviolet two-color photoelectric respone of voltage modulated |
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| CN104701391B (en) * | 2015-03-16 | 2017-03-15 | 中国科学院宁波材料技术与工程研究所 | A kind of photoelectric information conversion element and its application |
| CN106159035A (en) * | 2015-04-09 | 2016-11-23 | 纳米新能源（唐山）有限责任公司 | The method preparing ultraviolet light dependent sensor and the ultraviolet light dependent sensor prepared |
| CN106159035B (en) * | 2015-04-09 | 2018-02-09 | 纳米新能源（唐山）有限责任公司 | The ultraviolet light sensor for preparing the method for ultraviolet light sensor and being prepared |
| CN108511600A (en) * | 2018-02-28 | 2018-09-07 | 云南中烟工业有限责任公司 | A kind of sound causes the preparation method of atomization chip |
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