CN1696332A - Method for depositing thin oxide coating through oxygen ion beam in low energy and auxiliary impulse laser - Google Patents
Method for depositing thin oxide coating through oxygen ion beam in low energy and auxiliary impulse laser Download PDFInfo
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- CN1696332A CN1696332A CN 200410044605 CN200410044605A CN1696332A CN 1696332 A CN1696332 A CN 1696332A CN 200410044605 CN200410044605 CN 200410044605 CN 200410044605 A CN200410044605 A CN 200410044605A CN 1696332 A CN1696332 A CN 1696332A
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Abstract
A process for preparing the oxide film on substrate by deposition method includes putting the oxide target and clean substrate in growing chamber, vacuumizing, using pulse laser to irradiate the oxide target, and using low-energy oxygen ion leam generated by low-energy ion beam generator to bombard the substrate.
Description
Technical field
The present invention relates to film preparing technology and ion beam technology, be meant a kind of low energy oxygen ion beam satellite pulse laser deposition (PLD) method that is used for the oxide film material preparation especially.In the process of PLD method growing oxide film, introduce low energy oxygen ion beam assisting growth, the energy and the dose controlled of isotopic pure low energy oxonium ion, have characteristics such as the growth of promotion, low-temperature epitaxy and the oxygenating of realization ultrahigh vacuum(HHV), can effectively improve the sull quality of PLD method, particularly long wavelength's pulsed laser deposition.The auxiliary PLD method of low energy ion beam also can be used for the preparation of the difficult chemical combination thin-film material of other high-melting-points.
Background technology
The sull of using in various fields as semiconductor film, optical thin film, dielectric film and superconducting thin film etc., mostly has the difficult synthetic characteristic of high-melting-point.Be used for preparing these oxide film materials method commonly used pulsed laser deposition (Pulsed laser deposition (PLD)) (also claiming laser ablation evaporation (Laser Ablation) or laser molecular beam epitaxy (Laser-MBE)), magnetron sputtering, chemical vapor deposition (CVD), electron beam evaporation and plasma ion assisted deposition etc. are arranged.Because of the PLD method has that quality of forming film is good, technology is simple, save advantages such as starting material and deposition rate be fast,, more and more be applied to the preparation of various oxide film materials along with the maturation and the progress of high-power pulsed laser in recent years.PLD belongs to a kind of of physical vapor deposition, its principle is to adopt high power pulsed laser bundle ablation target, heat up rapidly under moment irradiation evaporation and eject the vapor slugs (also claiming material plumage group) that has the target composition of target utilizes the material plumage group deposition growing on substrate that is evaporated.PLD prepares in the process of sull, because of the pulse laser of different wave length can make the oxide target material that is evaporated decompose in various degree, long wavelength laser is bigger than the degree of decomposition that short wavelength laser causes, and this makes in thin film composition that growth obtains often anoxic.For replenishing the oxygen of disappearance, the logical a certain amount of oxygen in the growth room of being everlasting, film is grown in oxygen-enriched atmosphere, but this can reduce the vacuum tightness of growth room, and then influence the growth quality of thin-film material, in addition, the oxygen of molecular state is not fine because of chemically reactive, the effective dose of oxygenating is difficult to again grasp, and its effect is not fine sometimes.How to solve the anoxic problem of process of growth, obtain having the high-quality thin film of positive stoicheiometry, be still present PLD legal system and be equipped with the main difficulty that sull will overcome.
Summary of the invention
The objective of the invention is to, a kind of method of low energy oxygen ion beam satellite pulse laser deposition sull is provided, utilize the low energy oxonium ion assisting growth and the ultrahigh vacuum(HHV) oxygenating of isotopic pure.The dose controlled of this method oxygenating can effectively be improved the PLD legal system and be equipped with the quality of sull and realize low-temperature epitaxy, is applicable to various oxide film material preparations.The auxiliary PLD method of low energy ion beam also can be used for the difficult chemical combination thin-film material preparation of other high-melting-points.
The technical scheme that technical solution problem of the present invention is adopted is:
The method of a kind of low energy oxygen ion beam of the present invention satellite pulse laser deposition sull, the deposition growing of oxide film material is to carry out in the impulse laser deposition system of introducing the low energy ion bundle device, wherein: impulse laser deposition system is made of pulsed laser and ultrahigh vacuum(HHV) growth room two portions, and laser target and substrate are arranged in the ultrahigh vacuum(HHV) growth room; The low energy ion bundle device is made of ion source, magnetic analyzer, magnetic or electric quadrupole lens, electrostatic deflection plates and retarding lens and line dosage control device etc., and retarding lens is installed in the ultrahigh vacuum(HHV) growth room; The low energy ion bundle device is used for producing the isotopic pure low energy ion of satellite pulse laser deposition growth; It is characterized in that:
The deposition growing step of oxide film material is as follows:
Substrate after oxide target material and the cleaning is inserted the growth room;
The growth room is vacuumized;
Utilize the pulse laser irradiation oxide target material, the low energy oxygen ion beam bombardment substrate that produces with the low energy ion bundle device simultaneously, low energy oxonium ion do up the effect that assisting growth and additional pulsed laser deposition prepare the oxygen that lacks in the sull process.
The big I of energy of the low energy oxonium ion that low energy ion bundle device wherein provides is added in the voltage of retarding lens by adjustment, in tens accurately controls in the scope of hundreds of electron-volt; The rete that has in low-energy oxonium ion and substrate and the growth interacts, and increased the hot kinetic energy that the PLD method deposits to the oxide molecule on the substrate, plays to promote growth and local heat effect, reduced the growing and preparing temperature of sull.
Wherein said low energy ion bundle device is not destroy under growth room's UHV condition, provide the isotopic pure oxonium ion of atomic state to replenish the oxygen that lacks in the pulsed laser deposition growing oxide film process, the dosage of delivery of supplemental oxygen causes oxide target material to lack the degree of oxygen according to pulse laser, is accurately controlled by the line dosage control device of this device.
Wherein said ion beam apparatus is the multiple ion-beam device, and when introducing the multiple ion-beam device, with a branch of generation low energy oxonium ion assisting growth, other bundles produce dopant ion and carry out the composition doping.
The low energy oxonium ion that wherein said ion beam apparatus produces substitutes with nitrogen ion or carbon ion, can carry out the difficult bonded nitride of high-melting-point or the carbide thin film material preparation of pulsed laser deposition.
Wherein utilize the YAG pulse laser of the auxiliary long wavelength 532nm of low energy oxygen ion beam, prepare zinc-oxide film on the silicon substrate.
Description of drawings
For further specifying technology contents of the present invention, be described in detail as follows below in conjunction with embodiment and accompanying drawing, wherein:
Fig. 1 is the auxiliary PLD method of a low energy oxygen ion beam growing oxide film synoptic diagram, and wherein, 1 is pulse laser beam, and 2 is the laser target target, and 3 is the material plumage group of laser evaporation, and 4 is substrate, and 5 is the low energy oxygen ion beam, and 6 is the ultrahigh vacuum(HHV) growth room;
Fig. 2 is the auxiliary pulsed laser deposition composite technology of a low energy double-ion beam system schematic, and wherein, 1 is pulse laser beam, 2 is the laser target target, and 4 is substrate, and 5 is the low energy oxygen ion beam, 6 is the ultrahigh vacuum(HHV) growth room, and 7 is the YAG laser apparatus, and 8 is speculum, 9 is XPS, and 10 is RHEED, and 11 is ion source, 12 is magnetic analyzer, 13 be magnetic (or) quadrupole lens, 14 is electrostatic deflection plates, 15 is retarding lens;
Fig. 3 is the zinc oxide sample that the XRD result of zinc oxide films membrane sample: a has the auxiliary PLD method growth of low energy oxygen ion beam; B does not have the zinc oxide sample figure of the auxiliary PLD method growth of low energy oxonium ion;
Fig. 4 is the XPS and the AES test result figure of the zinc-oxide film of the auxiliary PLD method growth of low energy oxygen ion beam.
Embodiment
The preparation of sull is with reference to Fig. 1, Fig. 2, and detailed process is as follows: in the growth room of earlier substrate 4 after oxide target material 2 and the cleaning being packed into, growth room 6 is vacuumized, reach ultrahigh vacuum(HHV) (＜10
-5Pa) after, open YAG pulsed laser 7, the pulse laser beam 1 of its generation is imported in growth room's (target chamber) 6 through speculum 8, target 2 on the pulse laser 1 ablative laser target after the line focus, the layer at the target position evaporation that heats up rapidly at the moment of high power pulsed laser irradiation, eject the vapor slugs (also claiming material plumage group) 3 that has oxide components, in oxide material plumage group on substrate 4 in the deposition growing, utilize the low energy oxygen ion beam 5 bombardment substrates of a branch of generation of low energy double-ion beam system, carry out the oxygen that lacks in assisting growth and the additional process of growth.Oxygen ion beam 5 is to adopt carbon monoxide (CO) as working gas, by producing in Bai Nasi (Bernus) the type ion source 11 of ion beam system, the ionic fluid that produces from ion source is high energy (15KeV), after the magnetic field of magnetic analyzer 12 (also claiming mass analyzer) is selected to analyze, obtain the energetic oxygen ions bundle of isotopic pure, again through the electric deflection of the secondary focusing and the electrostatic deflection plates 14 of magnetic quadrupole lens 13, the energetic oxygen ions bundle of isotopic pure enters ultrahigh vacuum(HHV) growth room 6, before arriving substrate 4, by the retarding lens device 15 in the growth room, the energy of the energetic oxygen ions of isotopic pure is reduced to tens becomes low energy ion to hundreds of electron-volt (eV), with the low energy oxygen ion beam bombardment substrate surface of the isotopic pure that obtains, satellite pulse laser carries out film growth at last.The energy of the low energy oxonium ion of assistant depositing, dosage and oxide film growth temperature can be because of the wavelength of pulse laser 1, the different designs as the case may be of kind of growth material; The oxide film material that growth obtains can utilize XPS device 9 to carry out chemical state and composition analysis, and crystalline quality can utilize RHEED device 10 to characterize.
As adopt other ions (as N
+Or C
+) substitute oxygen ion beam of the present invention, also can carry out the preparation of the difficult chemical combination thin-film materials of other high-melting-points (as nitride or carbide) of PLD method.
The beneficial effect that the present invention is compared with prior art had:
Compare with the PLD method sull preparation of carrying out in the oxygen-enriched atmosphere of oxygen of in the growth room, leading to commonly used at present, the low energy oxygen ion beam assisting growth of the isotopic pure that the present invention adopts can be realized the ultrahigh vacuum(HHV) oxygenating under the vacuum degree condition that does not reduce the growth room; The oxonium ion of atomic state has better chemically reactive than the oxygen of molecular state, and the dose controlled of oxygenating; The lotus energy oxonium ion of assisting growth and the rete in substrate and the growth interact, and also can promote film growth and realize low-temperature epitaxy.The auxiliary PLD method of low energy oxygen ion beam can effectively be improved the quality that existing P LD legal system is equipped with sull.As with other ion substitution oxonium ions, the present invention also can be used as the difficult bonded thin-film materials preparation of other high-melting-points of PLD method.Low energy ion beam satellite pulse laser deposition (PLD) method is a kind of thin-film material preparation method with practical value.
Realize the best way of invention:
1, realize the major equipment of invention:
The compacting of pulsed laser deposition equipment, low energy ion beam device, vacuum apparatus (oil-sealed rotary pump, turbomolecular pump (or cryopump), ionic pump etc.), laser target, agglomerating plant etc.;
2. according to the particular case of growth apparatus, design the technological line of enforcement of the present invention.As optical maser wavelength that produces according to pulse laser and thin-film material (sull) classification that will prepare, determine energy, dosage and other growth parameter(s)s of the low energy ion (oxonium ion) of assistant depositing.
Specific embodiment:
Utilize low energy oxygen ion beam satellite pulse laser deposition (PLD) method, on silicon (Si) substrate, prepare zinc oxide (ZnO) film.Adopt common PLD method growing ZnO thin-film, the long laser of radiothermy (as the KrF laser of 248nm or the Nd:YAG laser of 266nm), in being arranged, all can realize the oxygen-enriched atmosphere of no oxygen the single-orientated high-quality growth of c-axle, and adopt long wavelength laser (as 532nm or 1064nm, Nd:YAG laser) even in the oxygen-enriched atmosphere of oxygen is arranged, also be difficult to realize the single-orientated growth of c-axle, this is because in the target plumage of the long wavelength laser carburation by evaporation group, the Zn of decomposition
+The content of composition is many than the short wavelength obviously, even grow on Si (100) substrate that is easy to the ZnO film growth, the c-axle of also all being unrealized is single-orientated, and the O/Zn ratio in the analyzing film can find out that oxygen level is obviously not enough in the film component, sees table 1 for details.
Table 1: the ZnO target plumage group of different wave length pulse laser evaporation characterizes with the composition analysis and the structure properties of prepared ZnO film sample
| Optical maser wavelength (nm) | ZnO target plumage group optical excitation spectrum | The O/Zn ratio of ZnO film sample | The XRD spectrum of ZnO film sample |
| ??1064 | The last one Zn +Excitation peak | ??0.49 | One weak ZnO peak |
| ??532 | One weak Zn +Excitation peak | ??0.80 | One weak ZnO (101) peak |
| ??248 | No Zn +Excitation peak | ??0.98 | The single-orientated ZnO of c-axle (002) peak |
In order to improve the quality of long wavelength's pulse laser growing ZnO thin-film, the present invention utilizes the common oxygen of low energy high purity oxygen ion substitution to carry out oxygenating and assisting growth.Adopt long wavelength's 532nmNd:YAG pulse laser, on Si (111) substrate, prepared and had the single oriented ZnO film of c-axle, the detailed experiments parameter sees Table 2, the experimental result of ZnO film sample is seen accompanying drawing 3,4, can find out have the ZnO film sample of low energy oxonium ion assisting growth obviously to improve from experimental result, the sufficient and approaching positive chemistry ratio of oxygen composition in the rete than the auxiliary quality of forming film of no low energy oxonium ion.Experimental result contrast with common PLD method sees Table 3, can find out that also the present invention has realized ultrahigh vacuum(HHV) oxygenating (5 * 10
-6And obviously improved the ZnO film quality (it is single-orientated to prepare the C-axle with height, near the high-quality thin film of positive chemical ratio) that the Nd:YAG laser of long wavelength 532nm is grown on the Si substrate Pa) and low-temperature epitaxy (200 ℃).
Table 2: adopt the auxiliary PLD legal system of low energy oxygen ion beam to be equipped with the experiment parameter of ZnO film sample
| The pulse laser parameter | Laser type | The Nd:YAG solid statelaser |
| Pulse laser wavelength | ??532nm | |
| Pulsewidth | ??20ns | |
| Energy density | ??5J/cm 2 | |
| Pulse- |
3 times/second | |
| The laser target material | The 99.99%ZnO powder forms through high-pressure sinter | |
| The distance of laser target and substrate | ??50mm | |
| Target plumage group deposits to Substrate Area | ??20mm×5mm | |
| The low energy ion beam parameter | The ion source material | CO gas |
| The ion of assisting growth | ??O + | |
| Ion energy | ??80eV | |
| Ion dose | ??5×10 13/s.cm 2 | |
| ZnO film growth parameter | Substrate | P-Si (111) (resistance is 7～11 Ω .cm) carries out organic solvent cleaning and deoxidation layer and handles before the growth |
| Growth temperature | ??200℃ | |
| Growth room's vacuum tightness | ??5×10
-6 | |
| Growth time | ||
| 6 hours | ||
| Sample area | ??20mm×20mm |
| The ZnO films test is analyzed | X-ray diffraction (XRD) | C-axle with height is single-orientated, and X ray rocking curve (XRC) halfwidth (FWHM) at ZnO (002) peak only is 2.2 ° |
| X-ray photoelectron power spectrum (XPS) | Film has the chemical structure state of ZnO | |
| Auger spectroscopy depth analysis (AES) | The distributed components of Zn and O in the rete approaches positive chemistry ratio |
Table 3: the auxiliary PLD method of low energy oxygen ion beam contrasts with the ZnO sample result of PLD method preparation usually
| The low energy oxygen ion beam is assisted the PLD method | Common PLD method | |
| The oxygenating mode | Low energy oxygen ion beam assisting growth | Logical oxygen is grown in oxygen-enriched atmosphere |
| Growth room's vacuum tightness | ??5×10 -6Pa | ??5×10 -1Pa |
| Growth temperature | ??200℃ | ??350-500℃ |
| Utilize the quality of the Nd:YAG Solid State Laser growing ZnO thin-film of 532 nm | It is single-orientated to prepare the c-axle with height on Si (111) substrate, near the high-quality thin film of positive chemical ratio | Can not realize having the single-orientated film growth of c-axle of positive chemical ratio |
Claims (6)
1, a kind of method of low energy oxygen ion beam satellite pulse laser deposition sull, the deposition growing of oxide film material is to carry out in the impulse laser deposition system of introducing the low energy ion bundle device, wherein: impulse laser deposition system is made of pulsed laser and ultrahigh vacuum(HHV) growth room two portions, and laser target and substrate are arranged in the ultrahigh vacuum(HHV) growth room; The low energy ion bundle device is made of ion source, magnetic analyzer, magnetic or electric quadrupole lens, electrostatic deflection plates and retarding lens and line dosage control device etc., and retarding lens is installed in the ultrahigh vacuum(HHV) growth room; The low energy ion bundle device is used for producing the isotopic pure low energy ion of satellite pulse laser deposition growth; It is characterized in that:
The deposition growing step of oxide film material is as follows:
Substrate after oxide target material and the cleaning is inserted the growth room;
The growth room is vacuumized;
Utilize the pulse laser irradiation oxide target material, the low energy oxygen ion beam bombardment substrate that produces with the low energy ion bundle device simultaneously, low energy oxonium ion do up the effect that assisting growth and additional pulsed laser deposition prepare the oxygen that lacks in the sull process.
2, the method for low energy oxygen ion beam satellite pulse laser deposition sull according to claim 1, it is characterized in that, the big I of energy of the low energy oxonium ion that low energy ion bundle device wherein provides is added in the voltage of retarding lens by adjustment, in tens accurately controls in the scope of hundreds of electron-volt; The rete that has in low-energy oxonium ion and substrate and the growth interacts, and increased the hot kinetic energy that the PLD method deposits to the oxide molecule on the substrate, plays to promote growth and local heat effect, reduced the growing and preparing temperature of sull.
3. the method for low energy oxygen ion beam satellite pulse laser deposition sull according to claim 1, it is characterized in that, wherein said low energy ion bundle device is not destroy under growth room's UHV condition, provide the isotopic pure oxonium ion of atomic state to replenish the oxygen that lacks in the pulsed laser deposition growing oxide film process, the dosage of delivery of supplemental oxygen causes oxide target material to lack the degree of oxygen according to pulse laser, is accurately controlled by the line dosage control device of this device.
4. the method for low energy oxygen ion beam satellite pulse laser deposition sull according to claim 1, it is characterized in that, wherein said ion beam apparatus is the multiple ion-beam device, when introducing the multiple ion-beam device, with a branch of generation low energy oxonium ion assisting growth, other bundles produce dopant ion and carry out the composition doping.
5. the method for low energy oxygen ion beam satellite pulse laser deposition sull according to claim 1, it is characterized in that, the low energy oxonium ion that wherein said ion beam apparatus produces substitutes with nitrogen ion or carbon ion, can carry out the difficult bonded nitride of high-melting-point or the carbide thin film material preparation of pulsed laser deposition.
6. according to the method for claim 1,2,3 described low energy oxygen ion beam satellite pulse laser deposition sulls, it is characterized in that, wherein utilize the YAG pulse laser of the auxiliary long wavelength 532nm of low energy oxygen ion beam, prepare zinc-oxide film on the silicon substrate.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101437644B (en) * | 2006-02-23 | 2012-07-04 | 皮科德昂有限公司 | Coating method |
| CN101094003B (en) * | 2006-05-30 | 2013-08-21 | 富士通株式会社 | System and method for independently adjusting multiple offset compensations applied to a signal |
| CN107884918A (en) * | 2017-11-13 | 2018-04-06 | 中国科学院合肥物质科学研究院 | High energy ultraviolet laser gatherer under a kind of high-intensity magnetic field |
| CN110144553A (en) * | 2019-04-09 | 2019-08-20 | 复旦大学 | Large area atom level precision laser MBE grown preparation system and method |
| CN114059022A (en) * | 2021-11-09 | 2022-02-18 | 西安交通大学 | PLD system provided with hollow cathode plasma and preparation method of film |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH05302163A (en) * | 1992-04-27 | 1993-11-16 | Sumitomo Electric Ind Ltd | Formation of multiple-oxide superconducting thin film |
| CN1042149C (en) * | 1993-05-21 | 1999-02-17 | 中国科学院上海冶金研究所 | Forming mould for platinum film deposition by ion beam and its technology |
| CN1094524C (en) * | 1999-12-24 | 2002-11-20 | 中国科学院上海冶金研究所 | Process for growing piezoelectric film of aluminium nitride on substrate of high-sound-velocity material |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101437644B (en) * | 2006-02-23 | 2012-07-04 | 皮科德昂有限公司 | Coating method |
| CN101094003B (en) * | 2006-05-30 | 2013-08-21 | 富士通株式会社 | System and method for independently adjusting multiple offset compensations applied to a signal |
| CN107884918A (en) * | 2017-11-13 | 2018-04-06 | 中国科学院合肥物质科学研究院 | High energy ultraviolet laser gatherer under a kind of high-intensity magnetic field |
| CN110144553A (en) * | 2019-04-09 | 2019-08-20 | 复旦大学 | Large area atom level precision laser MBE grown preparation system and method |
| CN110144553B (en) * | 2019-04-09 | 2024-04-23 | 复旦大学 | Large-area atomic-level precision laser molecular beam epitaxial film preparation system and method |
| CN114059022A (en) * | 2021-11-09 | 2022-02-18 | 西安交通大学 | PLD system provided with hollow cathode plasma and preparation method of film |
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|---|---|
| CN1332062C (en) | 2007-08-15 |
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