CN1392286A - Process for prapring vanadium oxide film - Google Patents
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- CN1392286A CN1392286A CN02138793A CN02138793A CN1392286A CN 1392286 A CN1392286 A CN 1392286A CN 02138793 A CN02138793 A CN 02138793A CN 02138793 A CN02138793 A CN 02138793A CN 1392286 A CN1392286 A CN 1392286A
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Abstract
The preparation process of vanadium oxide film includes: cleaning substrate surface; sputtering vanadium film to the substrate in vacuum chamber after the substrate and the target being cleaned with parallel particle beam and focused particle beam; oxidizing the vanadium film in an annealing furnace heated in argon atmosphere and filled with oxygen to prepare vanadium oxide film; annealing the vanadium oxide film in pure argon atmosphere; and cooling in argon environment to room temperature. The said process results in compact film with high adhesion to the substrate, no need of strict control in reaction gas flow rate, high repeatability and capacity of preparing vanadium oxide film with different chemical composition for different requirement.
Description
Technical field
The invention belongs to information science and technical field, be specifically related to a kind of method for preparing vanadium oxide film.
Background technology
Since Bell Laboratory found that first vanadium oxide film has the phase transition temperature characteristic, vanadium oxide film had caused various countries investigators' extensive interest from later 1950s Morin.Result of study shows: vanadium oxide film has reversible phase transition temperature characteristic, and at normal temperatures, vanadium oxide film presents the semi-conductor attitude, is tetragonal lattice structure, has higher resistivity and infrared waves transmitance; When the film temperature rising reached transformation temperature, the microtexture and the photoelectric characteristic of film were undergone mutation; This moment, vanadium oxide film changed monoclinic structure into by tetragonal lattice structure, and film presents metallic state, and resistivity reduces rapidly, and infrared waves is presented higher reflection potential, and this variation is a reversible.Because this characteristic of vanadium oxide film, so vanadium oxide thin film material all has good application prospects such as fields such as the automatic protections of novel light storage device, Novel MOS transistor switching circuit, the infrared glimmer switch of inversion of phases and anti-intense laser radiation.What is particularly worth mentioning is that, though with VO
2For the vanadium oxide mixed phase polycrystal film of base does not have the phase transition temperature characteristic when the room temperature, but because it has higher temperature coefficient of resistance, in the time of 25 ℃, the representative value of its temperature coefficient of resistance is-2.00 * 10
-2K
-1, be the common metal film 5-10 doubly, so vanadium oxide film also is the ideal material that is used for making the non-refrigeration infrared detector thermistor at present.In the not refrigerant infrared imaging system, also obtained to use very widely with the infrared focus plane of vanadium oxide film as thermistor.
The valency of vanadium has 2
+, 3
+, 4
+With 5
+Valency and can form nearly 13 kinds of different phase structures behind the oxygen reaction, and has at least the vanadium oxide of 8 kinds of phase structures to have the phase transition temperature characteristic.For VO
2, its typical transformation temperature is 68 ℃, stress and doping can change transformation temperature.There is several different methods can prepare vanadium oxide film at present, (sees C V Ramana, O M Hussain, B.Srinivasulu, et al.Spectroscopic characterization of electton-beam evaporated V as electron beam evaporation deposition
2O
5Thin films.Thin Solid Films.1997,305:219-266), the reactive ion sputter (is seen S D Hansen, C R Aita.Low temperature reactive sputterdopositon of vanadium oxide.J.Vac.Sci.Technol., 1985, A3 (3): 660-663), chemical vapour deposition (is seen E E Chain.Effect of oxygen in ion-beam sputter deposition of vanadium oxide.J.Vac.Sci.Technol., 1987, A5 (4): 1762-1766) and sol-gel (Sol-Gel) (see F C Case.Lowtemperature deposition of VO
2Thin films.J.Vac.Sci.Technil., 1990, A8 (3): 1395-1398) etc.Adopt the microtexture of different preparation method's prepared vanadium oxide films on different substrates and optics thereof, electricity, magnetism characteristic that bigger difference is all arranged, so the various countries investigator is in the novel method of trying to explore to prepare vanadium oxide film, good with processability, as to satisfy different demands vanadium oxide film.
Vanadium oxide film has multiple different phase structure, and the stable condition of various phase structures is seemingly closer again, and the stable condition of single phase is very narrow, thereby it is relatively more difficult to prepare the single phase oxidation vanadium with strict stoicheiometry.In preparation process, want strict each processing parameter of control, just can prepare the well behaved vanadium oxide film that satisfies the demands.Processing parameter changes a little, and the characteristic of then prepared vanadium oxide film will differ widely, and has reduced the repeatability of technology, has increased the control difficulty of technology.
The particle that ion beam sputtering goes out during ion beam sputtering deposition has than macro-energy, when plated film, can produce bombardment to existing rete, remove film defects, therefore the rete that adopts ion beam sputtering deposition to generate is generally dense, relatively good with the adhesivity of substrate, and the homogeneity of film also is guaranteed easily.Therefore, generally all adopt the method for reactive ion sputter coating to prepare vanadium oxide film both at home and abroad.The reactive ion sputter coating promptly is to feed an amount of reactant gases (O in the process of ion beam sputtering deposition
2), directly generate required vanadium oxide film.But in the process of reactive ion beam sputter coating, because the bombarding ion bundle generally all adopts the bigger Ar of ion beam energy
+Ionic fluid, in the sputter coating process, the energy that sputter generates produces bombardment than higher vanadium oxide particle to the lattice microtexture of the vanadium oxide film that generated, vanadium oxide film on the substrate had damaging action, reduced the phase-change characteristic of vanadium oxide film, though adopt annealing process compensated part to damage, near the prepared vanadium oxide film generally phase transformation effect transformation temperature is compared still slightly gap with additive method (as PECVD).And in the process of ion beam sputtering deposition, because reaction gas flow is subjected to ion beam energy, close flow density, all multifactor restrictions such as base vacuum and Ar airshed, make very important to the accurate control of reaction gas flow, this has just increased the difficulty of method greatly, and has reduced the repeatability of method.
Summary of the invention
The object of the present invention is to provide a kind of new method for preparing vanadium oxide film, this method can overcome the latent defect that the reactive ion sputtering film coating method exists, can avoid the damage of particle beam to the vanadium oxide membrane structure, the compactness of enhanced film and with the adhesivity of substrate; This method need strictness not controlled reaction gas flow in the process of sputter coating, can reduce preparation technology's difficulty, increases the repeatability of technology, can prepare the vanadium oxide film that has the different chemical proportioning, satisfies multiple demand.
For achieving the above object, the present invention may further comprise the steps successively:
(1) substrate surface cleans;
(2) sputter vanadium film:
(2.1) charge into argon gas to the vacuum chamber of laying substrate, adopt parallel particle beam, focusing respectively
Particle cleans substrate and rake thin;
(2.2) sputter is coated with the vanadium film, finishes until plated film;
(3) oxide-diffused and after annealing:
(3.1) heating anneal stove under argon gas atmosphere charges into oxygen after the intensification, oxygen and argon gas
Throughput ratio is 1: 10～10: 1;
(3.2) in addition oxidation of the vanadium film that step (2) is coated with, the preparation vanadium oxide film;
(3.3) after the vanadium film oxidation fully, close oxygen valve, vanadium oxide membrane is annealed in pure argon;
(3.4) after annealing finishes, close annealing furnace, vanadium oxide film at the ar gas environment internal cooling extremely
Room temperature.
The throughput ratio of oxygen and argon gas is 1: 2～2: 1 in the above-mentioned steps (3.1), better effects if when the intensification temperature is 350 ℃-500 ℃.
The contriver has carried out SEM and XPS analysis to the vanadium oxide polycrystal film of present method preparation, and its SEM photo and XPS spectrum figure are respectively as shown in Figures 2 and 3.As shown in Figure 2: prepared vanadium oxide film surface is tangible acicular grains shape, and film surface is smooth, fine and close, and good uniformity presents polycrystalline structure.The electricity of film and optical characteristics are respectively shown in accompanying drawing 4 and accompanying drawing 5, by among the figure as can be known: vanadium oxide film presents the resistivity catastrophe characteristics near transformation temperature (68 ℃), infrared (2.5um) transmitance of film variation before and after phase transformation has reached 60%, (electrology characteristic is seen embodiment 1, and optical characteristics sees it is embodiment 2).Data shows: if be coated with special film at film surface be, the change of infrared transmittivity will reach 90%, can satisfy infrared glimmer switch and the anti-light laser requirement of the required film of protection system automatically fully.
In order to be illustrated more clearly in the characteristics of present method, enumerate following table comparative illustration in addition.
Table 1 reactive ion beam sputter coating and present method contrast
| Method name | The reactive ion sputter coating | Ion beam sputtering plating vanadium film and rear oxidation annealing |
| The method flow difference | In coating process, feed reactant gases O 2The preparation vanadium oxide film | Do not feed reactant gases in the coating process, vanadium oxide membrane prepares vanadium oxide film |
| The after annealing method | Need the after annealing method | Need the after annealing method |
| The method difficulty | Need strict control reaction gas flow during sputter | When rear oxidation, need the pilot-gas throughput ratio |
| The method repeatability | Lower | Higher |
| Lattice damage | The part lattice damage | A small amount of lattice damage |
| Phase-change characteristic | Phase-change characteristic is arranged | Phase-change characteristic is obvious |
| Temperature coefficient of resistance | ????-0.018K -1 | ??-0.021K -1 |
| The infrared spectra transmitance changes before and after the phase transformation | 60% (under the more excellent method condition of strictness) | 60% (under the general method condition) |
Description of drawings:
Fig. 1 is Si
3N
4The SEM photo of V film on the substrate;
Fig. 2 is Si
3N
4The SEM photo of vanadium oxide film on the substrate;
Fig. 3 is Si
3N
4VO on the substrate
2The XPS spectrum figure of film;
Fig. 4 is the resistivity-temperature relation curve of vanadium oxide film;
Fig. 5 is the spectral transmittance-temperature curve of vanadium oxide film.
Embodiment
The present invention is further detailed explanation in the mode enumerated below.
Embodiment 1:(1) method purpose: preparation has the vanadium oxide film of high temperature coefficient of resistance, is used for the non-refrigeration infrared detector thermosensitive material film.(2) substrate material: Si (3) preparation flow: 1. clean substrate.Adopt the standard semiconductor purging method to clean substrate, substrate is cleaned up the back dry for standby.2. sputter vanadium film.Open vacuum chamber, put into the Si substrate, take out rough vacuum earlier, drive high valve then, pumping high vacuum.After pumping high vacuum arrives preset value, charge into argon gas and arrive operating air pressure.Open collimated source, clean the Si substrate with parallel ionic fluid earlier, close collimated source then, open the focusing source, clean rake thin, cleaning is opened baffle plate after finishing, the beginning sputter coating.The method parameter table of sputter coating is as shown in table 2:
Table 2: embodiment 1 sputter coating parameter list
3. oxidizing annealing.The substrate that is coated with the vanadium film is placed in the annealing furnace, feeds argon gas, annealing furnace begins heating, be heated to design temperature after, open oxygen valve, regulate oxygen and argon flow amount and after arriving preset value, begin vanadium oxide film.Method for oxidation is closed oxygen valve after finishing, and substrate is annealed in ar gas environment.Annealing is closed annealing furnace after finishing, and naturally cools to room temperature, closes argon gas.Method for annealing finishes.The method parameter tabulation is as shown in table 3:
| Base vacuum | ????＜3×10 -3Pa |
| Operating air pressure | ????2×10 -2Pa |
| Ion beam energy (cleaning substrate) | ????500eV |
| Screen-grid current (cleaning substrate) | ????40mA |
| Ion beam energy | ????800eV |
| Screen-grid current | ????70mA |
| The plated film time | ????3min |
| Underlayer temperature | ????200℃ |
Table 3 embodiment 1 oxidizing annealing method parameter table
(4) film characteristics
| Reactant gases | ????Ar，O2 |
| Gas flow ratio | ????2∶1 |
| Argon flow amount | 60 lattice |
| Oxidizing temperature | ????388-390℃ |
| Oxidization time | ????60min |
| Annealing time | ????60min |
Infrared eye is its temperature coefficient of resistance with the most important parameter of vanadium oxide film, adopts the temperature coefficient of resistance of the vanadium oxide film of present method preparation to reach-0.021K in room temperature (25 ℃) time
-1, than adopt the reactive ion sputter coating prepared-0.018K
-1Improved 14%.
Embodiment 2:(1) method purpose: preparation has the vanadium oxide film of high phase-change characteristic, is used for inversion of phases glimmer switch (2) substrate material: Si
3N
4(3) preparation flow: preparation flow and embodiment 1 are basic identical, but method parameter has difference slightly.Table 4, table 5 are respectively the method parameter tables of this embodiment
Table 4: embodiment 2 sputter coating parameter lists
Table 5 embodiment 2 oxidizing annealing method parameter tables
(4) film characteristics
| Base vacuum | ????＜3×10 -3Pa |
| Operating air pressure | ????2×10 -2Pa |
| Ion beam energy (cleaning substrate) | ????500eV |
| Screen-grid current (cleaning substrate) | ????40mA |
| Ion beam energy | ????800eV |
| Screen-grid current | ????70mA |
| The plated film time | ????10min |
| Underlayer temperature | ????250℃ |
| Reactant gases | ????Ar，O2 |
| Gas flow ratio | ????1∶2 |
| Argon flow amount | 60 lattice |
| Oxidizing temperature | ????400℃ |
| Oxidization time | ????90min |
| Annealing time | ????60min |
Inversion of phases glimmer switch important parameters is its phase-change characteristic, and phase-change characteristic is good more, shows that then the characteristic of vanadium oxide film is good more.Adopt present method at Si
3N
4The vanadium oxide film that substrate prepares above change in resistance before and after phase transformation can reach 3 orders of magnitude, the infrared spectra transmitance changes before and after phase transformation can reach 60%, can compare favourably with adopt the prepared vanadium oxide film of reactive ion beam under the rigorous method condition.Embodiment 3:(1) method purpose: preparation is used for the vanadium oxide film with high temperature coefficient of resistance (2) substrate material: the Si of infrared eye
3N
4(3) preparation flow: preparation flow and embodiment 1 are basic identical, but the oxidizing annealing parameter has slightly than big difference.
Table 6 is the oxidizing annealing parameter list of this embodiment
Embodiment 4:(1) method purpose: preparation is used for the vanadium oxide film with high phase-change characteristic of inversion of phases glimmer switch.(2) substrate material: SiO
2(3) preparation flow: preparation flow and embodiment 2 are basic identical, and only the oxidizing annealing parameter has difference slightly.
| Reactant gases | ????Ar，O2 |
| Gas flow ratio | ????10∶1 |
| Argon flow amount | 60 lattice |
| Oxidizing temperature | ????390℃ |
| Oxidization time | ????60min |
| Annealing time | ????60min |
Table 7 is the oxidizing annealing parameter list of this embodiment
| Reactant gases | ????Ar，O2 |
| Gas flow ratio | ????1∶10 |
| Argon flow amount | 60 lattice |
| Oxidizing temperature | ????420℃ |
| Oxidization time | ????90min |
| Annealing time | ????60min |
Claims (3)
1. method for preparing vanadium oxide film may further comprise the steps successively:
(1) substrate surface cleans;
(2) sputter vanadium film, its flow process is:
(2.1) charge into argon gas to the vacuum chamber of laying substrate, adopt parallel particle beam, focused particle respectively
Clean substrate and rake thin;
(2.2) sputter is coated with the vanadium film, finishes until plated film;
(3) oxide-diffused and after annealing, its flow process is:
(3.1) heating anneal stove under argon gas atmosphere charges into oxygen after the intensification, the stream of oxygen and argon gas
Amount is than being 1: 10～10: 1;
(3.2) in addition oxidation of the vanadium film that step (2) is coated with, the preparation vanadium oxide film;
(3.3) after the vanadium film oxidation fully, close oxygen valve, vanadium oxide membrane is annealed in pure argon;
(3.4) after annealing finishes, close annealing furnace, vanadium oxide film at the ar gas environment internal cooling to the chamber
Temperature.
2. the method for preparing vanadium oxide film according to claim 1 is characterized in that: the throughput ratio of oxygen and argon gas is 1: 2～2: 1 in the described step (3.1).
3. the method for preparing vanadium oxide film according to claim 1 and 2 is characterized in that: the intensification temperature is 350 ℃～500 ℃ in the described step (3.1).
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| CN1308482C (en) * | 2004-08-25 | 2007-04-04 | 华中科技大学 | Process for preparing vanadium oxide film capable of regulating phase change temp. |
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