CN107779831A - The method that magnetron sputtering prepares A phase hypovanadic oxide films - Google Patents

The method that magnetron sputtering prepares A phase hypovanadic oxide films Download PDF

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CN107779831A
CN107779831A CN201610744315.6A CN201610744315A CN107779831A CN 107779831 A CN107779831 A CN 107779831A CN 201610744315 A CN201610744315 A CN 201610744315A CN 107779831 A CN107779831 A CN 107779831A
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face
target
vanadium
phase hypovanadic
substrate
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CN107779831B (en
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曹逊
金平实
孙光耀
李�荣
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Shanghai Institute of Ceramics of CAS
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Shanghai Institute of Ceramics of CAS
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/0021—Reactive sputtering or evaporation
    • C23C14/0036—Reactive sputtering
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides
    • C23C14/083—Oxides of refractory metals or yttrium

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

The present invention relates to the method that magnetron sputtering prepares A phase hypovanadic oxide films, using vanadium metal target or vanadium oxide ceramic target as target, the target is sputtered using argon gas as sputter gas and by reacting gas of oxygen to form A phase hypovanadic oxide films on substrate.The cell parameter of A phase hypovanadic oxides is aA=0.844nm,bA=0.844nm,cA=0.767nm, substrate lattice parameter is used to be matched with A phase hypovanadic oxides for key of the invention.

Description

The method that magnetron sputtering prepares A phase hypovanadic oxide films
Technical field
Present invention relates particularly to a kind of method for preparing A phase hypovanadic oxide films in utilization magnetron sputtering, belong to new nothing Machine field of functional materials.
Background technology
The tetravalent oxide vanadium dioxide crystal phase structure species of vanadium is various, it is known that structure have Rutile Type structure (R phases), Monocline phase structure (M phases), three monoclinic phase structures (T-phase), and interphase A phases and B phases.M phases therein and R phase hypovanadic oxides due to Can mutually it convert, and phase transition temperature is close to room temperature, and receive significant attention, before Intelligent energy-saving window etc. has application Scape.And the research on the interphase A phases of vanadium dioxide is relatively fewer.
A phase hypovanadic oxides VO2(A) found first by Theobald, Oka has found VO for the first time afterwards2(A) phase transformation Characteristic, phase transition temperature is about 165 DEG C, and gives VO2(A) specific crystal structure and lattice parameter before and after phase transformation.But VO2(A) difficult, the only method of Hydrothermal Synthesiss, and VO in the document reported at present is prepared2(A) it is unstable so that prepare compared with Pure VO2(A) it is more difficult.
Research on vanadium dioxide film preparation method has just measured greatly like the mushrooms after rain since the seventies in last century Existing, in numerous synthetic methods, for physics magnetron sputtering method due to the prospect with extensive industrialization, product is uniform and stable, Repeated strong, automaticity is high and receives much concern.However, sputtering method prepares the current still blank of research of A phase hypovanadic oxides.
The content of the invention
The present invention prepares A phase hypovanadic oxide films using magnetron sputtering, it is therefore intended that makes up physical sputtering method and is preparing A phases The blank of vanadium dioxide film, enrich functional compounds preparation method.
Therefore, the invention provides a kind of method that magnetron sputtering prepares A phase hypovanadic oxide films, with vanadium metal target or oxygen Change vanadium ceramic target as target, the target is sputtered using argon gas as sputter gas and by reacting gas of oxygen with A phase hypovanadic oxide films are formed on substrate, the substrate is (110) face strontium titanates STO, (110) face lanthanum aluminate LAO, (110) Face PMN-PT PMN-PT, (110) face strontium aluminate tantalum lanthanum LAST, (110) face strontium aluminate tantalum neodymium NSAT, (110) face Gallic acid neodymium NdGaO3, (110) face scandium acid yttrium YScO3, (110) face scandium acid holmium HoScO3, (110) face scandium acid terbium TbScO3、(110) Face scandium acid dysprosium DyScO3, (110) face scandium acid gadolinium GdScO3At least one of.
The cell parameter of A phase hypovanadic oxides is aA=0.844nm, bA=0.844nm, cA=0.767nm, it is brilliant using substrate Lattice parameter is matched with A phase hypovanadic oxides as the key of the present invention.Therefore, the present invention using vanadium metal target or vanadium oxide ceramic target as Target, and from suitable substrate (for example, ((110) face strontium titanates STO, (110) face lanthanum aluminate LAO, (110) face magnoniobate Lead-lead titanates PMN-PT, (110) face strontium aluminate tantalum lanthanum LAST, (110) face strontium aluminate tantalum neodymium NSAT, (110) face gallic acid neodymium NdGaO3, (110) face scandium acid yttrium YScO3, (110) face scandium acid holmium HoScO3, (110) face scandium acid terbium TbScO3, (110) face scandium acid Dysprosium DyScO3, (110) face scandium acid gadolinium GdScO3Deng) prepare A phase hypovanadic oxides.Wherein described substrate is deposited with pure A phase hypovanadic oxides In following epitaxial relationshipcVO2(A)≈2aSubstrate, outside the growth of the suitable A phase hypovanadic oxides of substrate Prolong.By taking strontium titanates substrate as an example, strontium titanates is perovskite structure, cell parameter aSTO=0.3905nm, therefore for (110) face , epitaxial relationship be present in strontium titanates substrate cVO2(A)(=0.767nm) ≈ 2aSTO(0.781nm), therefore (110) face strontium titanates substrate suitable A phase hypovanadic oxides growth extension.
The present invention forms A phase hypovanadic oxide films without moving back by being sputtered to the target directly on substrate Fire processing.
In the present invention, the oxygen purity is more than 99.99%, the purity more than 99.99% of the argon gas.
In the present invention, the vanadium metal target is the vanadium metal that purity is more than 99.99%, or the vanadium oxide ceramic target is By hot pressed sintering after at least one of vanadic anhydride powder, hypovanadic oxide powder, vanadium trioxide powder uniformly mixing Into.
The present invention prepares A phase hypovanadic oxide films using magnetron sputtering, and its depositing temperature is 350~500 DEG C, deposition total head It is 1~5% for 0.5~5.0Pa, oxygen partial pressure.
The present invention prepares A phase hypovanadic oxide films using magnetron sputtering, and it is 5~10 × 10 to control back end vacuum-5Pa, sputtering Power is 50~150W, and sputtering time is 5~300 minutes.
The method of the invention is simple to operate, is easily controlled, and gained film can be used for battery, hydrogen storage and optoelectronic switch etc. Aspect.
Brief description of the drawings
The XRD diffraction patterns of vanadium dioxide film prepared by Fig. 1 embodiments 1；
The XRD diffraction patterns of vanadium dioxide film prepared by Fig. 2 embodiments 2.
Embodiment
The present invention is further illustrated below by way of following embodiments, it should be appreciated that following embodiments are merely to illustrate this Invention, is not intended to limit the present invention.
The present invention is that (target selects to depend on sputtering equipment target rifle for vanadium metal target or vanadium dioxide ceramic target using sputtering target material Size), sputter gas is argon gas, and reacting gas is oxygen.And depositing temperature (for example, 350~500 DEG C) is controlled, deposit total head The parameter such as (for example, 0.5~5.0Pa), oxygen partial pressure (for example, 1~5%), the A of high-purity is formed under the conditions of suitable substrate Phase hypovanadic oxide film.
Substrate can be selected as (110) face strontium titanates STO, (110) face lanthanum aluminate LAO, (110) face PMN-PT PMN-PT, (110) face strontium aluminate tantalum lanthanum LAST, (110) face strontium aluminate tantalum neodymium NSAT, (110) face gallic acid neodymium NdGaO3、(110) Face scandium acid yttrium YScO3, (110) face scandium acid holmium HoScO3, (110) face scandium acid terbium TbScO3, (110) face scandium acid dysprosium DyScO3、 (110) face scandium acid gadolinium GdScO3At least one of.
Argon gas and oxygen as sputter gas and reacting gas, which preferably use, passes through high-purity gas, equal for example with purity For more than 99.99% oxygen and argon gas respectively as reacting gas and sputter gas.
Vanadium metal target can be vanadium metal, the vanadium metal for being preferably more than 99.99% for purity.Or the vanadium oxide ceramics Target is burnt by hot pressing after at least one of vanadic anhydride powder, hypovanadic oxide powder, vanadium trioxide powder uniformly mixing Knot forms.As an example, the powder of selection vanadic anhydride and vanadium trioxide, according to 1.5:After 1 mol ratio proportioning Fine grinding is sufficiently mixed, the temperature of hot pressing can be 580~640 DEG C, and pressure can be 20~60MPa.
The present invention forms A phase hypovanadic oxide films without moving back by being sputtered to the target directly on substrate Fire processing.Wherein, it can be 5~10 × 10 to control back end vacuum-5Pa, sputtering power can be 50~150W, sputtering time can be 5~ 300 minutes.
Magnetron sputtering of the present invention prepares the purposes of the method for A phase hypovanadic oxide films, including as battery, hydrogen storage with And optoelectronic switch etc..
Embodiment is enumerated further below to describe the present invention in detail.It will similarly be understood that following examples are served only for this Invention is further described, it is impossible to is interpreted as limiting the scope of the invention, those skilled in the art is according to this hair Some nonessential modifications and adaptations that bright the above is made belong to protection scope of the present invention.Following examples are specific Technological parameter etc. is also only an example in OK range, i.e. those skilled in the art can be done properly by this paper explanation In the range of select, and do not really want to be defined in the concrete numerical value of hereafter example.
Embodiment 1
Using vanadium dioxide ceramic target, sputter gas is the argon gas of purity 99.99%, and reacting gas is the oxygen of purity 99.99% Gas, it is 1 × 10 to control back end vacuum-4450 DEG C of Pa, depositing temperature, deposit total head 3.0Pa, oxygen partial pressure 1%, sputtering power 100W, sputters vanadium dioxide film 70 minutes on the strontium titanates substrate of (110) face.Natural cooling cools after the completion of sputtering.
X-ray diffraction sign is carried out to the film of acquisition, as a result sees accompanying drawing 1.The use of X-ray diffraction is directional light incidence mould Formula, θ -2 θ scannings.It will be noted from fig. 1 that the sample obtained is A phase hypovanadic oxides, thin film epitaxy pattern is that (100) orientation is outer Prolong.Without other miscellaneous peaks in addition to substrate and A phase hypovanadic oxides in collection of illustrative plates, it was demonstrated that the sample thing phase purity of acquisition is high.
Embodiment 2
Using vanadium dioxide ceramic target, sputter gas is the argon gas of purity 99.99%, and reacting gas is the oxygen of purity 99.99% Gas, it is 8 × 10 to control back end vacuum-5500 DEG C of Pa, depositing temperature, deposit total head 3.0Pa, oxygen partial pressure 5%, sputtering power 70W, sputters vanadium dioxide film 120 minutes in the lanthanum aluminate substrate of (110) face.Natural cooling cools after the completion of sputtering.
X-ray diffraction sign is carried out to the film of acquisition, as a result sees accompanying drawing 2.The use of X-ray diffraction is directional light incidence mould Formula, θ -2 θ scannings.From fig. 2 it can be seen that the sample obtained is A phase hypovanadic oxides, thin film epitaxy pattern is that (100) orientation is outer Prolong.Without other miscellaneous peaks in addition to substrate and A phase hypovanadic oxides in collection of illustrative plates, it was demonstrated that the sample thing phase purity of acquisition is high.
Embodiment 3
Using vanadium dioxide ceramic target, sputter gas is the argon gas of purity 99.99%, and reacting gas is the oxygen of purity 99.99% Gas, it is 5 × 10 to control back end vacuum-5200 DEG C of Pa, depositing temperature, deposit total head 1.0Pa, oxygen partial pressure 3%, sputtering power 120W, in (110) face scandium acid dysprosium (DyScO3) vanadium dioxide film is sputtered on substrate 40 minutes.Natural cooling drops after the completion of sputtering Temperature.Sample is characterized, it was demonstrated that scandium acid dysprosium (DyScO3) (100) direction and VO2(A) phase Lattice Matching, A phase titanium dioxides are obtained Vanadium film.
Embodiment 4
Using vanadium metal target, sputter gas is the argon gas of purity 99.99%, and reacting gas is the oxygen of purity 99.99%, is controlled Back end vacuum is 8 × 10-5300 DEG C of Pa, depositing temperature, deposition total head 5.0Pa, oxygen partial pressure 5%, sputtering power 60W, (110) vanadium dioxide film is sputtered on face PMN-PT substrates 120 minutes.Natural cooling cools after the completion of sputtering.Sample is carried out Characterize, it was demonstrated that obtain A phase hypovanadic oxide films.
The present invention is described in detail above, apply specific example in text is illustrated to the present invention, this It is to be understood that for the ease of those skilled in the art and using the present invention.Those skilled in the art can be easy Various modifications are made on ground to these embodiments, and the thought in the present invention is applied in other embodiment without by creating The work of property.Therefore, the invention is not restricted to embodiment here, those skilled in the art are according to announcement of the invention, for this Invent the improvement made and modification all should be within protection scope of the present invention.

Claims (6)

1. a kind of method that magnetron sputtering prepares A phase hypovanadic oxide films, it is characterised in that with vanadium metal target or vanadium oxide ceramics Target is sputtered with substrate as target using argon gas as sputter gas and by reacting gas of oxygen to the target A phase hypovanadic oxide films are formed, the substrate is（110）Face strontium titanates STO,（110）Face lanthanum aluminate LAO,（110）Face magnoniobate Lead-lead titanates PMN-PT,（110）Face strontium aluminate tantalum lanthanum LAST,（110）Face strontium aluminate tantalum neodymium NSAT,（110）Face gallic acid neodymium NdGaO3、（110）Face scandium acid yttrium YScO3、（110）Face scandium acid holmium HoScO3、（110）Face scandium acid terbium TbScO3、（110）Face scandium acid Dysprosium DyScO3、（110）Face scandium acid gadolinium GdScO3At least one of.
2. according to the method for claim 1, it is characterised in that by being sputtered the target with directly on substrate A phase hypovanadic oxides film is formed without annealing.
3. method according to claim 1 or 2, it is characterised in that the oxygen purity is more than 99.99%, the argon gas Purity be 99.99%.
4. according to the method any one of claim 1-3, it is characterised in that the vanadium metal target is vanadium metal, preferably The vanadium metal for being more than 99.99% for purity, or the vanadium oxide ceramic target be by vanadic anhydride powder, hypovanadic oxide powder, Hot pressed sintering forms after at least one of vanadium trioxide powder uniformly mixes.
5. according to the method any one of claim 1-4, it is characterised in that depositing temperature is 350~500 DEG C, deposition Total head is 0.5~5.0Pa, and oxygen partial pressure is 1~5%.
6. according to the method any one of claim 1-5, it is characterised in that it is 5~10 × 10 to control back end vacuum-5 Pa, sputtering power are 50~150W, and sputtering time is 5~300 minutes.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108515009A (en) * 2018-04-12 2018-09-11 四川星明能源环保科技有限公司 A phase hypovanadic oxide films and preparation method thereof
WO2020125440A1 (en) * 2018-12-18 2020-06-25 深圳先进技术研究院 Method for preparing flexible vanadium oxide thin film by means of two-step method
CN117535624A (en) * 2024-01-10 2024-02-09 季华实验室 Infrared window with vanadium oxide film, and preparation method and application thereof

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CN101863511A (en) * 2010-07-05 2010-10-20 中国科学技术大学 Method for preparing monoclinic phase vanadium dioxide and doped nano powder thereof
TW201229268A (en) * 2011-01-04 2012-07-16 Hon Hai Prec Ind Co Ltd Coated article and method for making the same
CN103420420A (en) * 2013-07-13 2013-12-04 宿州学院 Preparation method for vanadium dioxide nanorod changed from phase B to phase A
CN104032278A (en) * 2014-06-12 2014-09-10 中国科学院上海技术物理研究所 Method for preparing vanadium dioxide film
CN105088166A (en) * 2015-08-24 2015-11-25 中国科学院上海微系统与信息技术研究所 Phase-change type vanadium oxide material and preparing method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101863511A (en) * 2010-07-05 2010-10-20 中国科学技术大学 Method for preparing monoclinic phase vanadium dioxide and doped nano powder thereof
TW201229268A (en) * 2011-01-04 2012-07-16 Hon Hai Prec Ind Co Ltd Coated article and method for making the same
CN103420420A (en) * 2013-07-13 2013-12-04 宿州学院 Preparation method for vanadium dioxide nanorod changed from phase B to phase A
CN104032278A (en) * 2014-06-12 2014-09-10 中国科学院上海技术物理研究所 Method for preparing vanadium dioxide film
CN105088166A (en) * 2015-08-24 2015-11-25 中国科学院上海微系统与信息技术研究所 Phase-change type vanadium oxide material and preparing method thereof

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108515009A (en) * 2018-04-12 2018-09-11 四川星明能源环保科技有限公司 A phase hypovanadic oxide films and preparation method thereof
WO2020125440A1 (en) * 2018-12-18 2020-06-25 深圳先进技术研究院 Method for preparing flexible vanadium oxide thin film by means of two-step method
CN117535624A (en) * 2024-01-10 2024-02-09 季华实验室 Infrared window with vanadium oxide film, and preparation method and application thereof
CN117535624B (en) * 2024-01-10 2024-04-05 季华实验室 Infrared window with vanadium oxide film, and preparation method and application thereof

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