CN109023276A - A method of the two-sided MgO film of homoepitaxy is prepared based on mid frequency sputtering - Google Patents
A method of the two-sided MgO film of homoepitaxy is prepared based on mid frequency sputtering Download PDFInfo
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- CN109023276A CN109023276A CN201810994465.1A CN201810994465A CN109023276A CN 109023276 A CN109023276 A CN 109023276A CN 201810994465 A CN201810994465 A CN 201810994465A CN 109023276 A CN109023276 A CN 109023276A
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- base band
- hastelloy
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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
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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
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive sputtering
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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
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
- C23C14/081—Oxides of aluminium, magnesium or beryllium
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- Organic Chemistry (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention belongs to technical field of film preparation, it is related on two sides while is coated with IBAD (ion beam assisted depositing)-MgO/SDP-Y2O3Hastelloy flexibility base band on two sides prepare homoepitaxy MgO film simultaneously, it is specially a kind of that two-sided while homoepitaxy MgO film is prepared based on intermediate frequency (MF) reactive magnetron sputtering.Venthole of the present invention using symmetrical structure in gas dispersion tube, uniform dispersion mixing gas, to solve the problems, such as that the membrane structure of medium frequency magnetron reaction sputtering preparation is non-uniform；The unidirectional design of venthole also target material surface be not directly contacted with oxygen to be oxidized to avoid metallic target, and such intake method improves sputtering yield, advantageously ensures that the uniformity and consistency of the MgO film that two sides is grown simultaneously.Compared to using high cost process complexity physical vapour deposition (PVD) (PVD) method of tradition, intermediate frequency saves buffer layer cost from extension MgO, improves superconducting tape cost performance, and deposition rate is high.
Description
Technical field
The invention belongs to technical field of film preparation, it is related to be coated with IBAD (ion beam assisted depositing)-MgO/SDP (molten
The planarization of liquid deposition)-Y2O3Metal flexible base band on two sides prepare homoepitaxy MgO film simultaneously, during specially one kind is based on
Frequently (MF) reactive magnetron sputtering prepares two-sided homoepitaxy MgO film.
Background technique
YBa2Cu3O7-x(YBCO) band have current-carrying is horizontal high, irreversibility field is high, superconductivity is good under magnetic field, cost compared with
Low advantage, market potential are huge.YBCO superconducting coating have the premise of superior critical current density jc first is that have it is excellent
Good texture orientation, so good texture orientation must be likewise supplied with by growing provided buffer layer substrate for it.It is so first
It pays close attention to and overcomes the problems, such as the substrate for being how to obtain preferable biaxial texture, then provide high quality template for ybco film
To guarantee that it obtains higher performance.And wherein, double-axle texture MgO buffer layer is to provide high quality for conductor of high-temperature superconductor coat
One of important component of template.
The MgO buffer layer mainstream preparation flow of conductor of high-temperature superconductor coat at present are as follows: first with ion-beam assisted deposition
(IBAD) the double-axle texture MgO film that a layer thickness is 8~12nm is deposited in base band, then passes through the method for electron beam evaporation
One layer of thicker MgO film (100nm or so) of homoepitaxy realizes grain-oriented optimization in film.But electron beam evaporation
The shortcomings that be the time required to it is longer, and most energy of electron beam will be taken away by crucible, thus its thermal efficiency is low；In addition it crosses
High heating power also can form stronger heat radiation to entire thin film deposition system, and the membrane structure and pattern prepared are not
Enough ideal (r.m.s. roughness is greater than 3nm).
Medium frequency magnetron reaction sputtering compared to electron beam evaporation growth efficiency it is higher, but intermediate frequency (MF) reactive magnetron sputtering by
It is very fast in the deposition rate when sputtering growing film, it is stringenter to the air-flow field distribution in reaction cavity, if air-flow field distribution
Unevenness then causes film that cannot continuously grow, it cannot be guaranteed that the surface homogeneity of film.
Summary of the invention
In view of the above problems, it in order to solve the deficiency during electron beam evaporation method prepares MgO homoepitaxy, drops
Low production cost improves product cost, optimizes film surface appearance.It is same based on mid frequency sputtering preparation that the present invention provides one kind
The method of the two-sided MgO film of matter extension replaces electron beam evaporation using intermediate frequency (MF) reactive magnetron sputtering, realizes MgO film two
Face is simultaneously from epitaxial growth.
Technical solution is as follows:
Step 1, by Hastelloy flexibility base band to be coated successively through the first winder, gas dispersion tube and volume Two around
Disk installation drives the first winder uniform rotation that Hastelloy flexibility base band is driven at the uniform velocity to move by stepper motor；It breathes out
Family name's alloy flexibility base band two sides is coated with IBAD-MgO/SDP-Y simultaneously2O3。
Gas dispersion tube is placed in the physical centre position among target；The internal cavity of gas dispersion tube is along the base band side of moving
To 4 one-way ventilating hole groups of setting, 4 one-way ventilating hole groups are constituted to be tied by the space of physical centre of Hastelloy flexibility base band
Structure；The venthole being arranged in each one-way ventilating hole group is arranged logical with equal angular towards Hastelloy flexibility base band
Stomata quantity is consistent, aperture is identical.So that the mixed gas sprayed from venthole can be uniformly dispersed in the two sides of base band, formed
Airflow field symmetrically and evenly, thus the film even compact that deposition obtains；And venthole unidirectionally faces Hastelloy flexibility base band,
The characteristics of back to metal targets, it can protect magnesium metal target nearby oxygen concentration be low and be not easy to be oxidized, and near baseband oxygen concentration is high,
Guarantee expeditiously grows two-sided MgO film.Hastelloy flexibility base band to be coated is to the physical centre region among target
Pass through.
Magnesium metal target is respectively disposed on on target by step 2, distinguishes target the two poles of the earth of external intermediate frequency power supply, then to entire
Equipment carries out vacuumize process to 1.0 × 10-3Then Pa is hereinafter, heat Hastelloy flexibility base band；
Step 3 rises to 480-550 degree to Hastelloy flexibility base band temperature, passes through each venthole of gas dispersion tube
It is passed through the mixed gas of argon gas and oxygen；It is then turned on intermediate frequency power supply, using constant voltage mode, keeps voltage constant, current control
In 6A-8A, sputtering power is in 990-1155W；Aura is formed to be formed about plasma bombardment to target, stepper motor drives Kazakhstan
Alloy flexibility base band starts at the uniform velocity through aura area deposition MgO film.
Step 4, after Hastelloy flexibility base band completely at the uniform velocity by closing intermediate frequency power supply behind aura region, stop heating,
Gas inlet pipe is simultaneously closed off, stops molecular pump and mechanical pump, is taken out after Temperature fall, can be prepared by MgO film.
The present invention uniformly disperses reaction gas using the venthole of symmetrical structure in gas dispersion tube, thus in solving
The non-uniform problem of membrane structure of frequency reactive magnetron sputtering preparation.The unidirectional design of venthole also makes target material surface not direct
Contact oxygen is oxidized to avoid metallic target, and such intake method improves sputtering yield, improves the quality of MgO film, has
Conducive to the uniformity and consistency of the MgO film for guaranteeing two sides growth.Compared to using the high cost process complexity physical vapor of tradition
(PVD) method of deposition, intermediate frequency save buffer layer cost from extension MgO, improve superconducting tape cost performance, and deposition rate is high.
Detailed description of the invention
Fig. 1 is the apparatus structure schematic diagram of embodiment；
Fig. 2 is gas dispersion tube structural schematic diagram；
Fig. 3 is that embodiment is two-sided while preparing high energy diffracted electrons rifle (RHEED) diffraction pattern of MgO film；
Fig. 4 be embodiment it is two-sided and meanwhile prepare the X-ray diffractometer of MgO film (XRD) 2Theta figure；
Fig. 5 is that embodiment is two-sided while preparing X-ray diffractometer (XRD) the ω scanning spectra at MgO film (200) peak；
Fig. 6 is that embodiment is two-sided while preparing X-ray diffractometer (XRD) the Φ scanning spectra at MgO film (220) peak.
Appended drawing reference: the first winder of 1-；The second winder of 2-；3,4- magnesium metal target；5- Hastelloy flexibility base band；6-
Mid frequency sputtering reaction chamber；7- air inlet pipe；8- parallelepiped gas dispersion pipe；9- venthole；10,11- self-heating electrode unit；12,
13- intermediate frequency power supply interface；14- DC current source.
Specific embodiment
With reference to the accompanying drawings and examples, technical solution of the present invention is described in detail.
Embodiment: intermediate frequency (MF) reactive magnetron sputtering is used, uses magnesium target as metal sputtering target, is being coated with IBAD-
MgO/SDP-Y2O3500mm long, 10mm wide Hastelloy flexibility base band on medium frequency magnetron sputtering is two-sided while homoepitaxy
One layer of MgO film.
Step 1, preparation, processing base band.By the two-sided IBAD-MgO/SDP-Y for respectively having deposited 10nm2O3Hastelloy it is soft
Property base band be fitted into the first winder 1, the base band other end introduce the second winder 2；Make Hastelloy flexibility base band two sides and oneself
The silver tungsten stick contact for heating electrode unit 10,11 is good, and Hastelloy flexibility base band 5 is at the uniform velocity moved under motor control
It is dynamic.
Step 2, by a length of 80 millimeters, width is 40 millimeters, is respectively symmetrically placed with a thickness of 5 millimeters of magnesium metal target, is formed
To target 3,4, the two poles of the earth of intermediate frequency power supply are connect respectively to target；Then chamber door is shut, successively mechanical pump is opened and molecular pump vacuumizes, make
6 vacuum of reaction chamber is down to 1.0 × 10-3Pa or less；Hastelloy flexibility base band is heated using self-heating mode: opening DC source
14, control electric current is raised slowly to 16A, and because base band and two lateral electrodes and DC source form current loop, flexible base band is because of itself
Resistance generates Joule heat.
Step 3, after electric current stablize after, base band temperature reach from extension MgO grow 500 degree of required temperature；It then passes to
0.5Pa argon gas, 2 × 10-3Pa oxygen, mixed gas are passed through cuboid dispersion pipe 8 by air inlet pipe 7, send forth out from venthole 9
Uniform gas forms uniform airflow field on 5 two sides of base band；
Then, intermediate frequency power supply is opened, intermediate frequency power supply is preheated, under constant power mode, setting power is 1000W, to target
3,4 it is formed about plasma bombardment formation aura.Until destroying the oxidation material on magnesium target surface；After aura is stablized, then it is arranged
Intermediate frequency power supply is constant voltage mode, keeps voltage 170V constant, sputtering power is in 1100W；
After aura is stablized, opens motor and rotate winder 1,2, react Hastelloy flexibility base band 5 in mid frequency sputtering
It is uniformly moved in room, keeping speed is 30 ms/h, and sputtering starts.
Step 4, after Hastelloy flexibility base band completely at the uniform velocity by closing intermediate frequency power supply behind aura region, stop heating,
Gas inlet pipe is simultaneously closed off, stops molecular pump and mechanical pump, is taken out after Temperature fall, can be prepared by MgO film.
High energy diffracted electrons rifle (RHEED) diffraction pattern and X-ray on the above-mentioned two sides two-sided MgO film a, b prepared spread out
Penetrating (XRD), test result is as follows:
Fig. 3 is high energy diffracted electrons rifle (RHEED) diffraction on the two sides a, b that is two-sided in embodiment while preparing MgO film
Figure；As can be seen from the figure the two sides a, b all occurs without annular layout, and diffraction spot is bright, illustrates that there is high twin shaft on two sides
Texture.
Fig. 4 is the XRD 2Theta scanning spectra on the two sides a, b that is two-sided in embodiment while preparing MgO film, can will be double
Face film can determine that (200) peak for MgO, and in addition to substrate peak, have no other miscellaneous peaks at 42.9 ° or so appearance, one strong peak.
Fig. 5 is the Omega scanning spectra at (200) peak on the two sides a, b that is two-sided in embodiment while preparing MgO film, two
Halfwidth is 3.36 ° and 3.71 ° outside the face of face MgO film, it is seen that the two-sided consistency of face external structure is fine.
Fig. 6 is the Phi scanning spectra at (220) peak on the two sides a, b that is two-sided in embodiment while preparing MgO film, two sides
Halfwidth distinguishes 6.40 ° and 6.82 ° in the face of MgO film, it is seen that prepared two-sided MgO film is biaxial texture, and in face
The two-sided consistency of structure is fine.
Claims (2)
1. a kind of method based on the mid frequency sputtering preparation two-sided MgO film of homoepitaxy, the specific steps are as follows:
Step 1 successively pacifies Hastelloy flexibility base band to be coated through the first winder, gas dispersion tube and the second winder
Dress drives the first winder uniform motion to drive Hastelloy flexibility base band uniform motion by stepper motor；Kazakhstan is closed
Golden flexibility base band two sides is coated with IBAD-MgO/SDP-Y simultaneously2O3；
Gas dispersion tube is placed in the physical centre position among target；The internal cavity of gas dispersion tube is set along the base band direction of motion
4 one-way ventilating hole groups are set, 4 one-way ventilating hole groups are constituted using Hastelloy flexibility base band as the space structure of physical centre；
The venthole being arranged in each one-way ventilating hole group is with equal angular towards Hastelloy flexibility base band, and the venthole being arranged
Quantity is consistent, aperture is identical；So that the mixed gas sprayed from venthole can be uniformly dispersed in the two sides of base band, formed symmetrical
Uniform and stable airflow field；Hastelloy flexibility base band to be coated passes through to the physical centre region among target；
Magnesium metal target is respectively disposed on on target by step 2, distinguishes target the two poles of the earth of external intermediate frequency power supply, then to whole equipment
Vacuumize process is carried out to 1.0 × 10-3Then Pa is hereinafter, heat Hastelloy flexibility base band；
Step 3 rises to 480-550 DEG C to Hastelloy flexibility base band temperature, is passed through by each venthole of gas dispersion tube
The mixed gas of argon gas and oxygen；It is then turned on intermediate frequency power supply, using constant voltage mode, keeps voltage constant, current control is in 6A-
8A, sputtering power is in 990-1155W；Aura is formed to be formed about plasma bombardment to target, stepper motor drives Hastelloy
Flexible base band starts at the uniform velocity by aura region to deposit MgO film；
Step 4, after Hastelloy flexibility base band completely at the uniform velocity by closing intermediate frequency power supply behind aura region, stop heating, simultaneously
Gas inlet pipe is closed, stops molecular pump and mechanical pump, is taken out after Temperature fall, can be prepared by MgO film.
2. the method as described in claim 1 based on the mid frequency sputtering preparation two-sided MgO film of homoepitaxy, it is characterised in that: institute
The heating method of Hastelloy flexibility base band is stated using self-heating mode.
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| CN201810994465.1A CN109023276A (en) | 2018-08-29 | 2018-08-29 | A method of the two-sided MgO film of homoepitaxy is prepared based on mid frequency sputtering |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110724922A (en) * | 2019-10-31 | 2020-01-24 | 汕头大学 | Epitaxial AZO film with controllable crystal orientation and polarity on flexible substrate and preparation method thereof |
| CN111607770A (en) * | 2020-06-19 | 2020-09-01 | 南京大学 | Magnetron sputtering equipment compatible with reflection type high-energy electron diffraction measurement |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102255040A (en) * | 2011-04-13 | 2011-11-23 | 电子科技大学 | Continuous preparation method of double-sided superconducting strip buffer layer |
| CN103695859A (en) * | 2013-12-11 | 2014-04-02 | 电子科技大学 | Preparation method of double-sided LaMnO3 buffer layer for superconductive strip |
| CN104021880A (en) * | 2014-06-03 | 2014-09-03 | 电子科技大学 | Preparation method of double-sided MgO buffer layer for coated conductor |
| CN108315697A (en) * | 2018-01-16 | 2018-07-24 | 电子科技大学 | A kind of preparation method of two-sided double-axle texture MgO film |
-
2018
- 2018-08-29 CN CN201810994465.1A patent/CN109023276A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102255040A (en) * | 2011-04-13 | 2011-11-23 | 电子科技大学 | Continuous preparation method of double-sided superconducting strip buffer layer |
| CN103695859A (en) * | 2013-12-11 | 2014-04-02 | 电子科技大学 | Preparation method of double-sided LaMnO3 buffer layer for superconductive strip |
| CN104021880A (en) * | 2014-06-03 | 2014-09-03 | 电子科技大学 | Preparation method of double-sided MgO buffer layer for coated conductor |
| CN108315697A (en) * | 2018-01-16 | 2018-07-24 | 电子科技大学 | A kind of preparation method of two-sided double-axle texture MgO film |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110724922A (en) * | 2019-10-31 | 2020-01-24 | 汕头大学 | Epitaxial AZO film with controllable crystal orientation and polarity on flexible substrate and preparation method thereof |
| CN111607770A (en) * | 2020-06-19 | 2020-09-01 | 南京大学 | Magnetron sputtering equipment compatible with reflection type high-energy electron diffraction measurement |
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Application publication date: 20181218 |