CN115323319A - Preparation of high quality Fe on MgO substrate 3 O 4 Method for making thin film - Google Patents
Preparation of high quality Fe on MgO substrate 3 O 4 Method for making thin film Download PDFInfo
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- CN115323319A CN115323319A CN202211089065.9A CN202211089065A CN115323319A CN 115323319 A CN115323319 A CN 115323319A CN 202211089065 A CN202211089065 A CN 202211089065A CN 115323319 A CN115323319 A CN 115323319A
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- 239000000758 substrate Substances 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 23
- 239000010409 thin film Substances 0.000 title claims description 11
- 238000002360 preparation method Methods 0.000 title claims description 9
- 238000004544 sputter deposition Methods 0.000 claims abstract description 20
- 238000000151 deposition Methods 0.000 claims abstract description 8
- 239000013077 target material Substances 0.000 claims abstract description 7
- 238000007781 pre-processing Methods 0.000 claims abstract description 3
- 239000010408 film Substances 0.000 claims description 39
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 25
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 18
- 229910052786 argon Inorganic materials 0.000 claims description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 9
- 239000001301 oxygen Substances 0.000 claims description 9
- 229910052760 oxygen Inorganic materials 0.000 claims description 9
- 239000007789 gas Substances 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 4
- 238000011109 contamination Methods 0.000 claims description 2
- 230000008021 deposition Effects 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 239000012535 impurity Substances 0.000 claims description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims 1
- 229910001882 dioxygen Inorganic materials 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 238000001755 magnetron sputter deposition Methods 0.000 abstract description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 31
- 238000000384 X-ray magnetic circular dichroism spectroscopy Methods 0.000 description 3
- 238000000137 annealing Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000001237 Raman spectrum Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 238000001451 molecular beam epitaxy Methods 0.000 description 2
- 238000002186 photoelectron spectrum Methods 0.000 description 2
- 238000004549 pulsed laser deposition Methods 0.000 description 2
- 239000012495 reaction gas Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 229910052596 spinel Inorganic materials 0.000 description 2
- 239000011029 spinel Substances 0.000 description 2
- 238000004506 ultrasonic cleaning Methods 0.000 description 2
- 229910001566 austenite Inorganic materials 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- -1 iron ions Chemical class 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 238000013507 mapping Methods 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000005289 physical deposition Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
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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
- C23C14/02—Pretreatment of the material to be coated
-
- 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
- C23C14/085—Oxides of iron group metals
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- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
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- Organic Chemistry (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention discloses a method for preparing high-quality Fe on an MgO (001) substrate 3 O 4 (001) Method for preparing high quality Fe on MgO (001) substrate using magnetron sputtering apparatus 3 O 4 (001) A film, mounting a target material to obtain a vacuum cavity; preprocessing a substrate; pre-sputtering; sputtering and depositing a film; in the step 1), high-purity Fe, namely the target with the purity of more than 99.95 percent is used, and the vacuum degree of a cavity reaches 1 x 10 ‑ 8 Torr above; the substrate temperature is kept at 300 ℃ during sputtering, the rotating speed of the sample stage is 5rpm, the baffle of the sample stage is opened to start to deposit the film, and the thickness of the deposited film is controlled according to the sputtering time; the power of the radio frequency power supply is 50W.
Description
Technical Field
The invention belongs to the technical field of ferrite film preparation, and particularly relates to a method for preparing high-quality Fe on an MgO (100) substrate by using a magnetron sputtering device 3 O 4 (001) A method of making a film.
Background
Ferroferric oxide (Fe) 3 O 4 ) Is of inverse spinel structure (AB) 2 O 4 ) Lattice constant of
O in lattice structure 2- The ions are stacked in face centered cubic structures, with tetrahedral and octahedral voids. The position of tetrahedral voids (A) being controlled by Fe 3+ The cations occupy, and the octahedral voids (B) are located by Fe 3+ /Fe 2+ And (4) cation occupation. 32O in the unit cell 2- Ions, 24 iron ions, are stacked to form 8 tetrahedral gaps and 16 octahedral gaps to form an inverse spinel structure of ferroferric oxide, and the chemical formula is Fe A 3+ [Fe 2+ Fe 3+ ] B (O -2 ) 4 。Fe 3 O 4 The film has the semimetal characteristic, the theoretical calculation spin polarizability is-100%, the Curie temperature is 858K, the film forming temperature is low, the resistivity is high, the film can be used as an ideal spin electron injection source in a self-selected electronic device, and the film has wide scientific research and application values in the field of spin electronics.
Production of Fe by physical deposition 3 O 4 The main methods of the thin film include Molecular Beam Epitaxy (MBE), pulsed Laser Deposition (PLD), sputtering (Sputtering), and the like. The molecular beam epitaxy equipment is expensive, the experimental conditions are strict, and the film preparation speed is low. The pulse laser deposition method is only suitable for the growth and preparation of small-area films, and the deposited large-area films are easy to generate non-uniform phenomenon, thereby seriously affecting the performance of the films. The magnetron sputtering deposition method has low cost, high speed and good quality, can deposit large-area films, and is one of the most widely applied film preparation methods in the industrial production of the microelectronic industry.
There have been researchers to deposit Fe by magnetron sputtering 3 O 4 The film has achieved related results, but all deposited on MgO (001) substrate are polycrystalline films or epitaxial with multiple orientationsThin films (CN 1010038393A, CN 101235484A, CN 101497986A, CN 101497987A). And all suffer from the following disadvantages: using Fe which is more difficult to obtain 2 O 3 The temperature of the target material and the growth substrate is higher (higher than 300 ℃), and the reaction gas is introduced into H 2 Epitaxial single crystal Fe with a certain risk and no high quality can be obtained 3 O 4 (100) A film.
Disclosure of Invention
In view of the disadvantages of the prior art, the invention aims to provide a method for preparing high-quality Fe 3 O 4 A method of making a film. The method uses magnetron sputtering to deposit high-quality Fe on a MgO (001) substrate 3 O 4 The single crystal film has controllable growth thickness and excellent film performance, and is favorable for industrial application.
The technical scheme adopted by the invention is to prepare high-quality Fe on an MgO (001) substrate 3 O 4 A method of making a film comprising the steps of:
1) Mounting a target material to obtain vacuum of a cavity;
2) Preprocessing a substrate;
3) Pre-sputtering;
4) Sputtering and depositing a film;
specifically, in the step 1), a high-purity Fe (purity greater than 99.95%) target material and a cavity are used. The vacuum degree must reach 1 × 10 -8 Torr above;
the step 2) is as follows: cleaning a MgO (001) substrate to remove oil contamination impurities on the surface of the substrate; after the cleaning and drying are finished, transferring the dried solution into a growth chamber through a vacuum system; the substrate is heated to 500 +/-50 ℃ and annealed for 30 +/-10 minutes, and then cooled to the sputtering growth temperature of 300 +/-30 ℃. The step 3) is as follows: introducing mixed gas of high-purity argon (99.999%) and oxygen (99.999%), regulating the pumping speed to make the sputtering pressure stable at 4X 10 -3 And (5) Torr. The proportion of oxygen and argon is controlled by an electrically controlled flow valve, and the volume of the argon is more than 30 times of that of the oxygen; the flow rate of oxygen was controlled to 1.5sccm and the flow rate of argon was controlled to about 50 sccm. And starting the pre-sputtering by using the radio frequency power supply with power of more than 30W, such as 50W and 60W, and the time is 15 +/-8 minutes.
In the step 4), the substrate temperature is maintained at 300 +/-30 ℃ during the deposition of the thin film, and the substrate is rotated at the speed of 2-10 rpm. By controlling the sputtering time, films with different thicknesses are deposited.
The invention has the beneficial effects that:
(1) Adopting a pure Fe target material which is easy to obtain;
(2) The reaction gas is less, and no pollution is caused;
(3) The process flow is simple and reliable, and the repeatability is high;
(4) The growth temperature is lower, 300 ℃;
(5) The magnetron sputtering mode is adopted, the efficiency is high, and the method is beneficial to being applied to industrial production.
Drawings
FIG. 1 shows a RHEED pattern according to an embodiment of the present invention.
Figure 2 is an XRD pattern of an example of the present invention.
FIG. 3 is an XPS spectrum of an example of the present invention.
FIG. 4 is a Raman spectrum of an example of the present invention.
FIGS. 5 and 6 are VSM and XMCD maps of examples of the present invention, respectively.
FIG. 7 is a spin-resolved photoelectron spectrum of an embodiment of the present invention;
FIG. 8 shows the spin polarizability of-42. + -. 3% for films grown by the method of the present invention.
Detailed description of the preferred embodiment
The invention adopts the magnetron sputtering method to prepare high-quality epitaxial single crystal Fe on the MgO (001) substrate 3 O 4 (001) A film. And the excellent performance of the film is characterized by a plurality of experimental means. The method has the advantages of simple process, repeatability, low cost, no pollution and suitability for industrial application.
To clarify the objects and advantages of the present invention, the following embodiments of the invention are described in connection with the following detailed description and the accompanying drawings:
installing high-purity Fe (99.95%) target material, vacuumizing the cavity, and ensuring that the vacuum degree needs to reach 1 x 10 -8 Torr。
Taking MgO (001) substrate with size of 10 × 10mm, and placingUltrasonic cleaning in acetone solution for 30 min, ultrasonic cleaning in absolute alcohol for 30 min, final ultrasonic cleaning in deionized water for 30 min, and blowing with nitrogen. And loading the cleaned substrate into a sample holder, and transferring the substrate into a magnetron sputtering growth chamber through a vacuum interconnection system. Then, the annealing temperature was set at 500 ℃ and annealing was carried out for 30 minutes at a set rotation speed of 5rpm. After annealing, the growth temperature is kept at 300 ℃, mixed gas of high-purity argon (99.999%) and oxygen (99.999%) is introduced, and the air pressure during sputtering is stabilized at 4 x 10 by adjusting the air extraction rate -3 About Torr is preferable. The proportion of oxygen and argon is controlled by an electrically controlled flow valve, the flow rate of oxygen is controlled to be 1.5sccm, and the flow rate of argon is controlled to be about 50 sccm. Using a radio frequency power supply, setting the power supply power to be 50W, and starting the pre-sputtering for 15 minutes.
Opening a baffle of a sample table, starting to deposit the film, closing the baffle after 15 minutes and 13 seconds to obtain Fe with the thickness of 50nm 3 O 4 (100) A film. The film with different thickness can be deposited by changing the time.
The RHEED (reflection high energy electron diffractometer) pattern of fig. 1 shows that the epitaxial relationship of the thin film is Fe 3 O 4 (001)[001]//MgO(001)[001]。Fe 3 O 4 (001) The surface appears clear
Reconstruction is carried out, and RHEED stripes are clear and long, so that the fact that the film grown by the method is flat in surface and good in crystallinity is proved.
FIG. 2 shows an XRD pattern illustrating Fe grown by the present method 3 O 4 (001) The films have a consistent orientation.
FIG. 3 shows Fe with standard X-ray photoelectron spectrum of the film 3 O 4 Film spectrum, no marked gamma-Fe observed around 718eV 2 O 3 The satellite peak of (a) appears.
FIG. 4 shows a Raman spectrum of a film typical of Fe 3 O 4 Film mapping.
FIG. 5 shows different thicknesses of Fe grown by the present method 3 O 4 VSM test junction for thin filmsThe maximum value of the saturation magnetization of the fruit reaches 407 +/-5 emu/cm 3 FIG. 6 shows 5nm Fe grown by this method 3 O 4 Fe L of thin film 2,3 Side XAS and XMCD lines. The atomic magnetic moment obtained by XMCD test is 3.31 +/-0.15 mu B /f.u.。
FIG. 7 shows 40nm Fe grown by this method 3 O 4 The spin resolution photoelectron spectrum of the film, the spin polarizability of-42 +/-3% obtained by the test of figure 8, is consistent with the value obtained by theoretical calculation.
In conclusion, the invention relates to a method for preparing a high-quality Fe3O4 (001) film on an MgO (001) substrate by using a magnetron sputtering device, which has the advantages of simple process flow, no pollution, high efficiency and suitability for industrial application.
Claims (5)
1. A method for preparing a high-quality Fe3O4 (001) thin film on an MgO (001) substrate, which is characterized in that,
1) Mounting a target material to obtain vacuum of a cavity;
2) Preprocessing a substrate;
3) Pre-sputtering;
4) Sputtering and depositing a film;
in the step 1), high-purity Fe, namely the target with the purity of more than 99.95 percent is used, and the vacuum degree of a cavity reaches 1 multiplied by 10 -8 Torr is higher than.
2. Preparation of high quality Fe on a MgO (001) substrate as claimed in claim 1 3 O 4 (001) The method of the film is characterized in that the MgO (001) substrate is cleaned to remove oil contamination impurities on the surface of the substrate; after the cleaning and drying, the mixture is conveyed into a growth chamber through a vacuum system; the substrate is heated to 500 +/-50 ℃ and annealed for 30 +/-10 minutes, and then cooled to the sputtering growth temperature of 300 +/-30 ℃.
3. Preparation of high quality Fe on a MgO (001) substrate as claimed in claim 2 3 O 4 (001) A step of thin film, characterized in that the step 3) is: introducing mixed gas of high-purity argon gas with the volume of 30 percent of that of oxygen gas and 99.999 percent of oxygen gasMore than twice.
4. Preparation of high quality Fe on a MgO (001) substrate as claimed in claim 3 3 O 4 (001) A step of forming a thin film, characterized in that the evacuation rate is adjusted so that the gas pressure during sputtering is stabilized at 4X 10 -3 Torr; the proportion of oxygen and argon is controlled by an electrically controlled flow valve, and pre-sputtering is started for 15 +/-8 minutes by using the power of a radio frequency power supply of more than 30W.
5. The process for preparing a high quality Fe3O4 (001) thin film on an MgO (001) substrate according to claim 2, wherein in the step 4), the substrate temperature is maintained at 300 ± 30 ℃ and rotated at a speed of 2-10rpm during the deposition of the thin film; and (3) depositing films with different thicknesses by controlling the sputtering time.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211089065.9A CN115323319A (en) | 2022-09-07 | 2022-09-07 | Preparation of high quality Fe on MgO substrate 3 O 4 Method for making thin film |
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| CN202211089065.9A CN115323319A (en) | 2022-09-07 | 2022-09-07 | Preparation of high quality Fe on MgO substrate 3 O 4 Method for making thin film |
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| CN202211089065.9A Pending CN115323319A (en) | 2022-09-07 | 2022-09-07 | Preparation of high quality Fe on MgO substrate 3 O 4 Method for making thin film |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101497986A (en) * | 2009-03-13 | 2009-08-05 | 天津大学 | Apparatus for preparing extension ferriferrous oxide film by facing-target reactive sputtering and operation method |
| US20140255798A1 (en) * | 2013-03-06 | 2014-09-11 | Uchicago Argonne Llc | Coating of porous carbon for use in lithium air batteries |
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2022
- 2022-09-07 CN CN202211089065.9A patent/CN115323319A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101497986A (en) * | 2009-03-13 | 2009-08-05 | 天津大学 | Apparatus for preparing extension ferriferrous oxide film by facing-target reactive sputtering and operation method |
| US20140255798A1 (en) * | 2013-03-06 | 2014-09-11 | Uchicago Argonne Llc | Coating of porous carbon for use in lithium air batteries |
Non-Patent Citations (1)
| Title |
|---|
| ZHE ZHANG等: "Direct observation of spin polarization in epitaxial Fe3O4(001)/MgO thin films grown by magnetron sputtering", 《APPL. PHYS. LETT.》, vol. 120, pages 2 * |
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