CN107742604B - Preparation method with room-temperature ferromagnetic hydrogen hafnium codope indium oxide film - Google Patents
Preparation method with room-temperature ferromagnetic hydrogen hafnium codope indium oxide film Download PDFInfo
- Publication number
- CN107742604B CN107742604B CN201710976639.7A CN201710976639A CN107742604B CN 107742604 B CN107742604 B CN 107742604B CN 201710976639 A CN201710976639 A CN 201710976639A CN 107742604 B CN107742604 B CN 107742604B
- Authority
- CN
- China
- Prior art keywords
- hydrogen
- codope
- temperature
- room
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02225—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer
- H01L21/0226—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process
- H01L21/02263—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase
- H01L21/02266—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase deposition by physical ablation of a target, e.g. sputtering, reactive sputtering, physical vapour deposition or pulsed laser deposition
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02109—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates
- H01L21/02112—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer
- H01L21/02172—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing at least one metal element, e.g. metal oxides, metal nitrides, metal oxynitrides or metal carbides
Abstract
A kind of preparation method with room-temperature ferromagnetic hydrogen hafnium codope indium oxide film, using direct current magnetron sputtering process.With hafnium oxide (HfO2) doping be 1.5~10wt.% In2O3Ceramic target is target, and monocrystalline silicon is used as sputter gas, is passed through hydrogen (H in sputtering process as substrate, the high-purity argon gas (Ar) of 99.99% or more purity2) deposited as doped source, obtain the hydrogen hafnium codope indium oxide film of different magnetization characteristics.
Description
Technical field
The present invention relates to a kind of method of magnetically controlled DC sputtering preparation room temperature ferromagnetic thin film, in particular to one kind passes through hydrogen
Gas doping regulates and controls the method for film magnetization characteristic.
Background technique
Dilute magnetic semiconductor combines the Charge Transport Proper ty of semiconductor and the information storage characteristic of magnetic material, because it is certainly
Application in rotation electronic device causes the interest studied extensively.Based on Dietl et al. [T.Dietl etc., Phys.Rev.B, 63,
195205 (2001)] the theoretical room-temperature ferromagnetic for having foretold wide bandgap semiconductor materials, transition metal element doped zinc oxide, two
The oxide lanthanon magnetic semiconductors material such as titanium oxide and indium oxide has attracted suitable concern.Currently, research obtains molybdenum [C.Y.Park
Deng Appl.Phys.Lett., 95,122502 (2009)], manganese [Y.K.An etc., Appl.Phys.Lett., 102,212411
(2013)], nickel [G.Peleckis etc., Appl.Phys.Lett., 89,022501 (2006)], iron [X.H.Xu etc.,
Appl.Phys.Lett., 94,212510 (2009)] doping, manganese chromium [F.X.Jiang etc., Appl.Phys.Lett., 96,
052503 (2010)], iron copper [Y.K.Yoo etc., Appl.Phys.Lett., 86,042506 (2005)], titanium vanadium chromium [A.Gupta
Deng J.Appl.Phys., 101,09N513 (2007)] room-temperature ferromagnetic of codope indium oxide film.So far, DC magnetic
Control sputtering prepares room-temperature ferromagnetic hydrogen hafnium codope indium oxide film and yet there are no relevant report.
Summary of the invention
It is an object of the present invention to provide a kind of magnetically controlled DC sputterings to prepare hydrogen hafnium codope indium sesquioxide (In2O3) ferromagnetism
The method of film (IHFO), in particular to a kind of method for regulating and controlling film magnetization characteristic by hydrogen doping.
The present invention uses HfO2Doping is the In of 1.5~10wt.%2O3Ceramic target, Ar gas are sputter gas, are sputtered
H is passed through in journey2As doped source, by regulating and controlling Sputtering power density, underlayer temperature, deposition pressure, H2Doping obtains different
The IHFO film of magnetic characteristic.It is realized by following steps:
Step 1, cleaning monocrystalline substrate
Monocrystalline substrate is put into deionized water, the dish detergent containing sodium alkyl benzene sulfonate, 80 DEG C of water-bath 1h or more are added.
Etc. cooling to lower than 40 DEG C, then ultrasonic 15min or more is rinsed with deionized water to no foam, pours into suitable alcohols, ultrasound
15min or more, then with deionized water flushing 5 times or more, appropriate amount of deionized water, then ultrasound 15min or more is added.
Step 2 prepares film
Cleaned monocrystalline substrate is fitted into magnetic control sputtering device, using HfO2Doping is 1.5~10wt.%'s
In2O3Ceramic target, when Chamber vacuum degree reaches 10-3When Pa, heating device is opened to silicon, 160 DEG C of heating temperature range
~500 DEG C, keep the temperature at least 30min.
Using Ar gas as sputter gas.H is passed through in sputtering process2As doped source, partial pressure of ar gas is 0.4~1.9Pa, hydrogen
Gas partial pressure is 2.5 × 10-2~0.125Pa and Sputtering power density are 1.5~5W/cm2, underlayer temperature be 160~500 DEG C,
Change Ar flow, H in sputtering process2One or several parameters in flow, Sputtering power density, underlayer temperature and air pressure, can
The IHFO film of different saturation magnetizations is prepared.
The present invention can prepare the IHFO film of different magnetization characteristics, and film crystal grain is fine and close, and uniformity is good, it can be achieved that large area
Deposition, and magnetization characteristic can be regulated and controled by control hydrogen flowing quantity, preparation process is easily-controllable.
Detailed description of the invention
The EDS of IHFO film prepared by Fig. 1 schemes；
The XRD diagram of IHFO film prepared by Fig. 2；
The M-H of hydrogen hafnium codope IHFO film prepared by Fig. 3 schemes.
Specific embodiment
1, monocrystalline substrate is cleaned
Monocrystalline substrate is put into deionized water, the dish detergent containing sodium alkyl benzene sulfonate is added, at 80 DEG C water-bath 1h with
On, it waits and cools to lower than 40 DEG C, then ultrasonic 15min or more is rinsed to not having foam with deionized water, suitable alcohols are added, surpassed
Sound 15min or more, then with deionized water flushing 5 times or more, appropriate amount of deionized water, ultrasonic 15min or more is added.
2, film is prepared:
The monocrystalline substrate cleaned up is put into the chamber of magnetic control sputtering device, using HfO2Doping be 1.5~
The In of 10wt.%2O3Ceramic target is evacuated to Chamber vacuum degree and reaches 10-3Pa opens heating device to silicon, heating
Temperature range is 160~500 DEG C, soaking time 30min or more.Argon gas is passed through as sputter gas, hydrogen is doped source, argon gas
Partial pressure is 0.4~1.9Pa, and hydrogen partial pressure is 2.5 × 10-2~0.125Pa, adjusting Sputtering power density are 1.5~5W/cm2, sink
0.5~2Pa of power is overstock, starts to prepare IHFO film.Etc. monocrystalline substrates temperature naturally cool to room temperature, take out prepared
IHFO film.
Embodiment 1
Monocrystalline substrate is put into deionized water, the dish detergent containing sodium alkyl benzene sulfonate is added, at 80 DEG C water-bath 1h with
On, it waiting and cools to lower than 40 DEG C, then ultrasonic 15min or more is rinsed to no foam with deionized water, suitable alcohols is added,
Ultrasonic 15min or more, then with deionized water flushing 5 times or more, appropriate amount of deionized water, ultrasonic 15min or more is added.
The substrate cleaned up is put into the chamber of magnetically controlled DC sputtering device, is evacuated to lower than 10-3Pa heats substrate
Temperature is 250 DEG C, soaking time 30min or more, is passed through Ar gas, partial pressure of ar gas 1.2Pa is passed through hydrogen, and hydrogen partial pressure is
0.08Pa, Sputtering power density 5W/cm2, IHFO film is prepared, underlayer temperatures is waited to naturally cool to room temperature, prepared by taking-up
IHFO film.
Performance test has been carried out to prepared IHFO film.As shown in Figure 1, energy spectrometer analysis ingredient obtain it is prepared
The mass percent of hafnium is 3.9wt.% in IHFO film.The X-ray diffraction curve of IHFO film as shown in Figure 2 shows this
Film is polycrystalline state.Curve A shown in Fig. 3 is the M-H curve for indicating prepared IHFO film magnetization characteristic, IHFO film table
Reveal apparent room-temperature ferromagnetic feature, saturation magnetization 13.35emucm-3。
Embodiment 2
Monocrystalline substrate is put into deionized water, the dish detergent containing sodium alkyl benzene sulfonate is added, at 80 DEG C water-bath 1h with
On, it waiting and cools to lower than 40 DEG C, then ultrasonic 15min or more is rinsed to no foam with deionized water, suitable alcohols is added,
Ultrasonic 15min or more, then with deionized water flushing 5 times or more, appropriate amount of deionized water, ultrasonic 15min or more is added.
The substrate cleaned up is put into the chamber of magnetically controlled DC sputtering device, is evacuated to lower than 10-3Pa heats substrate
Temperature is 500 DEG C, and soaking time 30min or more is passed through Ar gas, divides as 1.9Pa, is passed through hydrogen, divides as 0.125Pa, splashes
Penetrating power density is 1.5W/cm2, IHFO film is prepared, underlayer temperatures is waited to naturally cool to room temperature, takes out IHFO film.
Curve B is the M-H curve for indicating the magnetization characteristic of prepared IHFO film in Fig. 3, and IHFO film shows bright
Aobvious room-temperature ferromagnetic feature, saturation magnetization 6.17emucm-3。
Embodiment 3
Monocrystalline substrate is put into deionized water, the dish detergent containing sodium alkyl benzene sulfonate is added, at 80 DEG C water-bath 1h with
On, it waiting and cools to lower than 40 DEG C, then ultrasonic 15min or more is rinsed to no foam with deionized water, suitable alcohols is added,
Ultrasonic 15min or more, then with deionized water flushing 5 times or more, appropriate amount of deionized water is added, again ultrasound 15min or more.
The substrate cleaned up is put into the chamber of magnetically controlled DC sputtering device, is evacuated to vacuum degree lower than 10-3Pa, lining
Bottom temperature is 160 DEG C, is passed through Ar gas, partial pressure of ar gas 0.4Pa is passed through hydrogen, hydrogen partial pressure 2.5 × 10-2Pa, Sputtering power density
For 3W/cm2, IHFO film is prepared, underlayer temperatures is waited to naturally cool to room temperature, takes out prepared IHFO film.
Curve C is the M-H curve for indicating the magnetization characteristic of prepared IHFO film in Fig. 3, and IHFO film shows room
Warm ferromagnetism feature, saturation magnetization 2.28emucm-3。
Embodiment 4
Monocrystalline substrate is put into deionized water, the dish detergent containing sodium alkyl benzene sulfonate is added, at 80 DEG C water-bath 1h with
On, it waiting and cools to lower than 40 DEG C, then ultrasonic 15min or more is rinsed to no foam with deionized water, suitable alcohols is added,
Ultrasonic 15min or more, then with deionized water flushing 5 times or more, appropriate amount of deionized water is added, again ultrasound 15min or more.
The substrate cleaned up is put into the chamber of magnetic control sputtering device, is evacuated to vacuum degree lower than 10-3Pa, substrate temperature
Degree is 160 DEG C, is passed through Ar gas, partial pressure of ar gas 0.4Pa is passed through hydrogen, hydrogen partial pressure 7.5 × 10-2Pa, Sputtering power density are
3W/cm2, IHFO film is prepared, underlayer temperatures is waited to naturally cool to room temperature, takes out prepared IHFO film.
Curve D is the M-H curve for indicating prepared IHFO film magnetization characteristic in Fig. 3, and IHFO film is shown significantly
Room-temperature ferromagnetic feature, saturation magnetization 7.51emucm-3.Compared with 3 acquired results of embodiment, hydrogen partial pressure increases,
When other deposition parameters are constant, the saturation magnetization of prepared IHFO film increases.
Claims (4)
1. a kind of preparation method with room-temperature ferromagnetic hydrogen hafnium codope indium oxide film, it is characterized in that: the preparation method
Using hafnium oxide (HfO2) doping be 1.5~10wt.% In2O3Ceramic target, Ar gas is sputter gas, in sputtering process
It is passed through H2As doped source, by regulating and controlling Sputtering power density, underlayer temperature, deposition pressure, H2Doping obtains different magnetization
The IHFO film of feature；Specific step is as follows:
Step 1, cleaning monocrystalline substrate
Monocrystalline substrate is put into deionized water, the dish detergent containing sodium alkyl benzene sulfonate, 80 DEG C of water-bath 1h or more are added；Wait drop
To being lower than 40 DEG C, then ultrasonic 15min or more is rinsed with deionized water to no foam temperature, pours into suitable alcohols, ultrasound
15min or more, then with deionized water flushing 5 times or more, appropriate amount of deionized water, then ultrasound 15min or more is added；
Step 2 prepares film
Cleaned monocrystalline substrate is fitted into magnetic control sputtering device, using HfO2Doping is the In of 1.5~10wt.%2O3
Ceramic target；When Chamber vacuum degree reaches 10-3When Pa, heating device is opened to silicon, heating temperature range 160 DEG C~500
DEG C, keep the temperature at least 30min.
2. the preparation method according to claim 1 with room-temperature ferromagnetic hydrogen hafnium codope indium oxide film, feature
Be: the sputtering method is magnetically controlled DC sputtering.
3. the preparation method according to claim 1 with room-temperature ferromagnetic hydrogen hafnium codope indium oxide film, feature
Be: the Sputtering power density is 1.5~5W/cm2。
4. the preparation method according to claim 1 with room-temperature ferromagnetic hydrogen hafnium codope indium oxide film, feature
Be: the Ar gas partial pressure is 0.4~1.9Pa, and hydrogen partial pressure is 2.5 × 10-2~0.125Pa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710976639.7A CN107742604B (en) | 2017-10-19 | 2017-10-19 | Preparation method with room-temperature ferromagnetic hydrogen hafnium codope indium oxide film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710976639.7A CN107742604B (en) | 2017-10-19 | 2017-10-19 | Preparation method with room-temperature ferromagnetic hydrogen hafnium codope indium oxide film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107742604A CN107742604A (en) | 2018-02-27 |
| CN107742604B true CN107742604B (en) | 2019-10-29 |
Family
ID=61237836
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710976639.7A Active CN107742604B (en) | 2017-10-19 | 2017-10-19 | Preparation method with room-temperature ferromagnetic hydrogen hafnium codope indium oxide film |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107742604B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111647853B (en) * | 2020-06-10 | 2022-11-08 | 邢义志 | Preparation method of high-transparency high-conductivity ultrathin hydrogen-doped indium oxide film |
| CN115418609B (en) * | 2022-08-11 | 2023-11-14 | 天津大学 | Hafnium-doped indium oxide transparent conductive film and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101866860A (en) * | 2010-05-26 | 2010-10-20 | 上海大学 | Preparation method of ZnO thin film field-effect transistor |
| CN105002469A (en) * | 2015-07-10 | 2015-10-28 | 中国科学院宁波材料技术与工程研究所 | Ceramic-metal nanowire composite film and preparation method thereof |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004336019A (en) * | 2003-04-18 | 2004-11-25 | Advanced Lcd Technologies Development Center Co Ltd | Film forming method, forming method of semiconductor element, semiconductor element, forming method of indicating device, and indicating device |
| CN101454892B (en) * | 2006-05-26 | 2011-12-14 | 株式会社半导体能源研究所 | Semiconductor device and manufacturing method thereof |
| JP5679622B2 (en) * | 2008-01-31 | 2015-03-04 | 株式会社東芝 | Insulating film and semiconductor device using the same |
| KR102297760B1 (en) * | 2014-12-31 | 2021-09-03 | 엘지디스플레이 주식회사 | Liquid crystal display device with oxide thin film transistor |
| CN106435490B (en) * | 2015-08-06 | 2018-11-30 | 清华大学 | Sputtering target and oxide semiconductor film with and preparation method thereof |
| US20170194366A1 (en) * | 2016-01-04 | 2017-07-06 | Chunghwa Picture Tubes, Ltd. | Method for manufacturing thin-film transistor |
-
2017
- 2017-10-19 CN CN201710976639.7A patent/CN107742604B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101866860A (en) * | 2010-05-26 | 2010-10-20 | 上海大学 | Preparation method of ZnO thin film field-effect transistor |
| CN105002469A (en) * | 2015-07-10 | 2015-10-28 | 中国科学院宁波材料技术与工程研究所 | Ceramic-metal nanowire composite film and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107742604A (en) | 2018-02-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107742604B (en) | Preparation method with room-temperature ferromagnetic hydrogen hafnium codope indium oxide film | |
| CN106449971B (en) | A kind of automatically controlled magnetic structure and its preparation method and application based on NdFeB | |
| CN112359421B (en) | Method for preparing layered bismuth-oxygen-selenium semiconductor film by reverse airflow method | |
| CN107043914A (en) | A kind of batch (-type) magnetically controlled DC sputtering preparation method of amorphous cobalt based magnetic thin film | |
| Kumar et al. | The influence of substrate temperature and annealing on the properties of pulsed laser-deposited YIG films on fused quartz substrate | |
| CN107881475B (en) | A method of Ni-Co-Mn-Ti alloy firm is prepared by magnetron sputtering DC sputturing method | |
| Meng et al. | Preparation of highly c-axis oriented AlN films on Si substrate with ZnO buffer layer by the DC magnetron sputtering | |
| Qin et al. | Influence of substrate temperature on the morphology and structure of bismuth thin films deposited by magnetron sputtering | |
| Li et al. | Grain growth kinetics and magnetic properties of NiZn ferrite thin films | |
| CN108315705B (en) | Structure for improving crystallization resistance of amorphous metal film material and preparation method thereof | |
| JP2010238770A (en) | Oxide thin film, and method of manufacturing the same | |
| CN108914080A (en) | A method of it prepares with room temperature exchange bias effect manganese bismuth alloy film | |
| Siddheswaran et al. | Highly c-axis oriented ZnO: Ni thin film nanostructure by RF magnetron sputtering: Structural, morphological and magnetic studies | |
| CN109449077A (en) | A kind of preparation method of the excellent polynary amorphous metal oxide semiconductive thin film of photoelectric properties | |
| Sun et al. | Investigation of optoelectronic performance in In, Ga co-doped ZnO thin films with various In and Ga levels | |
| CN101615467A (en) | A kind of preparation method of Cr doped ZnO-based diluted magnetic semiconductor film material | |
| CN109652770B (en) | Method for regulating vapor deposition metal film texture by using semiconductor substrate | |
| Iriarte | Influence of the magnetron on the growth of aluminum nitride thin films deposited by reactive sputtering | |
| CN110777342A (en) | Magnetostrictive film and preparation method thereof | |
| Dellas et al. | Effect of deposition angle on fiber axis tilt in sputtered aluminum nitride and pure metal films | |
| CN105470116B (en) | A method of regulation dilute magnetic semiconductor material room temperature magnetism | |
| Matsuda et al. | Fabrication of ferromagnetic Ni epitaxial thin film by way of hydrogen reduction of NiO | |
| CN107958765A (en) | A kind of magnetic membrane material with perpendicular magnetic anisotropic and preparation method thereof | |
| Xi et al. | Growth and magnetic properties of soft ferrite films by pulsed laser deposition | |
| CN106960907B (en) | A kind of rare earth Er doping Ge2Sb2Te5Phase transiting storing thin-film material and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |