CN107742604A - 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
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- CN107742604A CN107742604A CN201710976639.7A CN201710976639A CN107742604A CN 107742604 A CN107742604 A CN 107742604A CN 201710976639 A CN201710976639 A CN 201710976639A CN 107742604 A CN107742604 A CN 107742604A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- 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
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- 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
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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, hydrogen (H is passed through in sputter procedure as substrate, the high-purity argon gas (Ar) of purity more than 99.99%2) 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 that magnetically controlled DC sputtering prepares room temperature ferromagnetic thin film, more particularly to one kind passes through hydrogen
Gas doping regulates and controls the method for film magnetization characteristic.
Background technology
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 widely studied interest.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 semiconductor material such as titanium oxide and indium oxide has attracted suitable concern.At present, 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.
The content of the invention
It is an object of the present invention to provide a kind of magnetically controlled DC sputtering to prepare hydrogen hafnium codope indium sesquioxide (In2O3) ferromagnetism
The method of film (IHFO), more particularly to a kind of method for regulating and controlling film magnetization characteristic by hydrogen doping.
The present invention uses HfO2Doping is 1.5~10wt.% In2O3Ceramic 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, obtain different
The IHFO films of magnetic characteristic.Realized by following steps：
Step 1, cleaning monocrystalline substrate
Monocrystalline substrate is put into deionized water, adds the dish detergent containing sodium alkyl benzene sulfonate, 80 DEG C of more than water-bath 1h.
Etc. cooling to less than 40 DEG C, ultrasonic more than 15min then with deionized water rinsing to no foam, pours into suitable alcohols, ultrasound
More than 15min, then with deionized water rinsing more than 5 times, add appropriate amount of deionized water, then ultrasonic more than 15min.
Step 2, prepare 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 10-3During Pa, heater is opened to silicon, 160 DEG C of heating temperature range
~500 DEG C, it is incubated at least 30min.
Using Ar gases as sputter gas.H is passed through in sputter procedure2As doped source, partial pressure of ar gas is 0.4~1.9Pa, hydrogen
Qi leel 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 flows, H in sputter procedure2One or several parameters in flow, Sputtering power density, underlayer temperature and air pressure, can
The IHFO films of different saturation magnetizations are prepared.
The present invention can prepare the IHFO films of different magnetization characteristics, and film crystal grain is fine and close, and uniformity is good, and large area can be achieved
Deposition, and magnetization characteristic can be regulated and controled by controlling hydrogen flowing quantity, preparation technology is easily-controllable.
Brief description of the drawings
The EDS figures of IHFO films prepared by Fig. 1；
The XRD of IHFO films prepared by Fig. 2；
The M-H figures of hydrogen hafnium codope IHFO films prepared by Fig. 3.
Embodiment
1st, monocrystalline substrate is cleaned
Monocrystalline substrate is put into deionized water, adds the dish detergent containing sodium alkyl benzene sulfonate, at 80 DEG C water-bath 1h with
On, wait and cool to less than 40 DEG C, ultrasonic more than 15min, then added suitable alcohols to not had foam with deionized water rinsing, surpassed
More than sound 15min, then with deionized water rinsing more than 5 times, add appropriate amount of deionized water, ultrasonic more than 15min.
2nd, film is prepared：
The monocrystalline substrate cleaned up is put into the chamber of magnetic control sputtering device, using HfO2Doping be 1.5~
10wt.% In2O3Ceramic target, it is evacuated to Chamber vacuum degree and reaches 10-3Pa, heater is opened to silicon, heating
Temperature range is 160~500 DEG C, more than soaking time 30min.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, regulation Sputtering power density are 1.5~5W/cm2, sink
0.5~2Pa of power is overstock, starts to prepare IHFO films.Room temperature is naturally cooled to etc. monocrystalline substrate temperature, is taken out prepared
IHFO films.
Embodiment 1
Monocrystalline substrate is put into deionized water, adds the dish detergent containing sodium alkyl benzene sulfonate, at 80 DEG C water-bath 1h with
On, wait and cool to less than 40 DEG C, ultrasonic more than 15min, then with deionized water rinsing to no foam, add suitable alcohols,
Ultrasonic more than 15min, then with deionized water rinsing more than 5 times, add appropriate amount of deionized water, ultrasonic more than 15min.
The substrate cleaned up is put into the chamber of magnetically controlled DC sputtering device, be evacuated to less than 10-3Pa, heat substrate
Temperature is 250 DEG C, more than soaking time 30min, 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 films are prepared, wait underlayer temperature to naturally cool to room temperature, prepared by taking-up
IHFO films.
Performance test has been carried out to prepared IHFO films.As shown in figure 1, energy spectrometer analysis composition obtain it is prepared
The mass percent of hafnium is 3.9wt.% in IHFO films.The X-ray diffraction curve of IHFO films as shown in Figure 2 shows, is somebody's turn to do
Film is polycrystalline state.Curve A shown in Fig. 3 is the M-H curves for representing prepared IHFO film magnetization characteristics, IHFO film tables
Reveal obvious room-temperature ferromagnetic feature, saturation magnetization 13.35emucm-3。
Embodiment 2
Monocrystalline substrate is put into deionized water, adds the dish detergent containing sodium alkyl benzene sulfonate, at 80 DEG C water-bath 1h with
On, wait and cool to less than 40 DEG C, ultrasonic more than 15min, then with deionized water rinsing to no foam, add suitable alcohols,
Ultrasonic more than 15min, then with deionized water rinsing more than 5 times, add appropriate amount of deionized water, ultrasonic more than 15min.
The substrate cleaned up is put into the chamber of magnetically controlled DC sputtering device, be evacuated to less than 10-3Pa, heat substrate
Temperature is 500 DEG C, more than soaking time 30min, is passed through Ar gas, partial pressure 1.9Pa, is passed through hydrogen, partial pressure 0.125Pa, splashes
It is 1.5W/cm to penetrate power density2, IHFO films are prepared, wait underlayer temperature to naturally cool to room temperature, take out IHFO films.
Curve B is the M-H curves for the magnetization characteristic for representing prepared IHFO films in Fig. 3, and IHFO films show bright
Aobvious room-temperature ferromagnetic feature, saturation magnetization 6.17emucm-3。
Embodiment 3
Monocrystalline substrate is put into deionized water, adds the dish detergent containing sodium alkyl benzene sulfonate, at 80 DEG C water-bath 1h with
On, wait and cool to less than 40 DEG C, ultrasonic more than 15min, then with deionized water rinsing to no foam, add suitable alcohols,
Ultrasonic more than 15min, then with deionized water rinsing more than 5 times, appropriate amount of deionized water is added, again ultrasonic more than 15min.
The substrate cleaned up is put into the chamber of magnetically controlled DC sputtering device, is evacuated to vacuum less 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 films are prepared, wait underlayer temperature to naturally cool to room temperature, take out prepared IHFO films.
Curve C is the M-H curves for the magnetization characteristic for representing prepared IHFO films in Fig. 3, and IHFO films show room
Warm ferromagnetism feature, saturation magnetization 2.28emucm-3。
Embodiment 4
Monocrystalline substrate is put into deionized water, adds the dish detergent containing sodium alkyl benzene sulfonate, at 80 DEG C water-bath 1h with
On, wait and cool to less than 40 DEG C, ultrasonic more than 15min, then with deionized water rinsing to no foam, add suitable alcohols,
Ultrasonic more than 15min, then with deionized water rinsing more than 5 times, appropriate amount of deionized water is added, again ultrasonic more than 15min.
The substrate cleaned up is put into the chamber of magnetic control sputtering device, is evacuated to vacuum less than 10-3Pa, substrate temperature
Spend for 160 DEG C, be passed through Ar gas, partial pressure of ar gas 0.4Pa, be passed through hydrogen, hydrogen partial pressure 7.5 × 10-2Pa, Sputtering power density are
3W/cm2, IHFO films are prepared, wait underlayer temperature to naturally cool to room temperature, take out prepared IHFO films.
Curve D is the M-H curves of IHFO film magnetization characteristics prepared by expression in Fig. 3, and IHFO films are shown significantly
Room-temperature ferromagnetic feature, saturation magnetization 7.51emucm-3.Compared with the acquired results of embodiment 3, hydrogen partial pressure increase,
When other deposition parameters are constant, the saturation magnetization increase of prepared IHFO films.
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 are sputter gas, in sputter procedure
It is passed through H2As doped source, by regulating and controlling Sputtering power density, underlayer temperature, deposition pressure, H2Doping, obtain different magnetization
The IHFO films of feature；Comprise the following steps that：
Step 1, cleaning monocrystalline substrate
Monocrystalline substrate is put into deionized water, adds the dish detergent containing sodium alkyl benzene sulfonate, 80 DEG C of more than water-bath 1h；Wait to drop
Temperature, which arrives, is less than 40 DEG C, ultrasonic more than 15min, then with deionized water rinsing to no foam, pours into suitable alcohols, ultrasound
More than 15min, then with deionized water rinsing more than 5 times, add appropriate amount of deionized water, then ultrasonic more than 15min；
Step 2, prepare film
Cleaned monocrystalline substrate is fitted into magnetic control sputtering device, using HfO2Doping is 1.5~10wt.% In2O3
Ceramic target；When Chamber vacuum degree reaches 10-3During Pa, heater is opened to silicon, heating temperature range 160 DEG C~500
DEG C, it is incubated at least 30min.
2. the preparation method of IHFO films according to claim 1, it is characterized in that：Described sputtering method is direct magnetic control
Sputtering.
3. the preparation method of IHFO films according to claim 1, it is characterized in that：Described Sputtering power density is 1.5
~5W/cm2。
4. the preparation method of IHFO films according to claim 1, it is characterized in that：Described Ar qi leels pressure for 0.4~
1.9Pa, hydrogen partial pressure are 2.5 × 10-2~0.125Pa.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111647853A (en) * | 2020-06-10 | 2020-09-11 | 邢义志 | Preparation method of high-transparency high-conductivity ultrathin hydrogen-doped indium oxide film |
| CN115418609A (en) * | 2022-08-11 | 2022-12-02 | 天津大学 | Hafnium-doped indium oxide transparent conductive film and preparation method thereof |
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| CN111647853A (en) * | 2020-06-10 | 2020-09-11 | 邢义志 | Preparation method of high-transparency high-conductivity ultrathin hydrogen-doped indium oxide film |
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| CN115418609A (en) * | 2022-08-11 | 2022-12-02 | 天津大学 | Hafnium-doped indium oxide transparent conductive film and preparation method thereof |
| CN115418609B (en) * | 2022-08-11 | 2023-11-14 | 天津大学 | Hafnium-doped indium oxide transparent conductive film and preparation method thereof |
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