CN106835052A - BiFeO is prepared using rf magnetron sputtering technique3The method of film resistance-variable storing device - Google Patents
BiFeO is prepared using rf magnetron sputtering technique3The method of film resistance-variable storing device Download PDFInfo
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- CN106835052A CN106835052A CN201710246585.9A CN201710246585A CN106835052A CN 106835052 A CN106835052 A CN 106835052A CN 201710246585 A CN201710246585 A CN 201710246585A CN 106835052 A CN106835052 A CN 106835052A
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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
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- 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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- 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
- C23C14/021—Cleaning or etching treatments
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/04—Coating on selected surface areas, e.g. using masks
- C23C14/042—Coating on selected surface areas, e.g. using masks using masks
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- 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
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
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Abstract
BiFeO is prepared the invention discloses using rf magnetron sputtering technique3The method of film resistance-variable storing device, this method selects NSTO as substrate, and perovskite structure BFO ferroelectric thin films are prepared by radio-frequency magnetron sputter method, then sputters at the top electrodes that 0.3mmx0.3mm is prepared on film by straight target.Compared with prior art, present invention process controllability is strong, easy to operate, low cost, product purity is obtained high.And film prepared by the present invention has superior resistive characteristic, and the unilateal conduction characteristic with diode, these superior characteristics can be such that BFO ferroelectric thin films are applied in resistance-variable storing device.
Description
Technical field
The invention belongs to thin film deposition machine resistance-variable storing device preparing technical field, more particularly to one kind is in Nb:SrTiO3
(NSTO) BiFeO is prepared on3The method of ferroelectric thin film resistance-variable storing device
Background technology
Resistance-variable storing device has read or write speed fast because of it, low in energy consumption, and integrated level is high and compatible with current semiconductor technology
The advantages of property is good, as one of most promising memory of new generation.BiFeO3(BFO) material is due to its excellent ferroelectricity
One of can, the characteristic such as photovoltaic performance and nontoxic pollution-free, the material attracted most attention as ferroelectric material field.Recently, study
Personnel have found that BFO films are also answered with resistive effect, cause people to the very big of BFO ferroelectric thin film resistance-variable storing device application studies
Interest.Many scientific research personnel pass through the methods such as pulsed laser deposition (PLD), sol-gal process (Sol-gel) and have prepared performance
Good ferroelectric thin film resistance-variable storing device, but these preparation methods are remained many not enough：Such as high cost, poor repeatability.Penetrate
Frequency magnetron sputtering method is one of the method for preparing high-quality large area film most cost performance, and the process is current half
One of important step of semiconductor process factory, it is good with current semiconductor process compatibility to have the advantages that.
But, up to the present, not yet have one kind that BFO films are prepared on NSTO substrates using radio-frequency magnetron sputter method
The method of resistance-variable storing device.
The content of the invention
The present invention is directed to deficiency of the prior art, it is proposed that a kind of preparation method easily and effectively.
To achieve the above object, the technical solution adopted by the present invention is thin using rf magnetron sputtering technique preparation BiFeO3
The method of film resistance-variable storing device, the method selects NSTO as substrate, and the BFO of advantages of good crystallization is prepared by radio-frequency magnetron sputter method
Film, then prepares the top electrodes of 0.3mmx0.3mm by sputtering method again.Obtain BFO film resistance-variable storing devices.
It is characterized in that：The method is comprised the following steps：
Step 1) cleaned NSTO substrates are fixed on pallet, vacuumized after shutting each air valve, until vacuum
Reach 3.2x10-4More than Pa, is passed through argon gas, and air pressure is adjusted to 3-5Pa by Molecular regulator pump push-pull valve.
Step 2) underlayer temperature as room temperature is set, radio frequency source build-up of luminance is opened, sputtering power is respectively 65W, target is carried out pre-
Sputtering 5 minutes, then opening baffle plate carries out sputtering sedimentation BiFeO3Plated film, uses tube annealing afterwards.
Step 3) Top electrode preparation；
Under the blocking of the mask plate with 0.3mmx0.3mm square holes, deposited on BFO ferroelectric thin films by sputtering method
The electrode of 0.3mmx0.3mm.
Step 1) in the cleaning process of NSTO be：First NSTO substrates are soaked with ethanol and with 5min is cleaned by ultrasonic, repeat three
It is secondary, then with acetone soak NSTO substrates and with being cleaned by ultrasonic, in triplicate, spontaneously dry afterwards finally deionized water with repeatedly.
Step 1) in target and substrate distance be 100mm.
Step 2) in deposition BFO films when be only passed through argon gas, flow is 40Sccm.
Step 2) in deposition BFO films when operating air pressure be 0.83Pa.
Step 2) in the BFO films that have deposited use tube annealing 30min for 600 DEG C in oxygen atmosphere.
Step 1) in deposition BFO films when sputtering time be 35~90min.
Using NSTO as substrate, its cleaning process is for film preparation：It is first with ethanol immersion NSTO substrates and clear with ultrasound
5min is washed, finally in triplicate, then with acetone soak NSTO substrates and with being cleaned by ultrasonic, in triplicate, deionized water with repeatedly
Rinse, spontaneously dry afterwards, and be placed on standby in sample box.This experiment (MSB-300B) on rf magnetron sputtering coating machine
Carry out thin film deposition.BFO targets use the ceramic target of 99.9% purity.
The preparation process of BFO ferroelectric thin film resistance-variable storing devices is as follows：The NSTO substrates that will have been cleaned are hidden with high temperature gummed tape
Firmly part surface, is then attached on sample carrier, shuts sputtering chamber and vacuumizes behind the door, until vacuum reaches 3.2x10-4During Pa,
Argon gas is passed through, push-pull valve is adjusted, sputtering chamber air pressure is adjusted to build-up of luminance air pressure, open radio frequency source build-up of luminance, then adjusting push-pull valve will
Sputtering chamber air pressure is adjusted to operating air pressure, and 5min is splashed in advance to target under identical power.In machine each side parameter stability one
After the section time, sample baffle plate is opened, start deposition film.After deposition certain hour, radio frequency source is closed, stop build-up of luminance.Finally will
The BFO films for having deposited use tube annealing 30min for 600 DEG C under oxygen atmosphere.
Under the blocking of the mask plate with 0.3mmx0.3mm square holes, deposited on BFO ferroelectric thin films by sputtering method
The electrode of 0.3mmx0.3mm.
Brief description of the drawings
Fig. 1 is the X ray diffracting spectrum of BFO ferroelectric thin films in the NSTO substrates of the preparation of embodiment 2.Be can see in collection of illustrative plates
The diffraction maximum of BFO, and have the second a small amount of phase, BFO films are oriented to (00l).
Fig. 2 is the atomic force microscopy diagram spectrum of the BFO ferroelectric thin films in NSTO substrates prepared by embodiment 1, from collection of illustrative plates
As can be seen that grain size is 150nm or so, the surface Root Mean Square roughness of BFO films is 12.5nm.
The leakage current test chart of the BFO ferroelectric thin films in Fig. 3 NSTO substrate of the preparation of embodiment 3, can from figure
The BFO ferroelectric thin films gone out in the NSTO substrates of present invention preparation show obvious unilateral conduction, and high/low currents ratio is
More than 1000.
The resistance state reversion figure of the BFO ferroelectric thin films in Fig. 4 NSTO substrate of the preparation of embodiment 1, as can be seen from the figure
The ratio of BFO ferroelectric thin films low resistance state high is more than 100.
The low resistance state retention performance test chart high of the BFO ferroelectric thin films in Fig. 5 NSTO substrate of the preparation of embodiment 1, from
It can be seen that the BFO ferroelectric thin films in the NSTO substrates of present invention preparation can keep 3600s in low resistance state high in figure, now just
The ratio of resistance state is 100 or so.
Specific embodiment
Embodiment 1
The NSTO substrate high temperature gummed tapes that will have been cleaned cover part surface, are then attached on sample carrier, shut and splash
Penetrate room to vacuumize behind the door, until vacuum reaches 3.2x10-4During Pa, 40Sccm argon gas is passed through, push-pull valve is adjusted, by sputtering chamber gas
Pressure is adjusted to the build-up of luminance air pressure of 4.5Pa, opens radio frequency source, and setting RF source power is 60W, after after target build-up of luminance, adjusts push-pull valve
Sputtering chamber air pressure is adjusted to the operating air pressure of 0.83Pa, 5min is splashed in advance to target under this power.Then machine each side is treated
Parameter stability for a period of time after, open sample baffle plate, start deposition film.After deposition 35min, radio frequency source is closed, stop build-up of luminance.
The BFO films that will finally deposit use tube annealing 30min for 600 DEG C under oxygen atmosphere.
Under the blocking of the mask plate with 0.3mmx0.3mm square holes, deposited on BFO ferroelectric thin films by sputtering method
The electrode of 0.3mmx0.3mm.
Embodiment 2
The NSTO substrate high temperature gummed tapes that will have been cleaned cover part surface, are then attached on sample carrier, shut and splash
Penetrate room to vacuumize behind the door, until vacuum reaches 3.2x10-4During Pa, 40Sccm argon gas is passed through, push-pull valve is adjusted, by sputtering chamber gas
Pressure is adjusted to the build-up of luminance air pressure of 4.5Pa, opens radio frequency source, and setting RF source power is 60W, after after target build-up of luminance, adjusts push-pull valve
Sputtering chamber air pressure is adjusted to the operating air pressure of 0.83Pa, 5min is splashed in advance to target under this power.Then machine each side is treated
Parameter stability for a period of time after, open sample baffle plate, start deposition film.After deposition 65min, radio frequency source is closed, stop build-up of luminance.
The BFO films that will finally deposit use tube annealing 30min for 600 DEG C under oxygen atmosphere.
Under the blocking of the mask plate with 0.3mmx0.3mm square holes, deposited on BFO ferroelectric thin films by sputtering method
The electrode of 0.3mmx0.3mm.
Embodiment 3
The NSTO substrate high temperature gummed tapes that will have been cleaned cover part surface, are then attached on sample carrier, shut and splash
Penetrate room to vacuumize behind the door, until vacuum reaches 3.2x10-4During Pa, 40Sccm argon gas is passed through, push-pull valve is adjusted, by sputtering chamber gas
Pressure is adjusted to the build-up of luminance air pressure of 4.5Pa, opens radio frequency source, and setting RF source power is 60W, after after target build-up of luminance, adjusts push-pull valve
Sputtering chamber air pressure is adjusted to the operating air pressure of 0.83Pa, 5min is splashed in advance to target under this power.Then machine each side is treated
Parameter stability for a period of time after, open sample baffle plate, start deposition film.After deposition 95min, radio frequency source is closed, stop build-up of luminance.
The BFO films that will finally deposit use tube annealing 30min for 600 DEG C under oxygen atmosphere.
Under the blocking of the mask plate with 0.3mmx0.3mm square holes, deposited on BFO ferroelectric thin films by sputtering method
The electrode of 0.3mmx0.3mm.
Film X-ray diffraction instrument involved in the present invention is D8Advance, (Bruker, Germany), test
The model of the AFM used by film surface appearance is Mutimode VIII (Bruker, Germany), testing film electric leakage
Stream, resistive effect is answered, and the model of the instrument used by resistive retention performance is that Agilent B1500 semiconductor analysis tester (is doing electricity
When learning performance test, protective current is disposed as 10mA).
Claims (10)
1. the method for preparing BiFeO3 film resistance-variable storing devices using rf magnetron sputtering technique, the method selects NSTO as lining
Bottom, the BFO films of advantages of good crystallization are prepared by radio-frequency magnetron sputter method, then prepare 0.3mmx0.3mm by sputtering method again
Top electrodes；Obtain BFO film resistance-variable storing devices；
It is characterized in that：The method is comprised the following steps：
Step 1) cleaned NSTO substrates are fixed on pallet, vacuumized after shutting each air valve, until vacuum reaches
3.2x10-4More than Pa, is passed through argon gas, and air pressure is adjusted to 3-5Pa by Molecular regulator pump push-pull valve；
Step 2) underlayer temperature as room temperature is set, radio frequency source build-up of luminance is opened, sputtering power is respectively 65W, and pre-sputtering 5 is carried out to target
Minute, then opening baffle plate carries out sputtering sedimentation BiFeO3Plated film, uses tube annealing afterwards；
Step 3) Top electrode preparation；
Under the blocking of the mask plate with 0.3mmx0.3mm square holes, deposited on BFO ferroelectric thin films by sputtering method
The electrode of 0.3mmx0.3mm.
2. the method that utilization rf magnetron sputtering technique according to claim 1 prepares BiFeO3 film resistance-variable storing devices,
It is characterized in that：Step 1) in the cleaning process of NSTO be：First NSTO substrates are soaked with ethanol and with 5min is cleaned by ultrasonic, repeat
Three times, then with acetone soak NSTO substrates and with being cleaned by ultrasonic, in triplicate, do naturally afterwards finally deionized water with repeatedly
It is dry.
3. the method that utilization rf magnetron sputtering technique according to claim 1 prepares BiFeO3 film resistance-variable storing devices,
It is characterized in that：Step 1) in target and substrate distance be 100mm.
4. the method that utilization rf magnetron sputtering technique according to claim 1 prepares BiFeO3 film resistance-variable storing devices,
It is characterized in that：Step 2) in deposition BFO films when be only passed through argon gas, flow is 40Sccm.
5. the method that utilization rf magnetron sputtering technique according to claim 1 prepares BiFeO3 film resistance-variable storing devices,
It is characterized in that：Step 2) in deposition BFO films when operating air pressure be 0.83Pa.
6. the method that utilization rf magnetron sputtering technique according to claim 1 prepares BiFeO3 film resistance-variable storing devices,
It is characterized in that：Step 2) in the BFO films that have deposited use tube annealing 30min for 600 DEG C in oxygen atmosphere.
7. the method that utilization rf magnetron sputtering technique according to claim 1 prepares BiFeO3 film resistance-variable storing devices,
It is characterized in that：Step 1) in deposition BFO films when sputtering time be 35~90min.
8. the method that utilization rf magnetron sputtering technique according to claim 1 prepares BiFeO3 film resistance-variable storing devices,
It is characterized in that：Using NSTO as substrate, its cleaning process is for film preparation：First NSTO substrates are soaked with ethanol and with ultrasonic
Cleaning 5min is in triplicate, then with acetone soak NSTO substrates and with being cleaned by ultrasonic, in triplicate, finally anti-with deionized water
It is multiple to rinse, spontaneously dry afterwards, and be placed on standby in sample box；Thin film deposition is carried out on rf magnetron sputtering coating machine；
BFO targets use the ceramic target of 99.9% purity.
9. the method that utilization rf magnetron sputtering technique according to claim 1 prepares BiFeO3 film resistance-variable storing devices,
It is characterized in that：The preparation process of BFO ferroelectric thin film resistance-variable storing devices is as follows：The NSTO substrate high temperature gummed tapes that will have been cleaned
Part surface is covered, is then attached on sample carrier, shut sputtering chamber and vacuumize behind the door, until vacuum reaches 3.2x10-4Pa
When, argon gas is passed through, push-pull valve is adjusted, sputtering chamber air pressure is adjusted to build-up of luminance air pressure, radio frequency source build-up of luminance is opened, then adjust push-pull valve
Sputtering chamber air pressure is adjusted to operating air pressure, 5min is splashed in advance to target under identical power；In machine each side parameter stability
After a period of time, sample baffle plate is opened, start deposition film；After deposition certain hour, radio frequency source is closed, stop build-up of luminance；Finally
The BFO films that will have been deposited use tube annealing 30min for 600 DEG C under oxygen atmosphere.
10. the method that utilization rf magnetron sputtering technique according to claim 1 prepares BiFeO3 film resistance-variable storing devices,
It is characterized in that：Under the blocking of the mask plate with 0.3mmx0.3mm square holes, sunk on BFO ferroelectric thin films by sputtering method
The electrode of product 0.3mmx0.3mm.
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Cited By (4)
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| CN110029308A (en) * | 2019-04-18 | 2019-07-19 | 武汉理工大学 | A kind of preparation method of bismuth ferrite photovoltaic film and its bismuth ferrite photovoltaic film of preparation |
| CN111816770A (en) * | 2020-06-12 | 2020-10-23 | 北京大学 | Perovskite thin film preparation method, perovskite thin film, solar cell device using perovskite thin film, and magnetron sputtering instrument |
| CN113913935A (en) * | 2021-10-26 | 2022-01-11 | 河北农业大学 | T-shaped BiFeO3Preparation method of ferroelectric thin film material |
| CN114214598A (en) * | 2021-12-23 | 2022-03-22 | 江苏籽硕科技有限公司 | Ion beam sputtering deposition equipment with high film preparation uniformity |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110029308A (en) * | 2019-04-18 | 2019-07-19 | 武汉理工大学 | A kind of preparation method of bismuth ferrite photovoltaic film and its bismuth ferrite photovoltaic film of preparation |
| CN110029308B (en) * | 2019-04-18 | 2020-09-08 | 武汉理工大学 | Preparation method of bismuth ferrite photovoltaic film and bismuth ferrite photovoltaic film prepared by same |
| CN111816770A (en) * | 2020-06-12 | 2020-10-23 | 北京大学 | Perovskite thin film preparation method, perovskite thin film, solar cell device using perovskite thin film, and magnetron sputtering instrument |
| CN113913935A (en) * | 2021-10-26 | 2022-01-11 | 河北农业大学 | T-shaped BiFeO3Preparation method of ferroelectric thin film material |
| CN113913935B (en) * | 2021-10-26 | 2023-11-21 | 河北农业大学 | T-shaped BiFeO 3 Method for preparing ferroelectric film material |
| CN114214598A (en) * | 2021-12-23 | 2022-03-22 | 江苏籽硕科技有限公司 | Ion beam sputtering deposition equipment with high film preparation uniformity |
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