CN109576659A - The magnetron sputtering preparation method of gradient auto-dope pure phase multi-element metal oxide film - Google Patents
The magnetron sputtering preparation method of gradient auto-dope pure phase multi-element metal oxide film Download PDFInfo
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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
- C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
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- 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
- C23C14/0042—Controlling partial pressure or flow rate of reactive or inert gases with feedback of measurements
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- 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
- C23C14/0084—Producing gradient compositions
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- 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
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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
- C23C14/3492—Variation of parameters during sputtering
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Abstract
The invention discloses a kind of magnetron sputtering preparation methods of gradient auto-dope pure phase multi-element metal oxide film, using magnetron co-sputtering, independent DC sputtering power is respectively adopted in target A and target B, and using the starting sputtering power and power fade rates of target A and target B during sputtering power ramp control device control cosputtering, regulate and control the ratio of metal ion in film；The sputtering power for sputtering component by controlling target A and target B during cosputtering, from film bottom to film, the change of gradient of metal ion A/B ratio is formed on top, the controllable adjustment of metal A/B ratio is realized within the scope of multi-element metal oxidation defect tolerance, under the premise of inhibiting miscellaneous phase to be precipitated, gradient auto-dope pure phase multi-element metal oxide is prepared.
Description
Technical field:
The present invention relates to the magnetron sputtering preparation methods of gradient auto-dope pure phase multi-element metal oxide film.
Background technique:
Gradient auto-dope is the novel semi-conductor modification technology being put forward for the first time in the world by wang et al in 2017, quilt
Confirming the photoelectric characteristic of semiconductive thin film can be effectively improved, only gradient auto-dope technology is to assist spraying by thermal diffusion at present
Mist pyrolysismethod realizes that the preparation method has the following deficiencies: that (1) assists forming A/B concentration gradient by thermal diffusion, however restricted
It in the thermal diffusion coefficient of A and B, is only capable of preparing the film of thickness < 550nm, is difficult to realize the regulation of A/B concentration gradient, film bottom
Portion is easy to appear with top and mutually separates；(2) thermal diffusion auxiliary inevitably needs to react at high temperature；(3) spray pyrolysis
Using organic solvent, inevitably in AxByOzSemiconductive thin film residual carbon impurity, defect level easy to form, greatly
Reduce the photoelectric characteristic of film.
Summary of the invention:
The object of the present invention is to provide a kind of gradient auto-dope pure phase multi-element metal oxide AxByOzThe magnetron sputtering of film
Preparation method, using magnetron co-sputtering, independent DC sputtering power is respectively adopted in target A and target B, and gradually using sputtering power
Become controller control cosputtering during target A and target B starting sputtering power and power fade rates, regulate and control film in metal from
The ratio of son；The sputtering power for sputtering component by controlling target A and target B during cosputtering, from film bottom to film top
Portion forms the change of gradient of metal ion A/B ratio, and metal A/B ratio is realized within the scope of multi-element metal oxidation defect tolerance
Controllable adjustment prepare gradient auto-dope pure phase multi-element metal oxide, which does not need under the premise of inhibiting mutually to separate
Thermal diffusion assists forming concentration gradient, therefore cosputtering reaction can carry out at room temperature.In addition, the technology is physical deposition, it can
Effectively to avoid existing spray pyrolysis from introducing the defect of carbon impurity, the gradient auto-dope pure phase for being suitable for basic research is obtained
AxByOzSemiconductive thin film solves the problems, such as that prior art thermal diffusion assistant spray pyrolysismethod exists.
The present invention is achieved by the following technical programs:
The magnetron sputtering preparation method of gradient auto-dope pure phase multi-element metal oxide film, using metal A as target A, with
Metal B controls cosputtering process using sputtering power ramp control device using argon gas and oxygen as cosputtering gas as target B
The starting sputtering power and power fade rates of middle target A and target B, carries out reactive sputtering, in substrate table under gradual change sputtering condition
Face sedimentation gradient auto-dope pure phase multi-element metal oxide (AxByOz, metal A, metal B, oxygen atom O is x with chemical dosage ratio:
The oxide of y:z composition) film, from film bottom to film, the change of gradient of metal ion A/B ratio is formed on top.
Wherein, target A and target B starting sputtering power is 20~500W, and the pre-sputtering time is 1~30min；Target A is splashed with originating
It penetrates on the basis of power, sputtering power is gradually successively decreased (incremental) with the fade rates of 1~30W/min, and target B is to originate sputtering power
Benchmark, sputtering power are gradually incremented by (successively decreasing) with the fade rates of 1~30W/min, and the cosputtering time is 1~60min.
Particularly, substrate is once purged is fixed in sputtering chamber on the sample stage of rotary heating, two target of target A and target B
With sample stage vertical central axis line at 20~60 ° of angles, the center target A and sample stage centre distance are 5~20cm, the center target B in axle center
It is 5~20cm with sample stage centre distance；The background vacuum upper limit is 10-2Pa, cosputtering reaction pressure are 0.1~1.5Pa, Ar
And O2Volume ratio be 1:4~1:1, range of flow be 1~100sccm；The sample stage speed of rotation is 5~30 revs/min.
Specifically includes the following steps:
1) cleaning meron is fixed in sputtering chamber on the sample stage of rotary heating, closes sample introduction hatch door, opened true
Sky pump and solenoid valve connected to it start to be evacuated to pressure lower than 10-2Pa opens sample stage rotation, is passed through cosputtering gas
Body opens power supply A and power supply B and carries out pre-sputtering, the power of pre-sputtering is starting sputtering to default 0.1~1.5Pa of pressure range
Power, starting sputtering power are 20~500W；The pre-sputtering time is 1~30min, flapper closure when pre-sputtering；
2) pre-sputtering completes baffle and automatically opens carry out reactive sputtering, and reactive sputtering pressure will be detected by vacuum meter, and
Pass through real-time monitoring cosputtering gas Ar/O2Feed rate, obtain preset 0.1~1.5Pa of reaction pressure；In sputtering process
Control the starting sputtering power and power gradual change speed of target A and target B during cosputtering respectively using sputtering power ramp control device
Rate carries out reactive sputtering under gradual change sputtering condition, and target A and target B starting sputtering power are 20~500W, and target A is to originate sputtering
On the basis of power, sputtering power is gradually successively decreased (incremental) with the fade rates of 1~30W/min, and target B is to originate sputtering power as base
Standard, sputtering power are gradually incremented by (successively decreasing) with the fade rates of 1~30W/min, and sputtering time is 1~60min；To the anti-of setting
It answers sputtering time to close baffle, closes shielding power supply, stop sample stage rotation, close the solenoid valve between vacuum pump and cavity,
Continuing pressure in logical Ar to cavity is atmospheric pressure, closes cosputtering gas inlet valve, takes out sample.
Target A's and target B has independent shielding power supply respectively, sputters in initial power (20~500W) and sputtering process gradually
Variable Rate (± 1~30W/min) can be arranged by sputtering power ramp control device.And pre-sputtering time, reaction cosputtering
Gas Ar/O2Ratio, gas flow range are, gradual change sputtering time, the sample stage speed of rotation can interact boundary in man-machine close friend
Face is configured, and realizes the Automatic Control during reaction cosputtering.
Compared with existing multi-element metal oxide gradient auto-dope method, the invention has the following advantages that
(1) existing thermal diffusion assistant spray pyrolysismethod be assist forming metal A/B concentration gradient by thermal diffusion, however
It is limited by the thermal diffusion coefficient of metal A and B, is only capable of preparing the film of thickness < 550nm, is difficult to realize metal A/B concentration gradient
Regulation, film bottom and top are easy to appear miscellaneous phase.The technology of the present invention can be easily by accurately controlling shielding power supply A and B
Incremented/decremented fade rates during cosputtering can create in different-thickness (nm~um grades) film from film bottom
To at the top of film can accuracy controlling metal A/B concentration gradient, can effectively avoid the precipitation of miscellaneous phase.
(2) existing thermal diffusion assistant spray pyrolysismethod needs to complete the thermal diffusion of metal A and B at high temperature heat, comes
Form metal A/B concentration gradient.The cosputtering reaction of the technology of the present invention does not need to carry out at high temperature, can obtain ladder at room temperature
Spend auto-dope film.
(3) it is related to a large amount of organic matter etc. in existing thermal diffusion assistant spray pyrolysismethod membrane-film preparation process, causes
Inevitably contain remaining carbon in gained multi-element metal oxide film, is easy to form defect energy in semiconductive thin film
Grade.The technology of the present invention is physical deposition, it is possible to prevente effectively from existing thermal diffusion assistant spray pyrolysismethod introduces the defect of carbon impurity,
Obtain the high-purity multi-element metal oxide film for being suitable for semiconductive thin film basic research.
Detailed description of the invention:
Fig. 1 is the structural schematic diagram of the power graded response cosputtering device of the embodiment of the present invention 1；
Wherein, 1, sputtering power ramp control device A；2, sputtering power ramp control device B；3, power supply A；4, power supply B；5, true
Sky meter；6, cavity；7, sample introduction hatch door；8, baffle；9,AxByOzFilm；10, sample stage；11, substrate；12, cosputtering gas inlet
Mouthful；13, flow controller；14, solenoid valve；15, vacuum pump；16, target A；17, target B.
Fig. 2 is the sample result figure of embodiment 1-2 and comparative example 1, wherein ordinate molar ratio refers to A/ (A+B) to A,
B is referred to B/ (A+B), the molar ratio of A and B are glow discharge optical emission spectrometry (GDOS) test result, and Depth is apart from thin
Distance at the top of film, scatter plot are test experiments as a result, solid line is linear fit；It (a) is embodiment 1, from film top the bottom of to
The gradient auto-dope A that portion x:y is reducedxByOz；It (b) is embodiment 2, from film top to the raised gradient auto-dope of bottom x:y
AxByOz；It (c) is comparative example 1, from film top to the constant no gradient A of bottom x:yxByOz。
Specific embodiment:
It is to further explanation of the invention, rather than limiting the invention below.
Embodiment 1: power graded response cosputtering device as shown in Figure 1, returning apparatus include sputtering chamber cavity, sputtering chamber
Sample stage, target A and the target B for the rotary heating being arranged in vivo, wherein target A's and target B has corresponding independent sputtering electricity respectively
Source current A and power supply B sputters the fade rates (± 1~30W/min) in initial power (20~500W) and sputtering process
Be arranged by corresponding sputtering power ramp control device A and B, described device further include solenoid valve, vacuum pump, vacuum meter, into
Sample hatch door, cosputtering gas inlet.Substrate is once purged to be fixed in sputtering chamber on the sample stage of rotary heating, target A and
The two target axle center target B and sample stage vertical central axis line angle, θ are 20~60 °, and the center target A and sample stage centre distance is 5~
20cm, the center target B and sample stage centre distance are 5~20cm.
The magnetron sputtering preparation method of gradient auto-dope pure phase multi-element metal oxide film, specifically includes the following steps:
1) cleaning meron is fixed in sputtering chamber on the sample stage of rotary heating, closes sample introduction hatch door, opened true
Sky pump and solenoid valve connected to it start to be evacuated to pressure lower than 10-2Pa opens sample stage rotation, is passed through cosputtering gas
Body opens power supply A and power supply B and carries out pre-sputtering, the power of pre-sputtering is starting sputtering to default 0.1~1.5Pa of pressure range
Power, starting sputtering power are 20~500W；The pre-sputtering time is 1~30min, flapper closure when pre-sputtering；
2) pre-sputtering completes baffle and automatically opens carry out reactive sputtering, and reactive sputtering pressure will be detected by vacuum meter, and
Pass through real-time monitoring cosputtering gas Ar/O2Feed rate, obtain preset 0.1~1.5Pa of reaction pressure；In sputtering process
Control the starting sputtering power and power gradual change speed of target A and target B during cosputtering respectively using sputtering power ramp control device
Rate carries out reactive sputtering under gradual change sputtering condition, and target A and target B starting sputtering power are 20~500W, and target A is to originate sputtering
On the basis of power, sputtering power is gradually successively decreased (incremental) with the fade rates of 1~30W/min, and target B is to originate sputtering power as base
Standard, sputtering power are gradually incremented by (successively decreasing) with the fade rates of 1~30W/min, and sputtering time is 1~60min；To the anti-of setting
It answers sputtering time to close baffle, closes shielding power supply, stop sample stage rotation, close the solenoid valve between vacuum pump and cavity,
Continuing pressure in logical Ar to cavity is atmospheric pressure, closes cosputtering gas inlet valve, takes out sample.
Embodiment 1:
With reference to specific embodiment, the difference is that: the center target A and sample stage centre distance are 10cm, the center target B with
Sample stage centre distance is 5cm, and the starting sputtering power of target A is 20W, and the starting sputtering power of target B is 100W, and target A is to originate
On the basis of sputtering power, sputtering power is gradually successively decreased with the fade rates of 1~30W/min, and target B is to originate sputtering power as base
Standard, sputtering power are gradually incremented by with the fade rates of 1~30W/min.The pre-sputtering time is 1min, the control of the sample stage speed of rotation
At 5 revs/min.The reaction cosputtering time is 1min.
Embodiment 2:
Reference implementation example 1, the difference is that: target A is on the basis of originating sputtering power, and sputtering power is with 1~30W/min
Fade rates be gradually incremented by, target B on the basis of originating sputtering power, sputtering power with the fade rates of 1~30W/min gradually
Successively decrease.
Comparative example 1:
Reference implementation example 1, the difference is that: for target A on the basis of originating sputtering power, sputtering power is unchanged, target B with
On the basis of originating sputtering power, sputtering power is unchanged.
Embodiment 3:
With reference to specific embodiment, the difference is that: the center target A and sample stage centre distance are 15~20cm, in target B
The heart and sample stage centre distance are 10~20cm.
Embodiment 4:
Reference implementation example 1, the difference is that: the setting pre-sputtering time is 10~60min, the control of the sample stage speed of rotation
At 20~30 revs/min.
Embodiment 5:
Reference implementation example 1, the difference is that: the reaction cosputtering time is 10~60min.
Claims (6)
1. the magnetron sputtering preparation method of gradient auto-dope pure phase multi-element metal oxide film, which is characterized in that with metal A work
It, using argon gas and oxygen as cosputtering gas, is controlled altogether using sputtering power ramp control device for target A using metal B as target B
The starting sputtering power and power fade rates of target A and target B, carries out reactive sputtering under gradual change sputtering condition in sputtering process,
In substrate surface sedimentation gradient auto-dope pure phase multi-element metal oxide film, from film bottom to film top formed metal from
The change of gradient of sub- A/B ratio, the multi-element metal oxide are AxByOz, wherein A is metal A, and B is metal B, and O is that oxygen is former
Son, x, y, z refer to metal A, metal B, the chemical dose of oxygen atom O.
2. the magnetron sputtering preparation method of gradient auto-dope pure phase multi-element metal oxide film according to claim 1,
It is characterized in that, target A and target B starting sputtering power are 20~500W, and the pre-sputtering time is 1~30min；Target A is to originate sputtering function
On the basis of rate, sputtering power is gradually successively decreased with the fade rates of 1~30W/min, and target B is on the basis of originating sputtering power, sputtering
Power is gradually incremented by with the fade rates of 1~30W/min, and the cosputtering time is 1~60min.
3. the magnetron sputtering preparation method of gradient auto-dope pure phase multi-element metal oxide film according to claim 1,
It is characterized in that, target A and target B starting sputtering power are 20~500W, and the pre-sputtering time is 1~30min；Target A is to originate sputtering function
On the basis of rate, sputtering power is gradually incremented by with the fade rates of 1~30W/min, and target B is on the basis of originating sputtering power, sputtering
Power is gradually successively decreased with the fade rates of 1~30W/min, and the cosputtering time is 1~60min.
4. the magnetron sputtering preparation method of gradient auto-dope pure phase multi-element metal oxide film according to claim 1 or claim 2,
It is fixed in sputtering chamber on the sample stage of rotary heating it is characterized in that, substrate is once purged, the two target axle center target A and target B
With sample stage vertical central axis line at 20~60 ° of angles, the center target A and sample stage centre distance are 5~20cm, the center target B and sample
Sample platform centre distance is 5~20cm；The background vacuum upper limit is 10-2Pa, cosputtering reaction pressure are 0.1~1.5Pa, Ar and O2
Volume ratio be 1:4~1:1, range of flow be 1~100sccm；The sample stage speed of rotation is 5~30 revs/min.
5. the magnetron sputtering preparation method of gradient auto-dope pure phase multi-element metal oxide film according to claim 1 or claim 2,
It is characterized in that, specifically includes the following steps:
Will cleaning meron be fixed in sputtering chamber on the sample stage of rotary heating, close sample introduction hatch door, open vacuum pump and
Solenoid valve connected to it starts to be evacuated to pressure lower than 10-2Pa opens sample stage rotation, is passed through cosputtering gas to pre-
If 0.1~1.5Pa of pressure range, open power supply A and power supply B and carry out pre-sputtering, the power of pre-sputtering is starting sputtering power, is risen
Beginning sputtering power is 20~500W；The pre-sputtering time is 1~30min, flapper closure when pre-sputtering；
Pre-sputtering completes baffle and automatically opens carry out reactive sputtering, and reactive sputtering pressure will be detected by vacuum meter, and pass through reality
When regulate and control cosputtering gas Ar/O2Feed rate, obtain preset 0.1~1.5Pa of reaction pressure；It uses and splashes in sputtering process
Starting sputtering power and power fade rates that power ramp control device controls target A and target B during cosputtering respectively are penetrated, gradually
Become under sputtering condition and carry out reactive sputtering, target A and target B starting sputtering power are 20~500W, and target A is to originate sputtering power as base
Standard, sputtering power are gradually successively decreased with the fade rates of 1~30W/min, and target B is on the basis of originating sputtering power, and sputtering power is with 1
The fade rates of~30W/min are gradually incremented by, or, target A is on the basis of originating sputtering power, sputtering power is with 1~30W/min's
Fade rates are gradually incremented by, and target B on the basis of originating sputtering power, gradually passed with the fade rates of 1~30W/min by sputtering power
Subtract, sputtering time is 1~60min；The reactive sputtering time to setting closes baffle, closes shielding power supply, stops sample stage rotation
Turn, close the solenoid valve between vacuum pump and cavity, continuing pressure in logical Ar to cavity is atmospheric pressure, close cosputtering gas into
Air valve takes out sample.
6. the magnetron sputtering preparation method of gradient auto-dope pure phase multi-element metal oxide film according to claim 1 or claim 2,
It is characterized in that, target A's and target B has independent shielding power supply respectively, the fade rates sputtered in initial power sputtering process are equal
It is arranged by sputtering power ramp control device, and pre-sputtering time, reaction cosputtering gas Ar/O2Ratio, gas flow model
It encloses, gradual change sputtering time, the sample stage speed of rotation are configured in man-machine friendly interactive interface, realization reaction cosputtering process
In Automatic Control.
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| CN201910022023.5A CN109576659A (en) | 2019-01-10 | 2019-01-10 | The magnetron sputtering preparation method of gradient auto-dope pure phase multi-element metal oxide film |
| PCT/CN2019/075648 WO2020143101A1 (en) | 2019-01-10 | 2019-02-21 | Magnetron sputtering preparation method for gradient self-doped pure-phase multi-element metal oxide thin film |
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| CN110158034A (en) * | 2019-05-10 | 2019-08-23 | 中国科学院上海技术物理研究所 | The method of a kind of More target sputtering together preparation heterogeneity and doping than film |
| CN112886033A (en) * | 2021-01-27 | 2021-06-01 | 浙江锋源氢能科技有限公司 | Polar plate structure, preparation method thereof, bipolar plate with polar plate structure and fuel cell |
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| CN112886033A (en) * | 2021-01-27 | 2021-06-01 | 浙江锋源氢能科技有限公司 | Polar plate structure, preparation method thereof, bipolar plate with polar plate structure and fuel cell |
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