CN107988629A - A kind of preparation method of low resistivity p-type cuprous oxide epitaxial film - Google Patents
A kind of preparation method of low resistivity p-type cuprous oxide epitaxial film Download PDFInfo
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- CN107988629A CN107988629A CN201711240726.2A CN201711240726A CN107988629A CN 107988629 A CN107988629 A CN 107988629A CN 201711240726 A CN201711240726 A CN 201711240726A CN 107988629 A CN107988629 A CN 107988629A
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- cuprous oxide
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- epitaxial film
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
- C30B23/02—Epitaxial-layer growth
- C30B23/025—Epitaxial-layer growth characterised by the substrate
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
- C30B23/02—Epitaxial-layer growth
- C30B23/06—Heating of the deposition chamber, the substrate or the materials to be evaporated
- C30B23/066—Heating of the material to be evaporated
Abstract
The present invention relates to a kind of preparation method of low resistivity p-type cuprous oxide epitaxial film, including (1) cleaning substrate monocrystal MgO (110);(2) by Cu2O ceramic targets are placed in settling chamber with substrate, and heating substrate opens oxygen ventilation valve, be passed through oxygen to settling chamber, the gas pressure intensity for adjusting settling chamber is 0.085 0.095Pa to 500 700 DEG C;(3) pulsed laser ablation Cu is passed through2O ceramic targets, deposit Cu on substrate2O epitaxial films, to obtain the final product.P-type Cu produced by the present invention2O Electrical good properties, possess the advantages of low-resistivity and high hall mobility, resistivity as low as 4.01 Ω cm, are Cu prepared by current PLD methods2The minimum value of O films, mobility are up to 34.86cm2v‑1s‑1, the optical energy gap of film is 2.56eV, possesses the prospect of being widely applied in solar cell and thin film transistor (TFT).
Description
Technical field
The present invention relates to a kind of low-resistivity (as low as 4.01 Ω cm), high mobility (up to 34.86cm2v-1s-1) it is high-quality
The preparation method of p-type cuprous oxide epitaxial film is measured, belongs to technical field of material.
Background technology
Cuprous oxide (Cu2O be) a kind of intrinsically p-type inorganic semiconductor material, energy gap between 2.0-2.6eV,
And since it is with high optical absorption coefficient and hole mobility, preparation process be simple, deposit is abundant and environmental-friendly etc. excellent
Point, has important application prospect in the field such as solar cell and thin film transistor (TFT) (TFT).
At present, based on Cu2The solar cell and thin film transistor (TFT) of O materials are by wide coverage, but its performance distance
Practical application still has larger gap.Document [T.Minami, Y.Nishi, T.Miyata, Heterojunction solar cell
With 6%efficiency based on an n-type aluminum-gallium-xide thin film and p-
type sodium-doped Cu2O sheet, Appl.Phys.Express, 8 (2015) 022301.] in use thermal oxidation method
The Cu of growth2O:Na can reach 6.1% electricity conversion as the heterojunction solar battery of light absorbing layer, still,
Make it difficult to reach Cu since it absorbs the problems such as layer resistivity is higher, carrier mobility is relatively low2O based solar batteries 20%
Theoretical electricity conversion.For the Cu reported at present2For O thin film transistor (TFT)s, its performance still has greatly improved
Space.Document [X.Zou, G.Fang, L.Yuan, M.Li, W.Guan, X.Zhao, Top-gate low-threshold
voltage p-Cu2O thin-film transistor grown on SiO2/Si substrate using a high-
Kappa HfON gate dielectric, IEEE Electron Device Lett, 31 (2010) 827-829.] use magnetic
It is 2.40cm that control sputtering method, which has obtained field mobility,2v-1s-1, on-off ratio be 3.96 × 104Cu2O thin film transistor (TFT)s.Document
[W.Maeng,S.-H.Lee,J.-D.Kwon,J.Park,J.-S.Park,Atomic layer deposited p-type
copper oxide thin films and the associated thin film transistor properties,
Ceram.Int., 42 (2016) 5517-5522.] to have prepared field mobility by atomic layer deposition method be 5.64cm2v-1s-1、
On-off ratio is 1.79 × 105, subthreshold swing be 0.75V/decade CuxO thin film transistor (TFT)s.The Cu reported at present2O bases are too
It is positive can battery and thin film transistor (TFT) performance it is not ideal enough, this crystal growth direction, microcosmic mainly due to its Cu2O film
The generation of structure and carrier and transport and cannot be regulated and controled well, cause the structure and electronic properties of film still to need to be carried
It is high.
In recent years, people have attempted distinct methods to grow Cu2O films, such as magnetron sputtering, thermal oxide, evaporation, pulse
Laser deposition (PLD), atomic layer deposition and electrochemical deposition method etc..Wherein, plasma of the PLD methods since kinetic energy can be produced
Body, can under relatively low growth temperature depositing high-quality film.However, Cu is prepared on PLD methods so far2O films
Report it is still rare, wherein on oxygen pressure to this method grow Cu2The research that O property of thin film influences is then more rare.
In addition, the Cu prepared with PLD methods reported at present2The resistivity of O films is all higher (generally 102-105Ω cm or so), it is unfavorable
In its practical application in related device.As document [K.Matsuzaki, K.Nomura, H.Yanagi, T.Kamiya,
M.Hirano,H.Hosono,Effects of post-annealing on(110)Cu2O epitaxial films and
origin of low mobility in Cu2O thin-film transistor,Phys.Status Solidi A,206
(2009) 2192-2197.] in use pure Cu to be used as substrate as target, MgO (110), growth temperature, 0.65Pa at 700 DEG C
Oxygen pressure under the Cu2O films that grow have~102The resistivity of Ω cm.It is well known that light is inhaled in thin-film solar cells
The optimal resistivity of layer is received in 0.1-1 Ω cm scopes.For high performance thin film transistor (TFT), the carrier concentration of its active layer is led to
Often 1016–1017cm-3Scope, hall mobility will generally exceed 10cm2v-1s-1, this causes its resistivity to be less than 102
Ωcm.Therefore, by exploring and studying new thin film growth process, obtain and have the high-quality of low-resistivity and high hall mobility concurrently
Measure Cu2O films, are to improve Cu2The necessary condition of O base function element performances.
To sum up, a variety of methods prepare Cu at present2O films, but film quality is poor, structure and electronic properties are all
Have much room for improvement.PLD methods are suitable for preparing high quality epitaxial film, but at present with the Cu of this method preparation2The universal resistivity of O films
It is higher, it is difficult to applied to devices such as solar cell and thin film transistor (TFT)s.
The content of the invention
In view of the deficiencies of the prior art, the high quality p-type the present invention provides a kind of low-resistivity, high mobility aoxidizes sub-
The preparation method of copper epitaxial film;
The technical scheme is that:
A kind of low-resistivity, high mobility high quality p-type cuprous oxide epitaxial film preparation method, including:
(1) substrate is cleaned, the substrate is monocrystalline MgO (110);
(2) by Cu2O ceramic targets are placed in the settling chamber of pulse laser deposition equipment with the substrate, heat the substrate
To 500-700 DEG C, oxygen ventilation valve is opened, is passed through oxygen to settling chamber, the gas pressure intensity for adjusting settling chamber is 0.085-
0.095Pa;
(3) Cu described in pulsed laser ablation is passed through2O ceramic targets, deposit Cu over the substrate2O epitaxial films, to obtain the final product.
Monocrystalline MgO (110) and Cu2O lattice mismatches are low, are advantageously implemented Cu2The epitaxial growth of O.Underlayer temperature and oxygen
Pressure meets Cu using Cu-O phasors as with reference to choosing2The thermal equilibrium condition of O growths, is easy to get to pure phase high quality Cu2O films.
Cu2O ceramic targets select market business finished product, and ripe target prepares industrial technology and causes Cu in the present invention2The preparation of O films is more
Inexpensively, it is convenient.
It is further preferred that in the step (2), the substrate is heated to 700 DEG C, the pressure for adjusting settling chamber is
0.09Pa。
Preferable according to the present invention, in the step (3), the frequency of pulse laser is 10-20Hz, the wavelength of pulse laser
For 248nm, pulse laser is in the Cu2O ceramic targets surface power density is 5-6J/cm2, when sedimentation time is 1 small, deposition knot
Shu Hou, cooled to room temperature, obtains p-type cuprous oxide epitaxial film.
Above-mentioned suitable growth conditions effectively reduces the resistivity of film, improves the carrier mobility of film.
It is further preferred that in the step (3), the frequency of pulse laser is 20Hz, and pulse laser is in the Cu2O makes pottery
Porcelain target surface power density is 6J/cm2。
The present invention have chosen 6J/cm2Laser energy density, larger energy cause film grow in particle kinetic energy more
Greatly so that film quality higher.The selection of the pulse laser frequency of 20Hz make it that film growth rate is very fast, saves film life
For a long time.
It is preferable according to the present invention, in the step (2), keep the vacuum of settling chamber to be less than 10-4Pa。
Preferable according to the present invention, the step (1), cleans substrate, including:Successively using enlightening health cleaning agent (Decon),
Deionized water, acetone, ethanol clean the substrate, spare after drying.
Adsorbed gas and the impurity of substrate surface are removed, improves the bond strength of sputtering layer and substrate and into film quality
Amount.
It is preferable according to the present invention, it is clear to the substrate using enlightening health cleaning agent (Decon), deionized water, acetone, ethanol
Wash 5min.
Beneficial effects of the present invention are:
1st, according to Cu2The architectural characteristic of O, the present invention use Cu2O ceramic targets, it is mono- in MgO using pulsed laser deposition
Brilliant Grown Cu2O films, by exploration and Optimizing Process Parameters, realize the regulation and control to membrane structure and electrical properties
And optimization.This preparation method technique is advanced, and informative data is repeated and workable.
2nd, detected by X-ray diffraction, transmission electron microscope and selective electron diffraction, product is monocrystalline Cu2O extensions
Film.P-type Cu produced by the present invention2O Electrical good properties, are provided simultaneously with the excellent of low-resistivity and high hall mobility
Point, resistivity as low as 4.01 Ω cm, are Cu prepared by current PLD methods2The minimum value of O films, mobility are up to 34.86cm2v-1s-1, the optical energy gap of film is 2.56eV.These outstanding performance parameters cause Cu prepared by this method2O films are in the sun
Possesses the prospect of being widely applied in energy battery and thin film transistor (TFT).
Brief description of the drawings
Fig. 1 is p-type Cu made from the embodiment of the present invention 12The XRD spectrum of O epitaxial films;
Fig. 2 is p-type Cu made from the embodiment of the present invention 12The high-resolution-ration transmission electric-lens figure of O epitaxial films;
Fig. 3 is p-type Cu made from the embodiment of the present invention 12The selective electron diffraction figure of O epitaxial films;
Fig. 4 is p-type Cu made from the embodiment of the present invention 12The transmitance collection of illustrative plates of O epitaxial films.
Embodiment
The present invention is further qualified with reference to Figure of description and embodiment, but not limited to this.
Embodiment 1
A kind of low-resistivity, high mobility high quality p-type cuprous oxide epitaxial film preparation method, including:
(1) 5min is respectively washed to substrate using enlightening health cleaning agent (Decon), deionized water, acetone, ethanol successively, blown
Spare after dry, substrate is monocrystalline MgO (110);Adsorbed gas and the impurity of substrate surface are removed, improves sputtering layer and substrate
Bond strength and quality of forming film.
(2) by Cu2During O ceramic targets are placed in the settling chamber of pulse laser deposition equipment with substrate, the substrate is heated extremely
700 DEG C, oxygen ventilation valve is opened, is passed through oxygen to settling chamber, the gas pressure intensity for adjusting settling chamber is 0.09Pa;
(3) pulsed laser ablation Cu is passed through2O ceramic targets, deposit Cu on substrate2O epitaxial films, the frequency of pulse laser
For 20Hz, the wavelength of pulse laser is 248nm, and pulse laser is in Cu2O ceramic targets surface power density is 6J/cm2, sedimentation time
1 it is small when, after deposition, cooled to room temperature, obtains p-type cuprous oxide epitaxial film.
P-type Cu made from embodiment 12The parameters of O epitaxial films are as shown in table 1:
Table 1
In table 1, μhFor film hole mobility, ρ is film resiativity, NhFor film hole, EgFor film
Optical energy gap.P-type Cu made from embodiment 12O epitaxial films resistivity as low as 4.01 Ω cm, are prepared by current PLD methods
Cu2The minimum value of O films, mobility are up to 34.86cm2v-1s-1, the optical energy gap of film is 2.56eV.These are outstanding
Performance parameter causes Cu prepared by this method2O films possess in solar cell and thin film transistor (TFT) be widely applied before
Scape.
P-type Cu made from embodiment 12The XRD spectrum of O epitaxial films is as shown in Figure 1;Cu is only existed in Fig. 12O(110)、
Cu2(220) three peaks of O (220) and MgO, from macroscopically illustrating Cu2O epitaxial films are monocrystal thin films.
P-type Cu made from embodiment 12The high-resolution-ration transmission electric-lens figure of O epitaxial films is as shown in Figure 2;Can from Fig. 2
To clearly atomic arrangement, can obtaining marked film through analysis, there are Cu with substrate2O (110) ∥ MgO (110) and Cu2O(111)
The relation of ∥ MgO (111), from microcosmic upper explanation Cu2O epitaxial films are monocrystal thin films.
P-type Cu made from embodiment 12The selective electron diffraction figure of O epitaxial films is as shown in Figure 3;By for point diffraction
Analysis and measuring and calculating, only a set of Cu2The diffraction pattern of O, illustrates Cu from microcosmic2O epitaxial films are monocrystal thin films.
P-type Cu made from embodiment 12The transmitance collection of illustrative plates of O epitaxial films is as shown in Figure 4;Pass through Fig. 4, it can be seen that sharp
The band edge of profit, illustrates Cu2Defect is few in O epitaxial films, and quality is high.
Embodiment 2
A kind of low-resistivity, high mobility high quality p-type cuprous oxide epitaxial film preparation method, including:
(1) 5min is respectively washed to substrate using enlightening health cleaning agent (Decon), deionized water, acetone, ethanol successively, blown
Spare after dry, substrate is monocrystalline MgO (110);Adsorbed gas and the impurity of substrate surface are removed, improves sputtering layer and substrate
Bond strength and quality of forming film.
(2) by Cu2During O ceramic targets are placed in the settling chamber of pulse laser deposition equipment with substrate, the substrate is heated extremely
600 DEG C, oxygen ventilation valve is opened, is passed through oxygen to settling chamber, the gas pressure intensity for adjusting settling chamber is 0.09Pa;
(3) Cu described in pulsed laser ablation is passed through2O ceramic targets, deposit Cu on substrate2O epitaxial films, pulse laser
Frequency is 20Hz, and the wavelength of pulse laser is 248nm, and pulse laser is in Cu2O ceramic targets surface power density is 6J/cm2, deposition
When time 1 is small, after deposition, cooled to room temperature, obtains p-type cuprous oxide epitaxial film.
P-type Cu made from embodiment 22O epitaxial films resistivity as low as 6.67 Ω cm, mobility are up to 23.75cm2v-1s
-1, the optical energy gap of film is 2.56eV.
Embodiment 3
A kind of low-resistivity, high mobility high quality p-type cuprous oxide epitaxial film preparation method, including:
(1) 5min is respectively washed to substrate using enlightening health cleaning agent (Decon), deionized water, acetone, ethanol successively, blown
Spare after dry, substrate is monocrystalline MgO (110);Adsorbed gas and the impurity of substrate surface are removed, improves sputtering layer and substrate
Bond strength and quality of forming film.
(2) by Cu2During O ceramic targets are placed in the settling chamber of pulse laser deposition equipment with substrate, the substrate is heated extremely
500 DEG C, oxygen ventilation valve is opened, is passed through oxygen to settling chamber, the gas pressure intensity for adjusting settling chamber is 0.09Pa;
(3) Cu described in pulsed laser ablation is passed through2O ceramic targets, deposit Cu on substrate2O epitaxial films, pulse laser
Frequency is 20Hz, and the wavelength of pulse laser is 248nm, and pulse laser is in Cu2O ceramic targets surface power density is 6J/cm2, deposition
When time 1 is small, after deposition, cooled to room temperature, obtains p-type cuprous oxide epitaxial film.
P-type Cu made from embodiment 22O epitaxial films resistivity as low as 15.87 Ω cm, mobility are up to 7.51cm2v-1s-1, the optical energy gap of film is 2.56eV.
Comparative example
Document [N.Kikuchi, K.Tonooka, Electrical and structural properties of Ni-
doped Cu2O films prepared by pulsed laser deposition,Thin Solid Films 486
(2005) 33-37] pulse laser method has been used, has selected CuO targets, SiO2Substrate, optical maser wavelength 248nm, pulse laser
Frequency is 10Hz, laser energy density 1.25J/cm2, depositing temperature is 500 DEG C, and when deposition is not passed through gas and keeps vacuum.
Cu prepared by comparative example2O film resiativities are 1 × 102–2×102Ω cm scopes, mobility is in 20-25cm2v-1s-1
Scope.
Table 2 is Cu prepared by the prior art2O epitaxial films and p-type Cu made from the method for the present invention2The performance of O epitaxial films
Parameter deck watch;In table 2, μhFor film hole mobility, ρ is film resiativity, NhFor film hole.
Table 2
As shown in Table 2, the prior art, Cu prepared by the method for the present invention are contrasted2O epitaxial films possess lower resistivity,
The hole mobility and carrier concentration of higher, therefore, the Cu prepared using the process conditions of the present invention2O epitaxial films are more suitable
For the relevant device such as solar cell and thin film transistor (TFT).
Claims (7)
- A kind of 1. preparation method of low resistivity p-type cuprous oxide epitaxial film, it is characterised in that including:(1) substrate is cleaned, the substrate is monocrystalline MgO (110);(2) by Cu2O ceramic targets are placed in the settling chamber of pulse laser deposition equipment with the substrate, heat the substrate to 500- 700 DEG C, oxygen ventilation valve is opened, is passed through oxygen to settling chamber, the gas pressure intensity for adjusting settling chamber is 0.085-0.095Pa;(3) Cu described in pulsed laser ablation is passed through2O ceramic targets, deposit Cu over the substrate2O epitaxial films, to obtain the final product.
- 2. a kind of preparation method of low resistivity p-type cuprous oxide epitaxial film according to claim 1, its feature exist In in the step (2), heating the substrate to 700 DEG C, the pressure for adjusting settling chamber is 0.09Pa.
- 3. a kind of preparation method of low resistivity p-type cuprous oxide epitaxial film according to claim 1, its feature exist In in the step (3), the frequency of pulse laser is 10-20Hz, and the wavelength of pulse laser is 248nm, and pulse laser is described Cu2O ceramic targets surface power density is 5-6J/cm2, when sedimentation time is 1 small, after deposition, cooled to room temperature, obtains To p-type cuprous oxide epitaxial film.
- 4. a kind of preparation method of low resistivity p-type cuprous oxide epitaxial film according to claim 3, its feature exist In in the step (3), the frequency of pulse laser is 20Hz, and the wavelength of pulse laser is 248nm, and pulse laser is described Cu2O ceramic targets surface power density is 6J/cm2, when sedimentation time is 1 small, after deposition, cooled to room temperature, obtains p Type cuprous oxide epitaxial film.
- 5. a kind of preparation method of low resistivity p-type cuprous oxide epitaxial film according to claim 1, its feature exist In, in the step (2), keep settling chamber vacuum be less than 10-4Pa。
- 6. a kind of preparation method of low resistivity p-type cuprous oxide epitaxial film according to claim 1, its feature exist In, the step (1), cleans substrate, including:Successively using enlightening health cleaning agent, deionized water, acetone, ethanol to the substrate Cleaned, it is spare after drying.
- 7. according to a kind of preparation method of any low resistivity p-type cuprous oxide epitaxial films of claim 1-6, it is special Sign is, 5min is cleaned to the substrate using enlightening health cleaning agent, deionized water, acetone, ethanol.
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Cited By (2)
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CN108642448A (en) * | 2018-05-16 | 2018-10-12 | 山东大学 | A kind of vacuum production method of low-resistivity N-shaped cuprous oxide film |
CN115376631A (en) * | 2022-08-16 | 2022-11-22 | 江苏科技大学 | Method for acquiring dielectric function and electronic correlation degree of p-type transparent conductive film |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108642448A (en) * | 2018-05-16 | 2018-10-12 | 山东大学 | A kind of vacuum production method of low-resistivity N-shaped cuprous oxide film |
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CN115376631A (en) * | 2022-08-16 | 2022-11-22 | 江苏科技大学 | Method for acquiring dielectric function and electronic correlation degree of p-type transparent conductive film |
CN115376631B (en) * | 2022-08-16 | 2023-06-23 | 江苏科技大学 | Method for acquiring dielectric function and electronic relevance of p-type transparent conductive film |
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