CN109449224B - Silicon-based photoelectric material and preparation method thereof - Google Patents
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- CN109449224B CN109449224B CN201811054222.6A CN201811054222A CN109449224B CN 109449224 B CN109449224 B CN 109449224B CN 201811054222 A CN201811054222 A CN 201811054222A CN 109449224 B CN109449224 B CN 109449224B
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- H01L31/032—
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- 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
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/02521—Materials
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- 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
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/02521—Materials
- H01L21/02551—Group 12/16 materials
- H01L21/02554—Oxides
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- 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
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/0257—Doping during depositing
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- H01L31/0321—
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- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
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- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Photovoltaic Devices (AREA)
- Luminescent Compositions (AREA)
Abstract
The invention is suitable for the technical field of photoelectricity, and provides a silicon-based photoelectric material, which is characterized by comprising the following components: a monocrystalline silicon wafer; er doped CeO attached to the monocrystalline silicon wafer2A film; and CeO doped attached to said Er2A layer of Ag particles on the surface of the film. Compared with the silicon-based Er doped CeO without deposited Ag particles, the silicon-based photoelectric material provided by the embodiment of the invention2The film material has the excitation peak shifted to the left and obviously raised photoluminescence intensity, especially Er3+The light-emitting peak intensity of the wavelength of 1540nm is obviously increased, the light-emitting efficiency is obviously improved, the light-emitting performance is greatly improved, and the method is more suitable for industrial application.
Description
Technical Field
The invention belongs to the technical field of photoelectricity, and particularly relates to a silicon-based photoelectric material and a preparation method thereof.
Background
Because of the compatibility with the existing integrated circuit technology and the excellent performance of the silicon-based optoelectronic material, the silicon-based optoelectronic material has been widely paid attention to and researched in recent years, and one of the keys for realizing the silicon-based optoelectronic interconnection is to realize effective light emission on the silicon substrate. However, silicon, which is a basic material in the conventional microelectronic industry, has a low light emitting efficiency as an indirect bandgap semiconductor material, and thus effective light emission cannot be realized.
Because of Ce4+The ionic radius is close to that of trivalent rare earth ions, more rare main ions are expected to be dissolved in solid solution to form a luminescent center, the luminescent center has strong absorption in a near ultraviolet region, and meanwhile, the phonon cut-off frequency is low, the optical transparency is good, the refractive index is high, and the luminescent center is favorable for obtaining high-efficiency rare earth ion luminescence by taking the luminescent center as a luminescent matrix material. More importantly, the excellent properties of the silicon-based composite material in the aspects of dielectric constant, energy band matching and band edge offset with silicon, thermodynamic stability and interface compatibility with silicon and the like are favorable for realizing the silicon-based composite materialThe photoelectric integration of (2). The rare earth Er ion has a special electronic layer structure, has the advantages of narrow spectral band, high color purity, wide wavelength distribution region, small temperature quenching, little influence of a substrate and the external environment, stable physicochemical properties and the like in luminescence, and has 1540nm luminescence with an optical communication waveband, so that the rare earth Er ion is widely researched as a future luminescent material. Currently, CeO2Has been demonstrated to be Er in photoluminescence and electroluminescence3+A suitable material for the ions, so that Er doped CeO is integrated on the silicon substrate2The light-emitting layer is a promising approach. Currently, Er is doped with CeO2Has been reported.
However, Er is doped with CeO2The luminous efficiency is still very low, and the luminous performance is a certain distance away from industrial application, so that the problem of providing a silicon-based optoelectronic material which has high luminous efficiency and is suitable for industrial application is urgently needed to be solved.
Disclosure of Invention
The embodiment of the invention provides a silicon-based photoelectric material, and aims to provide a silicon-based photoelectric material which is high in luminous efficiency and more suitable for industrial application.
The embodiment of the invention is realized in such a way that the silicon-based photoelectric material comprises:
a monocrystalline silicon wafer;
er doped CeO attached to the monocrystalline silicon wafer2A film; and
doped CeO attached to said Er2A layer of Ag particles on the surface of the film.
The embodiment of the invention also provides a preparation method of the silicon-based photoelectric material, which comprises the following steps:
obtaining a clean monocrystalline silicon wafer;
preparing Er doped with CeO on the surface of the monocrystalline silicon wafer2Film is obtained to obtain silicon-based Er doped CeO2A film;
the Er is doped with CeO2Preparing Ag film on the surface of the film to obtain silicon-based Er doped CeO2A thin film Ag film;
doping the silicon-based Er with CeO2Carrying out heat treatment on the film Ag film under the protection of Ar gas to ensure thatAnd forming Ag particles from Ag in the Ag film to obtain the silicon-based photoelectric material.
Compared with the silicon-based Er doped CeO without deposited Ag particles, the silicon-based photoelectric material prepared by the preparation method of the silicon-based photoelectric material provided by the embodiment of the invention2The film material has the excitation peak shifted to the left and obviously raised photoluminescence intensity, especially Er3+The light-emitting peak intensity of the wavelength of 1540nm is obviously increased, the light-emitting efficiency is obviously improved, the light-emitting performance is greatly improved, and the method is more suitable for industrial application.
Drawings
Fig. 1 is a schematic structural diagram of a silicon-based photovoltaic material according to an embodiment of the present invention;
FIG. 2 shows a silicon-based Er doped CeO provided by an embodiment of the present invention2SEM characterization of the films;
FIG. 3 shows CeO according to an embodiment of the present invention2The PLE patterns of the silicon-based photoelectric materials of the first embodiment, the second embodiment and the third embodiment are obtained without depositing Ag particles on the surface of the film;
FIG. 4 shows CeO according to an embodiment of the present invention2The photoluminescence spectra of the silicon-based photoelectric materials of the first embodiment, the second embodiment and the third embodiment are not deposited with Ag particles on the surface of the film.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Fig. 1 shows a structure of a silicon-based photovoltaic material provided by an embodiment of the present invention, which is described in detail below.
The silicon-based photoelectric material provided by the embodiment of the invention comprises a monocrystalline silicon piece and Er doped CeO attached to the monocrystalline silicon piece2Thin film and doped CeO attached to said Er2A layer of Ag particles on the surface of the film.
In the embodiment of the invention, the monocrystalline silicon piece is a heavily boron-doped monocrystalline silicon piece, the resistivity is 0.001-50 omega cm, and the orientation is <100 >. It is understood that, for the monocrystalline silicon wafer, other P-type or N-type doped monocrystalline silicon wafers may be used, and are not particularly limited.
In the embodiment of the invention, the Er is doped with CeO2The thickness of the film is 50-250nm, and the size of Ag particles in the Ag particle layer is 20-80 nm.
The preparation method of the silicon-based photoelectric material provided by the embodiment of the invention comprises the following steps: obtaining a clean monocrystalline silicon wafer; preparing Er doped with CeO on the surface of the monocrystalline silicon wafer2Film is obtained to obtain silicon-based Er doped CeO2A film; the Er is doped with CeO2Preparing Ag film on the surface of the film to obtain silicon-based Er doped CeO2A thin film Ag film; doping the silicon-based Er with CeO2And carrying out heat treatment on the film Ag film under the protection of Ar gas to enable the Ag film to form an Ag particle layer, thus obtaining the silicon-based photoelectric material.
The following examples are provided to illustrate the performance of the method for preparing a silicon-based photovoltaic material provided in the examples of the present invention.
The first embodiment is as follows:
carrying out RCA standard cleaning on the monocrystalline silicon wafer;
and (3) using HF: rinsing with a 1:4 HF solution to obtain a clean monocrystalline silicon wafer;
preparation of 150 nm-thick Er-doped CeO on surface of clean monocrystalline silicon wafer2A film;
doping Er with CeO2Preparing an Ag film with the thickness of 5nm on the surface of the film;
doping the silicon-based Er with CeO2Placing the film Ag film in heat treatment equipment, and introducing Ar gas until air in the heat treatment equipment is exhausted;
controlling the heat treatment equipment to heat up to 400 ℃ at the speed of 100 ℃/s under the condition of keeping introducing Ar gas, continuously preserving heat for 1min, and turning off a power supply;
and cooling to room temperature under the condition of keeping introducing Ar gas to obtain the product.
Example two:
carrying out RCA standard cleaning on the monocrystalline silicon wafer;
and (3) using HF: rinsing with a 1:4 HF solution to obtain a clean monocrystalline silicon wafer;
preparation of Er-doped CeO with thickness of 50nm on surface of clean monocrystalline silicon wafer2A film;
doping Er with CeO2Preparing an Ag film with the thickness of 10nm on the surface of the film;
doping the silicon-based Er with CeO2Placing the film Ag film in heat treatment equipment, and introducing Ar gas until air in the heat treatment equipment is exhausted;
controlling the heat treatment equipment to heat up to 450 ℃ at the speed of 150 ℃/s under the condition of keeping introducing Ar gas, continuously preserving heat for 1.5min, and turning off a power supply;
and cooling to room temperature under the condition of keeping introducing Ar gas to obtain the product.
Example three:
carrying out RCA standard cleaning on the monocrystalline silicon wafer;
and (3) using HF: rinsing with a 1:4 HF solution to obtain a clean monocrystalline silicon wafer;
preparation of Er-doped CeO with thickness of 250nm on surface of clean monocrystalline silicon wafer2A film;
doping Er with CeO2Preparing an Ag film with the thickness of 15nm on the surface of the film;
doping the silicon-based Er with CeO2Placing the film Ag film in heat treatment equipment, and introducing Ar gas until air in the heat treatment equipment is exhausted;
controlling the heat treatment equipment to heat up to 500 ℃ at the speed of 200 ℃/s under the condition of keeping introducing Ar gas, continuously preserving heat for 2min, and turning off a power supply;
and cooling to room temperature under the condition of keeping introducing Ar gas to obtain the product.
In the embodiment of the invention, Er doped with CeO can be prepared on the surface of a clean monocrystalline silicon wafer by a radio frequency magnetron sputtering method, a sol-gel method, a pulse laser sputtering deposition method and the like2The film is not particularly limited, and Er doped with CeO is prepared by utilizing a radio frequency magnetron sputtering method2Thin film for example, Er doped CeO is prepared on the surface of a clean monocrystalline silicon wafer2The procedure of the film is illustrated:
1. by doping with 0.5% (mol ratio) Er2O3CeO (B) of2The ceramic target is used as a target material;
2. putting the cleaned silicon wafer into a cavity of a magnetron sputtering device, and vacuumizing the cavity to 5 multiplied by 10-3Pa;
3. Then introducing argon gas with the flow of 30sccm, and adjusting a gate valve to enable the sputtering working pressure to be 1.2 Pa;
4. raising the temperature of the sample stage to 120 ℃, and adjusting the sputtering power acting on the ceramic target to 125W;
5. sputtering for 2h to obtain Er doped CeO with the thickness of about 100nm2A film.
6. The Er prepared by the method is doped with CeO2Placing the film into a tube furnace, and introducing O2Heat treatment is carried out for 6min at 800 ℃ to obtain the prepared silicon-based Er doped CeO2A film.
In the embodiment of the invention, CeO can be doped in Er by a high-vacuum multi-source thermal evaporation deposition method, an electron beam evaporation method, a direct-current magnetron sputtering method or the like2Preparing Ag layer on the surface of the film, wherein CeO is doped into Er by taking the example of preparing the Ag layer by using a high-vacuum multi-source thermal evaporation deposition method as an example2Preparation of Ag films on the film surface for illustration:
1. doping silicon-based Er with CeO2The film is fixed on a substrate in the thermal evaporation deposition cavity and is blocked by a baffle plate; shearing a proper amount of silver wires, wiping the surface with alcohol, and then putting the silver wires into a quartz boat in an evaporation deposition cavity;
2. the air pump is opened to pump the vacuum degree in the cavity to 5 multiplied by 10-3Pa;
3. Opening a thermal evaporation power supply and a film thickness meter, adjusting the current to 160-200A, opening a baffle plate, and displaying the deposition rate of 0.05-0.2nm/s by the film thickness meter;
4. and when the thickness of the film thickness meter shows that the deposition thickness is 5-20nm, closing the baffle and the thermal evaporation power supply.
In the embodiment of the present invention, the thermal processing apparatus is an RTP-300 rapid thermal processing apparatus, and it is understood by those skilled in the art that the selection of the thermal processing apparatus is merely an example, and in the practical application process, the selection may be specifically performed according to a specific finished product amount, and does not limit the protection scope of the present invention. The RTP-300 rapid thermal processing equipment can expel the air in the equipment by introducing Ar gas at the rate of 30sccm for 15 minutes.
In the embodiment of the invention, the Ar gas is firstly introduced to drive off the air in the equipment and the argon is continuously introduced in the whole heat treatment process, so that the problem that the enhanced luminescence is reduced or even the enhanced luminescence is not effective due to the oxidation of Ag in the rapid heat treatment process can be solved.
In the embodiment of the invention, the temperature rise rate, the heat preservation temperature and the heat preservation time are matched with each other to prepare the uniform Ag particles with good sphericity, so that the enhanced luminescence effect is maximized, and the problem that the enhanced luminescence is weakened or even does not work due to the poor matching of the temperature rise rate, the heat preservation temperature and the heat preservation time is solved.
In the implementation of the invention, the performance of the obtained silicon-based photoelectric material is characterized by the following method. Testing of Er-doped CeO Using a Cold Field Emission Scanning Electron Microscope (FESEM) model HITACHI S-4800 manufactured by Hitachi, Japan2And the Ag particle size is obtained according to the surface morphology of the film. The films were subjected to photoluminescence testing using a SpectraPro 2500i monochromator system from Acton Research Corporation and UV-visible spectroscopy using an FLS920P spectrometer from Edinburgh Corporation.
FIGS. 2(a), 2(b), and 2(c) are the silicon-based Er doped CeO of the first, second, and third embodiments, respectively2The SEM appearance of the film shows that the size of Ag particles increases with the increase of the deposition thickness of the Ag film, and the average particle size of the Ag particles is equal to about 22nm, 50nm and 78nm in sequence.
FIG. 3 shows silicon-based Er doped CeO2PLE (photoluminescence excitation spectrum, change of emission intensity of a substance at a certain wavelength under the action of excitation light with different wavelengths) of silicon-based photoelectric materials of example I, example II and example III, wherein Ag particles are not deposited on the surface of the film, and the change of emission intensity of a substance at a certain wavelength can be seen from the PLE spectrum3+The light with the wavelength of 548nm is emitted, the three groups of samples deposited with Ag are more shifted to the left than the samples not deposited with Ag particles, and the light with the corresponding wavelength of 548nm is emittedThe intensity peak of the emitted light is significantly increased.
FIG. 4 shows silicon-based Er doped CeO2The photoluminescence spectra of the silicon-based photoelectric materials of the first, second and third examples, on which no Ag particles are deposited, can be seen from the figure that the three groups of samples with Ag deposited thereon have significantly improved luminescence intensity, especially Er3+The intensity of the luminescence peak at a wavelength of-1540 nm is significantly increased.
In summary, the silicon-based photoelectric material prepared by the method for preparing the silicon-based photoelectric material provided by the embodiment of the invention is relatively to the silicon-based Er doped with CeO without depositing Ag particles2The film material has the excitation peak shifted to the left and obviously raised photoluminescence intensity, especially Er3+The light-emitting peak intensity of the wavelength of 1540nm is obviously increased, the light-emitting efficiency is obviously improved by 1.5 times to the maximum, the light-emitting performance is greatly improved, and the method is more suitable for industrial application.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (4)
1. A silicon-based photovoltaic material, comprising:
a monocrystalline silicon wafer;
er doped CeO attached to the monocrystalline silicon wafer2A film; and
doped CeO attached to said Er2The Ag particle layer on the surface of the film is characterized in that the average size of Ag particles in the Ag particle layer is 78nm, the Ag particles are spherical, and the Er is doped with CeO2The thickness of the film is 250nm, the Ag particle layer is formed by carrying out heat treatment on an Ag film under the protection of Ar gas, and the thickness of the Ag film is 15 nm; and the Ag film is treated under the following heat treatment conditions:
and under the condition of keeping introducing Ar gas, controlling the heat treatment equipment to heat up to 500 ℃ at the speed of 200 ℃/s, and continuously preserving heat for 2 min.
2. The silicon-based photovoltaic material according to claim 1, wherein the single crystal silicon wafer is a heavily boron-doped single crystal silicon wafer, and has a resistivity of 0.001 to 50 Ω -cm and an orientation of <100 >.
3. A preparation method of a silicon-based photoelectric material is characterized by comprising the following steps:
obtaining a clean monocrystalline silicon wafer;
preparing Er doped with CeO on the surface of the monocrystalline silicon wafer2Film is obtained to obtain silicon-based Er doped CeO2A film;
the Er is doped with CeO2Preparing Ag film on the surface of the film to obtain silicon-based Er doped CeO2A thin film Ag film;
doping the silicon-based Er with CeO2Carrying out heat treatment on the film Ag film under the protection of Ar gas to enable the Ag film to form an Ag particle layer, and obtaining the silicon-based photoelectric material; wherein the average size of Ag particles in the Ag particle layer is 78nm, the Ag particles are spherical, and the Er is doped with CeO2The thickness of the film is 250nm, and the thickness of the Ag film is 15 nm; and the heat treatment conditions are as follows:
doping the silicon-based Er with CeO2The method comprises the following steps of carrying out heat treatment on the film Ag film under the protection of Ar gas, and specifically comprises the following steps:
doping the silicon-based Er with CeO2Placing the film Ag film in heat treatment equipment, and introducing Ar gas until air in the heat treatment equipment is exhausted;
controlling the heat treatment equipment to heat up to 500 ℃ at the speed of 200 ℃/s under the condition of keeping introducing Ar gas, continuously preserving heat for 2min, and turning off a power supply;
and cooling to room temperature under the condition of keeping introducing Ar gas to obtain the product.
4. The method for preparing a silicon-based photovoltaic material according to claim 3, wherein the step of obtaining a clean monocrystalline silicon wafer comprises:
carrying out RCA standard cleaning on the monocrystalline silicon wafer;
and (3) using HF: rinsing with a 1:4 HF solution to obtain a clean monocrystalline silicon wafer.
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