CN103268858B - A kind of preparation method of near-infrared photoelectricity silicon materials - Google Patents
A kind of preparation method of near-infrared photoelectricity silicon materials Download PDFInfo
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- CN103268858B CN103268858B CN201310173942.5A CN201310173942A CN103268858B CN 103268858 B CN103268858 B CN 103268858B CN 201310173942 A CN201310173942 A CN 201310173942A CN 103268858 B CN103268858 B CN 103268858B
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- silicon chip
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- crystal silicon
- element sulphur
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Abstract
The invention discloses a kind of preparation method of near-infrared photoelectricity silicon materials, comprise crystal silicon chip heavy doping element sulphur, the crystal silicon chip of heavy doping element sulphur is placed in annealing device adopts electric field-assisted to anneal, the voltage swing of annealing electric field is for can not puncture silicon chip, annealing temperature is 550 DEG C, and annealing time is 6 hours.The method can hinder the precipitation of heavily doped element sulphur element sulphur in annealing process in surface of crystalline silicon, makes element sulphur in the heavily doped element sulphur layer of surface of crystalline silicon keep higher concentration, and can improve the photoelectric properties of near-infrared photoelectricity silicon materials.
Description
Technical field
The invention belongs to crystalline silicon technologies field, be specifically related to a kind of preparation method of near infrared light electric material.
Background technology
Heavy doping element sulphur silicon materials (sulfurhypedopedsilicon) are considered to the material that can form Intermediate Gray impurity energy level, and the research for it originates in the research to black silicon.Research finds, black silicon is the heavy doping of element sulphur in the light absorption physics root that near-infrared portion of energy is less than energy gap.Heavy doping sulphur in silicon, material there occurs not special phase transformation, and silicon materials are significantly improved in the absorption of infrared part.Therefore, heavy doping element sulphur silicon materials have very important application potential in photovoltaic cell, communication sensor field.
At present, in prior art, the method preparing heavy doping element sulphur silicon materials has laser assisted doping method and ion implantation, and wherein the doping content of laser assisted doping method (is the highlyest about 10
20atom/cm
3) (be the highlyest about 10 higher than the doping content of ion implantation
16atom/cm
3), laser assisted etching method is that silicon chip is placed in sulphur hexafluoride atmosphere, silicon face is scanned with femtosecond laser, downward 0 ~ 500nm the part in silicon top layer forms element sulphur heavy doping, by controlling background gas pressure, femtosecond (or nanosecond) laser pulse number, the parameters such as light intensity reach the object controlling inner element sulphur doped level; Ion implantation is the method for common doped semiconductor, due to it, there is controllable doped concentration and be not heated mechanical equilibrium condition restriction and widespread adoption in the heavy doping of semiconductor device.
Laser assisted doping method is better than ion implantation, but in annealing process, sulphion slowly can separate out silicon top layer, causes the decline of laser doping layer sulphion concentration, affects its photoelectric properties.
Summary of the invention
The object of this invention is to provide a kind of preparation method of near-infrared photoelectricity silicon materials, the method can hinder the precipitation of heavily doped element sulphur element sulphur in annealing process in surface of crystalline silicon, make element sulphur in the heavily doped element sulphur layer of surface of crystalline silicon keep higher concentration, and the photoelectric properties of near-infrared photoelectricity silicon materials can be improved.
Because electric field plays a part to hinder sulphion drift in annealing process, so by the crystal silicon chip of heavy doping element sulphur is placed in electric field when annealing, the element sulphur doping of larger concentration can be obtained on crystal silicon chip surface, form Intermediate Gray, and then make crystal silicon chip have better photoelectric property.
Above-mentioned purpose of the present invention is achieved by the following technical solution: a kind of preparation method of near-infrared photoelectricity silicon materials, comprise crystal silicon chip heavy doping element sulphur, the crystal silicon chip of heavy doping element sulphur is placed in annealing device adopts electric field-assisted to anneal, the voltage swing of annealing electric field is for can not puncture silicon chip, annealing temperature is 550 DEG C, and annealing time is 6 hours.
The anneal voltage of electric field of the present invention is preferably 10000V.
The present invention the crystal silicon chip of heavy doping element sulphur is placed in annealing device carry out electric field-assisted annealing time, make the positive pole of surface towards electric field of crystal silicon chip heavy doping element sulphur, and direction of an electric field is perpendicular to the surface of this crystal silicon chip heavy doping element sulphur.
As a modification of the present invention, in order to keep the heavily doped element sulphur concentration of surface of crystalline silicon consistent, electric field of the present invention is preferably uniform electric field.
Electric field of the present invention is preferably arranged on inside or the outside of annealing device.
The present invention carries out weight sulfur doping to adopting laser during crystal silicon chip heavy doping element sulphur.
Laser of the present invention is preferably femtosecond or nanosecond laser.
Crystal silicon chip is placed in chamber by the present invention, regulates chamber inner pressure to be preferably 1 × 10 by force
-3below pa, is filled with sulfurous gas and is preferably 0.5 ± 0.01Pa by force to chamber inner pressure, regulates laser intensity to be preferably 1.8J/cm
2, adopt femtosecond or nanosecond laser facula scanning surface of crystalline silicon, when laser inswept all silicon faces, the chamber being mounted with crystal silicon chip vacuumized process to vacuum degree and be preferably 1 × 10
-3below pa, is filled with inert gas and is preferably 0.5 ± 0.01Pa by force to chamber inner pressure, and taking-up crystal silicon chip is placed in electric field and carries out auxiliary annealing.
Sulfurous gas of the present invention is preferably SF
6; Described inert gas is preferably argon gas.
Crystal silicon chip of the present invention is preferably monocrystalline silicon piece.
Crystal silicon chip of the present invention need carry out ultrasonic cleaning process, and the solvent that described ultrasonic cleaning adopts is acetone.
Specifically, the preparation method of a kind of near-infrared photoelectricity silicon materials provided by the invention, comprises the following steps:
(1) clean is carried out to surface of crystalline silicon;
(2) weight sulfur doping is carried out to surface of crystalline silicon;
(3) crystal silicon chip after heavy sulfur doping is placed in annealing device and carries out electric field-assisted annealing.
Compared with prior art, tool of the present invention has the following advantages: the crystal silicon chip after counterweight sulfur doping of the present invention, adopt electric field-assisted when annealing, element sulphur is subject to the precipitation of electric field action to element sulphur and has hysteresis, thus the silicon materials that preparation is formed have very high near infrared absorption coefficient.
Accompanying drawing explanation
Fig. 1 is the flow chart of the preparation method of near-infrared photoelectricity silicon materials of the present invention;
Fig. 2 is electric field-assisted annealing schematic diagram in the embodiment of the present invention 1, and the electrode wherein forming electric field is placed in annealing furnace; Wherein 1 is annealing furnace, and 2 is heater strip, and 3 is high-voltage DC power supply, and 4 is positive pole, and 5 is T-shaped support, and 6 is negative pole;
Fig. 3 is electric field-assisted annealing schematic diagram in the embodiment of the present invention 2, and the electrode wherein forming electric field is placed on outside annealing furnace.
Fig. 4 does not use its inner element sulphur concentration of electric field along with the relation of the degree of depth in embodiment 1 and 2, abscissa is the degree of depth on distance crystal silicon chip surface, and ordinate is the concentration of element sulphur;
Fig. 5 has added its inner element sulphur concentration of electric field with depth relationship in embodiment 1 and 2, abscissa is the degree of depth on distance crystal silicon chip surface, and ordinate is the concentration of element sulphur;
Fig. 6 is that in embodiment 1 and 2, absorption coefficient, at non-added electric field, has added the performance in electric field and crystalline silicon, and abscissa is wavelength, and ordinate is the absorption coefficient of light.
Embodiment
Below in conjunction with drawings and Examples, the present invention is further illustrated.
embodiment 1
As shown in fig. 1, the preparation method of the near-infrared photoelectricity silicon materials that the present embodiment provides, containing following steps:
(1) monocrystalline silicon surface is cleaned, cleaning process comprises and is placed in acetone soln by silicon, is placed in sonication chamber, opens the switch of sonication chamber by the acetone soln soaking silicon chip, take out the silicon chip cleaned after 20 minutes, be loaded on the objective table of vacuum chamber;
(2) weight sulfur doping is carried out to crystal silicon chip, vacuum chamber is vacuumized, regulate pressure to be 1 × 10
-3below Pa, opens charging valve, pours background gas SF with the flow of 40sccm
6, to vacuum chamber, pressure is 0.5 ± 0.01pa, after gas pressure in vacuum is stable, opens femtosecond (or nanosecond) laser, laser intensity is adjusted to 1.8J/cm
2, open automatic control console, make the surface of femtosecond laser hot spot inswept monocrystalline silicon slowly, after the inswept all silicon faces of laser, vacuum chamber is evacuated to 1 × 10
-3below pa, is filled with argon gas to 0.5 ± 0.01pa, is taken out by monocrystalline silicon in vacuum chamber, is placed on annealing furnace objective table, carries out next step annealing in process;
(3) design of electric field-assisted annealing annealing furnace and electric field is as follows: be provided with resistive heater 2 at the outer wall position place, both sides of annealing furnace 1, the design of electric field as shown in Figure 2, the positive electrode 4 of generation electric field and negative electrode 6 are arranged on the inside of annealing device and annealing furnace 1, wherein positive electrode is positioned at top, negative electrode is positioned at below, monocrystalline silicon piece is placed between two electrode plate, the size of electrode is designed to about 10cm × 10cm, just, negative electrode is fixing in the lehr by T-shaped support 5 grade, wherein crystal silicon chip is positioned on the crossbearer of T-shaped support, negative pole can be fixed in the vertical frame of T-shaped support, the material of T-shaped support is insulating material, and can the high temperature of resistance to more than 1000 DEG C.Monocrystalline silicon is weighed the surface of sulfur doping just to positive pole by laser, on the inwall of annealing furnace, arbitrary position arranges an aperture, the radius of aperture can be about 5mm, and for the wire through connection positive and negative electrode, this wire is connected with the high-voltage DC power supply 6 of outside, wire is wanted and annealing body of heater keeps airtight, top electrode connects positive source, and bottom electrode connects power cathode, and electric field level setting model does not puncture air, do not puncture silicon chip, specifically depend on the circumstances.In the present invention, positive pole or negative pole fixed form is in the lehr not limited to enumerating in the present embodiment, is only citing herein, not limits it.
The surface of crystalline silicon of laser processing is placed towards positive pole, open annealing furnace, and open high voltage source, make direction of an electric field between pole plate perpendicular to silicon face, electric field level setting model does not puncture air simultaneously, do not puncture silicon chip, specifically depend on the circumstances, can adopt the high pressure of 10000v, adjustment annealing temperature is 550 DEG C, after 6 hours to be annealed, by silicon chip extracting.
With depth relationship as shown in Figure 4, the inner element sulphur of crystal silicon chip of the heavy doping element sulphur adopting the present embodiment electric field-assisted to anneal during annealing with depth relationship as shown in Figure 5 for the inner element sulphur of crystal silicon chip of the heavy doping element sulphur wherein not adopting electric field-assisted to anneal during annealing.As can be seen from the surperficial increase along with the degree of depth of the crystal silicon chip of the heavy doping element sulphur adopting the present embodiment electric field-assisted to anneal when annealing in Fig. 4 and Fig. 5, Fig. 5, what do not adopt electric field-assisted to anneal when the concentration decline of element sulphur is comparatively annealed is slow.
The crystal silicon chip absorption coefficient of light of the heavy doping element sulphur wherein not adopting electric field-assisted to anneal, adopt electric field-assisted annealing heavy doping element sulphur crystal silicon chip the absorption coefficient of light and without heavy doping element sulphur, the absorption coefficient of light of the common crystal silicon chip not adopting electric field-assisted to anneal as shown in Figure 6, as can be seen from Figure 6, adopt the crystal silicon chip absorption coefficient of light of the heavy doping element sulphur of electric field-assisted annealing relative to the crystal silicon chip absorption coefficient of light of the heavy doping element sulphur not adopting electric field-assisted to anneal with through heavy doping element sulphur, the absorption coefficient of light of the common crystal silicon chip not adopting electric field-assisted to anneal wants high.
embodiment 2
As shown in fig. 1, the preparation method of the near-infrared photoelectricity silicon materials that the present embodiment provides, containing following steps:
(1) monocrystalline silicon surface is cleaned, cleaning process comprises and silicon to be placed in acetone soln some minutes, the acetone soln soaking silicon chip is placed in sonication chamber, open the switch of sonication chamber, continue the silicon chip taking out to have cleaned for 20 minutes, be loaded on the objective table of vacuum chamber;
(2) weight sulfur doping is carried out to crystal silicon chip, vacuum chamber is vacuumized, regulate pressure to be 1 × 10
-3below Pa, opens charging valve, pours background gas SF with the flow of 40sccm
6, to vacuum chamber, pressure is 0.5 ± 0.01pa, after gas pressure in vacuum is stable, opens femtosecond (or nanosecond) laser, laser intensity is adjusted to 1.8J/cm
2, open automatic control console, make the surface of femtosecond laser hot spot inswept monocrystalline silicon slowly, after the inswept all silicon faces of laser, vacuum chamber is evacuated to 1 × 10
-3below pa, is filled with argon gas to 0.5 ± 0.01pa, is taken out by monocrystalline silicon in vacuum chamber, is placed on annealing furnace objective table, carries out next step annealing in process;
(3) design of electric field-assisted annealing annealing furnace and electric field is as follows: be provided with resistive heater at the outer wall position place, both sides of annealing furnace, the design of electric field as shown in Figure 3, the positive and negative electrode producing electric field is arranged on the outside of annealing device and annealing furnace, wherein positive electrode is positioned at above annealing furnace, negative electrode is positioned at below annealing furnace, the size of electrode is designed to about 20cm × 20cm, annealing furnace with a T-shaped stentplacement between two battery lead plates, making timbering material is insulating material, battery lead plate top electrode connects positive pole, bottom crown connects negative pole, monocrystalline silicon piece is arranged in annealing furnace, be provided with T-shaped support in the lehr, monocrystalline silicon is arranged on the crossbearer of T-shaped support, monocrystalline silicon is weighed the surface of sulfur doping just to positive pole by laser, the material of T-shaped support is insulating material, and can the high temperature of resistance to more than 1000 DEG C, in the present invention, the fixed form of positive pole or negative pole and monocrystalline silicon piece is not limited to enumerating in the present embodiment, is only citing herein, not limits it.
The surface of crystalline silicon of laser processing is placed towards positive pole, open annealing furnace, and open high voltage source, make direction of an electric field between pole plate perpendicular to silicon face, electric field level setting model does not puncture air simultaneously, do not puncture silicon chip, specifically depend on the circumstances, can adopt the high pressure of 10000v, adjustment annealing temperature is 550 DEG C, after 6 hours to be annealed, by silicon chip extracting.
With depth relationship as shown in Figure 4, the inner element sulphur of crystal silicon chip of the heavy doping element sulphur adopting the present embodiment electric field-assisted to anneal during annealing with depth relationship as shown in Figure 5 for the inner element sulphur of crystal silicon chip of the heavy doping element sulphur wherein not adopting electric field-assisted to anneal during annealing.As can be seen from the surperficial increase along with the degree of depth of the crystal silicon chip of the heavy doping element sulphur adopting the present embodiment electric field-assisted to anneal when annealing in Fig. 4 and Fig. 5, Fig. 5, what do not adopt electric field-assisted to anneal when the concentration decline of element sulphur is comparatively annealed is slow.
The crystal silicon chip absorption coefficient of light of the heavy doping element sulphur wherein not adopting electric field-assisted to anneal, adopt electric field-assisted annealing heavy doping element sulphur crystal silicon chip the absorption coefficient of light and without heavy doping element sulphur, the absorption coefficient of light of the common crystal silicon chip not adopting electric field-assisted to anneal as shown in Figure 6, as can be seen from Figure 6, adopt the crystal silicon chip absorption coefficient of light of the heavy doping element sulphur of electric field-assisted annealing relative to the crystal silicon chip absorption coefficient of light of the heavy doping element sulphur not adopting electric field-assisted to anneal with through heavy doping element sulphur, the absorption coefficient of light of the common crystal silicon chip not adopting electric field-assisted to anneal wants high.
The present invention will be described more than to enumerate specific embodiment.It is pointed out that above embodiment is only for the invention will be further described, do not represent protection scope of the present invention, the nonessential amendment that other people prompting according to the present invention is made and adjustment, still belong to protection scope of the present invention.
Claims (9)
1. the preparation method of near-infrared photoelectricity silicon materials, comprise crystal silicon chip heavy doping element sulphur, it is characterized in that: the crystal silicon chip of heavy doping element sulphur is placed in annealing device and adopts electric field-assisted to anneal, the voltage of annealing electric field is 10000V, annealing temperature is 550 DEG C, and annealing time is 6 hours.
2. the preparation method of near infrared light electric material according to claim 1, it is characterized in that: the crystal silicon chip of heavy doping element sulphur is placed in annealing device carry out electric field-assisted annealing time, make the positive pole of surface towards electric field of crystal silicon chip heavy doping element sulphur, and direction of an electric field is perpendicular to the surface of this crystal silicon chip heavy doping element sulphur.
3. the preparation method of near infrared light electric material according to claim 2, is characterized in that: described electric field is uniform electric field.
4. the preparation method of near infrared light electric material according to claim 1, is characterized in that: carry out weight sulfur doping to adopting laser during crystal silicon chip heavy doping element sulphur.
5. the preparation method of near infrared light electric material according to claim 4, is characterized in that: described laser is femtosecond or nanosecond laser.
6. the preparation method of near infrared light electric material according to claim 5, is characterized in that: during to crystal silicon chip heavy doping element sulphur, crystal silicon chip is placed in chamber, regulates chamber inner pressure to be by force 1 × 10
-3below pa, being filled with sulfurous gas to chamber inner pressure is by force 0.5 ± 0.01Pa, and adjustment laser intensity is 1.8J/cm
2, adopt femtosecond or nanosecond laser facula scanning surface of crystalline silicon, when laser inswept all silicon faces, the chamber being mounted with crystal silicon chip being vacuumized process to vacuum degree is 1 × 10
-3below pa, being filled with inert gas to chamber inner pressure is by force 0.5 ± 0.01Pa, and taking-up crystal silicon chip is placed in electric field and carries out auxiliary annealing.
7. the preparation method of near infrared light electric material according to claim 6, is characterized in that: described sulfurous gas is SF
6; Described inert gas is argon gas.
8. the preparation method of the near infrared light electric material according to any one of claim 1-7, is characterized in that: described crystal silicon chip is monocrystalline silicon piece.
9. the preparation method of near infrared light electric material according to claim 8, is characterized in that: described crystal silicon chip need carry out ultrasonic cleaning process, and the solvent that described ultrasonic cleaning adopts is acetone.
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| US7057256B2 (en) * | 2001-05-25 | 2006-06-06 | President & Fellows Of Harvard College | Silicon-based visible and near-infrared optoelectric devices |
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| CN1323061A (en) * | 2000-03-30 | 2001-11-21 | 国际商业机器公司 | DC or AC electric field auxiliary annealing |
| CN101824654A (en) * | 2009-03-04 | 2010-09-08 | 中国科学院半导体研究所 | Method for manufacturing black silicon material |
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