CN102534570A - Method for preparing microcrystalline silicon film by plasma-enhanced chemical vapor deposition - Google Patents
Method for preparing microcrystalline silicon film by plasma-enhanced chemical vapor deposition Download PDFInfo
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Abstract
The invention relates to a method for preparing a microcrystalline silicon film by plasma-enhanced chemical vapor deposition, belonging to the technical field of plasma application. The invention relates to a method for preparing the microcrystalline silicon film by the chemical vapor deposition technology which adopts a hollow cathode to enhance plasma, in particular to the technology which utilizes a micro-hollow cathode array electrode structure to increase the density of the plasma so as to further improve the deposition rate of the film. After the micro-hollow cathode array electrode structure is adopted, the discharge efficiency is improved, the monomer pyrolysis rate is further improved, and the density of active groups in the space can be increased, so that the deposition rate of the film is greatly improved, and the deposition temperature is reduced.
Description
Technical field:
The present invention relates to a kind of method that adopts hollow cathode to strengthen plasma activated chemical vapour deposition prepared microcrystalline silicon film, especially utilize microvoid the heart-yin utmost point array electrode structure can increase plasma density and then raising depositing of thin film speed.
Background technology:
Solar cell utilizes photovoltaic effect directly conversion of solar energy to be electric energy, is one of optimal novel energy.Silica-base film becomes current this hot research fields as a kind of high-level efficiency, solar cell material cheaply.People have found that the microcrystal silicon battery has better properties and lower cost in preparation amorphous silicon membrane process.During amorphous silicon membrane, change the film growth condition in preparation, can make that the part crystallization of silicon becomes little crystal grain in the film.This film that contains silicon microcrystal grain has material impact to the efficient and life-span of solar cell.
Microcrystal silicon has the optical band gap close with silicon single crystal (1.12eV), and spectral response range comprises ruddiness and region of ultra-red, and efficiency of conversion is higher, and does not almost have photic attenuating effect.And the optical band gap of non-crystalline silicon is 1.7eV, and greater band gap can not be utilized the ir radiation of ruddiness and long-wave band etc., and efficiency of conversion is low, and photic attenuating effect is arranged, and its efficiency of conversion can further reduce along with the time, made its development receive certain limitation.Photic decline that it is generally acknowledged non-crystalline silicon is relevant with its inner Si-Si bond disorder network structure, dangling bonds and other subsurface defects, therefore, eliminates the unordered network structure that this metastable state just must be improved film, and micritization is exactly an important approach.Microcrystal silicon can make with the preparation method identical with non-crystalline silicon, have low temperature process, consumptive material few, be convenient to advantage such as large-area preparation, can deposit on the cheap flexible substrate, be very promising solar cell material.
The current method for preparing microcrystalline silicon film mainly contains: solid phase crystallization method (SPC; Solid Phase C rystallization), liquid phase epitaxial method (LPE; Liquid Phase Epitaxy), chemical vapour deposition (CVD, Chemical Vapor Deposition) etc.
One, solid phase crystallization method (SPC).General deposited amorphous silicon thin film under lower temperature earlier, thermal annealing Siliciumatom that amorphous silicon membrane is under solid-state is activated and recombinates again, and then changes into microcrystalline silicon film.Solid phase crystallization method comprises High Temperature Furnaces Heating Apparatus annealing crystallization method, rapid thermal annealing crystallization method (RTA; Rapid Thermal Annealing), PRK revulsive crystallization method (ELA; Excimer Laser Annealing) and metal-induced crystallization method (MIC, Metal Induced Crystallization) etc.
High Temperature Furnaces Heating Apparatus annealing crystallization method is under vacuum or high pure nitrogen protection, to put into stove to amorphous silicon membrane to anneal, and makes it change polycrystalline state into by non-crystalline state.If adopt glass substrate or plastic, require annealing temperature lower, this can make the annealed time longer, and the speed that heats up has very big influence to grain size.
Rapid thermal annealing crystallization method be with halogen tungsten lamp as thermal source, utilize the heat effect of light and quantum effect that material is annealed, can increase bulk diffusion and surface diffusion coefficient, shorten annealing time greatly, reduce defect concentration simultaneously, can obtain crystallization effect preferably.But this method annealing temperature still belongs to high temperature process greater than 700 ℃.
PRK revulsive crystallization method; Utilize the high-energy of moment laser pulse generation to incide the amorphous silicon membrane surface; The degree of depth that only 100nm is thick on the film top layer produces heat effect; The a-Si film was reached about 1000 ℃ in moment, thereby realize the transformation of a-Si, do not have too much thermal energy conduction to substrate to p-Si.Choose reasonable Wavelength of Laser and power use LASER HEATING just can make the a-Si film reach the temperature of fusing and the temperature of assurance substrate is lower than 450 ℃.The microcrystalline silicon film crystal grain of PRK revulsive crystallization method preparation is big, spatial selectivity good, and doping efficiency is high, intracrystalline imperfection is few, electrology characteristic good, the mobility advantages of higher.But, this method is owing to grain-size is responsive to laser power, and large-area uniformity is relatively poor, poor repeatability, and equipment cost is high, safeguards complicacy, makes its application receive certain limitation.
The metal-induced crystallization method is utilized the atoms metal that exists in the non-crystalline material can reduce the required energy of material crystallization, and is made crystallisation process under lower temperature, to carry out.Before or after deposition a-Si film, vapor deposition last layer metal (Al, Ni, Pd) film makes it be converted into microcrystalline silicon film with heat-treating methods then.Because the existence of atoms metal makes the Si-Si covalent linkage change metallic bond Si-Al into, has greatly reduced excitation energy, thereby has reduced the crystallization temperature of non-crystalline silicon.But the atoms metal that contains in the film can become impurity, and the one-piece construction and the performance of solar cell impacted.
Two, liquid phase epitaxial method (LPE).At a certain temperature, silicon has certain solubleness in a lot of metals.Change the temperature of saturated solution, silicon will be separated out in solution, thereby possibly form the epitaxy of silicon, might obtain the film of microcrystal silicon structure.The microcrystalline silicon film of liquid phase epitaxial method preparation is grown under intimate thermally equilibrated condition, thereby has very low defect concentration and crystal boundary composite reactive, and epitaxial growth temperature is lower, and growth velocity is very fast.In addition, through the control growing condition, utilize liquid phase epitaxial method can directly prepare microcrystal silicon with suede structure.This method is difficult to avoid sneaking into of liquid phase impurity atoms.
Three, chemical vapor deposition (CVD).Chemical vapour deposition is through certain incentive mechanism; Reactant gas molecules is excited and resolves into various reactive groups or ion; These are excited or the ion that decomposites or group are diffused near the substrate and with it and react, finally deposition layer of even thin-film material on substrate.Chemical vapour deposition technique mainly comprises subatmospheric chemical Vapor deposition process (LPCVD; Low Pressure CVD); Hot-wire chemical sinks vapour deposition process (HWCVD, Hotwire CVD) and plasma enhanced chemical vapor deposition method (PECVD, Plasma enhanced CVD) or the like.
The microcrystalline silicon film quality of subatmospheric chemical Vapor deposition process preparation is good, and crystal grain has preferred orientation, but its grain-size is less, and carrier mobility is big inadequately, also usually is accompanied by the increase of surfaceness, and the electrical stability of device is had a negative impact.Hot filament CVD, the deposit film rapid speed, but in the preparation process, the tramp m. atom pollutes film easily.
The plasma enhanced chemical vapor deposition method is to make reactant gases resolve into atom, ion and other reactive groups with plasma body photoglow, at the substrate surface reactive deposition, finally generates microcrystalline silicon film or amorphous silicon membrane.Through optimizing preparation parameter, can make quality microcrystalline silicon film preferably, and temperature is very low, be particularly suitable on flexible substrate such as plastic film, preparing solar cell, received people's extensive concern.
But common plasma enhanced chemical vapor deposition method, the sedimentation rate of preparation microcrystalline silicon film is slower, and crystal grain is less.For this reason, we combine the advantage of hollow cathode discharge, have developed the method that plasma enhanced chemical vapor deposition unit that hollow cathode combines with plate armature prepares microcrystalline silicon film.The kind electrode structure can improve discharging efficiency, and then improves the monomer cleavage rate, increases the reactive group concentration in the space, improves depositing of thin film speed greatly, and can reduce depositing temperature.
Summary of the invention:
To above-mentioned technical problem, the present invention provides a kind of apparatus for atomic layer deposition with array hollow cathode structure,
A kind of apparatus for atomic layer deposition; It is characterized in that: this device comprises gas distributing system 1, vacuum chamber 2, array hollow cathode top electrode 3, flat ground connection lower electrode 4, pumped vacuum systems 5, power-supply system 6; The through hole that it is 1-3mm that said array hollow cathode top electrode 3 has a plurality of equally distributed diameter ranges; The spacing in adjacent hole is 2-4mm; Spacing between array hollow cathode top electrode 3 and the flat ground connection lower electrode 4 is 5-20mm, and array coreless armature 3 connects the air-supply duct of gas distributing system 1.The terminal stud of said formula hollow cathode array electrode 3 is connected to high voltage terminal one end of said power-supply system 6; And keeping insulation with the vacuum chamber of said device, flat ground connection lower electrode, the ground terminal of said power-supply system 6 is connected on said vacuum chamber 2 and the said plate electrode 4.
Said power-supply system 6 is unipolarity or in the bipolar pulse direct supply any of intermediate frequency power supply, the 10-60KHz of high-frequency radio frequency power supply, the 10-60KHz of VHF power supply, the 2-60MHz of 60-100MHz.Said power-supply system adopts pulse control mode can control and regulate the dutycycle in the discharge process.
Said plate electrode 4 is provided with heating unit.
The method steps of using above device is following:
Said gas distributing system 1 comprises two-way gas piping at least, and each gas piping comprises vacuum breaker, operated pneumatic valve switch and mass flowmeter; Wherein operated pneumatic valve closes the period 0.01～10 second scope, and time precision was less than 0.01 second.
Said power-supply system 6 out-put supply dutycycles 5～90%.
The apparatus for atomic layer deposition with array hollow cathode structure that the present invention relates to, said gas distributing system 1 can be controlled the serial or parallel connection of many gas circuits.
The apparatus for atomic layer deposition that the present invention relates to array hollow cathode structure; Said gas distributing system 1 comprises two-way gas piping at least; Air feed individually or simultaneously; The said gas piping of two-way at least has at least a gas circuit to supply argon gas by mass-flow gas meter and accurate solenoid control in the said gas piping of two-way at least.
The apparatus for atomic layer deposition with array hollow cathode structure that the present invention relates to, said pumped vacuum systems 5 can make the base vacuum of said vacuum chamber reach 1 * 10
-4Pa, according to the difference of processing condition, the air pressure during discharge can be controlled within the scope of 10-1000Pa.
The apparatus for atomic layer deposition that the present invention relates to array hollow cathode structure, the mode that said plate electrode 4 adopts downsides to place, as the substrate mounting table, said plate electrode 4 has heating function, and temperature is adjustable continuously in 40～600 ℃ of scopes.
The present invention provides a kind of novel method for preparing microcrystalline silicon film; Adopting little hollow cathode array discharge effect to increase on the basis of plasma density principle; Utilize radio frequency or VHF power supply excitation working gas to produce plasma body, the microcrystalline silicon film of on base materials such as organic film, glass or silicon single crystal, growing; This method specifically may further comprise the steps:
A. substrate pre-treatment: use organic film, monocrystalline silicon piece or sheet glass as substrate; To p type monocrystalline silicon piece with HF acid ultrasonic cleaning, to remove the SiO on surface
2Layer, and then use absolute ethyl alcohol, deionized water to carry out ultrasonic cleaning successively, clean until silicon chip surface, dry up with nitrogen then; Sheet glass directly carries out ultrasonic cleaning with absolute ethyl alcohol, deionized water successively, and is clean until glass sheet surface, dries up with nitrogen then; Adopt absolute ethyl alcohol wiping film surface when adopting organic film as substrate;
B. vacuum obtains and the base station heating: said substrate is placed on the lower electrode, is evacuated to 1 * 10 with molecular pump and mechanical pump
-2Pa-1 * 10
-4Pa; Open the base station heating simultaneously, 40～600 ℃ of control base station TRs;
C. thin film deposition: after vacuum tightness and base station temperature reach said b step and require; Open inlet system, alternately feed silicon source gas and hydrogen, when treating that air pressure satisfies the thin film deposition requirement; Power-on is discharged, and carries out the plasma enhanced chemical vapor deposition microcrystalline silicon film.
D. shutdown: thin film deposition finishes, and stops discharge earlier, closes silicon source gas and hydrogen then successively, and gas circuit and Vakuumkammer are washed with argon gas or nitrogen, closes all power supplys and source of the gas at last.
The method for preparing microcrystalline silicon film that the present invention relates to, wherein said silicon source gas adopts SiH
4, SiH
2Cl
2, SiHCl
3Or SiCl
4In any, or mix an amount of argon gas with the enhanced discharge effect, improve the quality of deposit film.
The method for preparing microcrystalline silicon film that the present invention relates to can produce the density plasma body higher than classic flat-plate electrode under radio frequency or the excitation of VHF power supply.
Description of drawings:
Fig. 1 is the apparatus for atomic layer deposition structural representation with array hollow cathode structure;
Fig. 2 is an array hollow cathode structure front elevational schematic;
Fig. 3 is an array hollow cathode structure schematic side view;
Fig. 4 is the gas distributing system synoptic diagram;
Fig. 5 is air pressure 220Pa, power 80W, the photo of plasma discharge under the interelectrode distance 18mm condition;
Fig. 6 is Raman (Raman) spectrogram of prepared microcrystalline silicon film;
Fig. 7 is the AFM three-dimensional appearance figure on prepared microcrystalline silicon film surface.
Embodiment
The present invention provides a kind of apparatus for atomic layer deposition that has array hollow cathode structure.This covering device comprises gas distributing system 1, vacuum chamber 2, array coreless armature 3, plate electrode 4, pumped vacuum systems 5, power-supply system 6.Utilize the hollow cathode discharge effect of array coreless armature 3; Can significantly improve ionisation of gas efficient; Improve the air pressure and the plasma density of discharge gas, and then improve the reaction monomers activation efficiency in the atomic layer deposition process, increase the reactive group concentration in the space; Improve depositing of thin film speed greatly, and can reduce depositing temperature.Measuring result shows that this array hollow discharge can increase plasma density to 10
11～10
13/ cm
3, reduce energy of plasma below 1eV, improve 5～10 times of depositing of thin film speed, depositing temperature is an envrionment temperature to 600 ℃.And this device can obtain in the 100mm diameter range, and homogeneity is less than 5%.
Array coreless armature 3 is the planar electrodes that have a lot of tiny through holes, and it forms the condenser coupling discharge electrode with plate electrode 4, and the spacing of two electrodes is adjustable, is the required electrical discharge zone of gas reaction between the two.Array coreless armature 3 connects the air-supply duct of gas distributing system 1, and the tiny through hole from the gas of gas distributing system is arranged through array earlier gets into Vakuumkammer again, can guarantee the air-flow distribution uniform of electrical discharge zone.Array coreless armature 3 is connected to high voltage terminal one end of power-supply system 6, and with vacuum chamber 2 are insulating.
Power-supply system 6; Can be the higher AC power of frequency (the high-frequency radio frequency power supply of 2-60MHz, or the VHF power supply of 60-100MHz, or the intermediate frequency power supply of 10-60KHz); Also can be unipolarity or the bipolar pulse direct supply of 10-60KHz, preferentially select the VHF power supply for use.The high-pressure side of power supply is connected on the terminal stud of array coreless armature 3, and keeps good insulation with miscellaneous part; The ground terminal of power supply is connected on vacuum chamber and the plate electrode 4.Through between 3 and 4, applying voltage, can ionization of gas be produced plasma body.Power-supply system adopts pulse control mode, can control and regulate the dutycycle in the discharge process.Power-supply system and gas distributing system can collaborative works through the unified control of ASIC micro computer.
Pumped vacuum systems 5 can make the base vacuum of vacuum chamber reach 1 * 10
-2Pa-1 * 10
-4Pa or better, according to the difference of processing condition, the air pressure during discharge can be controlled within the scope of 10-1000Pa.
Plate electrode 4, the mode that generally adopts downside to place can be used as the substrate mounting table.Plate electrode 4 has heating function, and TR is continuous adjustable from 40～600 ℃.
Prepare the little experimental installation of a cover according to content of the present invention; Top electrode is designed to the array hollow cathode structure (seeing accompanying drawing 2) of ladder hole; Porous uniform distribution, diameter range are 1-3mm, and the spacing in adjacent hole is 2-4mm; The planar electrode of the garden that the is shaped as shape in hole, hexagon, through hole such as square is selected stainless steel for use.Power-supply system is the radio-frequency power supply of frequency 27.12MHz, output rating 300W, has automatic adaptation.Vacuum pump system is selected rotary-vane vaccum pump and turbo-molecular pump system for use, and is furnished with the valve of regulating pumping speed.
Under the condition of base vacuum 0.1Pa, discharge air pressure 220Pa, argon flow amount 220sccm, lower discharge power 80W, interelectrode distance 18mm, only use argon gas discharging.Use langmuir probe, the electron density that records argon plasma can reach 115.2 * 10
10Cm
-3, be superior to the plasma electron density 28.4 * 10 of the plate electrode under the same terms
10Cm
-3The discharge photo is seen accompanying drawing 4.
To prepare silica-based can film be example very much, and the operating process and the result of use of this device is described.
With siliceous gas or liquid is silicon source presoma, is reducing gas with hydrogen; Under vacuum or rough vacuum condition, produce plasma body with radio frequency or the excitation of VHF power supply, realize that pulsed plasma strengthens the chemical vapour deposition microcrystalline silicon film.Technical process mainly was divided into for four steps: substrate pre-treatment, vacuum obtain and base station heating, thin film deposition, shutdown.
One. substrate pre-treatment: use organic film, monocrystalline silicon piece or sheet glass as substrate.To p type monocrystalline silicon piece with 20% HF acid ultrasonic cleaning 60 seconds, to remove the SiO on surface
2Layer, and then use absolute ethyl alcohol, deionized water to carry out ultrasonic cleaning successively, clean until silicon chip surface, dry up with clean nitrogen then; Substrates such as sheet glass directly carry out ultrasonic cleaning with absolute ethyl alcohol, deionized water, and are clean until glass sheet surface, dry up with nitrogen then.
Two. vacuum obtains and the base station heating: substrate is placed on the lower electrode, when vacuum tightness during less than 10Pa, opens molecular pump, simultaneously the power supply opening to the chip bench heating.Vakuumkammer is evacuated to 1 * 10
-3Pa, 100～600 ℃ of control base station TRs.
Three. thin film deposition: after vacuum tightness and base station temperature reach requirement, open gas distributing system.Import argon gas 5～100sccm earlier, 5～10 minutes, open plasma was carried out plasma surface to substrate and is cleaned scavenging period 5～10 minutes.Close the plasma discharge power supply; Continue to feed argon gas 5～10 minutes, close the argon gas input; Open silicon source gas, input 5～100sccm silicon source gas, 0.2～5 second time; Close silicon source gas; Input argon gas 5～100sccm, 1～5 second; Close argon gas; Open hydrogen gas, input 5～100sccm hydrogen gas, 0.2～5 second time, while open plasma power supply, plasma discharge power 30～400W; Close hydrogen gas, close plasma electrical source; Input argon gas 5～100sccm, 1～5 second; Close argon gas; This is an one-period.Then import silicon source gas, argon gas, hydrogen, argon gas etc. respectively and repeat, realize proportionally alternately feeding silicon source gas and hydrogen, carry out the deposition of plasma enhanced chemical vapor deposition microcrystalline silicon film.
Four. shutdown: thin film deposition finishes, and closes silicon source gas hydrogen then successively, and gas circuit and Vakuumkammer were washed 10～30 minutes with argon gas, closes argon gas at last, and molecular pump, mechanical pump and all power supplys.
Adopt the apparatus for atomic layer deposition of array hollow cathode structure of the present invention; In conjunction with hollow cathode plasma low temperature, efficient and accurate, the controlled advantage of ald; Have higher discharging efficiency and plasma density than classic flat-plate electrode structure, can improve the cleavage rate of reaction monomers greatly.This device has effectively solved the shortcoming that traditional ALD deposition needs heat, can deposit multiple function film at a lower temperature efficiently, helps reducing the production cost of film, promotes the development of film and related prods.
This device is specially adapted to accurately preparations such as the silica-base film, aluminum oxide film, titanium nitride membrane of nano thickness.
Has 520cm in the Raman spectrogram of the microcrystalline silicon film for preparing among this embodiment
-1The peak crystallization at wave number place, the percent crystallization in massecuite of this film sample are 51.8%, change the microcrystalline silicon film that film deposition conditions can make different percent crystallization in massecuites.
The cylindrical tip that has microcrystalline silicon film crystal grain among the AFM AFM three-dimensional appearance figure of the microcrystalline silicon film for preparing among this embodiment.
Adopt hollow cathode plasma to strengthen the method for chemical vapour deposition; Because the hollow cathode effect during discharge has higher discharging efficiency and plasma density than classic flat-plate electrode structure, can improve the cleavage rate of reaction monomers greatly; The operating air pressure of plasma body increases; Thereby improve depositing of thin film speed, help reducing the production cost of microcrystalline silicon film, promote the development of microcrystalline silicon film solar cell and related prods.
Claims (5)
1. the method for a plasma enhanced chemical vapor deposition microcrystalline silicon film; It is characterized in that: use with lower device; This device comprises gas distributing system (1), vacuum chamber (2), array hollow cathode top electrode (3), flat ground connection lower electrode (4), pumped vacuum systems (5), power-supply system (6); The through hole that it is 1-3mm that said array hollow cathode top electrode (3) has a plurality of equally distributed diameter ranges; The spacing in adjacent hole is 2-4mm, and the spacing between array hollow cathode top electrode (3) and the flat ground connection lower electrode (4) is 5-20mm, and array coreless armature (3) connects the air-supply duct of gas distributing system (1); The terminal stud of said formula hollow cathode array electrode (3) is connected to high voltage terminal one end of said power-supply system (6); And keeping insulation with the vacuum chamber of said device, flat ground connection lower electrode, the ground terminal of said power-supply system (6) is connected on said vacuum chamber (2) and the said plate electrode (4);
May further comprise the steps: gas distributing system (1) to said array coreless armature (3) air feed, earlier through the through hole on the said array coreless armature (3), gets into vacuum chamber (2) from the gas of said gas distributing system (1) with pulse alternative loop cycle mode again; Between said array hollow cathode electrode (3) and said plate electrode (4), apply voltage, ionization of gas is produced plasma body carry out thin film deposition, plasma discharge power 30～400W.
2. the apparatus for atomic layer deposition with array hollow cathode structure according to claim 1, said gas distributing system (1) comprises two-way gas piping at least, and each gas piping comprises vacuum breaker, operated pneumatic valve switch and mass flowmeter; Wherein operated pneumatic valve closes the period 0.01～10 second scope, and time precision was less than 0.01 second.
3. method according to claim 1 is characterized in that: said power-supply system (6) out-put supply dutycycle 5～90%.
4. method according to claim 1 is characterized in that: gas distributing system (1) with pulse alternative loop cycle mode to array coreless armature (3) supply response monomer gas and argon gas.
5. method according to claim 1 is characterized in that: said plate electrode (4) is heated to 40-600 ℃.
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| CN105483654A (en) * | 2016-01-22 | 2016-04-13 | 华北电力大学（保定） | Device for producing nano-crystalline silicon thin film |
| CN108048820A (en) * | 2017-12-22 | 2018-05-18 | 江苏鲁汶仪器有限公司 | Vapor deposition apparatus and vapor deposition method |
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| CN103938187A (en) * | 2014-04-29 | 2014-07-23 | 东莞职业技术学院 | Large-area thin-film deposition PECVD (Plasma Enhanced Chemical Vapor Deposition) electrode structure and equipment |
| CN103938187B (en) * | 2014-04-29 | 2016-07-06 | 东莞职业技术学院 | Large area film deposition PECVD electrode structure and equipment |
| CN105483654A (en) * | 2016-01-22 | 2016-04-13 | 华北电力大学（保定） | Device for producing nano-crystalline silicon thin film |
| CN110612363A (en) * | 2017-03-31 | 2019-12-24 | 迪罗拉科技有限公司 | System and method for coating a surface |
| CN110612363B (en) * | 2017-03-31 | 2021-12-21 | Agm集装箱控制公司 | System and method for coating a surface |
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| CN113163566A (en) * | 2021-04-27 | 2021-07-23 | 常州大学 | Device and method for modifying carbon material by plasma |
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