CN101413115B - Method for plasma assisted film deposition - Google Patents
Method for plasma assisted film deposition Download PDFInfo
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- CN101413115B CN101413115B CN200710181613XA CN200710181613A CN101413115B CN 101413115 B CN101413115 B CN 101413115B CN 200710181613X A CN200710181613X A CN 200710181613XA CN 200710181613 A CN200710181613 A CN 200710181613A CN 101413115 B CN101413115 B CN 101413115B
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Abstract
The invention relates to a film deposition system through the assistance of plasma and a method thereof. The system mainly consists of a plasma film deposition device and a plasma process monitoring device; the plasma film deposition device can be used for inputting pulse power and process reaction gas; the pulse power and process reaction gas act to produce an active species in reaction gas for a plasma discharge and dissociation process so as to carry out a film deposition process; the plasma process monitoring device comprises a plasma composition optical emission spectroscopy and a pulse plasma modulation program device; the value of spectral intensity of the active species in a plasma composition is measured through the plasma composition optical emission spectroscopy; and the spectral intensity ratio between the active species is calculated through pulse plasma modulation program device, so as to modulate the proper action time and power of the pulse power plasma, obtain high sedimentation rate within the sedimentation range of microcrystal silicon and master the optimal sedimentation quality of the film in real time.
Description
Technical field
The invention relates to a kind of plasma assisted film deposition System and method for, especially refer to a kind ofly use plasma composition optical emission spectroscopy instrument monitoring by the spectral intensity between the dissociated active specy of pulsed plasma, and via the spectral intensity ratio between plasma body modulation programunit calculating active specy, active modulation pulse power parameter, can in the scope of microcrystalline silicon deposition, obtain high deposition rate, and control the plasma assisted film deposition System and method for of best thin film deposition quality in real time.
Background technology
Press, microcrystal silicon (μ c-Si) film can be applicable to the repeatedly silicon film type solar battery structure of formula (tandem) of string, has the advantage of the photoelectric transformation efficiency that improves thin film solar cell; Generally be to obtain the micro-crystallization silicon film, yet be subject to low sedimentation rate, and be difficult to obtain high crystal structure, therefore cause the great bottleneck in the application, for example yield poorly, percent crystallization in massecuite is low etc. by auxiliary vapour deposition (PECVD) technology of plasma body; Especially, the required microcrystalline silicon film thickness of thin film solar cell reaches 1-2 μ m, and its depositing operation time is long, therefore needs badly and improves its sedimentation rate and crystalline quality effectively.
The auxiliary gas phase deposition technology of known plasma body often adopts high frequency pulse power supply (Highfrequency pulse power) can suppress a large amount of active species (radicals) that the continous way high frequency electric source produced and forms molecule powder (powder) because of polymerization, and causes the situation of amorphous silicon membrane in deposition surface.
The known day disclosure No. 20030421313, JP of application for a patent for invention " manufacture method of silicon-film solar-cell ", as shown in Figure 1, its by pulsed plasma action time of selecting the different depositional phases in advance than Pr (plasma body open (ON) time/(open (ON) time+plasma body of plasma body is closed (OFF) time)), in depositing operation initial time T1, adopt less action of plasma time ratio Pr1, treat that microcrystal silicon is after forming initial layers under the lower sedimentation rate, in technology later stage time T 2, adopt higher action of plasma time ratio Pr2 again, improve film deposition rate and finish whole layer, to obtain the microcrystalline silicon film of high deposition rate, can be applicable to make the high-level efficiency solar cell.
Only, in microcrystalline silicon deposition technology, for example silane gas (SiH4) and hydrogen (H
2) wait by the actual rate of plasma dissociation, dynamically can influence the sedimentation rate and the percent crystallization in massecuite of microcrystalline silicon film, aforementioned should Japan's publication by selecting segmentation pulsed plasma ratio action time, control above-mentioned two kinds of gases by stages by dissociated ratio, improve microcrystalline silicon film sedimentation rate and inhomogeneity purpose though can reach with waiting for quietly, monitored and quantitative analysis yet can't change to the gaseous constituent of dissociating in the thin film deposition processes; Fig. 1 only shows default two-part process time T and action of plasma time ratio Pr, during right practical application, as will obtaining optimal deposition speed, must precisely subdivided more multistage pulsed plasma ratio action time, and can only preset multistage processing condition, cause practical application and complicated operationization; In addition, this known patent belongs to out circuit system, process gas is dissociated ratio in long-time thin film deposition processes and mass production in the plasma body, easily because of airflow field disturbance, electrode surface deposition or the like making a difference property of factor, also can influence the accuracy of former default processing condition, cause the thin film deposition quality that can't obtain expecting.
Summary of the invention
The objective of the invention is to propose a kind of plasma assisted film deposition System and method for, can monitor the spectrum of detecting and analysis active specy in real time and calculate spectral intensity ratio, with the suitable pulse power parameter of modulation, under high deposition rate, the microcrystal silicon process stabilizing is controlled in the crystalline growth zone, can avoid the growth of silicon film non-crystalline silicon tissue, to obtain the fine microcrystalline silicon film.
For achieving the above object, plasma assisted film deposition provided by the invention system, it comprises:
One plasma body film deposition apparatus can supply input pulse power supply and process gas, produces plasma discharge by the pulse power and process gas effect, and the active specy of the plural number that can dissociate, to carry out thin film deposition processes; And
One plasma process monitoring device comprises:
One plasma body composition optical emission spectroscopy instrument is in order to the spectral intensity of this plural number active specy of detecting analysis;
One pulsed plasma modulation programunit is connected with this plasma body composition optical emission spectroscopy instrument and the pulse power, in order to calculate spectral intensity ratio and modulation pulse power parameter according to this.
Described plasma assisted film deposition system, wherein, this plasma body film deposition apparatus can be plasma auxiliary chemical vapor deposition apparatus.
Described plasma assisted film deposition system, wherein, this plural active specy is hydrogen (H
*) and silane gas (SiH
*).
Described plasma assisted film deposition system, wherein, the process gas of this input comprises hydrogen (H
2) and silane gas (SiH
4).
Described plasma assisted film deposition system, wherein, the pulsed plasma action time that this pulse power parameter is the pulse power.
Described plasma assisted film deposition system, wherein, this pulse power parameter comprises the power of the pulse power.
Plasma assisted film deposition method provided by the invention, it comprises:
One plasma body film deposition apparatus is provided, can supplies input pulse power supply and process gas, produce plasma discharge by the pulse power and process gas effect, and the active specy of the plural number that can dissociate, to carry out thin film deposition processes; And
One plasma process monitoring device is provided, analyzes the spectral intensity of this plural number active specy and give spectral intensity ratio r between the calculated complex active specy in order to detecting, and according to this ratio modulation pulse power parameter.
Described plasma assisted film deposition method, wherein, this plasma process monitoring device comprises:
One plasma body composition optical emission spectroscopy instrument is in order to the spectral intensity of this plural number active specy of detecting analysis; And
One pulsed plasma modulation programunit is connected with the plasma composition optical emission spectroscopy instrument and the pulse power, according to the spectral intensity ratio modulation pulse power parameter of calculating this plural number active specy.
Described plasma assisted film deposition system, wherein, this plural active specy is hydrogen (H
*) and silane gas (SiH
*).
Described plasma assisted film deposition system, wherein, the process gas of this input comprises hydrogen (H
2) and silane gas (SiH
4).
Described plasma assisted film deposition method, wherein, definition begins to take place non-crystalline silicon in the thin film deposition processes when organizing spectral intensity ratio (SiH between the active specy
*/ H
*)
TransitionBe crystallization conversion value R; This certain value will be monitored the spectral intensity ratio r=(SiH of gained with depositing operation ionic medium body technology monitoring device for judging whether deposition is the criterion of microcrystalline silicon film
*/ H
*)
ProcessCompare mutually.
Described plasma assisted film deposition method, wherein:
If the spectral intensity ratio r is greater than this crystallization conversion value R in the technology, then reduce pulsed plasma action time by this pulsed plasma modulation programunit modulation, can avoid the growth of silicon film non-crystalline silicon tissue;
If the spectral intensity ratio r is less than this crystallization conversion value R in the technology, then improve pulsed plasma action time by this pulsed plasma modulation programunit modulation, can in the scope of microcrystalline silicon deposition, obtain high deposition rate.
Described plasma assisted film deposition method, wherein, this pulsed plasma modulation program also can make up power or pulsed plasma action time of the modulation pulse power mutually.
Described plasma assisted film deposition method, wherein, the modulation program of this pulsed plasma action time calculates according to linear gauge formula shown below:
t
n+1＝t
n+k*t
n*(R-r)/R；
Wherein,
N is equal to or greater than 0 integer;
t
N+1It is next new pulsed plasma action time;
t
nIt is present pulsed plasma action time;
K is system characteristic correction weights;
R is the crystallization conversion value;
R is the spectral intensity ratio between active specy in the technology.
Description of drawings
Fig. 1 is that stage pulsed plasma action time of known day disclosure application for a patent for invention JP No. 20030421313 " manufacture method of silicon-film solar-cell " is than Pr and depositing operation time T graphic representation.
Fig. 2 is a system schematic of the present invention.
Fig. 3 is the spectrogram of the active specy detected of plasma process monitoring device of the present invention.
Fig. 4 is the linear modulation pulsed plasma of the present invention graphic representation of action time.
Fig. 5 is a method flow diagram of the present invention.
Main mark nomenclature in the accompanying drawing:
10-plasma assisted film deposition system
20-plasma foil deposition apparatus
The 21-cavity
211-technological reaction gas inlet
The 212-pneumatic outlet
213-has an X-rayed window
The 22-top electrode
The 23-lower electrode
The 24-pulse power
The 25-substrate
The 26-well heater
The 27-plasma discharge
30-plasma process monitoring device
31-plasma composition optical emission spectroscopy instrument
32-pulsed plasma modulation programunit
N-is equal to or greater than 0 integer
t
N+1-next new pulsed plasma action time
t
n-present pulsed plasma action time
K-system characteristic correction weights
R-crystallization inversion spectrum intensity rate
The spectral intensity ratio that records at present of r-active specy
T0-pulsed plasma initial value action time
Embodiment
Further understand and approval for having structure purpose of the present invention and effect, conjunction with figs. describe in detail as after.
Describe the present invention for reaching employed technique means of purpose and effect hereinafter with reference to accompanying drawing, and the cited embodiment of the following drawings only is an aid illustration, technique means of the present invention is not limited to cited accompanying drawing.
See also shown in Figure 2, plasma assisted film deposition provided by the invention system 10, it mainly is to be made of a plasma body film deposition apparatus 20 and a plasma process monitoring device 30.
This plasma body film deposition apparatus 20 can be plasma auxiliary chemical vapor deposition apparatus, as shown in Figure 2, it comprises a cavity 21, this cavity 21 has a technological reaction gas inlet 211 and a pneumatic outlet 212, in this cavity 21, be provided with a top electrode 22 and a lower electrode 23, this top electrode 22 reaches and is connected with the pulse power 24 1 ends, can carry the substrate 25 of deposit film on this lower electrode 23, make this substrate 25 be positioned at 23 of this top electrode 22 and lower electrodes, be provided with a well heater 26 in these lower electrode 23 belows again, simultaneously, this cavity 21, lower electrode 23 is connected with the pulse power 24 the other ends; By the gas supply device (not shown) gas that thin film deposition processes is required, be generally hydrogen (H
2) and silane gas (SiH
4) via in these technological reaction gas inlet 211 these cavitys 21 of input, by the pulse power 24 pulse power is sent in the cavity 21 simultaneously, in this top electrode 22 and 23 of lower electrodes and reactant gases generation plasma discharge 26, and can dissociate hydrogen (H
*) and silane gas (SiH
*) active specy that waits, simultaneously by 25 heating of 26 pairs of substrates of this well heater, make that to reach technology temperature required, and carry out thin film deposition in these substrate 25 surfaces; After thin film deposition, in this cavity 21 remaining gas and the gas that deposition reaction generated, then discharge by the pneumatic outlet 212 of this cavity 21, this pneumatic outlet 212 is communicated with the vacuum suction device (not shown), for example device such as vacuum pump detaches this cavity 21 with auxiliary fast with residual gas.
Characteristics of the present invention are this plasma process monitoring device 30, it is made of a plasma body composition optical emission spectroscopy instrument 31 and a pulsed plasma modulation programunit 32, this plasma body composition optical emission spectroscopy instrument 31 is analyzed the spectral intensity of active specy in order to detecting, 32 of this pulsed plasma modulation programunits are connected with this plasma body composition optical emission spectroscopy instrument 31 and the pulse power 24, in order to calculate the spectral intensity of the different activities species that this plasma body composition optical emission spectroscopy instrument 31 resolved, and calculate spectral intensity ratio r to each other according to this, carry out modulation pulse power parameter, for example power of the pulsed plasma action time and the pulse power or the like; The spectrum that is parsed is two main spectral values that influence microcrystalline silicon film sedimentation rate and film quality as shown in Figure 3, and one belongs to silane gas active specy (SiH for wavelength 414nm
*) spectral intensity, another then is that wavelength 656nm belongs to hydrogen active specy (H
*) spectral intensity.
Known to thin film deposition processes correlative technology field personage, as silane gas (SiH
*) spectral intensity is higher, the microcrystalline silicon film sedimentation rate is higher, however film is organized and easily is converted to the non-crystalline silicon tissue; Otherwise, as hydrogen active specy (H
*) spectral intensity is higher, then obtain good micro-crystallization tissue more easily, but sedimentation rate will reduce gradually.
Spectral intensity ratio (SiH between active specy when wherein, definition begins to take place non-crystalline silicon in the thin film deposition processes and organizes
*/ H
*)
TransitionBe crystallization conversion value R; This certain value will be monitored the spectral intensity ratio r=(SiH of gained with depositing operation ionic medium body technology monitoring device for judging whether deposition is the criterion of microcrystalline silicon film
*/ H
*)
ProcessCompare mutually.
Spectral intensity ratio r measured in technology is greater than crystallization conversion value R, though high sedimentation rate is arranged, yet because of the silane gas active specy (SiH in the plasma body
*) ionic weight increases easy polymerization, and then the formation powder is in deposition surface, so that generate the amorphous silicon membrane tissue.
Based on the above factor as can be known, by the spectral intensity ratio r between active specy in the control thin film deposition processes, make it as far as possible near and be not more than crystallization conversion value R, can take into account the highest microcrystalline silicon film sedimentation rate of acquisition under the thin film crystallization quality.
Plasma process monitoring device 30 provided by the present invention is the silane gas active specy (SiH by these plasma body composition optical emission spectroscopy instrument 31 real-time monitoring film depositing operations
*) and hydrogen active specy (H
*) spectral intensity of isoreactivity species, via the spectral intensity ratio r between these pulsed plasma modulation programunit 32 calculated activity species, carry out modulation pulse power parameter, with control film deposition rate and deposition quality according to the modulation process; As previously mentioned, this pulse power parameter comprises power of pulsed plasma action time, the pulse power or the like, at the action of plasma time (t) of the modulation pulse power, its modulation program is to calculate according to linear gauge formula shown below as shown in Figure 4:
t
n+1＝t
n+k*t
n*(R-r)/R；
Wherein,
N is equal to or greater than 0 integer;
t
N+1It is next new pulsed plasma action time;
t
nIt is present pulsed plasma action time;
K is system characteristic correction weights;
R is the crystallization conversion value;
R is the spectral intensity ratio between active specy in the technology.
Wherein these system characteristic correction weights k is greater than 0, according to the correction of different plasma system.
Wherein this n equals at 0 o'clock, and t0 is set at pulsed plasma initial value action time that thin film deposition processes begins.
See also the flow process 50 of plasma assisted film deposition method provided by the invention shown in Figure 5, it comprises the following steps:
51: thin film deposition processes begins;
52: set the action of plasma time initial value t0 of a lower pulse power, this plasma body initial value action time t0 makes according to the working experience value, though sedimentation rate is lower, can guarantee to obtain the microcrystalline silicon film tissue;
53: with the pulse power action of plasma time t behind initial or the modulation
nCarry out depositing operation (step 53), and judge whether to finish thin film deposition (step 54);
If finish thin film deposition processes then to finishing thin film deposition (step 56), right if also not finishing thin film deposition processes then enters this plasma process monitoring flow journey shown in the step 55 and carry out the pulsed plasma modulation of action time, this plasma process monitoring flow journey 55 comprises:
551: the spectral intensity ratio r of active specy in the technology is analyzed and is calculated in detecting;
552: spectral intensity ratio r and crystallization conversion value R in the more present technology;
553: judge that whether present spectral intensity ratio r is greater than crystallization conversion value R;
During depositing operation carries out, when present spectral intensity ratio r greater than crystallization conversion value R, expression is in non-crystalline silicon organizational growth zone, therefore this moment, the action of plasma time was too high, must be reset to initial action of plasma time t
0(step 554, to guarantee to be back to into microcrystal silicon organizational growth the zone, this step is to be carried out by this pulsed plasma modulation programunit 32 shown in Figure 2);
Otherwise,, then enter subordinate phase and judge (step 555) if the spectral intensity ratio r is not more than crystallization conversion value R at present;
555: judge whether present spectral intensity ratio r equals crystallization conversion value R;
When present spectral intensity ratio r equals crystallization conversion value R, expression is grown up regional at present at microcrystalline silicon film, and has high sedimentation rate, therefore keeps present pulsed plasma value action time, do not carry out modulation, and get back to the thin film deposition processes of step 53;
556: enter this step and be the spectral intensity ratio r less than crystallization conversion value R, though representative at present in the microcrystalline silicon film zone of growing up, sedimentation rate is slow, therefore can modulation increases the time (step 556) of pulsed plasma effect, to improve sedimentation rate;
According to linear gauge formula t
N+1=t
n+ k*t
n* (R-r)/R calculates the new action of plasma time of necessary modulation, replaces the present action of plasma time (step 557), returns the thin film deposition processes of step 53;
So continue to monitor the spectral intensity ratio modulation pulsed plasma action time between active specy in the plasma body, r=R is grown up with the microcrystalline silicon film that remains under the high deposition rate, finish (step 56) until finishing whole thin film deposition processes.
In sum, plasma assisted film deposition System and method for provided by the invention, its characteristics are to have a plasma process monitoring device, can monitor by the spectral intensity ratio between the spectral intensity of the dissociated active specy of pulsed plasma and calculated activity species, the action of plasma time of the active modulation pulse power, make and in the scope of microcrystalline silicon deposition, obtain high deposition rate, to promote the thin film deposition production capacity, what must emphasize is, except that preceding modulation action of plasma time method, can also make up the power in the modulation pulse power mutually, carry out according to aforesaid pulsed plasma modulation program; Moreover, the invention belongs to closed loop system, use the detecting of plasma composition optical emission spectroscopy instrument because of the airflow field disturbance, the variation of electrode surface deposition or the like dissociation effect that factor causes is also quantized to calculate spectral intensity ratio variation r, the processing parameter of the modulation pulse power in real time, as action of plasma time (Plasma duty time) and output rating (Power) or the like, has stable long microcrystalline silicon film depositing operation advantage, must be compared to known technology to preestablish the setting means of multistage processing condition, the present invention really can be more accurately according to the gaseous constituent ratio that dissociates in the plasma body, modulation microcrystalline silicon deposition thin-film technique parameter is to obtain high deposition rate, and avoid known technology to cause problem complicated on the technique initialization, have the enhancement on the effect.
Only the above only is embodiments of the invention, when not limiting the scope that the present invention is implemented with this.Promptly the equalization of doing according to claim of the present invention generally changes and modifies, and all should still belong in the scope that claim of the present invention contains.
Claims (7)
1. plasma assisted film deposition method, it comprises:
One plasma body film deposition apparatus is provided,, produces plasma discharge by the pulse power and process gas effect for input pulse power supply and process gas, and the active specy of the plural number that can dissociate, to carry out thin film deposition processes; And
One plasma process monitoring device is provided, analyzes the spectral intensity of this plural number active specy and give spectral intensity ratio r between the calculated complex active specy in order to detecting, and according to the action of plasma time and the power parameter of this ratio modulation pulse power.
2. plasma assisted film deposition method as claimed in claim 1, wherein, this plasma process monitoring device comprises:
One plasma body composition optical emission spectroscopy instrument is in order to the spectral intensity of this plural number active specy of detecting analysis; And
One pulsed plasma modulation programunit is connected with the plasma composition optical emission spectroscopy instrument and the pulse power, according to the action of plasma time and the power parameter of the spectral intensity ratio modulation pulse power that calculates this plural number active specy.
3. plasma assisted film deposition method as claimed in claim 1, wherein, this plural active specy is the active specy of hydrogen and silane gas.
4. plasma assisted film deposition method as claimed in claim 3, wherein, the process gas of this input comprises hydrogen and silane gas.
5. plasma assisted film deposition method as claimed in claim 3, wherein, definition begins to take place non-crystalline silicon in the thin film deposition processes when organizing spectral intensity ratio between the active specy
(SiH * / H * ) TransitionBe crystallization conversion value R; This certain value will be monitored the spectral intensity ratio r=(SiH of gained with depositing operation ionic medium body technology monitoring device for judging whether deposition is the criterion of microcrystalline silicon film
*/ H
*)
ProcessCompare mutually; SiH wherein
*Be the active specy of silane gas, H
*Active specy for hydrogen.
6. plasma assisted film deposition method as claimed in claim 5, wherein:
If the spectral intensity ratio r is greater than this crystallization conversion value R in the technology, then reduce pulsed plasma action time by this pulsed plasma modulation programunit modulation, avoid the growth of silicon film non-crystalline silicon tissue;
If the spectral intensity ratio r is less than this crystallization conversion value R in the technology, then improve pulsed plasma action time by this pulsed plasma modulation programunit modulation, in the scope of microcrystalline silicon deposition, obtain high deposition rate.
7. plasma assisted film deposition method as claimed in claim 6, wherein, the modulation program of this pulsed plasma action time calculates according to linear gauge formula shown below:
t
n+1＝t
n+k*t
n*(R-r)/R；
Wherein,
N is equal to or greater than 0 integer;
t
N+1It is next new pulsed plasma action time;
t
nIt is present pulsed plasma action time;
K is system characteristic correction weights;
R is the crystallization conversion value;
R is the spectral intensity ratio between active specy in the technology.
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|---|---|---|---|
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| CN101413115B true CN101413115B (en) | 2010-08-25 |
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| TWI465158B (en) * | 2011-01-12 | 2014-12-11 | Ind Tech Res Inst | A microwave-excited plasma device |
| CN108385073B (en) * | 2018-04-24 | 2020-12-22 | 信利（惠州）智能显示有限公司 | Method for manufacturing ITO film |
| KR102054372B1 (en) * | 2018-07-17 | 2019-12-10 | 차동호 | Gas Ingredient Monitoring Equipment for Gas Laser |
| CN114807893A (en) * | 2021-01-19 | 2022-07-29 | 圆益Ips股份有限公司 | Thin film forming method |
| CN113913778B (en) * | 2021-09-08 | 2023-09-08 | 核工业西南物理研究院 | Online surface coating siliconized wall treatment method for fusion device |
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| US6627463B1 (en) * | 2000-10-19 | 2003-09-30 | Applied Materials, Inc. | Situ measurement of film nitridation using optical emission spectroscopy |
| JP2005183620A (en) * | 2003-12-18 | 2005-07-07 | Sharp Corp | Method for manufacturing silicon thin film solar battery |
| US20060065654A1 (en) * | 2004-09-30 | 2006-03-30 | Watlow Electric Manufacturing Compamy | Modular layered heater system |
| CN1800830A (en) * | 2005-01-05 | 2006-07-12 | 中国科学院长春光学精密机械与物理研究所 | Spectrum detection method for instructing plasma assisted semiconductor material preparation |
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|---|---|---|---|---|
| US5347460A (en) * | 1992-08-25 | 1994-09-13 | International Business Machines Corporation | Method and system employing optical emission spectroscopy for monitoring and controlling semiconductor fabrication |
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