Embodiment
Please refer to Fig. 1, Fig. 1 is the plasma CVD device synoptic diagram, comprising: reaction chamber 101, be positioned at the pedestal 102 of cavity bottom, temperature regulating device 104, the gas spray equipment 107 that is used for distributing gas that base-plate temp is controlled and the plasma producing apparatus 106 that is used to produce plasma body.Wherein said pedestal 102 is used to place the substrate (not shown) for the treatment of deposit film, has the resistance wire (not shown) that is used to heat in the described pedestal.Described temperature regulating device 104 is electrically connected the control processing that is used for pedestal is carried out gradient of temperature with described pedestal 102.Described gas spray equipment 107 is positioned at chamber roof, is oppositely arranged with described pedestal 102.
Adopt the temperature regulating device 104 of above-mentioned plasma CVD device directly resistance wire to be applied power with pedestal 102 heating, the base-plate temp fluctuating range surpasses more than 10 degree, the base-plate temp fluctuating range is big especially to solar cell amorphous silicon membrane or microcrystalline silicon film influence greatly, the contriver is through discovering, reason is that the film grain size that the base-plate temp fluctuating range causes greatly forming amorphous silicon membrane or microcrystalline silicon film differs, homogeneity is poor, thereby the quality of the feasible film that forms is low, unstable properties.And the film of other types is not responsive especially to the base-plate temp fluctuating range, therefore can not produce above-mentioned problem.
For this reason, the present inventor provides a kind of plasma activated chemical vapour deposition base-plate temp control method, and the target temperature of plasma activated chemical vapour deposition pedestal with resistance wire and pedestal heating is provided; According to the original temperature of pedestal and the target temperature of pedestal heating, the total temperature that obtains target temperature and original temperature is poor; Numerical range according to temperature in the number of total temperature difference decision design temperature gradient and each thermograde; According to the thermograde of setting, heating heats up pedestal successively according to the numerical range of temperature in each thermograde to resistance wire, wherein, intensification parameter to last thermograde is controlled, make base-plate temp fluctuating range of base-plate temp after reaching target temperature satisfy process requirements, described process requirements is the fluctuating range of the requirement of deposition of amorphous silicon films or microcrystalline silicon film, with the deposition of amorphous silicon films is example, satisfying the process requirements temperature fluctuation is that amplitude is less than 5 ℃, adopt above-mentioned base-plate temp control method in being warming up to the process of target temperature, accurate control is accomplished in intensification.
Wherein, base-plate temp when described target temperature is deposition of amorphous silicon or microcrystalline silicon film, the original temperature of pedestal is the starting temperature of pedestal, it needs to be noted, described according to total temperature difference decision design temperature gradient number and each thermograde in the numerical range of temperature act as and avoid in the temperature-rise period temperature fluctuation amplitude excessive, concrete, decide the numerical range of temperature in the number of thermograde and each thermograde according to the processing requirement of deposition concrete non-crystalline silicon or microcrystalline silicon film, in other words, with the deposition of amorphous silicon films is example, preferred temperature gradient is 3, the numerical range of the temperature of each thermograde is followed successively by 15%~25% of total temperature difference, 75%~85% of total temperature difference, 3%~5% of total temperature difference, the numerical range of the thermograde of above-mentioned setting and the temperature of thermograde can obtain higher amorphous silicon membrane, avoids the grain size of amorphous silicon membrane to differ; With the deposition micro crystal silicon film is example, preferred temperature gradient is 4, the numerical range of the temperature of each thermograde is followed successively by 15%~25% of total temperature difference, 50%~60% of total temperature difference, 20%~30% of total temperature difference, 3%~5% of total temperature difference, the numerical range of the above-mentioned thermograde and the temperature of thermograde can obtain higher microcrystalline silicon film, avoid the grain size of microcrystalline silicon film to differ, in other embodiments, can also be according to concrete thin-film technique requirement, set the numerical range of the temperature of the thermograde for the treatment of deposit film and thermograde, thereby obtain to treat preferably deposition film quality.
Further, the present inventor is through discovering the temperature rise rate by the resistance wire of controlling last thermograde, the heating-up time of last thermograde, the numerical range of last thermograde can realize that the fluctuating range of base-plate temp is little.
Particularly, the resistance wire temperature rise rate that the contriver finds to control last thermograde is lower than the resistance wire temperature rise rate of its last thermograde, can reduce of the heating mode interference of last thermograde heating mode to last thermograde, make under the temperature control method of minute thermograde, the temperature rise rate of last thermograde is stable, thereby reduces the fluctuating range of base-plate temp.
The present inventor after further research, discovery is according to the thermograde of setting, the heating mode of selecting temperature rise rate to successively decrease successively, to resistance wire heating until pedestal successively according to each thermograde in the numerical range of temperature heat up, adopt above-mentioned mode, carry out the transition to the gradient of back one temperature reposefully from last thermograde, thereby make that the base-plate temp fluctuating range is little, the intensification meeting of pedestal is more accurate.
The present inventor also finds, if the heating-up time sufficiently long of last thermograde, thus interior intensification enough steadily of thermograde in the end made, and then make the temperature of pedestal heat up steadily, reach the little purpose of fluctuating range.
And if the numerical range of last thermograde is enough little, the fluctuating range of base-plate temp is played certain restriction, and then make the temperature of pedestal heat up steadily, reach the little purpose of fluctuating range.
As shown in Figure 2, plasma activated chemical vapour deposition base-plate temp control method of the present invention comprises the steps:
Step S101 provides the target temperature of plasma activated chemical vapour deposition pedestal with resistance wire and pedestal heating;
Step S102, according to the original temperature of pedestal and the target temperature of pedestal heating, the total temperature that obtains target temperature and original temperature is poor;
Step S103 is according to the numerical range of temperature in the number of total temperature difference decision design temperature gradient and each thermograde;
Step S104, according to the thermograde of setting, heating heats up pedestal successively according to the numerical range of temperature in each thermograde to resistance wire, wherein, intensification parameter to last thermograde is controlled, and makes base-plate temp fluctuating range of base-plate temp after reaching target temperature satisfy process requirements.
Particularly, the plasma activated chemical vapour deposition pedestal is used to place the substrate for the treatment of deposit film, base-plate temp when described target temperature can be for deposition of amorphous silicon or microcrystalline silicon film, theoretical can be any temperature of suitable deposition of amorphous silicon or microcrystalline silicon film, and common target temperature can be 100 ℃, 200 ℃, 140 ℃, 90 ℃, 210 ℃ or 150 ℃.
The original temperature of described pedestal is the starting temperature of pedestal, can be any temperature in theory, and for example 20 ℃, 100 ℃, 16 ℃, 200 ℃, 350 ℃ or 76 ℃, the original temperature of pedestal is the room temperature of cleaning chamber usually, is generally 25 ℃.
Thermograde is the temperature rise period that the resistance wire of article on plasma body chemical vapor phase growing pedestal adopts identical temperature rise rate.When using plasma chemical vapour deposition deposition of amorphous silicon or microcrystalline silicon film, be generally staged and increase progressively intensification, select the heat up numerical range of temperature of this thermograde of different resistance wire temperature rise rates in each thermograde, and base material is generally the metallic substance of good heat conductivity, aluminium for example, make the pedestal of heat conduction heat up to the resistance wire heating, reach target temperature until pedestal.
In the present invention, determine at least 2 thermogrades, and come the heating mode of preferred each thermograde, thereby optimize the pedestal temperature-rise period, reduce the fluctuating range that base-plate temp reaches target temperature according to the numerical range of the temperature of thermograde according to the total temperature difference.
Preferred temperature gradient is 3 or 4, in other embodiments, thermograde can be 7,9,11,20 ..., wherein, the thermograde number is many more, it is accurate more to heat up, the fluctuating range that reaches target temperature is more little, but, the thermograde number too much can influence the intensification efficient of pedestal, takes all factors into consideration pedestal intensification efficient and base-plate temp fluctuating range, and preferred temperature gradient is 3 or 4, if thermograde is 3, the numerical range of the temperature of each thermograde is followed successively by 15%~25% of total temperature difference, 75%~85% of total temperature difference, 3%~5% of total temperature difference.If thermograde is 4, the numerical range of the temperature of each thermograde be followed successively by the total temperature difference 15%~25%, the total temperature difference 50%~60%, the total temperature difference 20%~30%, the total temperature difference 3%~5%.
Also need to prove, the present invention also comprises: the numerical range of last thermograde that heats up the time, light the step of the plasma body of plasma CVD device, bring extra energy to cause the temperature of pedestal that the phenomenon of fluctuation is arranged to avoid lighting plasma body, improve the stability of base-plate temp.
Below being warming up to 150 ℃ from 25 ℃, thermograde is 3 and is example, and first embodiment of plasma activated chemical vapour deposition temperature control method of the present invention is done exemplary illustrated.
In the present embodiment, the original temperature of pedestal is the room temperature of cleaning chamber, is generally 25 ℃.
Target temperature is 150 ℃, described 150 ℃ is the depositing temperature of solar cell amorphous silicon membrane or microcrystalline silicon film, need to prove that in other embodiments, target temperature also can be set at the depositing temperature of other solar cell amorphous silicon membranes or microcrystalline silicon film.
It is poor that wherein target temperature and original temperature have total temperature, and described total temperature difference is 125 ℃.
Differing from 125 ℃ of definite thermograde numbers according to total temperature is 3, and the numerical range of the temperature of each thermograde is followed successively by 25 ℃, 95 ℃ and 5 ℃.
When heating up first thermograde, temperature rise rate can be 5 ℃/minute, is warming up to 50 ℃ in 5 minutes; When heating up second thermograde, temperature rise rate can be 10 ℃/minute, is warming up to 145 ℃ in 9.5 minutes; When heating up the 3rd thermograde, temperature rise rate can be 0.5 ℃/minute, is warming up to 150 ℃ in 10 minutes.
Wherein, the change of temperature rise rate can obtain by existing resistance wire heat regulation method, for example: the parameters such as heat-up time of change the resistance wire heating power, regulating resistance wire, here do not give unnecessary details one by one.
Need to prove, in the present embodiment, the temperature rise rate of last thermograde (i.e. the 3rd thermograde) is 0.5 ℃/minute, be lower than 10 ℃/minute of its last thermogrades (i.e. second thermograde), last thermograde has the temperature rise rate lower than last thermograde and has the advantage of optimizing the pedestal temperature-rise period, thereby reduces the fluctuating range that base-plate temp reaches target temperature.
Please refer to Fig. 3, Fig. 3 is the base-plate temp heating curve figure of first embodiment of employing plasma activated chemical vapour deposition temperature control method of the present invention, from the temperature heating curve figure of pedestal as can be seen, the first thermograde T1 is that 25 ℃, the second thermograde T2 are that 95 ℃, the 3rd thermograde T3 are 5 ℃, after pedestal reaches target temperature, basicly stable at 150 ℃, temperature fluctuation range is lower than 5 ℃.
Below being warming up to 150 ℃ from room temperature, thermograde is 4 and is example, and second embodiment of plasma activated chemical vapour deposition temperature control method of the present invention is done exemplary illustrated.
In the present embodiment, it is poor that target temperature and original temperature have total temperature, and described total temperature difference is 125 ℃.Determine that according to the total temperature difference thermograde number is 4, the numerical range of the temperature of each gradient is followed successively by 25 ℃, 70 ℃, 25 ℃ and 5 ℃.
In the present embodiment, the numerical range of the temperature of first gradient is 25 ℃, and when resistance wire was heated up the numerical range of temperature of first gradient, temperature rise rate was 5 ℃/minute, is warming up to 50 ℃ in 5 minutes.
The numerical range of the temperature of second gradient is 70 ℃, and when resistance wire was heated up the numerical range of temperature of second gradient, temperature rise rate was 4 ℃/minute, is warming up to 120 ℃ in 17.5 minutes.
The numerical range of the temperature of the 3rd gradient is 25 ℃, and when resistance wire was heated up the numerical range of temperature of the 3rd gradient, temperature rise rate was 3 ℃/minute, is warming up to 145 ℃ in 8.33 minutes.
The numerical range of the temperature of the 4th gradient is 5 ℃, and when resistance wire was heated up the numerical range of temperature of the 4th gradient, temperature rise rate was 0.5 ℃/minute, is warming up to 150 ℃ in 10 minutes.
In the present embodiment, the contriver takes all factors into consideration practicality and efficient, the temperature head of original temperature and target temperature is divided into 4 thermogrades, and in the numerical range of the temperature of each gradient that heats up, the heating mode of selecting temperature rise rate to reduce successively, make that temperature fluctuation range is little when reaching target temperature.
Please refer to Fig. 4, Fig. 4 is the base-plate temp heating curve figure of second embodiment of employing plasma activated chemical vapour deposition temperature control method of the present invention, from the temperature heating curve figure of pedestal as can be seen, the first thermograde t1 is that 25 ℃, the second thermograde t2 are that 70 ℃, the 3rd thermograde t3 are that 25 ℃, the 4th thermograde t4 are 5 ℃.After pedestal reached target temperature, basicly stable at 150 ℃, temperature fluctuation range was lower than 3 ℃.
Below to be warming up to 150 ℃ from room temperature, thermograde is 4 and is example, and in temperature-rise period, light the plasma body of plasma CVD device, the 3rd embodiment of plasma activated chemical vapour deposition temperature control method of the present invention is done exemplary illustrated.
In the present embodiment, it is poor that target temperature and original temperature have total temperature, and described total temperature difference is 125 ℃.Determine that according to the total temperature difference thermograde number is 4, the numerical range of the temperature of each gradient is followed successively by 25 ℃, 70 ℃, 25 ℃ and 5 ℃.
First of intensification present embodiment, second, the numerical range of the temperature of the 3rd gradient can be with reference to second embodiment, adopt 5 ℃/minute temperature rise rate that resistance wire was heated up 5 minutes successively, 4 ℃/minute temperature rise rate heated up 17.5 minutes to resistance wire, 3 ℃/minute temperature rise rate heated up 8.33 minutes to resistance wire, adopt above-mentioned heating mode, heat up after 30.83 minutes, light the plasma body of plasma CVD device, light the moment of the plasma body of plasma CVD device, plasma cognition is brought extra energy, cause the temperature of pedestal that fluctuation is arranged, simultaneously, adopting temperature rise rate is the numerical range (5 ℃) of temperature of 0.5 ℃/minute intensification the 4th gradient, heating-up time is 10 minutes, reaches target temperature until the plasma activated chemical vapour deposition pedestal.When the numerical range of the temperature of the 4th gradient that heats up, the temperature fluctuation meeting of plasma activated chemical vapour deposition pedestal settles out gradually, thereby makes that temperature fluctuation range was little when the plasma activated chemical vapour deposition base-plate temp reached target temperature.
Below to be warming up to 150 ℃ from room temperature, thermograde is 4 and is example, and when the numerical range of the temperature of the 4th gradient that heats up, light the plasma body of plasma CVD device, the 4th embodiment of plasma activated chemical vapour deposition temperature control method of the present invention is done exemplary illustrated.
In the present embodiment, it is poor that target temperature and original temperature have total temperature, and described total temperature difference is 125 ℃.Determine that according to the total temperature difference thermograde number is 4, the numerical range of the temperature of each gradient is followed successively by 25 ℃, 70 ℃, 25 ℃ and 5 ℃.
First of intensification present embodiment, second gradient, the numerical range of the 3rd temperature can be with reference to second embodiment, adopt 5 ℃/minute temperature rise rate that resistance wire was heated up 5 minutes successively, 4 ℃/minute temperature rise rate heated up 17.5 minutes to resistance wire, 3 ℃/minute temperature rise rate heated up 8.33 minutes to resistance wire, adopt above-mentioned heating mode, heat up after 30.83 minutes, then, when resistance wire is heated up the numerical range of temperature of the 4th gradient, adopt 0.5 ℃/minute temperature rise rate that resistance wire was heated up 10 minutes, after resistance wire heated up 1 minute, light the plasma body of plasma CVD device, light the moment of the plasma body of plasma CVD device, plasma cognition is brought extra energy, cause the temperature of pedestal that fluctuation is arranged, in this process, keep 0.5 ℃/minute temperature rise rate that resistance wire is heated up, reach target temperature until the plasma activated chemical vapour deposition pedestal.When the numerical range of the temperature of the 4th gradient that heats up, because the resistance wire temperature rise rate of the 4th thermograde is lower, plasma body brings extra energy to be digested in this temperature-rise period, almost not influence when base-plate temp is reached target temperature, when the numerical range of the temperature of the 4th gradient that heats up, the temperature fluctuation meeting of plasma activated chemical vapour deposition pedestal settles out gradually, thereby makes that temperature fluctuation range was little when the plasma activated chemical vapour deposition base-plate temp reached target temperature.
In sum, the present invention is by becoming at least two thermogrades according to target temperature with the total temperature difference of original temperature, consider efficient and practicality, preferred 3 thermogrades or 4 thermogrades, wherein, when being divided into 3 thermogrades, the numerical range of the temperature of each gradient be followed successively by the total temperature difference 15%~25%, the total temperature difference 75%~85%, the total temperature difference 3%~5%; Adopt the resistance wire temperature rise rate of last thermograde to be lower than the resistance wire temperature rise rate of its last thermograde, thereby make that when base-plate temp reached target temperature, temperature fluctuation range was little.
Further, when the numerical range of intensification thermograde, the heating mode that adopts temperature rise rate to reduce successively successively makes that temperature fluctuation further reduces when reaching target temperature.
Especially, the present invention is when heating up the numerical range of last thermograde, light the plasma body of plasma CVD device, can avoid lighting plasma body brings extra energy to cause the temperature of pedestal that the phenomenon of fluctuation is arranged, improve the stability of base-plate temp, thereby avoid the amorphous silicon membrane of the formation that temperature fluctuation brings or the film grain size of microcrystalline silicon film to differ, homogeneity difference problem improves film forming quality.
Below being warming up to 150 ℃ from 25 ℃, thermograde is 3 and is example, and the 5th embodiment of plasma activated chemical vapour deposition temperature control method of the present invention is done exemplary illustrated.
Differing from 125 ℃ of definite thermograde numbers according to total temperature is 3, and the numerical range of the temperature of each thermograde is followed successively by 25 ℃, 95 ℃ and 5 ℃.
When heating up first thermograde, temperature rise rate can be 5 ℃/minute, is warming up to 50 ℃ in 5 minutes; When heating up second thermograde, temperature rise rate can be 10 ℃/minute, is warming up to 145 ℃ in 9.5 minutes; When heating up the 3rd thermograde, selecting the heating-up time is 40 minutes, and this moment, temperature rise rate was 0.125 ℃/minute.In other embodiments, the heating-up time can also be 1 hour, 2 hours, and 2 hours 30 minutes ...; Need to prove that the contriver finds that the heating-up time is selected long more, when base-plate temp reached target temperature, temperature fluctuation range was little, and still, the heating-up time is long more, and intensification efficient can be low more, takes all factors into consideration production efficiency, and the preferred heating-up time is 40 minutes.
In the present embodiment, determine 3 thermogrades according to the total temperature difference, and the numerical range of the temperature of each thermograde that heats up successively, and the heating-up time of controlling last thermograde is when base-plate temp reaches target temperature, temperature fluctuation range is little, and avoids the big defective of single heating mode base-plate temp fluctuation.
Below being warming up to 150 ℃ from 25 ℃, thermograde is 3 and is example, and the 6th embodiment of plasma activated chemical vapour deposition temperature control method of the present invention is done exemplary illustrated.
Differing from 125 ℃ of definite thermograde numbers according to total temperature is 3, and the numerical range of the temperature of each thermograde is followed successively by 25 ℃, 99 ℃ and 1 ℃.
When heating up first thermograde, temperature rise rate can be 5 ℃/minute, is warming up to 50 ℃ in 5 minutes; When heating up second thermograde, temperature rise rate can be 10 ℃/minute, is warming up to 149 ℃ in 9.9 minutes; When heating up the 3rd thermograde, because the numerical range of the 3rd thermograde is 1 ℃, follow-up intensification can be adopted lower temperature rise rate, for example 0.125 ℃/minute, 1 ℃/minute etc., the numerical range of 1 ℃ the 3rd thermograde plays certain restriction to the fluctuating range of base-plate temp, and then make the temperature of pedestal heat up steadily, reach the little purpose of fluctuating range.
Below only be described at the uniform velocity heating up in each gradient temperature, so, according to spirit of the present invention, as long as the heating-up time of each thermograde of control and the numerical range that needs to heat up, wherein the temperature temperature rise rate in each thermograde can be for quickening, slow down or setting arbitrarily according to process requirements.
Though oneself discloses the present invention as above with preferred embodiment, the present invention is defined in this.Any those skilled in the art without departing from the spirit and scope of the present invention, all can do various changes and modification, so protection scope of the present invention should be as the criterion with claim institute restricted portion.