CN101667605A - Phosphorus gettering process of silicon chip - Google Patents
Phosphorus gettering process of silicon chip Download PDFInfo
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- CN101667605A CN101667605A CN200910034600A CN200910034600A CN101667605A CN 101667605 A CN101667605 A CN 101667605A CN 200910034600 A CN200910034600 A CN 200910034600A CN 200910034600 A CN200910034600 A CN 200910034600A CN 101667605 A CN101667605 A CN 101667605A
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Abstract
The invention relates to a phosphorus gettering process of silicon chips in the manufacture of solar cells, which comprises the following steps: putting sueded silicon chips into a diffusion furnace for pre-deposition, removing a phosphorosilicate glass layer after diffusion, soaking the silicon chips through distributed processing in a hydrofluoric acid solution, and removing oxide layers from the surfaces of the silicon chips; then putting the silicon chips after washing into the diffusion furnace for secondary diffusion processing, taking the silicon chips out from the diffusion furnace after the processing of the secondary diffusion working procedure, cooling the silicon chips to room temperature, and measuring the square resistance of the silicon chips. The invention can effectively decrease heavily doped 'dead layers' and greatly prolong the average minority carrier lifetime of the silicon chips; after the processes including etching, PECVD, silk screen sintering and the like arefinished according to the normal process of a cell chip, the average transformation efficiency of the made cell chip is further improved, and the cell chip has better electrical performance parameters.
Description
Technical field
The invention belongs to the photovoltaic technology field, particularly relate to the phosphorus gettering process of a kind of silicon chip in the solar cell manufacturing.
Background technology
Along with industrialized development, non-renewable energy resources such as electric power, coal, oil signal for help repeatedly, and energy problem becomes the bottleneck of restriction international community economic development day by day, and more and more countries comes into effect " sunlight program ", develop solar energy resources, seek the new power of economic development.Under the promotion of international photovoltaic market great potential, the solar cell manufacturing industry of various countries not only falls over each other to drop into huge fund, enlarges to produce, and the also numerous and confused research and development institution that sets up oneself researches and develops new battery project, improves the quality and the transformation efficiency of product.Yet silicon chip is made solar battery mono-crystal silicon as basis material and is had microdefect and metal impurities, and these impurity and defective are introduced multiple deep energy level in the silicon forbidden band, become the complex centre of minority carrier, have had a strong impact on the photoelectric conversion efficiency of solar cell.
In monocrystalline silicon, because impurity and impurity, migration and coacervation again can take place in the interaction between impurity and the defective, beavy metal impurity or microdefect at a certain temperature, utilize this phenomenon, introduce mechanical damage, defective or precipitate a certain film in silicon chip back, also can introduce defective in vivo, make beavy metal impurity be enriched to these special region, promptly be called the absorption of impurity from the working region of device, the former is called outer gettering, and the latter is an intrinsic gettering.Impurity-absorbing technique is to reduce the processing of silicon chip and the pollution of device technology process, improves a kind of very effective method of the performance of device.Utilize impurity to introduce defective and form the impurity enriched zone to the characteristic of the region clustering of imperfection with lattice, damage field with this one deck impurity enriched removes then, just can get to the purpose of removing partial impurities in the silicon chip, reduce minority carrier recombination center in the silicon chip, improve the short circuit current of battery, thereby improve photoelectric conversion efficiency of the solar battery.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, a kind of heavy doping " dead layer " that effectively reduces is provided, improve the battery short wave response, the phosphorus gettering process of the Isc of improvement battery and the silicon chip of Voc.Purpose of the present invention realizes by following technical scheme: described phosphorus gettering process comprises the steps:
(1) pre-deposition: the silicon chip that will prepare matte is put in the diffusion furnace and is spread, and this operation was divided into for six steps, and the feeding amount of the time in per step, temperature and all gases is as follows in detail:
(a), first step diffusion: be 300～400s diffusion time, the fire door temperature is 870～880 ℃, and temperature is 820～830 ℃ in the stove, and stove tail temperature is 820～830 ℃, the feeding amount of nitrogen is 22000～23000ml, and the feeding amount of phosphorus oxychloride and oxygen is 0ml;
(b), second step diffusion: be 120～180s diffusion time, the fire door temperature is 880～890 ℃, and temperature is 840～850 ℃ in the stove, and stove tail temperature is 860～870 ℃, the feeding amount of nitrogen is 22000～23000ml, and the feeding amount of phosphorus oxychloride and oxygen is 0ml;
(c), the 3rd step diffusion: be 360～420s diffusion time, the fire door temperature is 870～880 ℃, and temperature is 850～860 ℃ in the stove, and stove tail temperature is 840～860 ℃, the feeding amount of nitrogen is 22000～23000ml, and the feeding amount of phosphorus oxychloride and oxygen is 0ml;
(d), the 4th step diffusion: be 1200～1300s diffusion time, the fire door temperature is 890～900 ℃, temperature is 860～880 ℃ in the stove, stove tail temperature is 870～890 ℃, the feeding amount of nitrogen is 25000～26000ml, the feeding amount of phosphorus oxychloride is 1900～2100ml, and the feeding amount of oxygen is 0ml;
(e), the 5th step diffusion: be 300～420s diffusion time, and the fire door temperature is 840～860 ℃, and temperature is 820～830 ℃ in the stove, stove tail temperature is 820～830 ℃, the feeding amount of nitrogen is 22000～23000ml, the feeding amount 0ml of phosphorus oxychloride, and the feeding amount of oxygen is 3000～4000ml;
(f), the 6th step diffusion: be 300～400s diffusion time, and the fire door temperature is 840～860 ℃, and temperature is 820～830 ℃ in the stove, stove tail temperature is 820～830 ℃, the feeding amount of nitrogen is 22000～23000ml, the feeding amount 0ml of phosphorus oxychloride, and the feeding amount of oxygen is 3000～4000ml;
After treating that diffusion is finished, silicon chip is taken out and be cooled to room temperature from diffusion furnace, measure the square resistance of silicon chip, the square resistance of control diffusion back silicon chip is between 100 Ω～110 Ω;
(2) dephosphorization silica glass layer: the silicon chip surface after above-mentioned pre-deposition is handled can form the thin phosphorosilicate glass layer of one deck, it is that 5%～6% hydrofluoric acid solution soaks 50～60s that silicon chip after will handling through pre-deposition is put into concentration, removes the phosphorosilicate glass layer on the silicon chip surface;
(3) distribute: will above-mentionedly remove silicon chip behind the phosphorosilicate glass layer and put into once more that diffusion furnace carries out high-temperature oxydation and gettering is handled, this operation is divided into 4 and goes on foot, and the feeding amount of the time in per step, temperature and all gases is as follows in detail again:
(a), first step diffusion: be 300～400s diffusion time, and the fire door temperature is 1020～1040 ℃, and temperature is 1010～1030 ℃ in the stove, stove tail temperature is 1010～1030 ℃, the feeding amount of nitrogen is 0ml, and the feeding amount of trichloroethanes is 0ml, and the feeding amount of oxygen is 20000～21000ml;
(b), second step diffusion: be 1620～1800s diffusion time, and the fire door temperature is 1000～1100 ℃, and temperature is 1000～1100 ℃ in the stove, stove tail temperature is 1000～1100 ℃, the feeding amount of nitrogen is 0ml, the feeding amount 500ml of trichloroethanes, and the feeding amount of oxygen is 20000～21000ml;
(c), the 3rd step diffusion: be 180～360s diffusion time, and the fire door temperature is 1020～1040 ℃, and temperature is 1010～1030 ℃ in the stove, stove tail temperature is 1010～1030 ℃, the feeding amount of nitrogen is 20000～22000ml, the feeding amount 0ml of trichloroethanes, and the feeding amount of oxygen is 0ml;
(d), the 4th step diffusion: be 300～400s diffusion time, and the fire door temperature is 1020～1040 ℃, and temperature is 1000～1100 ℃ in the stove, stove tail temperature is 1000～1100 ℃, the feeding amount of nitrogen is 20000～22000ml, and the feeding amount of trichloroethanes is 0ml, and the feeding amount of oxygen is 0ml;
After treating that the 4th step finished, after silicon chip taken out and being cooled to room temperature, measure the square resistance of silicon chip from diffusion furnace, control square resistance between 70 Ω-80 Ω;
(4) deoxidation layer: through forming the oxide-film of one deck blueness on the silicon chip surface after the distribution process again, will put into concentration through the silicon chip after the distribution process again is that 5%～6% hydrofluoric acid solution soaks 300～400s,, remove the oxide layer on the silicon chip surface;
(5) secondary diffusion: above-mentioned being put into through the silicon chip of getting rid of surface oxide layer after cleaning carried out DIFFUSION TREATMENT once more in the diffusion furnace, this operation was divided into for seven steps, and the feeding amount of the time in per step, temperature and all gases is as follows in detail:
(a), first step diffusion: be 300～400s diffusion time, and the fire door temperature is 900～910 ℃, and temperature is 850～860 ℃ in the stove, stove tail temperature is 850～870 ℃, the feeding amount of nitrogen is 28000～30000ml, the feeding amount 0ml of phosphorus oxychloride, and the feeding amount of oxygen is 0ml;
(b), second step diffusion: be 360～420s diffusion time, and the fire door temperature is 910～920 ℃, and temperature is 870～880 ℃ in the stove, stove tail temperature is 880～890 ℃, the feeding amount of nitrogen is 28000～30000ml, the feeding amount 0ml of phosphorus oxychloride, and the feeding amount of oxygen is 0ml;
(c), the 3rd step diffusion: be 120～210s diffusion time, and the fire door temperature is 920～930 ℃, and temperature is 890～900 ℃ in the stove, stove tail temperature is 890～900 ℃, the feeding amount of nitrogen is 22000～23000ml, the feeding amount 0ml of phosphorus oxychloride, and the feeding amount of oxygen is 3000～4000ml;
(d), the 4th step diffusion: be 460～580s diffusion time, the fire door temperature is 930～940 ℃, temperature is 880～890 ℃ in the stove, stove tail temperature is 890～900 ℃, the feeding amount of nitrogen is 22000～23000ml, the feeding amount 2000～2100ml of phosphorus oxychloride, the feeding amount of oxygen is 3000～4000ml;
(e), the 5th step diffusion: be 920～1200s diffusion time, the fire door temperature is 930～940 ℃, temperature is 880～890 ℃ in the stove, stove tail temperature is 890～900 ℃, the feeding amount of nitrogen is 22000～23000ml, the feeding amount 2200～2300ml of phosphorus oxychloride, the feeding amount of oxygen is 3000～4000ml;
(f), the 6th step diffusion: be 300～420s diffusion time, and the fire door temperature is 890～900 ℃, and temperature is 850～860 ℃ in the stove, stove tail temperature is 860～870 ℃, the feeding amount of nitrogen is 22000～23000ml, the feeding amount 0ml of phosphorus oxychloride, and the feeding amount of oxygen is 3000～4000ml;
(g), the 7th step diffusion: be 300～400s diffusion time, and the fire door temperature is 900～910 ℃, and temperature is 850～860 ℃ in the stove, stove tail temperature is 860～870 ℃, the feeding amount of nitrogen is 22000～23000ml, the feeding amount 0ml of phosphorus oxychloride, and the feeding amount of oxygen is 0ml;
After the secondary diffusion finishes, silicon chip is taken out and be cooled to room temperature from diffusion furnace, measure the minority carrier life time and the square resistance of silicon chip, the square resistance of control secondary diffusion back silicon chip is between 30 Ω-40 Ω.
The present invention compares with traditional handicraft, and advantage is: the average minority carrier lifetime of handling the back silicon chip improves greatly; Finish technologies such as etching, PECVD, silk screen sintering according to the normal process of battery sheet after, the average transformation efficiency of making of battery sheet further improves, and every unit for electrical property parameters of battery sheet is more excellent.
Embodiment
Below in conjunction with concrete enforcement the present invention is further described.
Embodiment 1
Select for use level of efficiency on the production line the silicon chip of 125 * 125 models of the monocrystalline below 15% totally 300 carry out the phosphorus gettering and handle, concrete steps are as follows:
(1) pre-deposition: the silicon chip that will prepare matte is put in the diffusion furnace and is spread, and this operation was divided into for six steps, and the feeding amount of the time in per step, temperature and all gases is as follows in detail:
(a), be 360s diffusion time, the fire door temperature is 875 ℃, temperature is 825 ℃ in the stove, stove tail temperature is 825 ℃, the feeding amount of nitrogen is 22500ml, the feeding amount of phosphorus oxychloride and oxygen is 0ml;
(b), be 150s diffusion time, the fire door temperature is 885 ℃, temperature is 845 ℃ in the stove, stove tail temperature is 865 ℃, the feeding amount of nitrogen is 22500ml, the feeding amount of phosphorus oxychloride and oxygen is 0ml;
(c), be 390s diffusion time, the fire door temperature is 875 ℃, temperature is 855 ℃ in the stove, stove tail temperature is 855 ℃, the feeding amount of nitrogen is 22500ml, the feeding amount of phosphorus oxychloride and oxygen is 0ml;
(d), be 1250s diffusion time, the fire door temperature is 895 ℃, temperature is 870 ℃ in the stove, stove tail temperature is 880 ℃, the feeding amount of nitrogen is 25500ml, the feeding amount of phosphorus oxychloride is 2000ml, the feeding amount of oxygen is 0ml;
(e), be 360s diffusion time, the fire door temperature is 850 ℃, temperature is 825 ℃ in the stove, stove tail temperature is 825 ℃, the feeding amount of nitrogen is 22500ml, the feeding amount 0ml of phosphorus oxychloride, the feeding amount of oxygen is 3500ml;
(f), be 360s diffusion time, the fire door temperature is 850 ℃, temperature is 825 ℃ in the stove, stove tail temperature is 825 ℃, the feeding amount of nitrogen is 22500ml, the feeding amount 0ml of phosphorus oxychloride, the feeding amount of oxygen is 3500ml;
After treating that diffusion is finished, silicon chip is taken out and be cooled to room temperature from diffusion furnace, with the square resistance of four-point probe measurment silicon chip, the square resistance of silicon chip is 105 Ω after this process DIFFUSION TREATMENT;
(2) dephosphorization silica glass layer: the silicon chip surface after above-mentioned pre-deposition is handled can form the thin phosphorosilicate glass layer of one deck, and will put into concentration through the silicon chip after the pre-deposition processing is that 5.5% hydrofluoric acid solution soaks 56s, removes the phosphorosilicate glass layer on the silicon chip surface;
(3) distribute: will above-mentionedly remove silicon chip behind the phosphorosilicate glass layer and put into once more that diffusion furnace carries out high-temperature oxydation and gettering is handled, this operation is divided into 4 and goes on foot, and the feeding amount of the time in per step, temperature and all gases is as follows in detail again:
(a), be 360s diffusion time, the fire door temperature is 1030 ℃, temperature is 1020 ℃ in the stove, stove tail temperature is 1020 ℃, the feeding amount of nitrogen is 0ml, the feeding amount of trichloroethanes is 0ml, the feeding amount of oxygen is 20500ml;
(b), be 1760s diffusion time, the fire door temperature is 1050 ℃, temperature is 1050 ℃ in the stove, stove tail temperature is 1050 ℃, the feeding amount of nitrogen is 0ml, the feeding amount 500ml of trichloroethanes, the feeding amount of oxygen is 20500ml;
(c), be 320s diffusion time, the fire door temperature is 1030 ℃, temperature is 1020 ℃ in the stove, stove tail temperature is 1020 ℃, the feeding amount of nitrogen is 21000ml, the feeding amount 0ml of trichloroethanes, the feeding amount of oxygen is 0ml;
(d), be 360s diffusion time, the fire door temperature is 1030 ℃, temperature is 1050 ℃ in the stove, stove tail temperature is 1050 ℃, the feeding amount of nitrogen is 2100ml, the feeding amount of trichloroethanes is 0ml, the feeding amount of oxygen is 0ml;
After treating that the 4th step finished, after silicon chip taken out from diffusion furnace and being cooled to room temperature, the square resistance of usefulness four-point probe measurment silicon chip, this square resistance through silicon chip after the distribution process again is about 75 Ω;
(4) deoxidation layer: through forming the oxide-film of one deck blueness on the silicon chip surface after the distribution process again,, will put into concentration through the silicon chip after the distribution process again is that 5.5% hydrofluoric acid solution soaks 350s, removes the oxide layer on the silicon chip surface;
(5) secondary diffusion: above-mentioned being put into through the silicon chip of getting rid of surface oxide layer after cleaning carried out DIFFUSION TREATMENT once more in the diffusion furnace, this operation was divided into for seven steps, and the feeding amount of the time in per step, temperature and all gases is as follows in detail:
(a), be 360s diffusion time, the fire door temperature is 905 ℃, temperature is 855 ℃ in the stove, stove tail temperature is 860 ℃, the feeding amount of nitrogen is 29000ml, the feeding amount 0ml of phosphorus oxychloride, the feeding amount of oxygen is 0ml;
(b), be 390s diffusion time, the fire door temperature is 915 ℃, temperature is 875 ℃ in the stove, stove tail temperature is 885 ℃, the feeding amount of nitrogen is 29000ml, the feeding amount 0ml of phosphorus oxychloride, the feeding amount of oxygen is 0ml;
(c), be 180s diffusion time, the fire door temperature is 925 ℃, temperature is 895 ℃ in the stove, stove tail temperature is 895 ℃, the feeding amount of nitrogen is 22500ml, the feeding amount 0ml of phosphorus oxychloride, the feeding amount of oxygen is 3500ml;
(d), be 520s diffusion time, the fire door temperature is 935 ℃, temperature is 885 ℃ in the stove, stove tail temperature is 895 ℃, the feeding amount of nitrogen is 22500ml, the feeding amount 2050ml of phosphorus oxychloride, the feeding amount of oxygen is 3500ml;
(e), be 1080s diffusion time, the fire door temperature is 935 ℃, temperature is 885 ℃ in the stove, stove tail temperature is 895 ℃, the feeding amount of nitrogen is 22500ml, the feeding amount 2250ml of phosphorus oxychloride, the feeding amount of oxygen is 3400ml;
(f), be 360s diffusion time, the fire door temperature is 895 ℃, temperature is 855 ℃ in the stove, stove tail temperature is 865 ℃, the feeding amount of nitrogen is 22500ml, the feeding amount 0ml of phosphorus oxychloride, the feeding amount of oxygen is 3300ml;
(g), be 380s diffusion time, the fire door temperature is 905 ℃, temperature is 855 ℃ in the stove, stove tail temperature is 865 ℃, the feeding amount of nitrogen is 22000ml, the feeding amount 0ml of phosphorus oxychloride, the feeding amount of oxygen is 0ml;
After the secondary diffusion finishes, silicon chip is taken out and is cooled to room temperature from diffusion furnace, with the minority carrier life time of minority carrier life time instrument measurement silicon chip, with the square resistance of four-point probe measurment silicon chip; Through measuring, about the high 6.0 μ s of minority carrier life time after the average minority carrier lifetime of silicon chip spreads than traditional handicraft after the PROCESS FOR TREATMENT of the present invention, the square resistance of silicon chip is about 35 Ω.
Finish technologies such as etching, PECVD, silk screen sintering according to the normal process of battery sheet after, the average transformation efficiency of making of battery sheet reaches 16.26%, has improved about 2% than traditional handicraft.
Embodiment 2
Select for use level of efficiency on the production line the silicon chip of 125 * 125 models of the monocrystalline below 15% totally 300 carry out the phosphorus gettering and handle, concrete steps are as follows:
(1) pre-deposition: the silicon chip that will prepare matte is put in the diffusion furnace and is spread, and this operation was divided into for six steps, and the feeding amount of the time in per step, temperature and all gases is as follows in detail:
(a), be 300s diffusion time, the fire door temperature is 870 ℃, temperature is 820 ℃ in the stove, stove tail temperature is 823 ℃, the feeding amount of nitrogen is 22100ml, the feeding amount of phosphorus oxychloride and oxygen is 0ml;
(b), be 120s diffusion time, the fire door temperature is 880 ℃, temperature is 840 ℃ in the stove, stove tail temperature is 860 ℃, the feeding amount of nitrogen is 22100ml, the feeding amount of phosphorus oxychloride and oxygen is 0ml;
(c), be 360s diffusion time, the fire door temperature is 870 ℃, temperature is 850 ℃ in the stove, stove tail temperature is 840 ℃, the feeding amount of nitrogen is 22000ml, the feeding amount of phosphorus oxychloride and oxygen is 0ml;
(d), be 1200s diffusion time, the fire door temperature is 890 ℃, temperature is 860 ℃ in the stove, stove tail temperature is 870 ℃, the feeding amount of nitrogen is 25000ml, the feeding amount of phosphorus oxychloride is 1900ml, the feeding amount of oxygen is 0ml;
(e), be 300s diffusion time, the fire door temperature is 840 ℃, temperature is 820 ℃ in the stove, stove tail temperature is 820 ℃, the feeding amount of nitrogen is 22000ml, the feeding amount 0ml of phosphorus oxychloride, the feeding amount of oxygen is 3000ml;
(f), be 300s diffusion time, the fire door temperature is 840 ℃, temperature is 820 ℃ in the stove, stove tail temperature is 820 ℃, the feeding amount of nitrogen is 22000ml, the feeding amount 0ml of phosphorus oxychloride, the feeding amount of oxygen is 3000ml;
After treating that diffusion is finished, silicon chip is taken out and be cooled to room temperature from diffusion furnace, with the square resistance of four-point probe measurment silicon chip, the square resistance of silicon chip is about 110 Ω after this process DIFFUSION TREATMENT;
(2) dephosphorization silica glass layer: dephosphorization silica glass layer: the silicon chip surface after above-mentioned pre-deposition is handled can form the thin phosphorosilicate glass layer of one deck, it is that 5% hydrofluoric acid solution soaks 60s that silicon chip after will handling through pre-deposition is put into concentration, removes the phosphorosilicate glass layer on the silicon chip surface;
(3) distribute: will above-mentionedly remove silicon chip behind the phosphorosilicate glass layer and put into once more that diffusion furnace carries out high-temperature oxydation and gettering is handled, this operation is divided into 4 and goes on foot, and the feeding amount of the time in per step, temperature and all gases is as follows in detail again:
(a), be 300s diffusion time, the fire door temperature is 1020 ℃, temperature is 1010 ℃ in the stove, stove tail temperature is 1010 ℃, the feeding amount of nitrogen is 0ml, the feeding amount of trichloroethanes is 0ml, the feeding amount of oxygen is 20000ml;
(b), be 1620s diffusion time, the fire door temperature is 1000 ℃, temperature is 1000 ℃ in the stove, stove tail temperature is 1000 ℃, the feeding amount of nitrogen is 0ml, the feeding amount 500ml of trichloroethanes, the feeding amount of oxygen is 20000ml;
(c), be 180s diffusion time, the fire door temperature is 1020 ℃, temperature is 1010 ℃ in the stove, stove tail temperature is 1010 ℃, the feeding amount of nitrogen is 20000ml, the feeding amount 0ml of trichloroethanes, the feeding amount of oxygen is 0ml;
(d), be 300s diffusion time, the fire door temperature is 1020 ℃, temperature is 1030 ℃ in the stove, stove tail temperature is 1010 ℃, the feeding amount of nitrogen is 20000ml, the feeding amount of trichloroethanes is 0ml, the feeding amount of oxygen is 0ml;
After treating that the 4th step finished, after silicon chip taken out from diffusion furnace and being cooled to room temperature, the square resistance of usefulness four-point probe measurment silicon chip, this square resistance through silicon chip after the distribution process again is about 80 Ω;
(4) deoxidation layer: through forming the oxide-film of one deck blueness on the silicon chip surface after the distribution process again,, will put into concentration through the silicon chip after the distribution process again is that 5% hydrofluoric acid solution soaks 400s, removes the oxide layer on the silicon chip surface;
(5) secondary diffusion: above-mentioned being put into through the silicon chip of getting rid of surface oxide layer after cleaning carried out DIFFUSION TREATMENT once more in the diffusion furnace, this operation was divided into for seven steps, and the feeding amount of the time in per step, temperature and all gases is as follows in detail:
(a), be 300s diffusion time, the fire door temperature is 900 ℃, temperature is 850 ℃ in the stove, stove tail temperature is 850 ℃, the feeding amount of nitrogen is 28000ml, the feeding amount 0ml of phosphorus oxychloride, the feeding amount of oxygen is 0ml;
(b), be 360s diffusion time, the fire door temperature is 910 ℃, temperature is 870 ℃ in the stove, stove tail temperature is 880 ℃, the feeding amount of nitrogen is 28030ml, the feeding amount 0ml of phosphorus oxychloride, the feeding amount of oxygen is 0ml;
(c), be 120s diffusion time, the fire door temperature is 920 ℃, temperature is 890 ℃ in the stove, stove tail temperature is 890 ℃, the feeding amount of nitrogen is 22000ml, the feeding amount 0ml of phosphorus oxychloride, the feeding amount of oxygen is 3000ml;
(d), be 460s diffusion time, the fire door temperature is 930 ℃, temperature is 880 ℃ in the stove, stove tail temperature is 890 ℃, the feeding amount of nitrogen is 22000ml, the feeding amount 2000ml of phosphorus oxychloride, the feeding amount of oxygen is 3000ml;
(e), be 920s diffusion time, the fire door temperature is 930 ℃, temperature is 880 ℃ in the stove, stove tail temperature is 890 ℃, the feeding amount of nitrogen is 22000ml, the feeding amount 2200ml of phosphorus oxychloride, the feeding amount of oxygen is 3000ml;
(f), be 300s diffusion time, the fire door temperature is 890 ℃, temperature is 850 ℃ in the stove, stove tail temperature is 860 ℃, the feeding amount of nitrogen is 22000ml, the feeding amount 0ml of phosphorus oxychloride, the feeding amount of oxygen is 3000ml;
(g), be 300s diffusion time, the fire door temperature is 900 ℃, temperature is 850 ℃ in the stove, stove tail temperature is 860 ℃, the feeding amount of nitrogen is 22000ml, the feeding amount 0ml of phosphorus oxychloride, the feeding amount of oxygen is 0ml;
After the secondary diffusion finishes, silicon chip is taken out and is cooled to room temperature from diffusion furnace, with the minority carrier life time of minority carrier life time instrument measurement silicon chip, with the square resistance of four-point probe measurment silicon chip; Through measuring, about the high 4.6 μ s of minority carrier life time after the average minority carrier lifetime of silicon chip spreads than traditional handicraft after the PROCESS FOR TREATMENT of the present invention, the square resistance of silicon chip is about 40 Ω.
Finish technologies such as etching, PECVD, silk screen sintering according to the normal process of battery sheet after, the average transformation efficiency of making of battery sheet reaches 15.80%, has improved about 1.6% than traditional handicraft.
Embodiment 3
Select for use level of efficiency on the production line the silicon chip of 125 * 125 models of the monocrystalline below 15% totally 300 carry out the phosphorus gettering and handle, concrete steps are as follows:
(1) pre-deposition: the silicon chip that will prepare matte is put in the diffusion furnace and is spread, and this operation was divided into for six steps, and the feeding amount of the time in per step, temperature and all gases is as follows in detail:
(a), be 400s diffusion time, the fire door temperature is 880 ℃, temperature is 830 ℃ in the stove, stove tail temperature is 830 ℃, the feeding amount of nitrogen is 23000ml, the feeding amount of phosphorus oxychloride and oxygen is 0ml;
(b), be 180s diffusion time, the fire door temperature is 890 ℃, temperature is 850 ℃ in the stove, stove tail temperature is 870 ℃, the feeding amount of nitrogen is 23000ml, the feeding amount of phosphorus oxychloride and oxygen is 0ml;
(c), be 420s diffusion time, the fire door temperature is 880 ℃, temperature is 860 ℃ in the stove, stove tail temperature is 860 ℃, the feeding amount of nitrogen is 23000ml, the feeding amount of phosphorus oxychloride and oxygen is 0ml;
(d), be 1300s diffusion time, the fire door temperature is 900 ℃, temperature is 880 ℃ in the stove, stove tail temperature is 890 ℃, the feeding amount of nitrogen is 26000ml, the feeding amount of phosphorus oxychloride is 2100ml, the feeding amount of oxygen is 0ml;
(e), be 420s diffusion time, the fire door temperature is 860 ℃, temperature is 830 ℃ in the stove, stove tail temperature is 830 ℃, the feeding amount of nitrogen is 23000ml, the feeding amount 0ml of phosphorus oxychloride, the feeding amount of oxygen is 4000ml;
(f), be 400s diffusion time, the fire door temperature is 860 ℃, temperature is 830 ℃ in the stove, stove tail temperature is 830 ℃, the feeding amount of nitrogen is 23000ml, the feeding amount 0ml of phosphorus oxychloride, the feeding amount of oxygen is 4000ml;
After treating that diffusion is finished, silicon chip is taken out and be cooled to room temperature from diffusion furnace, with the square resistance of four-point probe measurment silicon chip, the square resistance of silicon chip is about 100 Ω after this process DIFFUSION TREATMENT;
(2) dephosphorization silica glass layer: the silicon chip surface after above-mentioned pre-deposition is handled can form the thin phosphorosilicate glass layer of one deck, and will put into concentration through the silicon chip after the pre-deposition processing is that 6% hydrofluoric acid solution soaks 50s, removes the phosphorosilicate glass layer on the silicon chip surface;
(3) distribute: will above-mentionedly remove silicon chip behind the phosphorosilicate glass layer and put into once more that diffusion furnace carries out high-temperature oxydation and gettering is handled, this operation is divided into 4 and goes on foot, and the feeding amount of the time in per step, temperature and all gases is as follows in detail again:
(a), be 400s diffusion time, the fire door temperature is 1040 ℃, temperature is 1030 ℃ in the stove, stove tail temperature is 1030 ℃, the feeding amount of nitrogen is 0ml, the feeding amount of trichloroethanes is 0ml, the feeding amount of oxygen is 21000ml;
(b), be 1800s diffusion time, the fire door temperature is 1100 ℃, temperature is 1100 ℃ in the stove, stove tail temperature is 1100 ℃, the feeding amount of nitrogen is 0ml, the feeding amount 500ml of trichloroethanes, the feeding amount of oxygen is 21000ml;
(c), be 360s diffusion time, the fire door temperature is 1040 ℃, temperature is 1030 ℃ in the stove, stove tail temperature is 1030 ℃, the feeding amount of nitrogen is 22000ml, the feeding amount 0ml of trichloroethanes, the feeding amount of oxygen is 0ml;
(d), be 400s diffusion time, the fire door temperature is 1040 ℃, temperature is 1100 ℃ in the stove, stove tail temperature is 1100 ℃, the feeding amount of nitrogen is 22000ml, the feeding amount of trichloroethanes is 0ml, the feeding amount of oxygen is 0ml;
After treating that the 4th step finished, after silicon chip taken out from diffusion furnace and being cooled to room temperature, the square resistance of usefulness four-point probe measurment silicon chip, this square resistance through silicon chip after the distribution process again is about 70 Ω;
(4) deoxidation layer: through forming the oxide-film of one deck blueness on the silicon chip surface after the distribution process again,, will put into concentration through the silicon chip after the distribution process again is that 6% hydrofluoric acid solution soaks 300s, removes the oxide layer on the silicon chip surface;
(5) secondary diffusion: above-mentioned being put into through the silicon chip of getting rid of surface oxide layer after cleaning carried out DIFFUSION TREATMENT once more in the diffusion furnace, this operation was divided into for seven steps, and the feeding amount of the time in per step, temperature and all gases is as follows in detail:
(a), be 400s diffusion time, the fire door temperature is 910 ℃, temperature is 860 ℃ in the stove, stove tail temperature is 870 ℃, the feeding amount of nitrogen is 30000ml, the feeding amount 0ml of phosphorus oxychloride, the feeding amount of oxygen is 0ml;
(b), be 420s diffusion time, the fire door temperature is 920 ℃, temperature is 880 ℃ in the stove, stove tail temperature is 890 ℃, the feeding amount of nitrogen is 30000ml, the feeding amount 0ml of phosphorus oxychloride, the feeding amount of oxygen is 0ml;
(c), be 210s diffusion time, the fire door temperature is 930 ℃, temperature is 900 ℃ in the stove, stove tail temperature is 900 ℃, the feeding amount of nitrogen is 23000ml, the feeding amount 0ml of phosphorus oxychloride, the feeding amount of oxygen is 4000ml;
(d), be 580s diffusion time, the fire door temperature is 940 ℃, temperature is 890 ℃ in the stove, stove tail temperature is 900 ℃, the feeding amount of nitrogen is 23000ml, the feeding amount 2100ml of phosphorus oxychloride, the feeding amount 4000ml of oxygen;
(e), be 1200s diffusion time, the fire door temperature is 940 ℃, temperature is 890 ℃ in the stove, stove tail temperature is 900 ℃, the feeding amount of nitrogen is 23000ml, the feeding amount 2200～2300ml of phosphorus oxychloride, the feeding amount of oxygen is 4000ml;
(f), be 420s diffusion time, the fire door temperature is 900 ℃, temperature is 860 ℃ in the stove, stove tail temperature is 870 ℃, the feeding amount of nitrogen is 23000ml, the feeding amount 0ml of phosphorus oxychloride, the feeding amount of oxygen is 4000ml;
(g), be 400s diffusion time, the fire door temperature is 910 ℃, temperature is 860 ℃ in the stove, stove tail temperature is 870 ℃, the feeding amount of nitrogen is 23000ml, the feeding amount 0ml of phosphorus oxychloride, the feeding amount of oxygen is 0ml;
After the secondary diffusion finishes, silicon chip is taken out and is cooled to room temperature from diffusion furnace, with the minority carrier life time of minority carrier life time instrument measurement silicon chip, with the square resistance of four-point probe measurment silicon chip; Find that through measuring about the high 4.8 μ s of minority carrier life time after the average minority carrier lifetime of silicon chip spreads than traditional handicraft after the PROCESS FOR TREATMENT of the present invention, the square resistance of silicon chip is about 30 Ω.
Finish technologies such as etching, PECVD, silk screen sintering according to the normal process of battery sheet after, the average transformation efficiency of making of battery sheet reaches 15.60%, has improved about 1.4% than traditional handicraft.
Claims (1)
1, a kind of phosphorus gettering process is characterized in that comprising the steps:
(1) pre-deposition: the silicon chip that will prepare matte is put in the diffusion furnace and is spread, and this operation was divided into for six steps, and the feeding amount of the time in per step, temperature and all gases is as follows in detail:
(a), first step diffusion: be 300～400s diffusion time, and the fire door temperature is 870～880 ℃, and temperature is 820～830 ℃ in the stove, and stove tail temperature is 820～830 ℃, and the feeding amount of nitrogen is 22000～23000ml;
(b), second step diffusion: be 120～180s diffusion time, and the fire door temperature is 880～890 ℃, and temperature is 840～850 ℃ in the stove, and stove tail temperature is 860～870 ℃, and the feeding amount of nitrogen is 22000～23000ml;
(c), the 3rd step diffusion: be 360～420s diffusion time, and the fire door temperature is 870～880 ℃, and temperature is 850～860 ℃ in the stove, and stove tail temperature is 840～860 ℃, and the feeding amount of nitrogen is 22000～23000ml;
(d), the 4th step diffusion: be 1200～1300s diffusion time, the fire door temperature is 890～900 ℃, and temperature is 860～880 ℃ in the stove, and stove tail temperature is 870～890 ℃, the feeding amount of nitrogen is 25000～26000ml, and the feeding amount of phosphorus oxychloride is 1900～2100ml;
(e), the 5th step diffusion: be 300～420s diffusion time, and the fire door temperature is 840～860 ℃, and temperature is 820～830 ℃ in the stove, and stove tail temperature is 820～830 ℃, and the feeding amount of nitrogen is 22000～23000ml, and the feeding amount of oxygen is 3000～4000ml;
(f), the 6th step diffusion: be 300～400s diffusion time, the fire door temperature is 840～860 ℃, and temperature is 820～830 ℃ in the stove, and stove tail temperature is 820～830 ℃, the feeding amount of phosphorus oxychloride is 22000～23000ml, and the feeding amount of oxygen is 3000～4000ml;
After treating that diffusion is finished, silicon chip is taken out and be cooled to room temperature from diffusion furnace, measure the square resistance of silicon chip, the square resistance of control diffusion back silicon chip is between 100 Ω～110 Ω;
(2) dephosphorization silica glass layer: the silicon chip surface after above-mentioned pre-deposition is handled can form the thin phosphorosilicate glass layer of one deck, it is that 5%～6% hydrofluoric acid solution soaks 50～60s that silicon chip after will handling through pre-deposition is put into concentration, removes the phosphorosilicate glass layer on the silicon chip surface;
(3) distribute: will above-mentionedly remove silicon chip behind the phosphorosilicate glass layer and put into once more that diffusion furnace carries out high-temperature oxydation and gettering is handled, this operation is divided into 4 and goes on foot, and the feeding amount of the time in per step, temperature and all gases is as follows in detail again:
(a), first step diffusion: be 300～400s diffusion time, and the fire door temperature is 1020～1040 ℃, and temperature is 1010～1030 ℃ in the stove, and stove tail temperature is 1010～1030, and the feeding amount of oxygen is 20000～21000ml;
(b), second step diffusion: be 1620～1800s diffusion time, the fire door temperature is 1000～1100 ℃, and temperature is 1000～1100 ℃ in the stove, and stove tail temperature is 1000～1100 ℃, the feeding amount 500ml of trichloroethanes, the feeding amount of oxygen is 20000～21000ml;
(c), the 3rd step diffusion: be 180～360s diffusion time, and the fire door temperature is 1020～1040 ℃, and temperature is 1010～1030 in the stove, and stove tail temperature is 1010～1030 ℃, and the feeding amount of nitrogen is 20000～22000ml;
(d), the 4th step diffusion: be 300～400s diffusion time, and the fire door temperature is 1020～1040 ℃, and temperature is 1000～1100 in the stove, and stove tail temperature is 1000～1100, and the feeding amount of nitrogen is 20000～22000ml;
After treating that the 4th step finished, after silicon chip taken out and being cooled to room temperature, measure the square resistance of silicon chip from diffusion furnace, control square resistance between 70-80 Ω;
(4) deoxidation layer: through forming the oxide-film of one deck blueness on the silicon chip surface after the distribution process again, will put into concentration through the silicon chip after the distribution process again is that 5%～6% hydrofluoric acid solution soaks 300～400s,, remove the oxide layer on the silicon chip surface;
(5) secondary diffusion: above-mentioned being put into through the silicon chip of getting rid of surface oxide layer after cleaning carried out DIFFUSION TREATMENT once more in the diffusion furnace, this operation was divided into for seven steps, and the feeding amount of the time in per step, temperature and all gases is as follows in detail:
(a), first step diffusion: be 300～400s diffusion time, and the fire door temperature is 900～910 ℃, and temperature is 850～860 ℃ in the stove, and stove tail temperature is 850～870 ℃, and the feeding amount of nitrogen is 28000～30000ml;
(b), second step diffusion: be 360～420s diffusion time, and the fire door temperature is 910～920 ℃, and temperature is 870～880 ℃ in the stove, and stove tail temperature is 880～890 ℃, and the feeding amount of nitrogen is 28000～30000ml;
(c), the 3rd step diffusion: be 120～210s diffusion time, and the fire door temperature is 920～930 ℃, and temperature is 890～900 ℃ in the stove, and stove tail temperature is 890～900 ℃, and the feeding amount of nitrogen is 22000～23000ml, and the feeding amount of oxygen is 3000～4000ml;
(d), the 4th step diffusion: be 460～580s diffusion time, the fire door temperature is 930～940 ℃, temperature is 880～890 ℃ in the stove, stove tail temperature is 890～900 ℃, the feeding amount of nitrogen is 22000～23000ml, the feeding amount 2000～2100ml of phosphorus oxychloride, the feeding amount of oxygen is 3000～4000ml;
(e), the 5th step diffusion: be 920～1200s diffusion time, the fire door temperature is 930～940 ℃, temperature is 880～890 ℃ in the stove, stove tail temperature is 890～900 ℃, the feeding amount of nitrogen is 22000～23000ml, the feeding amount 2200～2300ml of phosphorus oxychloride, the feeding amount of oxygen is 3000～4000ml;
(f), the 6th step diffusion: be 300～420s diffusion time, and the fire door temperature is 890～900 ℃, and temperature is 850～860 ℃ in the stove, and stove tail temperature is 860～870 ℃, and the feeding amount of nitrogen is 22000～23000ml, and the feeding amount of oxygen is 3000～4000ml;
(g), the 7th step diffusion: be 300～400s diffusion time, and the fire door temperature is 900～910 ℃, and temperature is 850～860 ℃ in the stove, and stove tail temperature is 860～870 ℃, and the feeding amount of nitrogen is 22000～23000ml;
After the secondary diffusion finishes, silicon chip is taken out and be cooled to room temperature from diffusion furnace, measure the square resistance of silicon chip, the square resistance of control secondary diffusion back silicon chip is between 30 Ω-40 Ω.
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