CN104404626B - The phosphorus diffusion method of Physical Metallurgy polysilicon solar cell - Google Patents
The phosphorus diffusion method of Physical Metallurgy polysilicon solar cell Download PDFInfo
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Abstract
The invention provides a kind of phosphorus diffusion method of Physical Metallurgy polysilicon solar cell, including, 1) silicon chip after cleaning and texturing is carried out into the first constant temperature heat treatment；2) by through step 1) treatment after silicon chip carry out the second constant temperature heat treatment；3) by through step 2) treatment after silicon chip carry out oxidation processes；4) to step 3) the logical phosphorus source of silicon chip after treatment carries out phosphorus diffusion process；5) by through step 4) treatment after silicon chip made annealing treatment.Method of diffusion of the invention is applied in the preparation of Physical Metallurgy silicon solar cell, it is cost-saved, production capacity is improved, the PN junction for being formed, surface impurity concentration is low, Impurity Distribution is uniform, diffusion uniformity is good, reduces dead layer effect, is conducive to the collection of electronics, loss in efficiency of the solar cell caused by being combined is reduced, so as to improve the final photoelectric transformation efficiency of cell piece.
Description
Technical field
The present invention relates to the diffusion technique in solar cell manufacture, specially a kind of Physical Metallurgy polycrystalline silicon solar electricity
The phosphorus diffusion method in pond.
Background technology
Solar cell is a kind of device that luminous energy can be converted into electric energy, because its application has cleaning, ring
Guarantor, free of contamination advantage, therefore receive much concern, just progressively turn into the optimal new energy for being hopeful to replace traditional energy.
In the solar cell of numerous kinds, polycrystalline silicon solar cell price is relatively low and conversion efficiency is higher, in photovoltaic city
Absolute leading position is occupied in, and this trend is difficult to change in a short time.Therefore continue to improve the polysilicon sun
Battery conversion efficiency, reduce production cost, make polycrystalline silicon solar cell generate electricity can be at war with traditional energy have become work as
Modern field of photovoltaic technology problem demanding prompt solution.
Current solar-grade polysilicon production generally uses chemical method (Siemens Method, improved Siemens or fluid bed
Method), the method is needed polycrystalline silicon purifying to certain purity, is doped into high purity boron further according to needing to re-melt polysilicon, greatly
Increased cost greatly.And the technology is present, and cost of investment is too high, apparatus and process is complicated, high energy consumption, production capacity are low, byproduct of reaction
The shortcomings of being difficult to treatment, the space that cost declines is very limited, seriously governs the development of solar energy industry.And Physical is purified
, used as a kind of emerging technique for producing solar energy level silicon, with process is simple, low cost, production capacity is big, pollute the features such as lacking for technology.
Increasing research institution and manufacturer start to focus on the polysilicon that Physical is purified.Therefore, from reduction
From the aspect of cost, raising production capacity and environmental benefit etc., Physical polycrystalline silicon purifying technology has good development space and pole
Competitive market prospects.
Boron in silicon materials, is directly purified to required purity, it is not necessary to right again by Physical Metallurgy method purifying polycrystalline silicon
Polysilicon is re-melted and is doped into high purity boron, and the resistivity of general polysilicon is lower than what chemical method was purified, i.e., boron is dense in polysilicon
Degree is relatively higher, and resistivity evenness is poor.Be there is also in Physical polysilicon production process simultaneously more
The microdefects such as crystal boundary, the dislocation of metal impurities and higher density, these metal impurities and defect finally can all form complex centre,
So as to influence battery conversion efficiency.
In order to improve the efficiency and reliability of Physical Metallurgy method polycrystal silicon cell, optimization is not only set about in terms of material,
Also need to be improved in terms of battery production technology.And in the preparation process of polycrystal silicon cell, diffusion PN junction belongs to core
Heart technology, the quality of made PN junction can directly influence the photoelectric transformation efficiency of solar cell.
At present, POCl3 (POCl is mostly used in polycrystal silicon cell production process3) liquid source diffusion method, its principle
It is：POCl3By N2It is carried along into Quartz stove tube, PCl is decomposed under the high temperature conditions5And P2O5, PCl5With O2Reaction generation P2O5
And Cl2, P2O5Again with silicon chip reaction generation P simple substance and SiO2, P atoms spread in silicon chip under high temperature, and form N-type region domain, and
Substrate together form PN junction.The PN junction even structure obtained using the method, diffusion layer surface is good, and production efficiency
Height, is conducive to making solar energy in large area battery, is to apply most method of diffusion at present.
In conventional diffusion technique, diffusion flow is generally divided into：Enter boat → constant temperature → TongYuan's diffusion → intensification propulsion → drop
Temperature → go out boat, in diffusion process, POCl3 reacts with silicon chip surface under the high temperature conditions, and by silicon chip surface internally
Slow diffusion.Because silicon chip is difficult to obtain and week in Quartz stove tube apart from very little (about 2.5mm), therefore the centre of silicon chip
The phosphorus source of equivalent is enclosed, sheet resistance uniformity is deteriorated after diffusion, may cause that silicon chip centre impurity concentration is low, and sheet resistance is higher, electricity
Piece final photoelectric transformation efficiency in pond is relatively low.Also, spread in order to stablize each warm area temperature before starting, existing process uses one
Step constant temperature, each warm area temperature fluctuation is larger, and stability is poor, therefore the temperature drift produced after temperature rising in thermostatic process
It is larger, it is necessary to constant temperature time it is more long.
Additionally, TongYuan's diffusing step and intensification forward step of conventional art are completed using same temperature, by polycrystalline
Silicon silicon sheet at low temperature deposits to control total impurities.To ensure that concentration is lightly doped, POCl3 source flux can not be big, otherwise adulterates
Concentration can be high, and so also resulting in sheet resistance uniformity becomes poor, influences electrical performance of cell parameter.In order to meet PN junction depth
Requirement with impurities concentration distribution is, it is necessary to the total amount in the foreign matter of phosphor of silicon chip surface deposition is more than foreign matter of phosphor solid solubility in silicon
The total amount of phosphorus atoms.In intensification progradation, a part of phosphorus impurities that can be deposited polysilicon surface are advanced by high temperature
(solubility of the phosphorus impurities in polysilicon is raised at high temperature, therefore the phosphorus atoms on surface can be in height in being pushed into polysilicon
Dissolved to polysilicon internal penetration under temperature).Although the phosphorus of silicon chip surface can be pushed into polysilicon, also a certain amount of
Phosphorus atoms be deposited on the surface of polysilicon, it is impossible to provide electronics as alms giver, thus formed one layer have it is certain thickness not
" dead layer " of easy conductive.
All conventional diffusion technique is optimized in order to improve many companies of battery efficiency, is replaced by alternating temperature diffusion technique
Constant temperature spreads.Because Cryogenic Temperature Swing diffusion technique can more effectively reduce the recombination rate of minority carrier, while phosphorus gettering
It is more abundant that effect is also played.But because temperature-controlling system shakiness causes each warm area temperature unstable, can also make diffusion uniformity
Difference, sheet resistance fluctuation becomes big, and doping concentration gradient can not be formed, and requirement higher thus be proposed to sintering process, greatly
Increased technology difficulty and complexity.
Either constant temperature diffusion or alternating temperature diffusion, it is all based on a TongYuan, distribution one of the phosphorus impurities in silicon chip
As meet Gaussian Profile or remaining error distribution.Simple is all difficult to solve the above problems by changing temperature, concentration or time,
Degree of optimization is limited.Therefore a kind of diffusion uniformity is sought preferably, sheet resistance is uniform and silicon chip surface and internal impurities concentration distribution
Uniformly, so that the polysilicon solar cell method of diffusion for improving the final photoelectric transformation efficiency of cell piece is particularly important.
The content of the invention
In order to solve the above technical problems, the invention provides a kind of phosphorus diffused sheet of Physical Metallurgy polysilicon solar cell
Method, including, 1) silicon chip after cleaning and texturing is carried out into the first constant temperature heat treatment；2) by through step 1) silicon chip after treatment carries out the
Two constant temperature are heat-treated；3) by through step 2) treatment after silicon chip carry out oxidation processes；4) to step 3) the logical phosphorus of silicon chip after treatment
Source carries out phosphorus diffusion process；5) by through step 4) treatment after silicon chip made annealing treatment.
According to an embodiment of the present invention, wherein the step 4) phosphorus diffusion process include the first DIFFUSION TREATMENT and the
Two DIFFUSION TREATMENTs, first DIFFUSION TREATMENT includes low temperature pre-deposition step and heating step, and second DIFFUSION TREATMENT includes
A) low temperature depositing；B) heat up propulsion；C) it is redeposited；D) high temperature propulsion；E) high temperature redistribution.
Another implementation method of the invention, first DIFFUSION TREATMENT includes：
In 770~790 DEG C, lead to big nitrogen, oxygen to the silicon chip and take the small nitrogen in source, big nitrogen flow be 20000~
21000sccm, oxygen flow is 200~350sccm, takes the small nitrogen flow in source for 300~450sccm, and the time is 60~150s；And
In 790~810 DEG C, to leading to big nitrogen and oxygen through the silicon chip after above-mentioned treatment, big nitrogen flow is 20000~
21000sccm, oxygen flow is 200~400sccm, and the time is 90~220s.
Another implementation method of the invention, second DIFFUSION TREATMENT includes：
A) in 790~810 DEG C, to through the silicon chip after first DIFFUSION TREATMENT leading to big nitrogen, oxygen and take the small nitrogen in source, big nitrogen
Flow is 22000~24000sccm, and oxygen flow is 600~1000sccm, takes the small nitrogen flow in source for 900~1100sccm, when
Between be 200~400s；
B) in 810~830 DEG C, big nitrogen being led to the silicon chip after being processed through step a), big nitrogen flow is 20000~
22000sccm, the time is 200~400s；
C) in 810~830 DEG C, lead to big nitrogen, oxygen to the silicon chip after being processed through step b) and take the small nitrogen in source, big nitrogen flow is
22000~24000sccm, oxygen flow is 700~1100sccm, takes the small nitrogen flow in source for 900~1400sccm, and the time is
200~400s；
D) in 830~850 DEG C, big nitrogen being led to the silicon chip after being processed through step c), big nitrogen flow is 20000~
22000sccm, the time is 200~400s；
E) in 830~850 DEG C, lead to big nitrogen, oxygen to the silicon chip after being processed through step d) and take the small nitrogen in source, big nitrogen flow is
22000~24000sccm, oxygen flow is 700~1100sccm, takes the small nitrogen flow in source for 900~1400sccm, and the time is
400~700s.
Another implementation method of the invention, wherein first constant temperature heat treatment includes, in 670~820 DEG C, to institute
State silicon chip and lead to big nitrogen, big nitrogen flow is 19000~20000sccm, and the time is 200~400s.
Another implementation method of the invention, wherein second constant temperature heat treatment includes, in 770~820 DEG C, Xiang Jing
The silicon chip of the first constant temperature heat treatment leads to big nitrogen, and big nitrogen flow is 19000~20000sccm, and the time is 180~360s.
Another implementation method of the invention, wherein the step 3) include, in 770~820 DEG C, to through the second constant temperature
The silicon chip for the treatment of leads to big nitrogen and dry oxygen, and big nitrogen flow is 19000~20000sccm, and oxygen flow is 700~1200sccm, oxygen
The change time is 200~300s.
Invention further provides a kind of phosphorus diffusion method of Physical Metallurgy polysilicon solar cell, including, 1) will
Silicon chip after cleaning and texturing carries out constant temperature heat treatment；2) by through step 1) treatment after silicon chip carry out oxidation processes；3) to step
2) the logical phosphorus source of silicon chip after processing carries out phosphorus diffusion process；4) by through step 3) treatment after silicon chip made annealing treatment；Wherein,
The step 3) phosphorus diffusion process include the first DIFFUSION TREATMENT and the second DIFFUSION TREATMENT, first DIFFUSION TREATMENT include low temperature
Pre-deposition step and heating step；Second DIFFUSION TREATMENT includes a) low temperature depositing；B) heat up propulsion；C) it is redeposited；D) it is high
Temperature propulsion；E) high temperature redistribution.
According to an embodiment of the present invention, first DIFFUSION TREATMENT includes：
In 770~790 DEG C, lead to big nitrogen, oxygen to the silicon chip and take the small nitrogen in source, big nitrogen flow be 20000~
21000sccm, oxygen flow is 200~350sccm, takes the small nitrogen flow in source for 300~450sccm, and the time is 60~150s；And
In 790~810 DEG C, to leading to big nitrogen and oxygen through the silicon chip after above-mentioned treatment, big nitrogen flow is 20000~
21000sccm, oxygen flow is 200~400sccm, and the time is 90~220s.
Another implementation method of the invention, second DIFFUSION TREATMENT includes：
A) in 790~810 DEG C, to through the silicon chip after first DIFFUSION TREATMENT leading to big nitrogen, oxygen and take the small nitrogen in source, big nitrogen
Flow is 22000~24000sccm, and oxygen flow is 600~1000sccm, takes the small nitrogen flow in source for 900~1100sccm, when
Between be 200~400s；
B) in 810~830 DEG C, big nitrogen being led to the silicon chip after being processed through step a), big nitrogen flow is 20000~
22000sccm, the time is 200~400s；
C) in 810~830 DEG C, lead to big nitrogen, oxygen to the silicon chip after being processed through step b) and take the small nitrogen in source, big nitrogen flow is
22000~24000sccm, oxygen flow is 700~1100sccm, takes the small nitrogen flow in source for 900~1400sccm, and the time is
200~400s；
D) in 830~850 DEG C, big nitrogen being led to the silicon chip after being processed through step c), big nitrogen flow is 20000~
22000sccm, the time is 200~400s；
E) in 830~850 DEG C, lead to big nitrogen, oxygen to the silicon chip after being processed through step d) and take the small nitrogen in source, big nitrogen flow is
22000~24000sccm, oxygen flow is 700~1100sccm, takes the small nitrogen flow in source for 900~1400sccm, and the time is
400~700s.
Method of diffusion of the invention is applied in the preparation of Physical Metallurgy silicon solar cell, cost-effective, improves production capacity, institute's shape
Into PN junction, surface impurity concentration is low, and Impurity Distribution is uniform, and diffusion uniformity preferably, reduces dead layer effect, is conducive to electronics
Collection, reduce solar cell because be combined caused by loss in efficiency, so as to improve cell piece final opto-electronic conversion imitate
Rate.And also help the situation that the battery crystal structure caused due to high temperature is deteriorated that improves.
Brief description of the drawings
Fig. 1 is the flow chart of the phosphorus diffusion method of the Physical Metallurgy polysilicon solar cell of an embodiment of the present invention.
Specific embodiment
Embodying feature of present invention will describe in detail in the following description with the exemplary embodiments of advantage.It should be understood that this
Invention can have various changes in different embodiments, and it is neither departed from the scope of the present invention, and it is therein explanation and
Diagram is treated as purposes of discussion in itself, and is not used to the limitation present invention.Wherein, as diluent gas when big nitrogen refers to diffusion
Pure nitrogen gas；The small nitrogen in source is taken, refers to the nitrogen that phosphorus source is carried by phosphorus source bottle；Dry-oxygen oxidation, be using the pure oxygen of drying as
Oxidizing atmosphere, at high temperature oxygen directly with pasc reaction generate silica.
The invention provides a kind of phosphorus diffusion method of Physical Metallurgy polysilicon solar cell, including, 1) cleaning is made
Silicon chip after suede carries out the first constant temperature heat treatment；2) by through step 1) treatment after silicon chip carry out the second constant temperature heat treatment；3) will
Through step 2) treatment after silicon chip carry out oxidation processes；4) to step 3) the logical phosphorus source of silicon chip after treatment carries out phosphorus diffusion process；
5) by through step 4) treatment after silicon chip made annealing treatment.
In one embodiment of the present invention, step 3) phosphorus diffusion process include at the first DIFFUSION TREATMENT and the second diffusion
Reason.
Method of diffusion of the invention adds two step constant temperature heat treatment technics of optimization, can be with very effective control diffusion furnace
The fluctuation of each warm area temperature, shortens constant temperature time, improves yield, and to diffused sheet resistance uniformity and cell piece conversion efficiency
All it is greatly improved.
As shown in figure 1, the phosphorus diffusion method of the Physical Metallurgy polysilicon solar cell of an embodiment of the present invention, will be clear
Wash clean and make matte Physical polysilicon chip be placed on diffusion furnace in be diffused, specific steps include：
Enter boat
Silicon chip after cleaning and texturing enters in diffusion furnace, is passed through greatly to the air inlet pipe of diffusion furnace during silicon chip enters boat
Nitrogen, big nitrogen flow is 22000~27000sccm, enters the boat time for 500~700s.
Constant temperature is heat-treated
First constant temperature is heat-treated：Each warm area temperature of diffusion furnace is set in 670~820 DEG C, keeps logical in thermostatic process
Enter big nitrogen, big nitrogen flow is 19000~20000sccm, and the heating-up time is 200~400s.
Second constant temperature is heat-treated：Each warm area temperature of diffusion furnace is set in 770~820 DEG C, to being passed through big nitrogen in diffusion furnace,
Big nitrogen flow is 19000~20000sccm, and the heating-up time is 180~360s.
Dry-oxygen oxidation
The temperature for keeping diffusion furnace is 770~820 DEG C, and to big nitrogen and dry oxygen is passed through in diffusion furnace, big nitrogen flow is 19000
~20000sccm, oxygen flow is 700~1200sccm, and oxidization time is 200~300s.
Prediffusion
Low temperature pre-deposition：The temperature for keeping diffusion furnace is 770~790 DEG C, to being passed through big nitrogen, oxygen in diffusion furnace and take
The small nitrogen in source；Big nitrogen flow is 20000~21000sccm, and oxygen flow is 200~350sccm, small nitrogen flow is 300~
450sccm, the low temperature pre-deposition time is 60~150s.
Heat up：Diffusion furnace is warming up to 790~810 DEG C, to being passed through big nitrogen and oxygen in diffusion furnace；Big nitrogen flow is
20000~22000sccm, oxygen flow is 200~400sccm, and the time is 90~220s.
Diffusion
Low temperature depositing：The temperature for keeping diffusion furnace is 790~810 DEG C, to being passed through big nitrogen, oxygen in diffusion furnace and take source
Small nitrogen；Big nitrogen flow is 22000~24000sccm, and oxygen flow is 600~1000sccm, small nitrogen flow is 900~
1100sccm, sedimentation time is 200~400s.
Heat up propulsion：Diffusion furnace is warming up to 810~830 DEG C, to being passed through big nitrogen in diffusion furnace；Big nitrogen flow is 20000~
22000sccm, the time is 200~400s.
It is redeposited：The temperature for keeping diffusion furnace is 810~830 DEG C, to being passed through big nitrogen, dry oxygen in diffusion furnace and to take source small
Nitrogen；Big nitrogen flow is 22000~24000sccm, and oxygen flow is 700~1100sccm, small nitrogen flow is 900~
1400sccm, the redeposited time is 200~400s.
High temperature is advanced：Diffusion furnace is warming up to 835~850 DEG C, to being passed through big nitrogen in diffusion furnace；Big nitrogen flow is 20000~
22000sccm, the time is 200~400s.
High temperature is redistributed：The temperature for keeping diffusion furnace is 835~850 DEG C, to being passed through big nitrogen, dry oxygen in diffusion furnace and take
The small nitrogen in source；Big nitrogen flow is 22000~24000sccm, and oxygen flow is 700~1100sccm, small nitrogen flow is 900~
1400sccm, the time is 400~700s.
Cooling annealing
In 680~730 DEG C, stop it is logical takes the small nitrogen in source and oxygen, continue to lead to big nitrogen, big nitrogen flow is 22500~
24500sccm, annealing time is 1500~1800s.
Go out boat
Big nitrogen is passed through in continuing to stove during silicon chip releases diffusion furnace；Big nitrogen flow is 22000~27000sccm,
Go out the boat time for 500~640s.
Method of diffusion of the invention is applied in the preparation of Physical Metallurgy silicon solar cell, can pass through changing for diffusion technique parameter
Become, square resistance is 65~100 Ω after making diffusion, cost-saved, production capacity is improved, with good result.The PN junction for being formed,
Surface impurity concentration is low, and Impurity Distribution is uniform, and diffused sheet resistance uniformity preferably, reduces dead layer effect, is conducive to the receipts of electronics
Collection, reduces loss in efficiency of the solar cell caused by being combined, so as to improve the final photoelectric transformation efficiency of cell piece.And
And the situation that the battery crystal structure caused due to high temperature is deteriorated that improves is also helped, reduce battery optical attenuation.
In one embodiment of the present invention, application two step constant temperature and two step prediffusion technologies before diffusion.
Diffusion starts preceding in order to stablize each warm area temperature, shortening constant temperature time, raising yield, by existing step constant temperature
It is changed into two step constant temperature.As needed the first step constant temperature setting each warm area temperature it is lower than final thermostat temperature, and exist compared with
Big difference, resets second step thermostat temperature, and each warm area temperature difference is smaller, the temperature for making full use of temperature-rise period to produce
Drift, makes each warm area temperature reach stable state in a short time, therefore constant temperature time is greatly shortened, and has not only saved electricity
Can, and production capacity raising.
Prediffusion is divided into two steps is carried out, and on the one hand can form one layer of prediffusion layer improves battery surface oxidation Rotating fields；
On the other hand it also avoid spreading the gas containing phosphorus source for starting rear silicon chip surface directly contact big flow, form non-equilibrium diffusion table
Face and influence the uniformity of follow-up diffused sheet resistance.
Start normally to diffuse to form PN junction after the completion of prediffusion, normal diffusion point multistep is carried out, and final step is high-temperature constant
Determine phosphorus source diffusion redistribution, improve the phosphorus concentration of surface N-type layer, the top thin layer in battery surface N areas is formed heavy doping N+
Layer.N+Layer can effectively ensure that battery surface forms good Ohmic contact with silver electrode, reduce the series resistance of battery, improve electricity
The short circuit current in pond.
Additionally, method of diffusion of the invention, reduces the usage amount of nitrogen, POCl3 and dry oxygen, when shortening technique
Between, save production cost.
Below, the phosphorus diffusion method of Physical Metallurgy polysilicon solar cell of the invention done in conjunction with specific embodiments into
One step explanation.Wherein, the silicon chip that each embodiment is used all is p-type Physical Metallurgy polysilicon chip, and resistivity is 0.6~3.0 Ω
cm。
Comparative example
After being optimized to conventional diffusion technique as a comparison case, 400 Physical Metallurgy polysilicon chips of matte will be made
Being placed on after cleaning up in diffusion furnace carries out shield and dissipates, and diffusion target sheet resistance is 85 Ω, specifically includes following steps：
Enter boat
Silicon chip after making herbs into wool enters in diffusion furnace, is passed through big nitrogen to the air inlet pipe of diffusion furnace during silicon chip enters boat, greatly
Nitrogen flow is 24000sccm, enters the boat time for 640s；
Constant temperature
The temperature of each warm area in quartz ampoule is set as：815 DEG C of fire door, 2 810 DEG C of warm area, 3 806 DEG C of warm area, warm area four
804 DEG C, 802 DEG C of stove tail, keep being passed through big nitrogen in thermostatic process, and big nitrogen flow is 22000sccm, and constant temperature time is 660s.
Dry-oxygen oxidation
It is 805~815 DEG C to keep diffusion furnace each warm area temperature, and to being passed through big nitrogen and dry oxygen in diffusion furnace, big nitrogen flow is
20000sccm, oxygen flow is 900sccm, and oxidization time is 350s.
Diffusion
TongYuan deposits：It is 805~815 DEG C to keep diffusion furnace each warm area temperature, to be passed through in diffusion furnace big nitrogen, oxygen and
The small nitrogen in source is taken, big nitrogen flow is 27400sccm, and oxygen flow is 1050sccm, and small nitrogen flow is 1280sccm, and sedimentation time is
1300s。
Heat up propulsion：To 845~860 DEG C, stopping is passed through the small nitrogen in the source of taking and dry oxygen to each temperature-raising region temperature raising of diffusion furnace, continues to expansion
Big nitrogen is passed through in scattered stove, big nitrogen flow is 20000sccm, and the time is 800s.
Cooling annealing
The temperature of diffusion furnace is down to 730 DEG C, and to big nitrogen is passed through in diffusion furnace, big nitrogen flow is 23000sccm, annealing time
It is 1800s.
Go out boat
Big nitrogen is passed through in continuing to stove during silicon chip releases diffusion furnace, big nitrogen flow is 23000sccm, goes out the boat time
It is 550s.
Embodiment 1
Using the two steps constant temperature technology of the invention after optimization on the basis of traditional handicraft comparative example, as embodiment 1,
To make matte 400 Physical Metallurgy polysilicon chips clean up after be placed in diffusion furnace and carry out shield and dissipate, spread target side
It is 85 Ω to hinder, and specifically includes following steps：
Enter boat
Silicon chip after making herbs into wool enters in diffusion furnace, is passed through big nitrogen to the air inlet pipe of diffusion furnace during silicon chip enters boat, greatly
Nitrogen flow is 24000sccm, enters the boat time for 640s；
Constant temperature is heat-treated
First constant temperature is heat-treated：The temperature of each warm area in quartz ampoule is set as：815 DEG C of fire door, 2 740 DEG C of warm area, temperature
3 730 DEG C of area, 4 710 DEG C of warm area, 805 DEG C of stove tail；Keep being passed through big nitrogen in thermostatic process；Big nitrogen flow is 20000sccm,
Constant temperature time is 300s.
Second constant temperature is heat-treated：The temperature of each warm area in quartz ampoule is set as：815 DEG C of fire door, 2 813 DEG C of warm area, temperature
3 812 DEG C of area, 4 810 DEG C of warm area, 810 DEG C of stove tail；Keep being passed through big nitrogen in thermostatic process；Big nitrogen flow is 20000sccm,
Constant temperature time is 200s；
Dry-oxygen oxidation
It is 810~815 DEG C to keep diffusion furnace each warm area temperature, and to being passed through big nitrogen and dry oxygen in diffusion furnace, big nitrogen flow is
20000sccm, oxygen flow is 900sccm, and oxidization time is 350s.
Diffusion
TongYuan deposits：It is 810~815 DEG C to keep diffusion furnace each warm area temperature, to be passed through in diffusion furnace big nitrogen, oxygen and
The small nitrogen in source is taken, big nitrogen flow is 27400sccm, and oxygen flow is 1050sccm, and small nitrogen flow is 1280sccm, and sedimentation time is
1300s。
Heat up propulsion：To 845~860 DEG C, stopping is passed through the small nitrogen in the source of taking and dry oxygen to each temperature-raising region temperature raising of diffusion furnace, continues to expansion
Big nitrogen is passed through in scattered stove, big nitrogen flow is 20000sccm, and the time is 800s.
Cooling annealing
The temperature of diffusion furnace is down to 730 DEG C, and to big nitrogen is passed through in diffusion furnace, big nitrogen flow is 23000sccm, annealing time
It is 1800s.
Go out boat
Big nitrogen is passed through in continuing to stove during silicon chip releases diffusion furnace, big nitrogen flow is 23000sccm, goes out the boat time
It is 550s.
Embodiment 2
Diffusing step of the invention is individually used on the basis of traditional handicraft comparative example, as embodiment 2, matte will be made
400 Physical Metallurgy polysilicon chips clean up after be placed in diffusion furnace and carry out shield and dissipate, diffusion target sheet resistance is 85 Ω, tool
Body is comprised the following steps：
Enter boat
Silicon chip after making herbs into wool enters in diffusion furnace, is passed through big nitrogen to the air inlet pipe of diffusion furnace during silicon chip enters boat, greatly
Nitrogen flow is 24000sccm, enters the boat time for 640s；
Constant temperature
The temperature of each warm area in quartz ampoule is set as：790 DEG C of fire door, 2 788 DEG C of warm area, 3 786 DEG C of warm area, warm area four
785 DEG C, 785 DEG C of stove tail, keep being passed through big nitrogen in thermostatic process, and big nitrogen flow is 22000sccm, and constant temperature time is 660s.
Dry-oxygen oxidation
It is 785~790 DEG C to keep diffusion furnace each warm area temperature, and to being passed through big nitrogen and dry oxygen in diffusion furnace, big nitrogen flow is
20000sccm, oxygen flow is 900sccm, and oxidization time is 350s.
Prediffusion
Low temperature pre-deposition：It is 785~790 DEG C to keep diffusion furnace each warm area temperature, to be passed through in diffusion furnace big nitrogen, oxygen with
And the small nitrogen in source is taken, big nitrogen flow is 20000sccm, and oxygen flow is 260sccm, and small nitrogen flow is 300sccm, low temperature pre-deposition
Time is 90s.
Heat up：Each temperature-raising region temperature raising of diffusion furnace to 800~802 DEG C, to being passed through big nitrogen and oxygen, big nitrogen flow in diffusion furnace
It is 20000sccm, oxygen flow is 200sccm, and the time is 200s.
Diffusion
Low temperature depositing：It is 800~802 DEG C to keep diffusion furnace each warm area temperature, to be passed through in diffusion furnace big nitrogen, oxygen and
The small nitrogen in source is taken, big nitrogen flow is 22000sccm, and oxygen flow is 780sccm, and small nitrogen flow is 1100sccm, and sedimentation time is
320s。
Heat up propulsion：To 820~823 DEG C, to being passed through big nitrogen in diffusion furnace, big nitrogen flow is each temperature-raising region temperature raising of diffusion furnace
20000sccm, the time is 280s.
It is redeposited：It is 820~823 DEG C to keep diffusion furnace each warm area temperature, to being passed through big nitrogen, dry oxygen in diffusion furnace and take
The small nitrogen in source, big nitrogen flow is 22000sccm, and oxygen flow is 800sccm, and small nitrogen flow is 1220sccm, and the redeposited time is
290s。
High temperature is advanced：To 845~848 DEG C, to being passed through big nitrogen in diffusion furnace, big nitrogen flow is each temperature-raising region temperature raising of diffusion furnace
20000sccm, the time is 300s.
High temperature is redistributed：It is 845~848 DEG C to keep diffusion furnace each warm area temperature, to be passed through in diffusion furnace big nitrogen, dry oxygen with
And take the small nitrogen in source, big nitrogen flow is 22000sccm, and oxygen flow is 810sccm, and small nitrogen flow is 1250sccm, and the time is
450s。
Cooling annealing
The temperature of diffusion furnace is down to 730 DEG C, and to big nitrogen is passed through in diffusion furnace, big nitrogen flow is 23000sccm, annealing time
It is 1800s.
Go out boat
Big nitrogen is passed through in continuing to stove during silicon chip releases diffusion furnace, big nitrogen flow is 23000sccm, goes out the boat time
It is 550s.
Embodiment 3
To make matte 400 Physical Metallurgy polysilicon chips clean up after be placed in diffusion furnace and carry out shield and dissipate, expand
It is 75 Ω to dissipate target sheet resistance, specifically includes following steps：
Enter boat
Silicon chip after making herbs into wool enters in diffusion furnace, is passed through big nitrogen to the air inlet pipe of diffusion furnace during silicon chip enters boat, greatly
Nitrogen flow is 23000sccm, enters the boat time for 640s.
Constant temperature
First constant temperature is heat-treated：The temperature of each warm area in quartz ampoule is set as：785 DEG C of fire door, 2 720 DEG C of warm area, temperature
3 710 DEG C of area, 4 670 DEG C of warm area, 783 DEG C of stove tail, keep being passed through big nitrogen in thermostatic process, and big nitrogen flow is 20000sccm,
Constant temperature time is 280s.
Second constant temperature is heat-treated：The temperature of each warm area in quartz ampoule is set as：788 DEG C of fire door, 2 787 DEG C of warm area, temperature
3 785 DEG C of area, 4 785 DEG C of warm area, 785 DEG C of stove tail, keep being passed through big nitrogen in thermostatic process, and big nitrogen flow is 20000sccm,
Constant temperature time is 190s.
Dry-oxygen oxidation
It is 785~788 DEG C to keep diffusion furnace each warm area temperature, and to being passed through big nitrogen and dry oxygen in diffusion furnace, big nitrogen flow is
20000sccm, oxygen flow is 800sccm, and oxidization time is 240s.
Prediffusion
Low temperature pre-deposition：It is 785~788 DEG C to keep diffusion furnace each warm area temperature, to be passed through in diffusion furnace big nitrogen, oxygen with
And the small nitrogen in source is taken, big nitrogen flow is 20000sccm, and oxygen flow is 260sccm, and small nitrogen flow is 300sccm, low temperature pre-deposition
Time is 90s.
Heat up：Each temperature-raising region temperature raising of diffusion furnace to 800~802 DEG C, to being passed through big nitrogen and oxygen, big nitrogen flow in diffusion furnace
It is 20000sccm, oxygen flow is 200sccm, and the time is 200s.
Diffusion
Low temperature depositing：It is 800~802 DEG C to keep diffusion furnace each warm area temperature, to be passed through in diffusion furnace big nitrogen, oxygen and
The small nitrogen in source is taken, big nitrogen flow is 22000sccm, and oxygen flow is 780sccm, and small nitrogen flow is 1100sccm, and sedimentation time is
320s。
Heat up propulsion：To 820~823 DEG C, to being passed through big nitrogen in diffusion furnace, big nitrogen flow is each temperature-raising region temperature raising of diffusion furnace
20000sccm, the time is 280s.
It is redeposited：It is 820~823 DEG C to keep diffusion furnace each warm area temperature, to being passed through big nitrogen, dry oxygen in diffusion furnace and take
The small nitrogen in source, big nitrogen flow is 22000sccm, and oxygen flow is 800sccm, and small nitrogen flow is 1220sccm, and the redeposited time is
290s。
High temperature is advanced：To 845~848 DEG C, to being passed through big nitrogen in diffusion furnace, big nitrogen flow is each temperature-raising region temperature raising of diffusion furnace
20000sccm, the time is 300s.
High temperature is redistributed：It is 845~848 DEG C to keep diffusion furnace each warm area temperature, to be passed through in diffusion furnace big nitrogen, dry oxygen with
And take the small nitrogen in source, big nitrogen flow is 22000sccm, and oxygen flow is 810sccm, and small nitrogen flow is 1250sccm, and the time is
450s。
Cooling annealing
The temperature of diffusion furnace is down to 730 DEG C, and to big nitrogen is passed through in diffusion furnace, big nitrogen flow is 23000sccm, annealing time
It is 1800s.
Go out boat
Big nitrogen is passed through in continuing to stove during silicon chip releases diffusion furnace, big nitrogen flow is 23000sccm, goes out the boat time
It is 550s.
Embodiment 4
To make matte 400 Physical Metallurgy polysilicon chips clean up after be placed in diffusion furnace and carry out shield and dissipate, expand
It is 85 Ω to dissipate target sheet resistance, specifically includes following steps：
Enter boat
Silicon chip after making herbs into wool enters in diffusion furnace, is passed through big nitrogen to the air inlet pipe of diffusion furnace during silicon chip enters boat, greatly
Nitrogen flow is 24000sccm, enters the boat time for 640s；
Constant temperature
First constant temperature is heat-treated：The temperature of each warm area in quartz ampoule is set as：788 DEG C of fire door, 2 720 DEG C of warm area, temperature
3 700 DEG C of area, 4 725 DEG C of warm area, 783 DEG C of stove tail, keep being passed through big nitrogen in thermostatic process, and big nitrogen flow is 20000sccm,
Constant temperature time is 270s.
Second constant temperature is heat-treated：The temperature of each warm area in quartz ampoule is set as：790 DEG C of fire door, 2 788 DEG C of warm area, temperature
3 785 DEG C of area, 4 785 DEG C of warm area, 785 DEG C of stove tail, keep being passed through big nitrogen in thermostatic process, and big nitrogen flow is 20000sccm,
Constant temperature time is 220s.
Dry-oxygen oxidation
It is 785~790 DEG C to keep diffusion furnace each warm area temperature, and to being passed through big nitrogen and dry oxygen in diffusion furnace, big nitrogen flow is
20000sccm, oxygen flow is 800sccm, and oxidization time is 240s.
Prediffusion
Low temperature pre-deposition：It is 785~790 DEG C to keep diffusion furnace each warm area temperature, to be passed through in diffusion furnace big nitrogen, oxygen with
And the small nitrogen in source is taken, big nitrogen flow is 20000sccm, and oxygen flow is 260sccm, and small nitrogen flow is 300sccm, low temperature pre-deposition
Time is 100s.
Heat up：Each temperature-raising region temperature raising of diffusion furnace to 802~806 DEG C, to being passed through big nitrogen and oxygen, big nitrogen flow in diffusion furnace
It is 20000sccm, oxygen flow is 200sccm, and the time is 200s.
Diffusion
Low temperature depositing：It is 802~806 DEG C to keep diffusion furnace each warm area temperature, to be passed through in diffusion furnace big nitrogen, oxygen and
The small nitrogen in source is taken, big nitrogen flow is 22000sccm, and oxygen flow is 780sccm, and small nitrogen flow is 1100sccm, and sedimentation time is
270s。
Heat up propulsion：To 822~826 DEG C, to being passed through big nitrogen in diffusion furnace, big nitrogen flow is each temperature-raising region temperature raising of diffusion furnace
20000sccm, the time is 280s.
It is redeposited：It is 822~828 DEG C to keep diffusion furnace each warm area temperature, to being passed through big nitrogen, dry oxygen in diffusion furnace and take
The small nitrogen in source, big nitrogen flow is 22000sccm, and oxygen flow is 800sccm, and small nitrogen flow is 1220sccm, and the redeposited time is
280s。
High temperature is advanced：To 840~844 DEG C, to being passed through big nitrogen in diffusion furnace, big nitrogen flow is each temperature-raising region temperature raising of diffusion furnace
20000sccm, the time is 280s.
High temperature is redistributed：It is 840~844 DEG C to keep diffusion furnace each warm area temperature, to be passed through in diffusion furnace big nitrogen, dry oxygen with
And take the small nitrogen in source, big nitrogen flow is 22000sccm, and oxygen flow is 810sccm, and small nitrogen flow is 1250sccm, and the time is
430s。
Cooling annealing
The temperature of diffusion furnace is down to 730 DEG C, and to big nitrogen is passed through in diffusion furnace, big nitrogen flow is 23000sccm, annealing time
It is 1800s.
Go out boat
Big nitrogen is passed through in continuing to stove during silicon chip releases diffusion furnace, big nitrogen flow is 23000sccm, goes out the boat time
It is 550s.
Silicon chip after comparative example and embodiment 1 to 4 are spread carries out square resistance test, and specific data are shown in Table 1.Meanwhile,
Silicon chip after embodiment 1 to 4 and comparative example diffusion, the method according to prior art are used to prepare specification 156mm × 156mm's
Physical Metallurgy polycrystal silicon cell, the performance parameter test of obtained battery the results are shown in Table 2.
Table 1
Table 2
| Voc(V) | Isc(A) | Rs(mΩ) | Rsh(Ω) | FF (%) | Ncel (%) | |
| Comparative example | 0.624 | 8.38 | 2.28 | 76.4 | 78.35 | 17.12 |
| Embodiment 1 | 0.626 | 8.39 | 1.89 | 78.7 | 79.42 | 17.20 |
| Embodiment 2 | 0.627 | 8.45 | 1.70 | 81.8 | 79.99 | 17.42 |
| Embodiment 3 | 0.626 | 8.50 | 1.63 | 82.5 | 80.09 | 17.52 |
| Embodiment 4 | 0.630 | 8.53 | 1.78 | 52.5 | 79.77 | 17.64 |
Be can be seen that compared with comparative example traditional handicraft with reference to the data of comparative example and embodiment 1 in table 1,2, the present invention
Using after two step constant temperature steps, constant temperature time can substantially shorten embodiment 1, after diffusion between square resistor disc in uniformity and piece
Uniformity is obtained for and is obviously improved, and battery efficiency also increases.
The as shown by data of comparative example and embodiment 2 in table 1,2, compared with comparative example traditional handicraft, the embodiment of the present invention 2 is adopted
Spread with multistep, although square resistance homogeneity and being not improved after diffusion, battery efficiency is but significantly improved.And tie
Close specific process parameter to can be seen that under diffused sheet resistance same case, after diffusing step is divided into multistep, it is possible to reduce trichlorine
Oxygen phosphorus and dry oxygen usage amount, it is cost-effective.
The data explanation of comparative example and embodiment 3,4, permanent using two step of the invention compared with traditional handicraft in table 1,2
Monolithic sheet resistance difference is can be controlled within 8% after temperature and diffusion technique, and sheet resistance difference is greatly improved within 5% between piece
The uniformity of diffused sheet resistance.Make open-circuit voltage (Voc) average value of the efficient physical metallurgy polycrystalline silicon solar cell of production from original
0.624~the 0.625V for coming brings up to more than 0.626V, and short circuit current (Isc) average value is improved from 8.30 original~8.40A
To more than 8.45A, ensureing sintering circuit under normal circumstances, cell series resistance (Rs) is average from 2.2~2.4m Ω, is reduced to
1.6~1.8m Ω, the fill factor, curve factor (FF) of battery close to 80%, average conversion efficiency from 17.10% or so original raising to
More than 17.4%.
Unless limited otherwise, term used herein is the implication that those skilled in the art are generally understood that.
Implementation method described in the invention is not used to limit the scope of the invention merely for exemplary purpose,
Those skilled in the art can be made within the scope of the invention various other replacements, changes and improvements, thus, the invention is not restricted to
Above-mentioned implementation method, and be only defined by the claims.
Claims (7)
1. a kind of phosphorus diffusion method of Physical Metallurgy polysilicon solar cell, including,
1) silicon chip after cleaning and texturing is carried out into the first constant temperature heat treatment；
2) by through step 1) treatment after silicon chip carry out the second constant temperature heat treatment；
3) by through step 2) treatment after silicon chip carry out oxidation processes；
4) to step 3) the logical phosphorus source of silicon chip after treatment carries out phosphorus diffusion process；The phosphorus diffusion process includes the first DIFFUSION TREATMENT
With the second DIFFUSION TREATMENT, first DIFFUSION TREATMENT include low temperature pre-deposition step and heating step, second DIFFUSION TREATMENT
Including：
A) in 790~810 DEG C, to through the silicon chip after first DIFFUSION TREATMENT leading to big nitrogen, oxygen and take the small nitrogen in source, big nitrogen flow
It is 22000~24000sccm, oxygen flow is 600~1000sccm, takes the small nitrogen flow in source for 900~1100sccm, the time is
200~400s；
B) in 810~830 DEG C, big nitrogen is led to the silicon chip after being processed through step a), big nitrogen flow is 20000~22000sccm, when
Between be 200~400s；
C) in 810~830 DEG C, lead to big nitrogen, oxygen to the silicon chip after being processed through step b) and take the small nitrogen in source, big nitrogen flow is
22000~24000sccm, oxygen flow is 700~1100sccm, takes the small nitrogen flow in source for 900~1400sccm, and the time is
200~400s；
D) in 830~850 DEG C, big nitrogen is led to the silicon chip after being processed through step c), big nitrogen flow is 20000~22000sccm, when
Between be 200~400s；
E) in 830~850 DEG C, lead to big nitrogen, oxygen to the silicon chip after being processed through step d) and take the small nitrogen in source, big nitrogen flow is
22000~24000sccm, oxygen flow is 700~1100sccm, takes the small nitrogen flow in source for 900~1400sccm, and the time is
400~700s；
5) by through step 4) treatment after silicon chip made annealing treatment.
2. method according to claim 1, first DIFFUSION TREATMENT includes：
In 770~790 DEG C, lead to big nitrogen, oxygen to the silicon chip and take the small nitrogen in source, big nitrogen flow is 20000~21000sccm,
Oxygen flow is 200~350sccm, takes the small nitrogen flow in source for 300~450sccm, and the time is 60~150s；And
In 790~810 DEG C, to big nitrogen and oxygen is led to through the silicon chip after above-mentioned treatment, big nitrogen flow is 20000~21000sccm,
Oxygen flow is 200~400sccm, and the time is 90~220s.
3. method according to claim 1, wherein first constant temperature heat treatment includes, in 670~820 DEG C, to described
Silicon chip leads to big nitrogen, and big nitrogen flow is 19000~20000sccm, and the time is 200~400s.
4. method according to claim 1, wherein second constant temperature heat treatment includes, in 770~820 DEG C, Xiang Jingsuo
The silicon chip for stating the heat treatment of the first constant temperature leads to big nitrogen, and big nitrogen flow is 19000~20000sccm, and the time is 180~360s.
5. method according to claim 1, wherein the step 3) include, in 770~820 DEG C, at through the second constant temperature
The silicon chip of reason leads to big nitrogen and dry oxygen, and big nitrogen flow is 19000~20000sccm, and oxygen flow is 700~1200sccm, oxidation
Time is 200~300s.
6. a kind of phosphorus diffusion method of Physical Metallurgy polysilicon solar cell, including,
1) silicon chip after cleaning and texturing is carried out into constant temperature heat treatment；
2) by through step 1) treatment after silicon chip carry out oxidation processes；
3) to step 2) the logical phosphorus source of silicon chip after treatment carries out phosphorus diffusion process；
4) by through step 3) treatment after silicon chip made annealing treatment；
Wherein, the step 3) phosphorus diffusion process include the first DIFFUSION TREATMENT and the second DIFFUSION TREATMENT, at first diffusion
Reason includes low temperature pre-deposition step and heating step；Second DIFFUSION TREATMENT includes：
A) in 790~810 DEG C, to through the silicon chip after first DIFFUSION TREATMENT leading to big nitrogen, oxygen and take the small nitrogen in source, big nitrogen flow
It is 22000~24000sccm, oxygen flow is 600~1000sccm, takes the small nitrogen flow in source for 900~1100sccm, the time is
200~400s；
B) in 810~830 DEG C, big nitrogen is led to the silicon chip after being processed through step a), big nitrogen flow is 20000~22000sccm, when
Between be 200~400s；
C) in 810~830 DEG C, lead to big nitrogen, oxygen to the silicon chip after being processed through step b) and take the small nitrogen in source, big nitrogen flow is
22000~24000sccm, oxygen flow is 700~1100sccm, takes the small nitrogen flow in source for 900~1400sccm, and the time is
200~400s；
D) in 830~850 DEG C, big nitrogen is led to the silicon chip after being processed through step c), big nitrogen flow is 20000~22000sccm, when
Between be 200~400s；
E) in 830~850 DEG C, lead to big nitrogen, oxygen to the silicon chip after being processed through step d) and take the small nitrogen in source, big nitrogen flow is
22000~24000sccm, oxygen flow is 700~1100sccm, takes the small nitrogen flow in source for 900~1400sccm, and the time is
400~700s.
7. method according to claim 6, first DIFFUSION TREATMENT includes：
In 770~790 DEG C, lead to big nitrogen, oxygen to the silicon chip and take the small nitrogen in source, big nitrogen flow is 20000~21000sccm,
Oxygen flow is 200~350sccm, takes the small nitrogen flow in source for 300~450sccm, and the time is 60~150s；And
In 790~810 DEG C, to big nitrogen and oxygen is led to through the silicon chip after above-mentioned treatment, big nitrogen flow is 20000~21000sccm,
Oxygen flow is 200~400sccm, and the time is 90~220s.
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| CN107316831B (en) * | 2017-05-15 | 2020-07-10 | 湖南红太阳光电科技有限公司 | Quartz boat and solar cell diffusion process |
| CN107507887B (en) * | 2017-08-25 | 2019-09-20 | 苏州阿特斯阳光电力科技有限公司 | A method of control doping curve conformity |
| CN109616543A (en) * | 2017-09-04 | 2019-04-12 | 通威太阳能（成都）有限公司 | Solar battery sheet diffusion technique |
| CN107946402B (en) * | 2017-10-09 | 2020-08-04 | 东莞南玻光伏科技有限公司 | Solar cell diffusion method |
| CN109103081A (en) * | 2018-07-02 | 2018-12-28 | 浙江启鑫新能源科技股份有限公司 | A kind of diffusion technique of crystal silicon solar energy battery |
| CN114188436B (en) * | 2020-09-15 | 2024-03-15 | 一道新能源科技股份有限公司 | Silicon substrate preparation method and solar cell |
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