CN106087070B - A kind of method of diamond wire silicon chip recrystallization wet-method etching - Google Patents
A kind of method of diamond wire silicon chip recrystallization wet-method etching Download PDFInfo
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Abstract
A kind of method of diamond wire silicon chip recrystallization wet-method etching, includes the following steps：(1) diamond wire silicon chip is sent to the high-temperature region of equipment；(2) silicon chip stops some time in the high-temperature region, and silicon chip surface is heated, and non-crystalline silicon melts, and the main body of silicon chip is non-fusible；(3) after the amorphous silicon layer of the silicon chip surface completes fusing or slightly superfuses, the silicon chip is sent out into the high-temperature region, the silicon chip surface cooling recrystallization forms polycrystalline structure；(4) silicon chip is subjected to wet process acid making herbs into wool.The albedo measurement of complete set solar spectrum is carried out to the silicon chip surface matte, the silicon wafer suede reflectivity is less than the reflectivity in existing common polycrystalline silicon chip acid making herbs into wool face.The present invention is recrystallized by non-crystalline silicon, solves the problems, such as that diamond wire silicon chip directly uses wet process acid making herbs into wool to fail, the low ideal matte of sun light reflectivity has been made, while improving the transfer efficiency of photovoltaic cell, has also reduced the cost of entire photovoltaic generation.
Description
Technical field
The present invention relates to a kind of methods of diamond wire silicon wafer wool making more particularly to a kind of diamond wire silicon chip to recrystallize wet method system
The method of suede.
Background technology
The sustainable development of the energy and environment is one of the problem of mankind most pay close attention to always.Current main stream still with
Based on fossil energy, coal and oil also greatly polluted environment for the survival of mankind while bringing human progress, by
Step changes energy consumption structure, and it is to solve the problems, such as this unique selection to greatly develop cleaning source technology.
Solar energy is inexhaustible with its, nexhaustible and pollution-free etc. exclusive advantage, becomes the focus of new energy.The sun
Can energy utilization, at present for mainly photovoltaic generation, photovoltaic generation be by means of photoelectric conversion device by solar energy turn
It is melted into electric energy, is cleaned since photovoltaic generation has, is pollution-free, transmission is convenient, the advantages that can storing, promotes it in the energy, environment
Sustainable development in occupy an important position.Currently, photovoltaic cell development type it is very much, such as have crystal silicon battery,
Thin-film solar cells, polymer solar battery, perovskite solar cell, wherein crystal silicon solar batteries development most at
It is ripe.
The industrial chain path of crystal silicon battery is：Metallic silicon-HIGH-PURITY SILICON-silicon ingot-silicon chip-cell piece-component-system, wherein
Silicon chip is formed by silicon ingot multi-wire saw, for producing cell piece.Wherein multi-wire saw is the hard mill for bringing joint-cutting into steel wire
Grain carries out silicon ingot to cut effect.Can being divided into free abrasive multi-wire saw cutting by abrasive type, (mortar is cut, and abrasive material is carbonization
Silicon) and the multi-thread saw cut of concretion abrasive (also referred to as diamond wire saw, abrasive material is diamond).Due to the multi-wire saw of free abrasive
Low production efficiency, consumptive material is more and of high cost, and pollutes environment, and the production of solar silicon wafers is gradually to the work of Buddha's warrior attendant wire cutting at present
Skill shifts, therefore the silicon chip of our current Buddha's warrior attendant wire cuttings is referred to as diamond wire silicon chip.
Cell piece is the device for solar energy being converted into electric energy, and the refractive index of crystalline silicon is 3.42, is radiated at
Sunlight on silicon chip is greatly reflected, and silion cell is not high to the utilization rate of sunlight, to make the conversion of battery
Efficiency reduces；Common method is that coarse suede structure is made in silicon chip surface before battery is formed, which can be with
The reflection of battery surface light is reduced to increase light absorption, the transformation efficiency of solar cell can increase.
The usually industrial method using alkali or sour chemical attack modifies wafer topography, makes silicon chip surface
Form rough matte light trapping structure.Wherein polysilicon chip occupies 80% or more market part in crystal silicon battery field
Volume is the mainstream in market, and polysilicon chip is then the method progress making herbs into wool for taking acid corrosion.But common polycrystalline silicon chip is general
The method of wet method acid corrosion making herbs into wool but fails substantially to diamond wire polysilicon chip, is mainly shown as that corrosion is slow, cutting stria without
Method removes.The failure of the acid etch of diamond wire polysilicon chip is related with silicon chip surface characteristic, but the country is to diamond wire polysilicon
The research of piece is less, up to the present, industry also fail to find it is suitable, with the matched inexpensive diamond wire polycrystalline of battery process
The process for etching of silicon chip.
Find that there are the amorphous silicon films of one layer of micron order thickness on its diamond wire wafer sections surface by related experiment, generally
Think that the film is caused by intense plastic strain in mechanical cutting procedure.The amorphous silicon film has the acid etch of wet method bright
Aobvious barrier effect, this also just directly results in diamond wire polysilicon chip during sour making herbs into wool and corrodes uneven, the apparent shape in part
Looks are difficult to change, and cannot reach expected making herbs into wool effect.
Although academia and industrial circle, which are proposed some, may solve the making herbs into wool scheme of diamond wire polysilicon chip, such as sandblasting
Technology, the black silicon technology of wet method and dry plasma technology claim (RIE technologies).But sandblast technology, RIE technologies are both needed to
It is replaced with new etching device, fringe cost is high, and complex process, industrial circle is difficult to receive；And the black silicon technology of wet method is pre-
It is first reacted in silicon chip surface and generates nano-noble metal particle and be used as the catalyst of acid corrosion, although the black silicon making herbs into wool of wet method can be with
Existing wet method equipment compatibility, but the introducing of noble silver virtually increases cost, and also if subsequent processing is improper, pole holds
Metallic pollution easily is caused to cell piece, and then influences transfer efficiency.
Invention content
The technical problem to be solved by the present invention is to overcome drawbacks described above of the existing technology, providing one kind making Buddha's warrior attendant
Line silicon chip is convenient for the method for forming the diamond wire silicon chip recrystallization wet-method etching of good light trapping structure, can be made using this method
Sun light reflectivity is less than the matte of traditional silicon chip, to improve the absorption efficiency of light, improves the opto-electronic conversion effect of photovoltaic cell
Rate.
The technical solution adopted by the present invention to solve the technical problems is：A kind of diamond wire silicon chip recrystallization wet-method etching
Method includes the following steps：
(1) diamond wire silicon chip is sent to the high-temperature region of equipment；Hot-zone with 2 different temperatures sections in equipment, respectively
For preheating zone, high-temperature region, the temperature of the high-temperature region is less than the fusing point of crystalline silicon；
(2) the diamond wire silicon chip of step (1) is stopped into some time, the diamond wire silicon chip surface in the high-temperature region
Heated, amorphous layer melts, and the main body of the diamond wire silicon chip is constant；
It (3), will be described after the amorphous silicon layer of the diamond wire silicon chip surface of step (2) completes fusing or slightly superfuses
Diamond wire silicon chip sends out the high-temperature region, and the diamond wire silicon chip surface is cooled down and is recrystallized, and forms polycrystalline structure；
(4) wet process acid making herbs into wool will be carried out after step (3) treated diamond wire silicon chip cooling.
Further, in step (1), the temperature range of the high-temperature region is 600-1400 DEG C；Preferred range is 1000-
1350℃。
Further, in step (2), the diamond wire silicon chip is 10-300 seconds in the high-temperature region residence time；It is preferred that stopping
It is 30-120 seconds to stay the time.
Further, in step (2), the heated mode of the diamond wire silicon chip surface is laser irradiation, microwave heating, resistance
It heats, one kind in infrared heating.
Further, in step (4), it is H that the etchant solution ingredient of the wet process acid making herbs into wool, which presses mol ratio,2O：HF：HNO3=
(2-3):1:(3-3.5), making herbs into wool corrosion reaction temperature are 8-10 DEG C, and the corrosion reaction time is 50-100 seconds.
Further, the diamond wire silicon chip is the solar-grade polysilicon piece of multi-thread Buddha's warrior attendant wire cutting production.
Further, the diamond wire silicon chip goes out pan feeding mode, by the way of high-temperature resistant belt conveyer or film trap, the gold
After rigid line silicon chip surface non-crystalline silicon fusing, infiltration or adhesion are not generated with support plate.
Since non-crystalline silicon does not have complete cell configuration, non-crystalline silicon has many qualitative differences with crystal silicon, especially
It is that fusing point, density and the hardness of non-crystalline silicon is all far below crystal silicon (namely silicon chip itself), it is only golden therefore in technical process
The non-crystalline silicon fusing of rigid line silicon chip surface, and silicon chip itself is without influence.Only so that diamond wire silicon chip surface amorphous layer recrystallizes, shape
At the polycrystalline structure for being conducive to wet method acid corrosion, subsequent polysilicon chip wet process acid making herbs into wool is then carried out；And diamond wire silicon chip
The recrystallization on surface is also a kind of preparation process of light trapping structure.Recrystallize the diamond wire silicon chip of processing and untreated diamond wire
It after silicon wafer wool making, is compared with scanning electron microscope (SEM) photograph, it can be found that treated that silicon chip surface occurs is numerous, uniform for recrystallization
Micro/nano level etch pit, form effective extinction matte, and apparent corruption then occurs in the silicon chip for not recrystallizing processing
Non-uniform phenomenon is lost, making herbs into wool effect has been seriously affected.
Silicon chip prepared by the method for the present invention completes follow-up diffusion, the batteries blade technolgy such as plated film and metallization, and detects
Battery efficiency, there are about 0.1% or so promotions for battery absolute efficiency, are mainly manifested in the promotion of short circuit current, this is mainly
Since absorbing incident light enhances.
Compared with prior art, the present invention has the following advantages：
(1) present invention carries out surface heating recrystallization processing by treating the diamond wire polysilicon chip of making herbs into wool, has melted gold
The amorphous silicon layer of rigid line silicon chip surface, has been cooled into the polysilicon structure consistent with silicon chip substrate so that subsequent wet acid system
Suede can be easy to happen, and so as to which the ideal matte that sun light reflectivity is less than 20% is made, increase the absorption of light, in turn
The photoelectric conversion efficiency of photovoltaic cell can be improved；
(2) present invention is easy to operate, increases only one of a diamond wire silicon chip surface amorphous silicon layer fusing recrystallization
Process, the wet method chain type texturing process compatible with the prior art；Production cost is relatively low, industrialized production easy to implement；And silicon
The recrystallization on piece surface is also a kind of preparation process of light trapping structure, can reach the making herbs into wool requirement of further battery piece.
Description of the drawings
Fig. 1 is that the diamond wire silicon chip surface of the embodiment of the present invention 1 recrystallizes forward and backward Raman spectrogram；
Fig. 2 is the scanning electron microscope (SEM) photograph of matte after the diamond wire silicon chip surface of the embodiment of the present invention 1 recrystallizes；
Fig. 3 is the scanning electron microscope (SEM) photograph of matte after the diamond wire silicon chip surface of the embodiment of the present invention 2 recrystallizes；
Fig. 4 is the scanning electron microscope (SEM) photograph a of the diamond wire silicon wafer suede of the prior art；
Fig. 5 is the scanning electron microscope (SEM) photograph b of the diamond wire silicon wafer suede of the prior art.
Specific implementation mode
Below in conjunction with drawings and the specific embodiments, the invention will be further described.
Embodiment 1
A kind of method of diamond wire silicon chip recrystallization wet-method etching of the present embodiment, includes the following steps：
(1) diamond wire silicon chip is sent to the high-temperature region of equipment；There is preheating warm area temperature to be set as 600 DEG C in equipment,
High-temperature region is set as 1400 DEG C, and cooling zone is set as 500 DEG C；The temperature of the high-temperature region is less than the fusing point (1420 of crystalline silicon
℃)；
(2) the diamond wire silicon chip of step (1) is stopped 10 seconds in the high-temperature region, the diamond wire silicon chip surface
Heated, the heated mode of the diamond wire silicon chip surface is laser irradiation, and amorphous silicon layer melts, and the diamond wire silicon chip
Main body it is non-fusible；
(3) after the amorphous silicon layer of the diamond wire silicon chip surface of step (2) completes fusing, the diamond wire silicon chip is passed
The high-temperature region is sent out, into the cooling zone, the diamond wire silicon chip surface cooling recrystallization forms polysilicon structure；This
It is as shown in Figure 1 that the diamond wire silicon chip surface of embodiment recrystallizes forward and backward Raman spectrogram；
It (4) will treated carries out wet process acid making herbs into wool after the diamond wire silicon chip is cooled to room temperature through step (3)；It is described wet
The etchant solution ingredient of method acid making herbs into wool is H by mol ratio2O：HF：HNO3=2:1:3.5, making herbs into wool corrosion reaction temperature is 8 DEG C,
The corrosion reaction time is 100 seconds.
The diamond wire silicon chip is the solar-grade polysilicon piece of multi-thread Buddha's warrior attendant wire cutting production.
The diamond wire silicon chip goes out pan feeding mode, using high-temperature resistant belt conveyer, the diamond wire silicon chip surface non-crystalline silicon
After fusing, infiltration or adhesion are not generated with support plate.
Fig. 2 is compared with Fig. 4, Fig. 5, it can be found that recrystallization treated that diamond wire silicon chip surface occurs is numerous,
The etch pit of uniform micro/nano level, forms effective extinction matte, and the diamond wire silicon chip for not recrystallizing processing then occurs
The apparent non-uniform phenomenon of corrosion, has seriously affected making herbs into wool effect.
The albedo measurement of D8 complete set solar spectrums is carried out to diamond wire polysilicon chip matte made from the present embodiment, it is described
Silicon wafer suede average reflectance is 18%, less than the reflectivity (20%- of the silicon wafer suede on normal (prior art) production line
21%).Diamond wire polysilicon chip prepared by the present embodiment method is applied to photovoltaic cell：The polysilicon chip is subsequently expanded
It dissipates, the batteries blade technolgy such as plated film, is prepared into complete cell piece, measurement obtains the (prior art work of average cell efficiency 18.38%
The average cell efficiency of industry production is 18.30%), than the photovoltaic cell high conversion efficiency 0.08% of prior art production.
Embodiment 2
The present embodiment is differed only in embodiment 1：
Step (1) preheating warm area temperature is set as 350 DEG C, and high-temperature region is set as 600 DEG C, and cooling zone is set as 300 DEG C；
Step (2) the diamond wire silicon chip stops 300 seconds in high-temperature region, the heated mode of the diamond wire silicon chip surface
For microwave heating；
After the amorphous silicon layer of step (3) the diamond wire silicon chip surface is slightly superfused, the diamond wire silicon chip is sent out
The high-temperature region, into cooling zone；
The etchant solution ingredient of step (4) the wet process acid making herbs into wool is H by mol ratio2O：HF：HNO3=3:1:3, making herbs into wool
Corrosion reaction temperature is 10 DEG C, and the corrosion reaction time is 50 seconds.
The diamond wire silicon chip goes out pan feeding mode, and by the way of film trap, the diamond wire silicon chip surface non-crystalline silicon is molten
After change, infiltration or adhesion are not generated with support plate.
Fig. 3 is compared with Fig. 4, Fig. 5, it can be found that recrystallization treated that diamond wire silicon chip surface occurs is numerous,
The etch pit of uniform micro/nano level, forms effective extinction matte, and the diamond wire silicon chip for not recrystallizing processing then occurs
The apparent non-uniform phenomenon of corrosion, has seriously affected making herbs into wool effect.
The albedo measurement of D8 complete set solar spectrums is carried out to diamond wire polysilicon chip matte made from the present embodiment, it is described
Silicon wafer suede average reflectance is 18.5%, less than the reflectivity (20%- of the silicon wafer suede on normal (prior art) production line
21%).Diamond wire polysilicon chip prepared by the present embodiment method is applied to photovoltaic cell：The polysilicon chip is subsequently expanded
It dissipates, the batteries blade technolgy such as plated film, is prepared into complete cell piece, measurement obtains the (prior art work of average cell efficiency 18.39%
The average cell efficiency of industry production is 18.30%), than the photovoltaic cell high conversion efficiency 0.09% of prior art production.
Remaining is the same as embodiment 1.
Embodiment 3
The present embodiment is differed only in embodiment 1：
Step (1) preheating warm area temperature is set as 500 DEG C, and high-temperature region is set as 1350 DEG C, and cooling zone is set as 450 DEG C；
Step (2) the diamond wire silicon chip stops 30 seconds in high-temperature region, the heated mode of the diamond wire silicon chip surface
For Resistant heating；
The etchant solution ingredient of step (4) the wet process acid making herbs into wool is H by mol ratio2O：HF：HNO3=2.5:1:3.3
Making herbs into wool corrosion reaction temperature is 9 DEG C, and the corrosion reaction time is 75 seconds.
The albedo measurement of D8 complete set solar spectrums is carried out to diamond wire polysilicon chip matte made from the present embodiment, it is described
Silicon wafer suede average reflectance is 17.2%, less than the reflectivity (20%- of the silicon wafer suede on normal (prior art) production line
21%).Diamond wire polysilicon chip prepared by the present embodiment method is applied to photovoltaic cell：The polysilicon chip is subsequently expanded
It dissipates, the batteries blade technolgy such as plated film, is prepared into complete cell piece, measurement obtains the (prior art work of average cell efficiency 18.41%
The average cell efficiency of industry production is 18.30%), than the photovoltaic cell high conversion efficiency 0.11% of prior art production.
Remaining is the same as embodiment 1.
Embodiment 4
The present embodiment is differed only in embodiment 1：
Step (1) preheating warm area temperature is set as 550 DEG C, and high-temperature region is set as 1000 DEG C, and cooling zone is set as 500 DEG C；
Step (2) the diamond wire silicon chip stops 120 seconds in high-temperature region, the heated mode of the diamond wire silicon chip surface
For infrared heating；
The etchant solution ingredient of step (4) the wet process acid making herbs into wool is H by mol ratio2O：HF：HNO3=2.8:1:3.4
Making herbs into wool corrosion reaction temperature is 9 DEG C, and the corrosion reaction time is 80 seconds.
The albedo measurement of D8 complete set solar spectrums is carried out to diamond wire polysilicon chip matte made from the present embodiment, it is described
Silicon wafer suede average reflectance is 17.5%, less than the reflectivity (20%- of the silicon wafer suede on normal (prior art) production line
21%).Diamond wire polysilicon chip prepared by the present embodiment method is applied to photovoltaic cell：The polysilicon chip is subsequently expanded
It dissipates, the batteries blade technolgy such as plated film, is prepared into complete cell piece, measurement obtains the (prior art work of average cell efficiency 18.40%
The average cell efficiency of industry production is 18.30%), than the photovoltaic cell high conversion efficiency 0.10% of prior art production.
Remaining is the same as embodiment 1.
Embodiment 5
The present embodiment is differed only in embodiment 1：
Step (1) preheating warm area temperature is set as 500 DEG C, and high-temperature region is set as 1200 DEG C, and cooling zone is set as 300 DEG C；
Step (2) the diamond wire silicon chip stops 75 seconds in high-temperature region, the heated mode of the diamond wire silicon chip surface
For microwave heating；
The etchant solution ingredient of step (4) the wet process acid making herbs into wool is H by mol ratio2O：HF：HNO3=2:1:3.5, system
Suede corrosion reaction temperature is 10 DEG C, and the corrosion reaction time is 90 seconds.
The albedo measurement of D8 complete set solar spectrums is carried out to diamond wire polysilicon chip matte made from the present embodiment, it is described
Silicon wafer suede average reflectance is 17.8%, less than the reflectivity (20%- of the silicon wafer suede on normal (prior art) production line
21%).Diamond wire polysilicon chip prepared by the present embodiment method is applied to photovoltaic cell：The polysilicon chip is subsequently expanded
It dissipates, the batteries blade technolgy such as plated film, is prepared into complete cell piece, measurement obtains the (prior art work of average cell efficiency 18.42%
The average cell efficiency of industry production is 18.30%), than the photovoltaic cell high conversion efficiency 0.12% of prior art production.
Remaining is the same as embodiment 1.
In summary, the present invention solves the table of diamond wire polysilicon chip by high temperature melting non-crystalline silicon-recrystallization technology
Face amorphous silicon layer hinders the problem of wet method acid corrosion, while good compatibility；Polysilicon wet process acid process for etching suitable for mainstream；
In addition, after being handled by recrystallization, the corrosion of silicon chip surface becomes uniformly mild, and suede structure is consistent, the reflectivity of sunlight
Also it decreases, and then battery efficiency increases.It is calculated according to the transfer efficiency 18.3% of current polysilicon chip battery, it can
The battery conversion efficiency for improving 0.1% or so, by every watt of 2.1 yuan of price, then the price of polycrystalline silicon battery plate can increase by 0.15
Member/piece, while diamond wire microtomy makes 0.40 yuan/piece of the cost reduction of silicon chip, therefore the economic benefit of the present invention again
It is fairly obvious.
The above is only presently preferred embodiments of the present invention, is not imposed any restrictions to the present invention, every according to the present invention
Technical spirit still belongs to technical solution of the present invention to any modification, change and equivalent structure transformation made by above example
Protection domain.
Claims (7)
1. a kind of method of diamond wire silicon chip recrystallization wet-method etching, which is characterized in that include the following steps：
(1) diamond wire silicon chip is sent to the high-temperature region of equipment；The temperature range of the high-temperature region is 1000-1350 DEG C；
(2) by the diamond wire silicon chip of step (1) the high-temperature region stop 10-300 seconds, the diamond wire silicon chip surface by
Heat, amorphous layer melt, and the main body of the diamond wire silicon chip is non-fusible；
(3) after the amorphous silicon layer of the diamond wire silicon chip surface of step (2) being completed fusing or slightly being superfused, by the gold
Rigid line silicon chip sends out the high-temperature region, and the diamond wire silicon chip surface is cooled down and is recrystallized, and forms polycrystalline structure；
(4) wet process acid making herbs into wool will be carried out after step (3) treated diamond wire silicon chip cooling.
2. the method for diamond wire silicon chip recrystallization wet-method etching as described in claim 1, which is characterized in that in step (2), institute
It is 30-120 seconds that diamond wire silicon chip, which is stated, in the high-temperature region residence time.
3. the method for diamond wire silicon chip recrystallization wet-method etching as claimed in claim 1 or 2, which is characterized in that step (2)
In, the heated mode of the diamond wire silicon chip surface is laser irradiation, microwave heating, resistance heating, one kind in infrared heating.
4. the method for the diamond wire silicon chip recrystallization wet-method etching as described in one of claims 1 or 2, which is characterized in that step
(4) in, it is H that the etchant solution ingredient of the wet process acid making herbs into wool, which presses mol ratio,2O：HF：HNO3=(2-3):1:(3-3.5).
5. the method for diamond wire silicon chip recrystallization wet-method etching as claimed in claim 4, which is characterized in that in step (4), institute
The corrosion reaction temperature for stating wet process acid making herbs into wool is 8-10 DEG C.
6. the method for diamond wire silicon chip recrystallization wet-method etching as claimed in claim 4, which is characterized in that in step (4), institute
The corrosion reaction time for stating wet process acid making herbs into wool is 50-100 seconds.
7. the method for the diamond wire silicon chip recrystallization wet-method etching as described in claim 1,2,5 or 6, which is characterized in that described
Diamond wire silicon chip is the solar-grade polysilicon piece of multi-thread Buddha's warrior attendant wire cutting production.
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| CN106087070A (en) | 2016-11-09 |
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