CN101626048A - Low-temperature growth method of silicon quantum dots for solar battery - Google Patents
Low-temperature growth method of silicon quantum dots for solar battery Download PDFInfo
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- CN101626048A CN101626048A CN200910094696A CN200910094696A CN101626048A CN 101626048 A CN101626048 A CN 101626048A CN 200910094696 A CN200910094696 A CN 200910094696A CN 200910094696 A CN200910094696 A CN 200910094696A CN 101626048 A CN101626048 A CN 101626048A
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Abstract
The invention relates to a low-temperature growth method of silicon quantum dots for a solar battery, which belongs to the technical field of silicon quantum dot material. The method comprises the following steps: alternately growing a silicon compound dielectric layer of the stoichiometric proportion and a silicon compound layer containing Si which is several nanometers thick in stoichiometric ratio on a silicon wafer or a quartz sheet or a glass sheet or a stainless steel sheet or high-temperature resistant polymer substrate material at the temperature lower than 450 DEG C by using the plasma chemical vapour deposition (PCVD) technology; carrying out post annealing treatment at the temperature lower than or equal to 550 DEG C by using the rapid photo-thermal annealing technology, so that the residual Si in the silicon compound layer containing Si generates diffusion transfer and solid phase crystallization to form the Si quantum dots, wherein the formed Si quantum dots are arranged in a layered mode, the size of each Si quantum dot is controlled by the thickness of the originally-grown silicon compound layer containing Si, and the density of each Si quantum dot is determined by the content of Si in the original SiN<x> layer containing Si. The invention has the advantages of low depositing temperature, quick speed and good technology controllability and repeatability, thus the uniformity of the grown silicon quantum dot material is good; and the invention is favorable for integrated manufacture and cost reduction of devices.
Description
Technical field:
The present invention relates to a kind of low-temperature growth method of silicon quantum dots for solar battery, belong to silicon quantum dot material technology field.
Background technology:
In order to strengthen the competitiveness with conventional energy resource, high efficiency, low cost and long-life solar cell are the targets that people pursue always.The commercial at present solar cell of using mainly is based on the first generation solar cell of silicon wafer, and it is ripe that this technology has been tending towards, and its photoelectric conversion efficiency is also near physics limit, but its cost is limited by raw material (being silicon wafer) itself day by day.Over the past two decades, the second generation solar cell of based semiconductor thin-film material has obtained flourish.Owing to adopted film deposition techniques, to compare with first generation solar cell, the cost of second generation solar cell significantly reduces, and the gap of the photoelectric conversion efficiency of its photoelectric conversion efficiency and first generation solar cell is day by day dwindled.But along with the maturation of technology, it is more and more littler that the photoelectric conversion efficiency of second generation solar cell improves the space.Theoretical research shows, the theoretical upper limit of the photoelectric conversion efficiency of the unijunction solar cell of standard about 31% (being called the Shochkley-Queisser limit efficiency), and surpassing 90% by the limit of the solar photovoltaic conversion efficient of law of thermodynamics decision, this shows the photoelectric conversion efficiency of the solar cell space that also improves a lot.Based on this, University of New South Wales (University of New South Wales) and U.S. regenerative resource National Laboratory (NREL) have proposed the notion of third generation solar cell respectively.Third generation solar cell combines the advantage of the first generation and second generation solar cell, overcome deficiencies such as first generation solar cell cost is higher, second generation photoelectric conversion efficiency of the solar battery is lower simultaneously, in the photovoltaic market in future, will have good development prospect.
Third generation solar cell has adopted novel nano structural material, and semiconductor-quantum-point material wherein receives much attention.The characteristic size of semiconductor-quantum-point is all comparable or littler with the de Broglie wavelength of electronics on three dimensions, so electronics motion therein is subjected to three-dimensional restriction, and promptly the energy of electronics all is quantized on three dimensions.Geometry and size by the control quantum dot can change its electronic state structure, realize the electricity of quantum dot device and " cutting out " of optical property.The physical characteristic of using relevant quantum dot with third generation solar cell mainly contains three: (1) quantum size effect: quantum dot light absorbing features wavelength is difference with the variation of quantum spot size, the quantum dot that size is little absorbs the sunlight of high-energy scope, the quantum dot that size is big absorbs the sunlight of low-yield scope, helps improving the matching degree of solar cell spectral response and solar spectrum like this; (2) energization transit time: quantum dot is because energy level discrete, the energy changing of its electronics slow than in the bulk semiconductor, thereby, emitting before phonon causes energy loss, might take out high-energy electron; (3) formation of multipotency band: because the coupling between quantum dot, in conduction band and valence band, form little can band (mini-band), utilize little optics that can interband to shift and the process of complexity such as photonic absorption, can improve matching degree with solar spectrum.
For realizing low cost, high efficiency, long-life and eco-friendly target, third generation solar cell requires that its material has that raw material resources is abundant, nontoxic, environmental friendliness, can adopt conventional film deposition techniques to carry out characteristics such as scale large-area preparation.In numerous semi-conducting materials, only silicon (Si) material can satisfy this requirement, and because its relevant device technology is very ripe, therefore can utilize the existing processes basis, reduces the manufacturing cost of solar cell.Based on this, the Si quantum dot is expected to become the core material of third generation solar cell.
The technology of preparing that is suitable for the Si quanta point material that solar cell uses is based on evaporating deposition technique, concrete grammar has two kinds at present: the one, and solid-phase crystallization forms the nanocrystalline quantum dot of Si, the 2nd, gas phase growth in situ Si quantum dot when growing with matrix film in the dielectric film of rich Si.Usually, if adopt first method, then high temperature after annealing (about 1100 ℃) is handled and is absolutely necessary, and this will increase the complexity and the production cost of technology, also may cause the fire damage of solar cell; Second method does not need after annealing to handle, but difficulty is very big, and the controllability of growth course and repeated relatively poor.
Summary of the invention:
The objective of the invention is to overcome the deficiency of prior art, and provide a kind of depositing temperature low, speed is fast, process controllability and good reproducibility, and the low-temperature growth method of the silicon quantum dots for solar battery of the good uniformity of the silicon quantum dot material of being grown.
Technical scheme of the present invention is:
At first using plasma strengthens chemical vapour deposition (CVD) (PECVD) technology, on the selected backing material under＜450 ℃ of temperature conditions the silicon compound (SiO of the stoichiometric proportion of several nanometer thickness of alternating growth
2, Si
3N
4, SiC) silicon compound (SiO of dielectric layer and rich Si
x, SiN
x, Si
1-xC
x) layer; Utilize then photo-thermal annealing (RPTA) technology of the film annealing technology that latest development gets up-fast at low temperatures (≤550 ℃) after annealing handle, make the silicon compound (SiO of rich Si
x, SiN
x, Si
1-xC
x) diffusive migration takes place Si more than needed in the layer, solid phase crystallization forms the Si quantum dot.The Si quantum dot that forms is that stratiform is arranged, and its size is by the silicon compound (SiO of the rich Si of original growth
x, SiN
x, Si
1-xC
x) layer THICKNESS CONTROL, the density of quantum dot is by the SiN of original rich Si
xSi content in the layer determines.
Plasma chemical vapor deposition technique of the present invention is radio frequency plasma or microwave plasma or Ecr plasma or very high frequency plasma enhancing chemical vapour deposition (CVD) (general designation PECVD) technology.
Quick photo-thermal annealing (RPTA) technology of the present invention is meant material is placed in the annealing furnace, utilize the lamp of tungsten halogen lamp or other wavelength that sample is carried out Fast Heating, be incubated certain hour not being higher than under 550 ℃ the equilibrium temperature, temperature retention time is determined according to the quantum dot size and dimension; Use then with the stove natural cooling, or the mode of air-cooled or water-cooled is lowered the temperature.
The invention has the advantages that: depositing temperature is low, has improved the flexibility that substrate is selected, and deposition velocity is fast, process controllability and good reproducibility, and the good uniformity of the Si quanta point material of being grown helps the integrated manufacturing of device and reduces manufacturing cost.
Description of drawings:
Fig. 1 is the schematic diagram of the forming process of Si quantum dot in the quick photo-thermal annealing process.
Embodiment:
The present invention not only limits to the following example.The embodiment of the invention is to adopt radio frequency plasma to strengthen chemical vapour deposition technique to grow with Si in conjunction with quick photo-thermal annealing technology
3N
4Si quanta point material for matrix.The plasma that the present invention also can encourage in different ways (comprising microwave plasma, Ecr plasma, very high frequency plasma) strengthens chemical vapour deposition technique and (comprises SiO in conjunction with quick photo-thermal annealing technology growth different substrates
2And SiC) Si quanta point material.
Embodiment 1:
Adopt radio frequency plasma to strengthen chemical vapour deposition technique, it is the Si sheet of 4 inch thickness 1mm that substrate is selected diameter, the Si that alternating growth 2nm is thick
3N
4The SiN of the rich Si of dielectric layer and 2nm
xLayer, Si
3N
4/ SiN
xDeposition cycle be 40.Sedimentary condition: rf frequency is 13.56MHz, radio-frequency power 60W, and the base vacuum degree reaches 1 * 10
-4Pa, reacting gas are N
2The SiH of dilution
4(gas volume N
2: SiH
41) and NH=1:
3, operating air pressure is 10Pa, depositing temperature is 300 ℃, deposition Si
3N
4During dielectric layer, reaction gas flow is N
2The SiH of dilution
4Be 30sccm (mark condition milliliter per minute), NH
3Be 30sccm, deposition rate 0.2nm/s deposits the SiN of rich Si
xDuring layer, reaction gas flow is N
2The SiH of dilution
4Be 100sccm, NH
3Be 30sccm, deposition rate 0.25nm/s; Film sample is placed in the quick photothermal treatment stove carries out annealing in process, utilize the light source of tungsten halogen lamp as photo-thermal annealing, the high pure nitrogen protection is placed on film sample on the monocrystalline silicon piece of quartzy box in the stove down.Annealing process is: 25 ℃/s of heating rate, and 500 ℃ of annealing temperatures, insulation 30min is then with stove natural cooling (air-cooled or water-cooled).Make Si diffusive migration more than needed, solid phase crystallization forms the Si quantum dot.The silicon quantum dot that present embodiment obtains is a layered arrangement, is shaped as sphere, and particle diameter is 2nm.
Embodiment 2:
Adopt microwave plasma to strengthen chemical vapour deposition technique, substrate is selected 20cm * 20cm, the simple glass sheet of thick 3mm, the SiO that alternating growth 2nm is thick
2The SiN of the rich Si of dielectric layer and 4nm
xLayer, SiO
2/ SiN
xDeposition cycle be 50.Sedimentary condition: rf frequency is 13.56MHz, radio-frequency power 60W, and the base vacuum degree reaches 1 * 10
-4Pa, reacting gas are N
2The SiH of dilution
4(gas volume N
2: SiH
41) and O=1:
2, operating air pressure is 10Pa, depositing temperature is 300 ℃, deposition SiO
2During dielectric layer, reaction gas flow is N
2The SiH of dilution
4Be 30sccm (mark condition milliliter per minute), O
2Be 30sccm, deposition rate 0.2nm/s deposits the SiN of rich Si
xDuring layer, reaction gas flow is N
2The SiH of dilution
4Be 100sccm, NH
3Be 30sccm, deposition rate 0.25nm/s; Film sample is placed in the quick photothermal treatment stove carries out annealing in process, utilize the thermal source of heating wire as thermal annealing, the high pure nitrogen protection is placed on film sample on the monocrystalline silicon piece of quartzy box in the stove down.Annealing process is: 25 ℃/s of heating rate, and 500 ℃ of annealing temperatures, insulation 30min uses then with stove natural cooling (air-cooled or water-cooled).Make Si diffusive migration more than needed, solid phase crystallization forms the Si quantum dot.The silicon quantum dot that present embodiment obtains is a layered arrangement, is shaped as sphere, and particle diameter is 4nm.
Embodiment 3:
Adopt Ecr plasma to strengthen chemical vapour deposition technique, substrate is selected 20cm * 30cm, the Stainless Steel sheet of thick 2mm, the SiN of SiC dielectric layer that alternating growth 3nm is thick and the rich Si of 6nm
xLayer, SiC/SiN
xDeposition cycle be 60.Sedimentary condition: rf frequency is 13.56MHz, radio-frequency power 60W, and the base vacuum degree reaches 1 * 10
-4Pa, reacting gas are N
2The SiH of dilution
4(gas volume N
2: SiH
41) and CH=1:
4, operating air pressure is 10Pa, and depositing temperature is 300 ℃, and during deposition SiC dielectric layer, reaction gas flow is N
2The SiH of dilution
4Be 30sccm (mark condition milliliter per minute), CH
4Be 30sccm, deposition rate 0.2nm/s deposits the SiN of rich Si
xDuring layer, reaction gas flow is N
2The SiH of dilution
4Be 100sccm, NH
3Be 30sccm, deposition rate 0.25nm/s; Film sample is placed in the quick photothermal treatment stove carries out annealing in process, utilize the light source of tungsten halogen lamp as photo-thermal annealing, the high pure nitrogen protection is placed on film sample on the monocrystalline silicon piece of quartzy box in the stove down.Annealing process is: 25 ℃/s of heating rate, and 500 ℃ of annealing temperatures, insulation 30min uses then with stove natural cooling (water-cooled or air-cooled).Make Si diffusive migration more than needed, solid phase crystallization forms the Si quantum dot.The silicon quantum dot that present embodiment obtains is a layered arrangement, is shaped as sphere, and particle diameter is 6nm.
Embodiment 4:
Adopt very high frequency plasma to strengthen chemical vapour deposition technique, substrate is selected 20cm * 30cm, the Stainless Steel sheet of thick 2mm, the Si that alternating growth 3nm is thick
3N
4The SiN of the rich Si of dielectric layer and 6nm
xLayer, Si
3N
4/ SiN
xDeposition cycle be 60.Sedimentary condition: rf frequency is 13.56MHz, radio-frequency power 60W, and the base vacuum degree reaches 1 * 10
-4Pa, reacting gas are N
2The SiH of dilution
4(gas volume N
2: SiH
41) and NH=1:
3, operating air pressure is 10Pa, depositing temperature is 300 ℃, deposition Si
3N
4During dielectric layer, reaction gas flow is N
2The SiH of dilution
4Be 30sccm (mark condition milliliter per minute), NH
3Be 30sccm, deposition rate 0.2nm/s deposits the SiN of rich Si
xDuring layer, reaction gas flow is N
2The SiH of dilution
4Be 100sccm, NH
3Be 30sccm, deposition rate 0.25nm/s; Film sample is placed in the quick photothermal treatment stove carries out annealing in process, utilize the light source of tungsten halogen lamp as photo-thermal annealing, the high pure nitrogen protection is placed on film sample on the monocrystalline silicon piece of quartzy box in the stove down.Annealing process is: 25 ℃/s of heating rate, and 500 ℃ of annealing temperatures, insulation 30min uses then with the stove natural cooling.Make Si diffusive migration more than needed, solid phase crystallization forms the Si quantum dot.The silicon quantum dot that present embodiment obtains is a layered arrangement, is shaped as sphere, and particle diameter is 6nm.
Claims (5)
1. the low-temperature growth method of a silicon quantum dots for solar battery, it is characterized in that this method is: using plasma strengthens chemical vapour deposition technique under＜450 ℃ of temperature, the silicon compound dielectric layer of the stoichiometric proportion of several nanometer thickness of alternately growing on backing material and the silicon compound layer of rich Si; Utilize quick photo-thermal annealing technology after annealing under≤550 ℃ temperature to handle then, make Si more than needed in the silicon compound layer of rich Si that diffusive migration take place, solid phase crystallization forms the Si quantum dot; The Si quantum dot that forms is that stratiform is arranged, and its size is by the THICKNESS CONTROL of the silicon compound layer of the rich Si of original growth, and the density of quantum dot is by the SiN of original rich Si
xSi content decision in the layer.
2. the low-temperature growth method of silicon quantum dots for solar battery as claimed in claim 1 is characterized in that plasma chemical vapor deposition technique is radio frequency plasma or Ecr plasma or microwave plasma or very high frequency plasma enhancing chemical vapour deposition technique.
3. the low-temperature growth method of silicon quantum dots for solar battery as claimed in claim 1 is characterized in that the silicon compound dielectric layer comprises SiO
2, Si
3N
4And SiC, the silicon compound layer of rich Si comprises SiO
x, SiN
xAnd Si
1-xC
x
4. the low-temperature growth method of silicon quantum dots for solar battery as claimed in claim 1, it is characterized in that quick photo-thermal annealing technology is meant is placed on material in the annealing furnace, utilize tungsten halogen lamp or heating wire mode of heating that sample is carried out Fast Heating, be incubated certain hour after reaching design temperature, temperature retention time is determined according to the quantum dot size and dimension; Use then with the stove natural cooling, or the mode of air-cooled or water-cooled is lowered the temperature.
5. the low-temperature growth method of silicon quantum dots for solar battery as claimed in claim 1, the growth substrates of Si quanta point material is selected silicon chip, quartz plate, sheet glass, stainless steel substrates or resistant to elevated temperatures polymer substrate.
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| CN101814555A (en) * | 2010-04-12 | 2010-08-25 | 浙江大学 | Method for improving efficiency of solar cell |
| CN102280500A (en) * | 2011-09-26 | 2011-12-14 | 华中科技大学 | Silicon quantum dot solar energy cell based on a heterojunction structure and preparation method thereof |
| CN102403378A (en) * | 2011-11-17 | 2012-04-04 | 华中科技大学 | Flexible film solar cell with quantum dot structure and preparation method thereof |
| CN102403376A (en) * | 2011-10-28 | 2012-04-04 | 华中科技大学 | N-i-p heterojunction solar cell with silicon quantum dot and preparation method thereof |
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| CN101814555A (en) * | 2010-04-12 | 2010-08-25 | 浙江大学 | Method for improving efficiency of solar cell |
| CN101814555B (en) * | 2010-04-12 | 2012-07-25 | 浙江大学 | Method for improving efficiency of solar cell |
| CN102280500A (en) * | 2011-09-26 | 2011-12-14 | 华中科技大学 | Silicon quantum dot solar energy cell based on a heterojunction structure and preparation method thereof |
| CN102403376B (en) * | 2011-10-28 | 2014-05-07 | 华中科技大学 | n-i-p heterojunction solar cell with silicon quantum dot and preparation method thereof |
| CN102403376A (en) * | 2011-10-28 | 2012-04-04 | 华中科技大学 | N-i-p heterojunction solar cell with silicon quantum dot and preparation method thereof |
| CN102403378B (en) * | 2011-11-17 | 2014-03-05 | 华中科技大学 | Flexible film solar cell with quantum dot structure and preparation method thereof |
| CN102403378A (en) * | 2011-11-17 | 2012-04-04 | 华中科技大学 | Flexible film solar cell with quantum dot structure and preparation method thereof |
| CN102751386A (en) * | 2012-07-11 | 2012-10-24 | 辽宁朝阳光伏科技有限公司 | Short wave response crystalline silicon solar battery preparation method based on multiple layers of silicon quantum dot |
| CN103618037A (en) * | 2013-11-25 | 2014-03-05 | 华中科技大学 | Doped silicon quantum dot light emitting diode device and preparation method thereof |
| CN103618037B (en) * | 2013-11-25 | 2017-04-19 | 华中科技大学 | Doped silicon quantum dot light emitting diode device and preparation method thereof |
| CN103972079A (en) * | 2014-04-01 | 2014-08-06 | 三峡大学 | Preparation method for ordered silicon quantum dots in three-dimensional space |
| CN103972079B (en) * | 2014-04-01 | 2016-06-01 | 三峡大学 | The preparation method of the orderly silicon quantum dot of a kind of three-dimensional spatial distribution |
| CN104952981A (en) * | 2015-07-07 | 2015-09-30 | 云南师范大学 | Method for preparing silicon quantum dot films through microwave annealing |
| CN107785447A (en) * | 2016-08-25 | 2018-03-09 | 比亚迪股份有限公司 | A kind of crystal silicon solar energy battery and preparation method thereof |
| CN108461386A (en) * | 2018-03-16 | 2018-08-28 | 三峡大学 | A kind of siliceous quantum dot multilayer film and preparation method thereof |
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