CN111200041A - Etching method and application of silicon nitride in crystalline silicon solar cell - Google Patents
Etching method and application of silicon nitride in crystalline silicon solar cell Download PDFInfo
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- 238000005530 etching Methods 0.000 title claims abstract description 71
- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 68
- 238000000034 method Methods 0.000 title claims abstract description 37
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 229910021419 crystalline silicon Inorganic materials 0.000 title claims abstract description 27
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 130
- 229910052709 silver Inorganic materials 0.000 claims abstract description 126
- 239000004332 silver Substances 0.000 claims abstract description 125
- SITVSCPRJNYAGV-UHFFFAOYSA-L tellurite Chemical compound [O-][Te]([O-])=O SITVSCPRJNYAGV-UHFFFAOYSA-L 0.000 claims abstract description 51
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 46
- 239000010703 silicon Substances 0.000 claims abstract description 45
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000011521 glass Substances 0.000 claims description 42
- 239000000843 powder Substances 0.000 claims description 29
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 21
- 238000002360 preparation method Methods 0.000 claims description 16
- 229910003069 TeO2 Inorganic materials 0.000 claims description 13
- 229910052760 oxygen Inorganic materials 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 9
- XHGGEBRKUWZHEK-UHFFFAOYSA-L tellurate Chemical compound [O-][Te]([O-])(=O)=O XHGGEBRKUWZHEK-UHFFFAOYSA-L 0.000 claims description 4
- WIKQEUJFZPCFNJ-UHFFFAOYSA-N carbonic acid;silver Chemical compound [Ag].[Ag].OC(O)=O WIKQEUJFZPCFNJ-UHFFFAOYSA-N 0.000 claims description 3
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- 229910052714 tellurium Inorganic materials 0.000 claims description 3
- 230000002194 synthesizing effect Effects 0.000 claims description 2
- XNRNVYYTHRPBDD-UHFFFAOYSA-N [Si][Ag] Chemical compound [Si][Ag] XNRNVYYTHRPBDD-UHFFFAOYSA-N 0.000 abstract description 13
- 238000005245 sintering Methods 0.000 abstract description 13
- 239000000126 substance Substances 0.000 abstract description 9
- 230000009286 beneficial effect Effects 0.000 abstract description 6
- 238000009766 low-temperature sintering Methods 0.000 abstract description 6
- 238000011065 in-situ storage Methods 0.000 abstract description 4
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- 229910004273 TeO3 Inorganic materials 0.000 description 71
- 238000006243 chemical reaction Methods 0.000 description 32
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- 238000002844 melting Methods 0.000 description 7
- 230000008018 melting Effects 0.000 description 7
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- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
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- C03—GLASS; MINERAL OR SLAG WOOL
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Abstract
The application discloses an etching method and application of silicon nitride in a crystalline silicon solar cell. The method for etching the silicon nitride in the crystalline silicon solar cell comprises the step of etching the silicon nitride of the crystalline silicon solar cell by silver tellurite. According to the etching method, the silicon nitride is etched by adopting the silver tellurite, the sintering temperature is low, the existing etching agent PbO can be completely replaced, and the lead-free low-temperature sintering is realized; in addition, the simple substance silver generated by etching the silver tellurite can be grown in situ in two dimensions on the silicon emitter to form nano silver, and the nano silver and the silicon of the emitter form good ohmic contact, thereby being beneficial to reducing the silver-silicon contact resistance and improving the efficiency of the solar cell.
Description
Technical Field
The application relates to the field of crystalline silicon solar cells, in particular to an etching method and application of silicon nitride in a crystalline silicon solar cell.
Background
Photovoltaic power generation is one of the most promising clean energy sources among renewable energy sources, and silicon solar cells account for more than 90% of the photovoltaic market share. High efficiency cells are the direction of future development, and one of the keys to improving the efficiency of silicon solar cells is metallization. In the production of the silicon solar cell, the metallization of the silicon solar cell is realized by screen printing silver paste and high-temperature sintering on a large scale. The sintering mechanism and the silver-silicon ohmic contact mechanism of the solar cell are important points of research in the field of silicon solar cells. Xiong adopts a contact terminal voltage measurement technology to deepen understanding of a silver-silicon contact forming process, so that a high-efficiency solar cell silver paste formula and a sintering process can be optimized. DieterK reviews ohmic contacts of solar cells and introduces the basic principles of metal-semiconductor contacts, including fermi level pinning of surface states, tunneling mechanisms of field emission, thermal/field emission and current transport, and studies on contact resistance of silicon with different materials. The measurement of ohmic contact is very critical, and the contact resistivity of the silicon solar cell is measured by Balif.C. with an atomic force microscope, and the minimum value of the silver-silicon contact is 10-7Ωcm2。
The glass frit contained in the silver paste is a very critical material and the basic function consists of etching the silicon nitride film (Si)3N4) And the anti-reflection layer and the silicon substrate form silver-silicon ohmic contact. Most of the ideas consider that silver in the silver grid line is dissolved and transmitted to the surface of the silicon emitter after glass powder is melted in the sintering process, silver is separated out on the surface of the silicon or in the glass layer when the temperature is reduced, the silver is in contact with silicon, and the photoelectric conversion efficiency of the battery can be improved due to good silver-silicon contact. Cai prepared a novel lead-free silver paste using TeO2A base glass frit for a front electrode of a crystalline silicon solar cell, the sintered front electrode having a resistivity of3.1-3.7 mu omega cm. Pi prepared a glass sample by a melt cooling method, and studied the glass powder to the antireflection film Si3N4Has been found to provide good silver to silicon bonding. Chunga studies the formation mechanism of solar cell contacts, and it is believed that silver is dissolved by interaction with atmospheric oxygen and forms Ag in molten glass+And then measure Ag+The concentration of (a) significantly increases with an increase in the oxygen partial pressure, and thus the oxidizing property of the atmosphere plays an important role in the sintering of the battery.
The method finds and develops a new material for the metallization of the existing crystalline silicon solar cell, realizes low-temperature sintering, reduces lead or lead-free metallization, researches the functions and the mechanism of the material, and is an important subject for the metallization of the solar cell.
Disclosure of Invention
The application aims to provide a novel method for etching silicon nitride in a crystalline silicon solar cell and application thereof.
The following technical scheme is adopted in the application:
the first aspect of the application discloses a method for etching silicon nitride in a crystalline silicon solar cell, which comprises the steps of adopting silver tellurite (Ag)2TeO3) And etching silicon nitride of the crystalline silicon solar cell.
Preferably, the etching method comprises the steps of adding silver tellurite into glass powder of the solar cell silver paste to prepare mixed glass powder, preparing the solar cell silver paste by adopting the mixed glass powder, preparing the silicon solar cell by adopting the solar cell silver paste containing the silver tellurite, and etching silicon nitride by using the silver tellurite at an etching temperature.
Preferably, the etching temperature of the silver tellurite starts at 545 ℃. Wherein, the etching temperature of 545 ℃ is only found by research in an implementation mode of the application, and Ag is obtained when the silver tellurite is about 545 DEG C2TeO3With Si3N4The TGA curve of the reaction begins to lose weight, indicating that a redox reaction has occurred; it will be appreciated that 545 ℃ is only a reaction node, and that redox reactions may also occur before this, but with less effectiveness or efficiency, and likewise oxidation at higher temperaturesThe original reaction can also occur, but higher heat energy is wasted; therefore, the optimum starting temperature for etching is 545 ℃.
It should be noted that, the application creatively discovers that the silver tellurite can etch silicon nitride of the crystalline silicon solar cell, and the etching temperature of the silver tellurite is only about 545 ℃, which is 160 ℃ lower than that of the traditional optimal etchant PbO, so that the silver tellurite can replace PbO to realize leadless low-temperature sintering; in addition, the etching product of the silver tellurite is conductive simple substance silver, which is beneficial to reducing the silver-silicon contact resistance and improving the efficiency of the solar cell.
It should be further noted that, in the present application, silver tellurite is used for silicon nitride etching, and may be directly used, or may be added into common oxide glass for etching, for example, added into glass powder to make solar cell slurry, so that the simple substance silver generated by etching can also optimize the silver-silicon interface, and improve the efficiency of the solar cell. In addition, the silicon nitride etching is carried out by adopting the silver tellurite, the silicon nitride can be etched at low temperature under various atmospheres, and the silicon nitride can be etched in an aerobic or anaerobic environment.
The second aspect of the application discloses a preparation method of a crystalline silicon solar cell, which comprises the step of etching silicon nitride of the crystalline silicon solar cell by adopting the silicon nitride etching method.
The preparation method of the crystalline silicon solar cell has the key point that the silicon nitride of the crystalline silicon solar cell is etched by the silicon nitride etching method; as for other steps, reference may be made to existing crystalline silicon solar cell preparation methods, which are not specifically limited herein.
The third aspect of the application discloses a crystalline silicon solar cell prepared by the preparation method.
It should be noted that, in the crystalline silicon solar cell of the present application, since silver tellurite is used for silicon nitride etching, the elemental silver generated by the etching can form good ohmic contact with silicon of the emitter by in-situ two-dimensional growth of nano silver on the silicon emitter, thereby improving the efficiency of the solar cell.
A fourth aspect of the present application discloses the use of silver tellurite in silicon nitride etching.
The key point of the method is that research finds that silver tellurite can etch silicon nitride; it is understood that this can not only be applied to the preparation of crystalline silicon solar cells, but also to other situations where silicon nitride etching is required, and is not particularly limited herein.
In a fifth aspect of the present application, a mixed glass frit is disclosed, which contains silver tellurite.
The sixth aspect of the application discloses a solar cell silver paste which contains silver tellurite.
It should be noted that the mixed glass powder or the silver paste for the solar cell of the present application can realize low-temperature sintering during the preparation of the solar cell due to the inclusion of silver tellurite, so that not only is the energy saved, but also the adverse effect of high-temperature sintering on the solar cell is avoided. More importantly, when the mixed glass powder containing silver tellurite or the silver paste of the solar cell is etched by silicon nitride, the simple substance silver product can form a two-dimensional nano structure growing in situ on a silicon emitter, so that the silicon emitter and the simple substance silver product form good ohmic contact, and the efficiency of the solar cell is improved.
The seventh aspect of the application discloses a preparation method of silver tellurite, which comprises the steps of adopting AgNO3、Ag2CO3、Ag2C2O4And Ag2At least one of O, Te and TeO2And tellurate, and heating to 250-1200 deg.c to synthesize the silver tellurite.
Preferably, the preparation method of silver tellurite specifically adopts AgNO3And TeO2And (4) synthesizing silver tellurite.
Compared with the existing preparation method, the preparation method of silver tellurite has the advantages of simpler and more direct synthesis steps, short synthesis process and avoidance of introduction of other metal impurities.
The beneficial effect of this application lies in:
according to the etching method, the silicon nitride is etched by adopting the silver tellurite, the sintering temperature is low, the existing etching agent PbO can be completely replaced, and the lead-free low-temperature sintering is realized; in addition, the simple substance silver generated by etching the silver tellurite can be grown in situ in two dimensions on the silicon emitter to form nano silver, and the nano silver and the silicon of the emitter form good ohmic contact, thereby being beneficial to reducing the silver-silicon contact resistance and improving the efficiency of the solar cell.
Drawings
FIG. 1 is a diagram showing the result of XRD analysis of silver tellurite in examples of the present application;
FIG. 2 is a DSC curve of silver tellurite in an example of the present application;
FIG. 3 shows the reaction of silver tellurite in O in the examples of the present application2TGA profile in an atmosphere;
FIG. 4 shows Ag in the examples of the present application2TeO3And Si3N4At O2Medium and differential thermal curves;
FIG. 5 shows Ag in the examples of the present application2TeO3With Si3N4In N2A TGA profile under ambient;
FIG. 6 shows Ag in the examples of the present application2TeO3Etching Si with PbO3N4The contrast curve of (1);
FIG. 7 shows Ag in the examples of the present application2TeO3With Si3N4XRD diffractogram of the powder;
FIG. 8 shows PbO and Si in the present embodiment3N4XRD diffractogram of the powder;
FIG. 9 shows Ag in the examples of the present application2TeO3XRD analysis result pattern of glass melted with oxide;
FIG. 10 shows Ag in the examples of the present application2TeO3Glass fused with oxides and Si3N4Mixing the powders in O2Thermogravimetric curve of medium heating reaction;
fig. 11 is a photograph of a silicon solar cell prepared in the example of the present application;
FIG. 12 is a cross-sectional view of a FIB slice of a silver grid line of a solar cell in an embodiment of the present application;
FIG. 13 is a block diagram of a silver-silicon contact interface in an embodiment of the present application;
FIG. 14 is a further enlarged interface view of Ag-Si contacts in an example of the present application;
FIG. 15 is a general area distribution diagram of the interface spectrum of the silver grid lines of the solar cell in the example of the present application;
FIG. 16 is a distribution diagram of Si in the interface spectrum of a silver grid line of a solar cell in an embodiment of the present application;
FIG. 17 is a distribution diagram of Ag in the interface spectrum of a silver grid line of a solar cell in an embodiment of the present application;
fig. 18 is a distribution diagram of O in the interface energy spectrum of the silver grid line of the solar cell in the example of the present application.
Detailed Description
The existing silicon nitride etching usually adopts an etchant PbO, so that the sintering temperature is high, and the use of lead has the problems of environmental unfriendliness and the like. In the research process of the crystalline silicon solar cell, the silicon nitride can be etched by the silver tellurite creatively, the sintering temperature is low, and the silver generated by etching can form good ohmic contact with the silicon of the emitter, so that the efficiency of the solar cell is improved.
Wherein, Ag2TeO3Is a compound with few reports, and the research on the performance and the application of the compound is rather lacked, and L.B.Sharma reports Ag2TeO3The synthesis method comprises the following steps: firstly adopting TeO2Reacting with sodium carbonate at high temperature to obtain Na2TeO3Mixing Na2TeO3Dissolving in water to form a solution; then preparing Ag by using a uniform precipitation method2TeO3I.e. AgNO3Adding Na into the solution uniformly2TeO3Precipitating Ag from the solution2TeO3Washing the precipitate and heat treating to obtain Ag2TeO3A crystal; ag prepared by the method2TeO3The characterization and thermal analysis are carried out, and the result shows that the Ag prepared by the precipitation method2TeO3Is a tetragonal crystal form.
On the basis of the above research and understanding, the present application further develops and developsNovel Ag2TeO3By the preparation of AgNO3、Ag2CO3、Ag2C2O4And Ag2At least one of O, Te and TeO2And tellurate, and directly heating to obtain Ag2TeO3. Ag thus prepared2TeO3The preparation method is simple, the synthesis process is shortened, and other metal impurities are prevented from being introduced; and can be fine satisfies this application and etches the user demand of silicon nitride.
The present application will be described in further detail with reference to specific examples. The following examples are intended to be illustrative of the present application only and should not be construed as limiting the present application.
Examples
1. Preparation of the Material
According to Ag2TeO3According to the metering ratio of (1), weighing AgNO with the purity of 99.9%3And TeO with purity of 99.99% and particle size D50 ═ 100nm2Mixing uniformly, placing in a muffle furnace, heating to 750 deg.C at a rate of 10 deg.C/min, keeping the temperature for 100min, cooling with the furnace, and grinding to particle size D50 ═ 10 μm for use to obtain Ag in the example2TeO3。
Ag to be prepared in this example2TeO3Adding the glass powder into glass powder of a solar cell silver paste to prepare mixed glass powder, preparing the solar cell silver paste by adopting the mixed glass powder, and preparing a silicon solar cell by adopting the solar cell silver paste containing silver tellurite, wherein the method specifically comprises the following steps:
weighing 70 g of prepared Ag2TeO3And melting the glass with other oxides, wherein the other oxides comprise: 1 g of Na2O, 2 g MgO, 0.5 g CaO, 0.2 g TiO23 g of P2O55g of SiO26 g of B2O320 g TeO2The specific condition for melting into glass is that the temperature is kept at 1000 ℃ for 2 hours, then the glass melt is poured into water for water quenching, the water quenched glass is put into an agate tank, and powder is milled by agate balls for 1 to 5 microns, thus obtaining the mixed glass powder of the embodiment.
The silver paste of the solar cell of the present example was obtained by mixing 5% of the mixed glass frit prepared in the present example, 85% of silver powder, 9% of an organic solvent, and 1% of a resin. The organic solvent and the resin are conventional general materials of the silver paste of the solar cell.
And (3) screen-printing silver grid lines with the line width of 30 mu m and the interval of 1mm on a silicon solar cell substrate by adopting a 400-mesh screen, and sintering the silver grid lines at 920 ℃ for 1min to form the cell.
2. Testing and characterization
XRD (Bruker, D8) was used, step size 0.1s, angle 10-80 °, to test Ag2TeO3、Ag2TeO3Glasses made by mixing with oxides, Ag2TeO3With Si3N4PbO and Si3N4X-ray diffraction pattern of the reaction product, wherein, Si3N4The purity of (2) was 99.95%, and the particle diameter D50 was 0.5. mu.m. Specifically, the thermal analyzer (Mettler-Toolido, TGA/DSC professional type) is used in O2Heating to 1000 deg.C at a rate of 10 deg.C/min under atmosphere, and measuring Ag2TeO3And Ag2TeO3PbO and Si3N4Differential and thermogravimetric curves of the powder; the solar cell efficiency was measured by a photoelectric simulator, and the interface element distribution and the morphology characteristics were observed by using FIB (FEI, Scios) samples and TEM (JEM-3200 FS).
3. Results and discussion
(1) XRD analysis result of silver tellurite sample
The XRD analysis results of the silver tellurite synthesized in this example are shown in FIG. 1, and the PDF card number is 83-1779, which shows that Ag is successfully synthesized in this example2TeO3. Compared with the existing Ag2TeO3Synthetic method, this example uses AgNO3And TeO2The synthesis is simpler, the pollution of other metal ions is avoided, and the experimental quality is improved.
(2) Silver tellurite thermal analysis results
The DSC curve of the silver tellurite synthesized in this example is shown in FIG. 2, and the melting point is 600 ℃ and TeO2And the melting points of PbO are 730 ℃ and 888 ℃ respectively,the melting point of silver tellurite is higher than that of TeO2130 ℃ lower than that of PbO, and 288 ℃ lower than that of PbO. The lower melting point of silver tellurite helps the etching reaction to proceed.
The silver tellurite synthesized in this example is in O2The TGA profile in the atmosphere, as shown in figure 3, shows that the material is stable before 800 ℃, starts to decompose after 800 ℃ and progresses in decomposition at 900 ℃.
(3)Ag2TeO3Etching of Si3N4
Ag2TeO3With Si3N4TGA profile of the reaction, as shown in FIG. 4, FIG. 4 is Ag2TeO3And Si3N4At O2Wherein the solid line is the thermogravimetric curve and the dashed line is the differential thermal curve.
In this example, 20mgAg was used2TeO3And 5mg of Si3N4Comparison of Ag2TeO3At O2The stable conditions under the environment are different, and the results in fig. 4 show that the curve of the sample begins to lose weight at about 545 ℃, which indicates that the redox reaction occurs, and the system releases N mainly according to the reaction equation (1)2Gas, the reaction occurs below the melting points of the two materials, indicating that the reaction is a solid phase reaction. The DSC curve shows that the heat is released at 450-800 ℃, and the temperature reaches the peak value at 600 ℃, which shows that the oxidation-reduction heat release reaction mainly occurs at about 600 ℃, which is beneficial to increasing the temperature of the system and accelerating the reaction.
6Ag2TeO3+Si3N4＝12Ag+3SiO2+6TeO2+2N2↑ (1)
2Ag2TeO3+Si3N4+2O2＝4Ag+3SiO2+2TeO2+2N2↑ (2)
The curve begins to increase weight around 750 ℃, and the peak value of the weight increase is reached at 900 ℃, which shows that the reaction is based on the equation (2). The TGA curve after 800 ℃ has obvious weight gain, but the heat release is weak, which indicates that the system absorbs oxygen as an endothermic reaction, and the heat release of the oxygen and the etching reaction can be mutually offset, thereby showing dynamic energy change.
This example also tested 10mgAg2TeO3With 2.5mg Si3N4In N2TGA profile under ambient conditions, the results are shown in figure 5. The results show that in N2The TGA curve under ambient conditions shows weight loss at the same temperature compared to aerobic conditions, the reaction is equation (1), and it is demonstrated that2Ag under environment2TeO3And Si3N4The weight gain after 750 ℃ is due to O2The participation in the reaction. Likewise, the weight loss after 900 ℃ is accelerated, Ag2TeO3And (5) decomposing.
(4)Ag2TeO3Etching Si with PbO3N4Comparison of (2)
Ag2TeO3Etching Si with PbO3N4Is shown in FIG. 6. in FIG. 6, the solid line shows the etching of Si by PbO3N4The dotted line is Ag2TeO3Etching of Si3N4Thermogravimetric curve of (c). The results in FIG. 6 show that the thermogravimetric curve of PbO remains substantially stable before 700 deg.C and the weight gain is accelerated after 710 deg.C without weight loss, indicating that PbO etches Si3N4Mainly by the presence of O in the environment2And (4) participating. The reaction equations are (3) and (4):
6PbO+Si3N4＝6Pb+3SiO2+2N2↑ (3)
2Pb+O2＝2PbO (4)
comparative Ag2TeO3The thermogravimetric curve of the material is obviously different from that of PbO, and Ag is2TeO3The etching reaction started at about 540 ℃ is 160 ℃ lower than that of lead oxide etching, and Ag2TeO3The weight loss of the etching thermogravimetric curve is first, which shows that the reaction mainly comes from Ag2TeO3Oxygen in (1), more environmental O as temperature increases2The curve begins to gain weight by participating in the reaction. Ag2TeO3Has the advantages of lower reaction temperature and richer oxygen source.
In this example, 10g of PbO and Ag were added2TeO3Each with 2.5g of Si3N4Powder ofAfter mixing and heating to 750 deg.C at 10K/min, XRD diffractogram of the product was measured, and the results are shown in FIGS. 7 and 8, in which FIG. 7 is Ag2TeO3With Si3N4XRD diffractogram of the powder, and FIG. 8 shows PbO and Si3N4XRD diffractogram of the powder. Comparative analysis of the results of FIGS. 7 and 8 shows that Ag2TeO3With Si3N4The powder reaction has a peak of the simple substance of silver, which indicates that silver is generated in the reaction product. Thus, Ag is added2TeO3The glass powder is added into the glass component of the silver paste, so that the sintering of the paste can be facilitated, and the interface conductivity can be improved. The reaction products of PbO are mainly amorphous glass and unreacted residues, and are free of metallic lead, i.e., do not generate conductive substances. Other reaction residues appear in the diffractogram, due to the SiO formed as a result of the reaction2The etching reaction is hindered from proceeding, resulting in incomplete reaction.
(4) Slurry and solar cell I-V, TEM
Ag to be prepared in this example2TeO3The XRD results of the mixed glass powder fused with the oxides to form glass are shown in FIG. 9. The results in fig. 9 show that the mixed glass frit material is predominantly disordered. Mixing glass with Si3N4The powders were mixed and the mixture was measured by TGA at O2The thermogravimetric curve of the medium heating reaction is shown in FIG. 10, and the results show the change of mass and Ag2TeO3With Si3N4The reaction is similar, which shows that Ag is successfully reacted2TeO3The performance of (2) is transplanted into the glass, namely the glass contains Ag2TeO3. Therefore, the silver paste prepared by the glass can better etch silicon nitride in the sintering process of the solar cell, generate more silver particles and improve the performance of the solar cell.
The above results show that Ag2TeO3Can effectively etch Si alone or added into oxide glass3N4And, low temperature etching can be achieved in various atmospheres, and etching can be performed in an oxygen-or oxygen-free environment.
In this example, seven silicon solar cell samples are repeatedly manufactured, and are sequentially marked as Solarcell-01 to Solarcell-07, the photo of the silicon solar cell is shown in fig. 11, and the parameter test results of the seven silicon solar cells are shown in table 1.
TABLE 1 silicon solar cell Performance test results
The results in Table 1 show that the current density of the battery reached 38.37mA/cm at the maximum2The open voltage is about 0.638V, the maximum photoelectric conversion efficiency reaches 18.41%, and the average value is more than 18%, which indicates that the silver grid line of the battery has good charge collection capability.
Fig. 12 to 14 show results of FIB section observation of the solar cell silver grid line of the silicon solar cell sample prepared in this example, in which fig. 12 is a cross-sectional view of the FIB section, fig. 13 is a structural view of a silver-silicon contact interface, and fig. 14 is an interface view of an Ag-Si contact. The results shown in fig. 12 to 14 show that the silver grid lines on the pyramid texture of the silicon-based surface have a contact interface structure with silicon; the surface of the silicon is formed with silver of thickness 50nm along the length of the surface of 300-500nm, which is Ag in the glass2TeO3Etching of Si3N4The product of (a); and the charges can be directly tunneled from the surface of the silicon emitter to the silver grid line, and the collection and transmission of the charges are completed.
The interface energy spectrum of the solar cell silver grid line is shown in fig. 15 to 18, wherein fig. 15 is a general surface distribution diagram, and fig. 16 to 18 are distribution diagrams of Si, Ag and O in sequence. As can be seen from the energy spectrum element distributions of fig. 15 to 18, silver and oxygen are separated, indicating that the interface etching product is a silver simple substance.
The distribution position and the morphology of the silver particles greatly influence the performance of the battery. Ballif measured the resistance of the direct silver-silicon contact and found that the resistivity of some regions was 4 orders of magnitude lower than the typical values, indicating that some silver-to-silicon contacts can significantly reduce the contact power of the cellAnd the charge is better collected. Liang studied key features of the battery interfacial micro-region: besides the residual SiNx, the other part of the silicon emitter is a thin glass layer with nano Ag colloid, and nano 10-100nm Ag particles are attached to the surface of the silicon emitter. However, it can also be seen that the silver particles are discretely distributed and interface-spaced at an average distance of more than 50nm, which is detrimental to electrical conductivity. Ballif measured the silver-silicon contact resistance and found that in a cross-sectional transmission electron microscope, the interface consisted of Ag crystals with a diameter of 200-500nm, which were penetrating 130nm on average through silicon, the smaller silver grains were in epitaxial relationship with the Si substrate, and it was considered that silver was grown from the glass melt. Likewise, the silver particles also exhibit a discrete distribution. While the nanosilver in this example shows a stripe shape in cross section, it is clear that it requires a higher concentration of silver ions during growth, which is in contrast to Ag2TeO3The addition being in direct relation, i.e. Ag2TeO3Etching of Si3N4More silver can then be produced, so that the separated silver particles continue at low concentrations. By Ag2TeO3The regenerated silver can be generated after the silicon nitride is etched, the regenerated silver is in direct contact with the silicon to collect charges, and then the charges are output through the silver grid lines, so that the efficiency of the solar cell is improved.
From the above results, it was revealed that Ag2TeO3When the glass is added into silver paste, on one hand, the low-temperature sintering of a silver grid line can be realized, and on the other hand, Ag2TeO3With Si3N4The product generated after the reaction is conductive metallic silver, the conductive advantage is very obvious compared with other materials, and the effect of improving the efficiency of the silicon solar cell is particularly outstanding.
Therefore, compared with the prior art, the method has the following advantages:
a. this example uses AgNO3And TeO2Directly synthesize Ag2TeO3The synthesis process is short, and other metal impurities are prevented from being introduced little; on the basis, the example further tests other raw materials, and the result shows that Ag can be used2CO3、Ag2C2O4Or Ag2Substitution of O for AgNO3Te sources other than TeO2Besides, Te or common tellurate can be directly adopted; can prepare Ag meeting the use requirement of the embodiment2TeO3Except that the temperature of heating is varied to be between about 250 c and 1200 c.
b. This example uses Ag2TeO3Etching of Si3N4The etching temperature is about 545 ℃, and the aim of Si-Si etching is realized3N4The etching temperature of the low-temperature etching is about 160 ℃ lower than that of PbO etching.
c. This example successfully converts Ag to2TeO3The method is applied to silicon solar cell silver paste, and the current density of the prepared cell reaches 38.37 mA-cm-2The average efficiency is greater than 18%.
d. The Ag-silicon interface was observed by TEM/EDS to find that the Ag was doped in the present example2TeO3And then growing silver with the length of 300-500nm and the thickness of 50nm along the surface of the silicon emitter. Description of Ag2TeO3Not only is an excellent low-temperature etching material, but also more importantly, silver ions with higher concentration are provided for an interface; the silver can better collect and transmit charges after being generated, and can collect and transmit the charges to the silver grid line, thereby being beneficial to reducing contact resistance and improving the efficiency of the solar cell.
e. The method opens up a new direction for the metallization of the silicon solar cell from the material development angle, and promotes the development of low-temperature sintered silver paste with less lead and no lead.
The foregoing is a more detailed description of the present application in connection with specific embodiments thereof, and it is not intended that the present application be limited to the specific embodiments thereof. It will be apparent to those skilled in the art from this disclosure that many more simple derivations or substitutions can be made without departing from the spirit of the disclosure.
Claims (10)
1. A method for etching silicon nitride in a crystalline silicon solar cell is characterized by comprising the following steps: the method comprises the step of etching silicon nitride of the crystalline silicon solar cell by silver tellurite.
2. The etching method according to claim 1, characterized in that: the method comprises the steps of adding silver tellurite into glass powder of the solar cell silver paste to prepare mixed glass powder, preparing the solar cell silver paste by adopting the mixed glass powder, preparing a silicon solar cell by adopting the solar cell silver paste containing the silver tellurite, and etching silicon nitride by using the silver tellurite at an etching temperature.
3. The etching method according to claim 2, characterized in that: the initial temperature of the etching temperature was 545 ℃.
4. A preparation method of a crystalline silicon solar cell is characterized by comprising the following steps: comprising etching silicon nitride of a crystalline silicon solar cell using the etching method as claimed in any one of claims 1 to 3.
5. The crystalline silicon solar cell prepared by the preparation method according to claim 4.
6. Application of silver tellurite in silicon nitride etching.
7. A mixed glass frit is characterized in that: the mixed glass powder contains silver tellurite.
8. The solar cell silver paste is characterized in that: the solar cell silver paste contains silver tellurite.
9. A preparation method of silver tellurite is characterized by comprising the following steps: comprises adopting AgNO3、Ag2CO3、Ag2C2O4And Ag2At least one of O, Te and TeO2And tellurate, and heating to 250-1200 deg.c to synthesize the silver tellurite.
10. The method of claim 9, wherein: in particular AgNO3And TeO2And synthesizing the silver tellurite.
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