WO2022052331A1 - 一种n型银铝浆用玻璃粉及其制备方法 - Google Patents

一种n型银铝浆用玻璃粉及其制备方法 Download PDF

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WO2022052331A1
WO2022052331A1 PCT/CN2020/132700 CN2020132700W WO2022052331A1 WO 2022052331 A1 WO2022052331 A1 WO 2022052331A1 CN 2020132700 W CN2020132700 W CN 2020132700W WO 2022052331 A1 WO2022052331 A1 WO 2022052331A1
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glass powder
containing compound
aluminum paste
type silver
mixture
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PCT/CN2020/132700
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English (en)
French (fr)
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毛平
郑金华
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南通天盛新能源股份有限公司
南通天晟新能源科技有限公司
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Priority to US17/777,945 priority Critical patent/US20230357074A1/en
Publication of WO2022052331A1 publication Critical patent/WO2022052331A1/zh

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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
    • C03C8/14—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions
    • C03C8/18—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions containing free metals
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C12/00—Powdered glass; Bead compositions
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/062—Glass compositions containing silica with less than 40% silica by weight
    • C03C3/07—Glass compositions containing silica with less than 40% silica by weight containing lead
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
    • C03C8/02—Frit compositions, i.e. in a powdered or comminuted form
    • C03C8/10—Frit compositions, i.e. in a powdered or comminuted form containing lead
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
    • C03C8/24—Fusion seal compositions being frit compositions having non-frit additions, i.e. for use as seals between dissimilar materials, e.g. glass and metal; Glass solders
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
    • H01B1/023—Alloys based on aluminium
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
    • H01B13/0016—Apparatus or processes specially adapted for manufacturing conductors or cables for heat treatment

Definitions

  • the invention belongs to the technical field of conductive materials containing metals or alloys, and particularly relates to a glass powder for N-type silver-aluminum paste and a preparation method thereof.
  • glass powder is an important factor in determining contact resistance, surface etching reaction and electrical properties of the entire cell, which requires it to have good electrical and mechanical properties.
  • the type and amount of glass powder also have a great influence on the open circuit voltage and the filling factor of the slurry under high temperature sintering conditions.
  • the glass frit in the silver-aluminum paste corrodes the SiNx anti-reflection film layer and is bonded to the underlying silicon. A sufficient and complete etching reaction can ensure the formation of a good ohmic contact.
  • glass powder not only promotes the adhesion of the silver-aluminum paste to the solar cell silicon substrate during the sintering process, but also affects the sintering kinetic properties of the conductive functional phase metal powder.
  • the glass powder for the front electrode silver-aluminum paste should be able to be completely etched with the silicon nitride anti-reflection film during the sintering process, and a contact layer should be formed between Ag and Si after sintering. , so that the silver powder and the silicon substrate can form a good ohmic contact, so as to achieve the purpose of effectively improving the photoelectric conversion efficiency of the solar cell.
  • Chinese patent CN200610011001.1 discloses the composition and preparation method of a silicon solar cell back field aluminum conductive paste.
  • thallium element is used as an inorganic binder in the application of the silicon solar cell back field aluminum conductive paste.
  • the bonding agent can have a good ohmic contact between the aluminum electrode and the silicon, thereby improving the photoelectric conversion efficiency, and the silicon-aluminum compound layer can also improve the adhesion strength of the aluminum film to the silicon substrate.
  • Chinese patent CN201210123378.1 discloses a conductive paste for solar cell back field, its preparation method and solar cell sheet.
  • aluminum-thallium alloy containing thallium and aluminum elements is used as conductive metal powder.
  • the surface of the back electric field metal film is smooth, the appearance is excellent, and the PP+ layer formed has excellent performance, the open circuit voltage of the battery is high, the photoelectric conversion efficiency is high, and the adhesion of the prepared metal film and the silicon wafer is strong, and the prepared solar cell is bent. degree is small.
  • the invention provides a glass powder for N-type silver-aluminum paste and a preparation method thereof.
  • the glass powder for N-type silver-aluminum paste contains thallium element, which can provide good silver melting ability and wettability to silicon wafers for solar cells.
  • the metal powder has good ohmic contact with the silicon surface, and the specific content of the present invention is as follows:
  • the purpose of the present invention is to provide a glass powder for N-type silver-aluminum paste, the technical point of which is that the glass powder for N-type silver-aluminum paste includes a lead-containing compound, a silicon-containing compound, a thallium-containing compound and a zinc-containing compound.
  • all the above-mentioned compounds can be at least one of oxides, halides, nitrate compounds, nitrite compounds, carbonate compounds, bicarbonate compounds, sulfate compounds and phosphate compounds kind.
  • the above-mentioned halide is at least one of chloride, fluoride, bromide and iodide.
  • the above-mentioned halide is chloride.
  • the above-mentioned glass frit for N-type silver-aluminum paste further includes a first main group metal element compound.
  • the above-mentioned first main group metal element compound is at least one of a lithium-containing compound, a sodium-containing compound, a potassium-containing compound, a rubidium-containing compound and a cesium-containing compound.
  • the above-mentioned glass powder for N-type silver aluminum paste is the composition of formula (I):
  • a, b, c, d, e and f represent the amount of elements contained in the glass powder for N-type silver-aluminum paste per 1 mol, where 0.6mol ⁇ a ⁇ 0.8mol, 0.05mol ⁇ b ⁇ 0.2mol , 0.03mol ⁇ c ⁇ 0.1mol, 0.01mol ⁇ d ⁇ 0.1mol, 0.001mol ⁇ e ⁇ 0.02mol, f is the amount of substances that balance the Pb element, Si element, Tl element, Zn element and M element group, where The M element is at least one of lithium element, sodium element, potassium element, rubidium element and cesium element.
  • the median particle size of the above-mentioned glass powder for N-type silver-aluminum paste is 0.5-2 ⁇ m.
  • the softening point of the above-mentioned glass frit for N-type silver-aluminum paste is 300-450°C.
  • Another object of the present invention is to provide a kind of glass powder for N-type silver aluminum paste, and its technical point is: the preparation method of the glass powder is as follows:
  • Step 1 Accurately weigh the amounts of the lead-containing compound, the silicon-containing compound, the thallium-containing compound and the zinc-containing compound by calculating, and uniformly mix and stir to obtain a mixture A;
  • Step 2 Place the mixture A obtained in the step 1 in a sintering furnace to promote sintering to obtain the mixture B, the sintering temperature of the sintering furnace is 900-1200°C, and the sintering time is 20-60min;
  • Step 3 The mixture B obtained in step 2 is placed in a cooling roll for cooling treatment to obtain mixture C.
  • the rotating speed of the cooling roller is 3-7rmp, and the processing time of the cooling roller is 1-2h;
  • Step 4 The mixture C obtained in the step 3 is placed in a ball mill for ball milling to obtain the mixture D, the rotational speed of the ball mill is 300-350rmp, and the ball milling time is 2-6h;
  • Step 5 The mixture D obtained in step 4 is placed in a 150-250 mesh vibrating screen for sieving, and then the sieved mixture D is placed in an oven and dried at a temperature of 80-150 ° C for 2-6h to obtain The N-type silver-aluminum paste is used for glass powder.
  • the glass powder for N-type silver-aluminum paste provided by the present invention includes a lead-containing compound, a silicon-containing compound, a thallium-containing compound and a zinc-containing compound, wherein the compound use of the thallium-containing compound and the lead-containing compound makes the glass powder have good melting
  • the prepared silver-aluminum paste has good wettability to the surface of the solar cell silicon wafer
  • the silicon-containing compound provides a more complete network structure for the glass powder
  • the zinc-containing compound reduces the softening temperature of the glass powder and further reduces the prepared N Type silver aluminum paste sintering temperature.
  • the glass powder for N-type silver-aluminum paste of the present application also contains a compound containing the first main group metal element, which can act with the zinc-containing compound to further reduce the softening temperature of the glass powder and further reduce the sintering of the prepared N-type silver-aluminum paste. temperature to improve the yield of N-type solar cells.
  • Fig. 1 is the flow chart of the preparation of a kind of N-type silver aluminum paste glass powder of the present invention
  • Example 2 is a DSC chart of the glass powder for N-type silver aluminum paste prepared in Example 1 of the present invention.
  • a glass powder for N-type silver-aluminum paste includes a lead-containing compound, a silicon-containing compound, a thallium-containing compound and a zinc-containing compound.
  • the compound here is at least one of oxides, halides, nitrate compounds, nitrite compounds, carbonate compounds, bicarbonate compounds, sulfate compounds and phosphate compounds, preferably the halide of the present application is chloride , at least one of fluoride, bromide and iodide, more preferably the halide of the present application is chloride, the compound use of thallium-containing compound and lead-containing compound makes the glass powder have good silver melting ability, and the prepared
  • the silver-aluminum paste has good wettability to the surface of the solar cell silicon wafer, the silicon-containing compound provides a more complete network structure for the glass powder, and the zinc-containing compound reduces the softening temperature of the glass powder and further reduces the sintering temperature of the prepared N-type silver-alumin
  • the glass powder for N-type silver-aluminum paste of the present invention also includes a first main group metal element compound, and the preferred first main group compound of the present invention is a lithium compound, a sodium-containing compound, a potassium-containing compound, a rubidium-containing compound and a cesium-containing compound At least one of the compounds can act with the zinc-containing compound to further reduce the softening temperature of the glass powder, further reduce the sintering temperature of the prepared N-type silver-aluminum paste, and improve the N-type solar cell preparation yield.
  • the glass powder for N-type silver-aluminum paste prepared by the present invention is the composition of formula (I):
  • a, b, c, d, e and f represent the amount of elements contained in the glass powder for N-type silver-aluminum paste per 1 mol, where 0.6mol ⁇ a ⁇ 0.8mol, 0.05mol ⁇ b ⁇ 0.2mol , 0.03mol ⁇ c ⁇ 0.1mol, 0.01mol ⁇ d ⁇ 0.1mol, 0.001mol ⁇ e ⁇ 0.02mol, f is the amount of substances that balance the Pb element, Si element, Tl element, Zn element and M element group, where The M element is at least one of lithium element, sodium element, potassium element, rubidium element and cesium element.
  • the prepared glass powder for N-type silver-aluminum paste has a median particle size of 0.5-2 ⁇ m and a softening point of 300-450° C.
  • the preparation method of a kind of N-type silver aluminum paste glass powder of the present invention is as follows:
  • Step 1 Accurately weigh the amounts of the lead-containing compound, the silicon-containing compound, the thallium-containing compound and the zinc-containing compound by calculating, and uniformly mix and stir to obtain a mixture A;
  • Step 2 Place the mixture A obtained in the step 1 in a sintering furnace to promote sintering to obtain the mixture B, the sintering temperature of the sintering furnace is 900-1200°C, and the sintering time is 20-60min;
  • Step 3 The mixture B obtained in step 2 is placed in a cooling roll for cooling treatment to obtain mixture C.
  • the rotating speed of the cooling roller is 3-7rmp, and the processing time of the cooling roller is 1-2h;
  • Step 4 The mixture C obtained in the step 3 is placed in a ball mill for ball milling to obtain the mixture D, the rotational speed of the ball mill is 300-350rmp, and the ball milling time is 2-6h;
  • Step 5 The mixture D obtained in step 4 is placed in a 150-250 mesh vibrating screen for sieving, and then the sieved mixture D is placed in an oven and dried at a temperature of 80-150 ° C for 2-6h to obtain The N-type silver-aluminum paste is used for glass powder.
  • the glass powder for N-type silver aluminum paste of the present invention is the composition of formula (I):
  • the preparation method of a kind of N-type silver aluminum paste glass powder of the present invention is as follows:
  • Step 1 Precisely weigh the amount of lead dioxide, silicon dioxide, thallium oxide, zinc oxide and sodium oxide by calculating, and mix and stir them to obtain mixture A;
  • Step 2 Place mixture A obtained in step 1 in a sintering furnace to promote sintering to obtain mixture B, where the sintering temperature of the sintering furnace is 1000° C. and the sintering time is 40 minutes;
  • Step 3 The mixture B obtained in step 2 is placed in a cooling roll for cooling treatment to obtain mixture C.
  • the rotating speed of the cooling roller is 5rmp, and the processing time of the cooling roller is 1h;
  • Step 4 The mixture C obtained in the step 3 is placed in a ball mill for ball milling to obtain the mixture D, the rotational speed of the ball mill is 325rmp, and the ball milling time is 4h;
  • Step 5 The mixture D obtained in step 4 is placed in a 200-mesh vibrating screen for sieving, and then the sieved mixture D is placed in an oven and dried at a temperature of 110 ° C for 4 hours to obtain the N-type silver aluminum Glass powder for paste.
  • the prepared glass powder for N-type silver-aluminum paste has a median particle size of 1 ⁇ m and a softening point of 321.96° C., as shown in the DSC chart of the glass powder of this embodiment as shown in FIG. 2 .
  • the glass powder for N-type silver aluminum paste of the present invention is the composition of formula (I):
  • the preparation method of a kind of N-type silver aluminum paste glass powder of the present invention is as follows:
  • Step 1 Accurately weigh the amounts of lead oxide, silicon dioxide, thallium oxide, zinc chloride and potassium chloride by calculation, and mix and stir to obtain mixture A;
  • Step 2 Place the mixture A obtained in the first step in a sintering furnace to promote sintering to obtain the mixture B, the sintering temperature of the sintering furnace is 900 ° C, and the sintering time is 60 minutes;
  • Step 3 The mixture B obtained in step 2 is placed in a cooling roll for cooling treatment to obtain mixture C.
  • the rotating speed of the cooling roller is 7rmp, and the processing time of the cooling roller is 1h;
  • Step 4 The mixture C obtained in the step 3 is placed in a ball mill for ball milling to obtain the mixture D, the rotational speed of the ball mill is 300rmp, and the ball milling time is 6h;
  • Step 5 The mixture D obtained in step 4 is placed in a 150-mesh vibrating screen for sieving, and then the sieved mixture D is placed in an oven and dried at a temperature of 150 ° C for 2 hours to obtain the N-type silver aluminum Glass powder for paste.
  • the median particle size of the prepared glass powder for N-type silver-aluminum paste was 0.5 ⁇ m, and the softening point was 450°C.
  • the glass powder for N-type silver aluminum paste of the present invention is the composition of formula (I):
  • the preparation method of a kind of N-type silver aluminum paste glass powder of the present invention is as follows:
  • Step 1 Accurately weigh the amounts of lead oxide, silicon dioxide, thallium oxide, zinc oxide, and lithium oxide by calculating, and uniformly mix and stir to obtain mixture A;
  • Step 2 Place mixture A obtained in step 1 in a sintering furnace to promote sintering to obtain mixture B, the sintering temperature of the sintering furnace is 1200°C, and the sintering time is 20 minutes;
  • Step 3 The mixture B obtained in step 2 is placed in a cooling roll for cooling treatment to obtain mixture C.
  • the rotating speed of the cooling roller is 7rmp, and the processing time of the cooling roller is 1h;
  • Step 4 The mixture C obtained in the step 3 is placed in a ball mill for ball milling to obtain the mixture D, the rotational speed of the ball mill is 350rmp, and the ball milling time is 2h;
  • Step 5 The mixture D obtained in step 4 is placed in a 250-mesh vibrating screen for sieving, and then the sieved mixture D is placed in an oven and dried at a temperature of 150 ° C for 2 hours to obtain the N-type silver aluminum Glass powder for paste.
  • the prepared glass powder for N-type silver-aluminum paste had a median particle size of 0.5 ⁇ m and a softening point of 300°C.
  • the glass powder for N-type silver aluminum paste of the present invention is the composition of formula (I):
  • the preparation method of a kind of N-type silver aluminum paste glass powder of the present invention is as follows:
  • Step 1 Accurately weigh the amounts of lead oxide, silicon dioxide, thallium oxide, zinc oxide, and lithium oxide by calculating, and uniformly mix and stir to obtain mixture A;
  • Step 2 Place mixture A obtained in step 1 in a sintering furnace to promote sintering to obtain mixture B, the sintering temperature of the sintering furnace is 1200°C, and the sintering time is 20 minutes;
  • Step 3 The mixture B obtained in step 2 is placed in a cooling roll for cooling treatment to obtain mixture C.
  • the rotating speed of the cooling roller is 7rmp, and the processing time of the cooling roller is 1h;
  • Step 4 The mixture C obtained in the step 3 is placed in a ball mill for ball milling to obtain the mixture D, the rotational speed of the ball mill is 350rmp, and the ball milling time is 2h;
  • Step 5 The mixture D obtained in step 4 is placed in a 250-mesh vibrating screen for sieving, and then the sieved mixture D is placed in an oven and dried at a temperature of 150 ° C for 2 hours to obtain the N-type silver aluminum Glass powder for paste.
  • the median particle size of the prepared glass powder for N-type silver-aluminum paste was 1.5 ⁇ m, and the softening point was 321°C.
  • the glass powder for N-type silver aluminum paste of the present invention is the composition of formula (I):
  • the preparation method of a kind of N-type silver aluminum paste glass powder of the present invention is as follows:
  • Step 1 Accurately weigh the amounts of lead oxide, silicon dioxide, thallium oxide, zinc chloride and potassium chloride by calculation, and mix and stir to obtain mixture A;
  • Step 2 Place the mixture A obtained in the first step in a sintering furnace to promote sintering to obtain the mixture B, the sintering temperature of the sintering furnace is 900 ° C, and the sintering time is 60 minutes;
  • Step 3 The mixture B obtained in step 2 is placed in a cooling roll for cooling treatment to obtain mixture C.
  • the rotating speed of the cooling roller is 7rmp, and the processing time of the cooling roller is 1h;
  • Step 4 The mixture C obtained in the step 3 is placed in a ball mill for ball milling to obtain the mixture D, the rotational speed of the ball mill is 300rmp, and the ball milling time is 6h;
  • Step 5 The mixture D obtained in step 4 is placed in a 250-mesh vibrating screen for sieving, and then the sieved mixture D is placed in an oven and dried at a temperature of 150 ° C for 2 hours to obtain the N-type silver aluminum Glass powder for paste.
  • the prepared glass powder for N-type silver-aluminum paste had a median particle size of 0.8 ⁇ m and a softening point of 341.2°C.
  • the glass powder of this comparative example does not contain thallium element, and the amount of lead element is the combination of thallium element and lead element in Example 1, and other operations are the same as those of Example 1.
  • the N-type silver-aluminum paste prepared in this comparative example is used for The median particle size of the glass powder is 0.5-2 ⁇ m, and the softening point is 300-450°C.
  • the N-type silver-aluminum pastes prepared from the glass frits of Examples 1-5 and Comparative Examples were screen-printed on a 156mm ⁇ 156mm N-type polycrystalline silicon wafer. After printing, it is dried and sintered at high temperature to test various properties, including open circuit voltage (Voc), photoelectric conversion efficiency (EFF), fill factor (FF), parallel resistance (Rsh), series resistance (Rs), short circuit current (Isc) ).
  • the test methods of each index are conventional methods in the field, and the specific test process and conditions all adopt unified test conditions, and the test results are shown in Table 1:
  • N-type silver-aluminum paste prepared from glass powder for N-type silver-aluminum paste in Example 1-5 of the present invention has good electrical performance characteristics.
  • EFF has excellent performance.

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Abstract

一种N型银铝浆用玻璃粉及其制备方法，包括含铅化合物、含硅化合物、含铊化合物和含锌化合物，其中含铊化合物和含铅化合物的复配使用使得玻璃粉具有好的熔银能力，且制备得到的银铝浆对太阳能电池硅片表面的浸润性好，含硅化合物为玻璃粉提供更加完整的网络结构，含锌化合物降低玻璃粉的软化温度，进一步降低制备得到的N型银铝浆烧结温度。该玻璃粉还含有含第一主族金属元素的化合物，该化合物可以和含锌化合物作用进一步降低玻璃粉的软化温度，进一步降低制备得到的N型银铝浆烧结温度，提高N型太阳能电池制备良率。

Description

一种N型银铝浆用玻璃粉及其制备方法 技术领域
本发明属于包含金属或合金的导电材料技术领域，具体涉及一种N型银铝浆用玻璃粉及其制备方法。
背景技术
对于N型太阳能电池银铝浆料来说，玻璃粉是决定接触电阻、表面蚀刻反应以及整个电池片电性能的重要因素，这就要求它具有良好的电学性能和机械性能。另外玻璃粉的种类以及用量也对开路电压以及高温烧结条件下浆料的填充因子有较大的影响。在太阳能电池制造工艺的烧结步骤中，银铝浆料中的玻璃粉通过腐蚀SiNx减反射膜层并和下层的硅接触粘合在一起，充分完全的蚀刻反应可以保证形成良好的欧姆接触。
虽然玻璃粉在浆料中占的比重比较小(1-5wt％)，但它在Ag-Si金属半导体接触形成过程中起到重要的作用，通过腐蚀SiNx减反射膜层与其发生蚀刻反应保证了其稳定的粘结性能。玻璃粉作为粘结相，不仅仅是在烧结过程中促进银铝浆与太阳能电池硅基板粘附在一起，同时也影响着导电功能相金属粉末的烧结动力学性能。正面电极银铝浆用玻璃粉除了要具备基本粘结相的相关性质外，还要能够在烧结过程中与氮化硅减反射膜蚀刻完全，烧结后在Ag和Si之间形成一层接触层，使银粉和硅基板能够形成良好的欧姆接触，以此来达到有效提高太阳能电池光电转换效率的目的。
中国专利CN200610011001.1公开了一种硅太阳能电池背场铝导电浆料组成及制备方法，在该技术中铊元素作为无机粘结剂在硅太阳能电池背场铝导电浆料的应用，该无机粘结剂能在铝电极与硅之间有良好的欧姆接触，从而提高光电转换效率，硅铝化合物层还可提高铝膜对硅基体附着强度。
中国专利CN201210123378.1公开了一种太阳能电池背电场用导电浆料、其制备方法及太阳能电池片，该技术中将含有铊元素和铝元素的铝-铊合金作为导电金属粉末，该组分制备的背电场金属膜表面光滑，外观优良，且形成的PP+层性能优异，电池的开路电压高，光电转换效率高，且制备的金属膜与硅片的附着力强，制备的太阳能电池片的弯曲度小。
发明内容
本发明提供了一种N型银铝浆用玻璃粉及其制备方法，该N型银铝浆用玻璃粉中含有铊元素能提供好的熔银能力，并且对太阳能电池用硅片的浸润性好，金属粉与硅表面良好的欧姆接触，本发明的具体内容如下：
本发明的目的在于提供一种N型银铝浆用玻璃粉，其技术点在于：所述N型银铝浆用玻璃粉包括含铅化合物、含硅化合物、含铊化合物和含锌化合物。
在本发明的有的实施例中，上述的所有化合物可以氧化物、卤化物、硝酸根化合物、亚硝酸根化合物、碳酸根化合物、碳酸氢根化合物、硫酸根化合物和磷酸根化合物中的至少一种。
在本发明的有的实施例中，上述的卤化物为氯化物、氟化物、溴化物和碘化物中的至少一种。
在本发明的有的实施例中，上述的卤化物为氯化物。
在本发明的有的实施例中，上述的N型银铝浆用玻璃粉还包括第一主族金属元素化合物。
在本发明的有的实施例中，上述的第一主族金属元素化合物为含锂化合物、含钠化合物、含钾化合物、含铷化合物和含铯化合物中的至少一种。
在本发明的有的实施例中，上述的N型银铝浆用玻璃粉为式(Ⅰ)的组合物：
Pb a-Si b-Tl c-Zn d-M e-O f，          式(Ⅰ)；
a、b、c、d、e和f表示每1mol所述N型银铝浆用玻璃粉中所含有的元素的物质的量，其中0.6mol≦a≦0.8mol，0.05mol≦b≦0.2mol，0.03mol≦c≦0.1mol，0.01mol≦d≦0.1mol，0.001mol≦e≦0.02mol，f为使Pb元素、Si元素、Tl元素、Zn元素和M元素组平衡的物质的量，其中M元素为锂元素、钠元素、钾元素、铷元素和铯元素中的至少一种。
在本发明的有的实施例中，上述的N型银铝浆用玻璃粉的中值粒径为0.5-2μm。
在本发明的有的实施例中，上述的N型银铝浆用玻璃粉的软化点为300-450℃。
本发明的另外一个目的在于提供一种N型银铝浆用玻璃粉，其技术点在于：所述玻璃粉的制备方法如下：
步骤一：通过计算精确称量含铅化合物、含硅化合物、含铊化合物和含锌化合物的量，将其通过混合搅拌均匀得到混合物A；
步骤二：将步骤一中得到的混合物A置于烧结炉中晋升烧结得到混合物B，所述烧结炉的烧结温度为900-1200℃，烧结时间为20-60min；
步骤三：将步骤二中得到的混合物B置于冷却辊中进行冷却处理得到混合物C。所述冷却辊的转速为3-7rmp，所述冷却辊的处理时间为1-2h；
步骤四：将步骤三中得到的混合物C置于球磨机中进行球磨处理得到混合物D，所述球磨机的转速为300-350rmp，球磨时间为2-6h；
步骤五：将步骤四中得到的混合物D置于150-250目的振动筛中进行筛分，然后将筛分后的混合物D置于烘箱中于80-150℃温度下烘干2-6h即得到所述N型银铝浆用玻璃粉。
与现有技术相比，本发明的有益效果在于：
本发明提供的一种N型银铝浆用玻璃粉包括含铅化合物、含硅化合物、含铊化合物和含锌化合物，其中含铊化合物和含铅化合物的复配使用使得玻璃粉具有好的熔银能力，且制备得到的银铝浆对太阳能电池硅片表面的浸润性好，含硅化合物为玻璃粉提供更加完整的网络结构，含锌化合物降低玻璃粉的软化温度，进一步降低制备得到的N型银铝浆烧结温度。本申请的N型银铝浆用玻璃粉还含有含第一主族金属元素的化合物，该化合物可以和含锌化合物作用进一步降低玻璃粉的软化温度，进一步降低制备得到的N型银铝浆烧结温度，提高N型太阳能电池制备良率。
附图说明
图1为本发明的一种N型银铝浆用玻璃粉制备的流程图；
图2为本发明实施例1制备得到的N型银铝浆用玻璃粉的DSC图。
具体实施方式
一种N型银铝浆用玻璃粉包括含铅化合物、含硅化合物、含铊化合物和含锌化合物。这里的化合物为氧化物、卤化物、硝酸根化合物、亚硝酸根化合物、碳酸根化合物、碳酸氢根化合物、硫酸根化合物和磷酸根化合物中的至少一种，优选本申请的卤化物为氯化物、氟化物、溴化物和碘化物中的至少一种，更优选本申请的卤化物为氯化物，含铊化合物和含铅化合物的复配使用使得玻璃粉具有好的熔银能力，且制备得到的银铝浆对太阳能电池硅片表面的浸润性好，含硅化合物为玻璃粉提供更加完整的网络结构，含锌化合物降低玻璃粉的软化温度，进一步降低制备得到的N型银铝浆烧结温度。本发明的N型银铝浆用玻璃粉还包括第一主族金属元素化合物，优选的本发明的第一主族化合物为锂化合物、含钠化合物、含钾化合物、含铷化合物和含铯化合物中的至少一种，该 化合物可以和含锌化合物作用进一步降低玻璃粉的软化温度，进一步降低制备得到的N型银铝浆烧结温度，提高N型太阳能电池制备良率。
本发明的制备得到的N型银铝浆用玻璃粉为式(Ⅰ)的组合物：
Pb a-Si b-Tl c-Zn d-M e-O f，         式(Ⅰ)；
a、b、c、d、e和f表示每1mol所述N型银铝浆用玻璃粉中所含有的元素的物质的量，其中0.6mol≦a≦0.8mol，0.05mol≦b≦0.2mol，0.03mol≦c≦0.1mol，0.01mol≦d≦0.1mol，0.001mol≦e≦0.02mol，f为使Pb元素、Si元素、Tl元素、Zn元素和M元素组平衡的物质的量，其中M元素为锂元素、钠元素、钾元素、铷元素和铯元素中的至少一种。制备得到的N型银铝浆用玻璃粉的中值粒径为0.5-2μm，软化点为300-450℃。
按照上述配方本发明的一种N型银铝浆用玻璃粉的制备方法如下：
步骤一：通过计算精确称量含铅化合物、含硅化合物、含铊化合物和含锌化合物的量，将其通过混合搅拌均匀得到混合物A；
步骤二：将步骤一中得到的混合物A置于烧结炉中晋升烧结得到混合物B，所述烧结炉的烧结温度为900-1200℃，烧结时间为20-60min；
步骤三：将步骤二中得到的混合物B置于冷却辊中进行冷却处理得到混合物C。所述冷却辊的转速为3-7rmp，所述冷却辊的处理时间为1-2h；
步骤四：将步骤三中得到的混合物C置于球磨机中进行球磨处理得到混合物D，所述球磨机的转速为300-350rmp，球磨时间为2-6h；
步骤五：将步骤四中得到的混合物D置于150-250目的振动筛中进行筛分，然后将筛分后的混合物D置于烘箱中于80-150℃温度下烘干2-6h即得到所述N型银铝浆用玻璃粉。
结合以下本发明的优选实施方法的详述以及包括的实施例可进一步地理解 本发明的内容。除非另有说明，本文中使用的所有技术及科学术语均具有与本申请所属领域普通技术人员的通常理解相同的含义。如果现有技术中披露的具体术语的定义与本申请中提供的任何定义不一致，则以本申请中提供的术语定义为准。
在本文中使用的，除非上下文中明确地另有指示，否则没有限定单复数形式的特征也意在包括复数形式的特征。还应理解的是，如本文所用术语“由…制备”与“包含”同义，“包括”、“包括有”、“具有”、“包含”和/或“包含有”，当在本说明书中使用时表示所陈述的组合物、步骤、方法、制品或装置，但不排除存在或添加一个或多个其它组合物、步骤、方法、制品或装置。此外，当描述本申请的实施方式时，使用“优选的”、“优选地”、“更优选的”等是指，在某些情况下可提供某些有益效果的本发明实施方案。然而，在相同的情况下或其他情况下，其他实施方案也可能是优选的。除此之外，对一个或多个优选实施方案的表述并不暗示其他实施方案不可用，也并非旨在将其他实施方案排除在本发明的范围之外。
实施例1
本发明的N型银铝浆用玻璃粉为式(Ⅰ)的组合物：
Pb a-Si b-Tl c-Zn d-Na e-O f，          式(Ⅰ)；
a、b、c、d、e和f表示每1mol所述N型银铝浆用玻璃粉中所含有的元素的物质的量，其中a＝0.7mol，b＝0.1mol，c＝0.065mol，d＝0.05，e＝0.01mol，f为使Pb元素、Si元素、Tl元素、Zn元素和M元素组平衡的物质的量。
按照上述配方本发明的一种N型银铝浆用玻璃粉的制备方法如下：
步骤一：通过计算精确称量二氧化铅、二氧化硅、氧化铊、氧化锌量和氧化钠，将其通过混合搅拌均匀得到混合物A；
步骤二：将步骤一中得到的混合物A置于烧结炉中晋升烧结得到混合物B，所述烧结炉的烧结温度为1000℃，烧结时间为40min；
步骤三：将步骤二中得到的混合物B置于冷却辊中进行冷却处理得到混合物C。所述冷却辊的转速为5rmp，所述冷却辊的处理时间为1h；
步骤四：将步骤三中得到的混合物C置于球磨机中进行球磨处理得到混合物D，所述球磨机的转速为325rmp，球磨时间为4h；
步骤五：将步骤四中得到的混合物D置于200目的振动筛中进行筛分，然后将筛分后的混合物D置于烘箱中于110℃温度下烘干4h即得到所述N型银铝浆用玻璃粉。制备得到的N型银铝浆用玻璃粉的中值粒径为1μm，软化点为321.96℃，如图2所示的本实施例的玻璃粉的DSC图。
实施例2
本发明的N型银铝浆用玻璃粉为式(Ⅰ)的组合物：
Pb a-Si b-Tl c-Zn d-K e-O f，           式(Ⅰ)；
a、b、c、d、e和f表示每1mol所述N型银铝浆用玻璃粉中所含有的元素的物质的量，其中a＝0.8mol，b＝0.2mol，c＝0.1mol，d＝0.1mol，e＝0.02mol，f为使Pb元素、Si元素、Tl元素、Zn元素和M元素组平衡的物质的量。
按照上述配方本发明的一种N型银铝浆用玻璃粉的制备方法如下：
步骤一：通过计算精确称量氧化铅、二氧化硅、氧化铊、氯化锌和氯化钾的量，将其通过混合搅拌均匀得到混合物A；
步骤二：将步骤一中得到的混合物A置于烧结炉中晋升烧结得到混合物B，所述烧结炉的烧结温度为900℃，烧结时间为60min；
步骤三：将步骤二中得到的混合物B置于冷却辊中进行冷却处理得到混合物C。所述冷却辊的转速为7rmp，所述冷却辊的处理时间为1h；
步骤四：将步骤三中得到的混合物C置于球磨机中进行球磨处理得到混合物D，所述球磨机的转速为300rmp，球磨时间为6h；
步骤五：将步骤四中得到的混合物D置于150目的振动筛中进行筛分，然后将筛分后的混合物D置于烘箱中于150℃温度下烘干2h即得到所述N型银铝浆用玻璃粉。制备得到的N型银铝浆用玻璃粉的中值粒径为0.5μm，软化点为450℃。
实施例3
本发明的N型银铝浆用玻璃粉为式(Ⅰ)的组合物：
Pb a-Si b-Tl c-Zn d-Li e-O f，          式(Ⅰ)；
a、b、c、d、e和f表示每1mol所述N型银铝浆用玻璃粉中所含有的元素的物质的量，其中a＝0.6mol，b＝0.05mol，c＝0.03mol，d＝0.01mol，e＝0.001mol，f为使Pb元素、Si元素、Tl元素、Zn元素和M元素组平衡的物质的量。
按照上述配方本发明的一种N型银铝浆用玻璃粉的制备方法如下：
步骤一：通过计算精确称量含氧化铅、二氧化硅、氧化铊、氧化锌、氧化锂的量，将其通过混合搅拌均匀得到混合物A；
步骤二：将步骤一中得到的混合物A置于烧结炉中晋升烧结得到混合物B，所述烧结炉的烧结温度为1200℃，烧结时间为20min；
步骤三：将步骤二中得到的混合物B置于冷却辊中进行冷却处理得到混合物C。所述冷却辊的转速为7rmp，所述冷却辊的处理时间为1h；
步骤四：将步骤三中得到的混合物C置于球磨机中进行球磨处理得到混合物D，所述球磨机的转速为350rmp，球磨时间为2h；
步骤五：将步骤四中得到的混合物D置于250目的振动筛中进行筛分，然后将筛分后的混合物D置于烘箱中于150℃温度下烘干2h即得到所述N型银铝 浆用玻璃粉。制备得到的N型银铝浆用玻璃粉的中值粒径为0.5μm，软化点为300℃。
实施例4
本发明的N型银铝浆用玻璃粉为式(Ⅰ)的组合物：
Pb a-Si b-Tl c-Zn d-Na e-O f，          式(Ⅰ)；
a、b、c、d、e和f表示每1mol所述N型银铝浆用玻璃粉中所含有的元素的物质的量，其中a＝0.7mol，b＝0.1mol，c＝0.065mol，d＝0.05，e＝0.01mol，f为使Pb元素、Si元素、Tl元素、Zn元素和M元素组平衡的物质的量。
按照上述配方本发明的一种N型银铝浆用玻璃粉的制备方法如下：
步骤一：通过计算精确称量含氧化铅、二氧化硅、氧化铊、氧化锌、氧化锂的量，将其通过混合搅拌均匀得到混合物A；
步骤二：将步骤一中得到的混合物A置于烧结炉中晋升烧结得到混合物B，所述烧结炉的烧结温度为1200℃，烧结时间为20min；
步骤三：将步骤二中得到的混合物B置于冷却辊中进行冷却处理得到混合物C。所述冷却辊的转速为7rmp，所述冷却辊的处理时间为1h；
步骤四：将步骤三中得到的混合物C置于球磨机中进行球磨处理得到混合物D，所述球磨机的转速为350rmp，球磨时间为2h；
步骤五：将步骤四中得到的混合物D置于250目的振动筛中进行筛分，然后将筛分后的混合物D置于烘箱中于150℃温度下烘干2h即得到所述N型银铝浆用玻璃粉。制备得到的N型银铝浆用玻璃粉的中值粒径为1.5μm，软化点为321℃。
实施例5
本发明的N型银铝浆用玻璃粉为式(Ⅰ)的组合物：
Pb a-Si b-Tl c-Zn d-K e-O f，         式(Ⅰ)；
a、b、c、d、e和f表示每1mol所述N型银铝浆用玻璃粉中所含有的元素的物质的量，其中a＝0.8mol，b＝0.2mol，c＝0.1mol，d＝0.1mol，e＝0.02mol，f为使Pb元素、Si元素、Tl元素、Zn元素和M元素组平衡的物质的量。
按照上述配方本发明的一种N型银铝浆用玻璃粉的制备方法如下：
步骤一：通过计算精确称量氧化铅、二氧化硅、氧化铊、氯化锌和氯化钾的量，将其通过混合搅拌均匀得到混合物A；
步骤二：将步骤一中得到的混合物A置于烧结炉中晋升烧结得到混合物B，所述烧结炉的烧结温度为900℃，烧结时间为60min；
步骤三：将步骤二中得到的混合物B置于冷却辊中进行冷却处理得到混合物C。所述冷却辊的转速为7rmp，所述冷却辊的处理时间为1h；
步骤四：将步骤三中得到的混合物C置于球磨机中进行球磨处理得到混合物D，所述球磨机的转速为300rmp，球磨时间为6h；
步骤五：将步骤四中得到的混合物D置于250目的振动筛中进行筛分，然后将筛分后的混合物D置于烘箱中于150℃温度下烘干2h即得到所述N型银铝浆用玻璃粉。制备得到的N型银铝浆用玻璃粉的中值粒径为0.8μm，软化点为341.2℃。
对比例1
本对比例的玻璃粉不含有铊元素，其中铅元素的物质的量为实施例1中铊元素和铅元素的综合，其余操作同实施例1，本对比例制备得到的N型银铝浆用玻璃粉的中值粒径为0.5-2μm，软化点为300-450℃。
实验例
将上述实施例1-5和对比例的玻璃粉制备的N型银铝浆用丝网印刷于 156mm×156mmN型多晶硅片上。印刷后经烘干，高温烧结，测试各项性能，包括开路电压(Voc)、光电转换效率(EFF)、填充因子(FF)、并联电阻(Rsh)、串联电阻(Rs)、短路电流(Isc)。各项指标的测试方法均为本领域常规方法，具体测试过程与条件均采用统一测试条件，测试结果见表1：
表1
  Voc/V Rsh/Ω Rs/Ω Isc/A EFF/％ FF/％
实施例1 0.6680 265.51 0.0023 9.5612 21.56 79.65
实施例2 0.6683 264.15 0.0024 9.4625 21.64 79.86
实施例3 0.6675 263.56 0.0025 9.6574 21.61 80.56
实施例4 0.6679 265.2 0.0021 9.5487 21.57 80.23
实施例5 0.6679 264.2 0.0026 9.6874 21.58 80.56
对比例 0.6656 282.6 0.00211 9.3254 21.30 79.21
由表1可知，本发明实施例1-5N型银铝浆用玻璃粉制备得到的N型银铝浆具有良好的电性能特点，在填充因子FF，接触电阻Rs、开路电压Voc和综合电性能EFF方面均具有优异的性能体现。
最后指出，以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本发明的保护范围之内。

Claims (10)

  1. 一种N型银铝浆用玻璃粉，其特征在于：所述N型银铝浆用玻璃粉包括含铅化合物、含硅化合物、含铊化合物和含锌化合物。
  2. 根据权利要求1所述的一种N型银铝浆用玻璃粉，其特征在于：所述化合物为氧化物、卤化物、硝酸根化合物、亚硝酸根化合物、碳酸根化合物、碳酸氢根化合物、硫酸根化合物和磷酸根化合物中的至少一种。
  3. 根据权利要求2所述的一种N型银铝浆用玻璃粉，其特征在于：所述卤化物为氯化物、氟化物、溴化物和碘化物中的至少一种。
  4. 根据权利要求3所述的一种N型银铝浆用玻璃粉，其特征在于：所述卤化物为氯化物。
  5. 根据权利要求1所述的一种N型银铝浆用玻璃粉，其特征在于：所述N型银铝浆用玻璃粉还包括第一主族金属元素化合物。
  6. 根据权利要求5所述的一种N型银铝浆用玻璃粉，其特征在于：所述第一主族金属元素化合物为含锂化合物、含钠化合物、含钾化合物、含铷化合物和含铯化合物中的至少一种。
  7. 根据权利要求1所述一种N型银铝浆用玻璃粉，其特征在于：所述N型银铝浆用玻璃粉为式(Ⅰ)的组合物：
    Pb a-Si b-Tl c-Zn d-M e-O f，     式(Ⅰ)；
    a、b、c、d、e和f表示每1mol所述N型银铝浆用玻璃粉中所含有的元素的物质的量，其中0.6mol≦a≦0.8mol，0.05mol≦b≦0.2mol，0.03mol≦c≦0.1mol，0.01mol≦d≦0.1mol，0.001mol≦e≦0.02mol，f为使Pb元素、Si元素、Tl元素、Zn元素和M元素组平衡的物质的量，其中M元素为锂元素、钠元素、钾元素、铷元素和铯元素中的至少一种。
  8. 根据权利要求7所述的一种N型银铝浆用玻璃粉，其特征在于：所述N型银 铝浆用玻璃粉的中值粒径为0.5-2μm。
  9. 根据权利要求7所述的一种N型银铝浆用玻璃粉，其特征在于：所述N型银铝浆用玻璃粉的软化点为300-450℃。
  10. 根据权利要求1所述的一种N型银铝浆用玻璃粉，其特征在于：所述玻璃粉的制备方法如下：
    步骤一：通过计算精确称量含铅化合物、含硅化合物、含铊化合物和含锌化合物的量，将其通过混合搅拌均匀得到混合物A；
    步骤二：将步骤一中得到的混合物A置于烧结炉中晋升烧结得到混合物B，所述烧结炉的烧结温度为900-1200℃，烧结时间为20-60min；
    步骤三：将步骤二中得到的混合物B置于冷却辊中进行冷却处理得到混合物C。所述冷却辊的转速为3-7rmp，所述冷却辊的处理时间为1-2h；
    步骤四：将步骤三中得到的混合物C置于球磨机中进行球磨处理得到混合物D，所述球磨机的转速为300-350rmp，球磨时间为2-6h；
    步骤五：将步骤四中得到的混合物D置于150-250目的振动筛中进行筛分，然后将筛分后的混合物D置于烘箱中于80-150℃温度下烘干2-6h即得到所述N型银铝浆用玻璃粉。
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