CN113461338A - Nano glass powder for PERC back silver and preparation method thereof - Google Patents

Nano glass powder for PERC back silver and preparation method thereof Download PDF

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Publication number
CN113461338A
CN113461338A CN202110878473.1A CN202110878473A CN113461338A CN 113461338 A CN113461338 A CN 113461338A CN 202110878473 A CN202110878473 A CN 202110878473A CN 113461338 A CN113461338 A CN 113461338A
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glass powder
oxide
drying
ball
preparation
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冷青松
张群
丰昭
李鹏
刘瑞鸿
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Jiangsu Zhengneng Electronic Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C12/00Powdered glass; Bead compositions
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B02CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02CCRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C17/00Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
    • B02C17/10Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls with one or a few disintegrating members arranged in the container
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B02CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02CCRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C17/00Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
    • B02C17/18Details
    • B02C17/20Disintegrating members

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  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Glass Compositions (AREA)

Abstract

The invention relates to the technical field of preparation of nano glass powder, in particular to nano glass powder for PERC back silver and a preparation method thereof, which comprises the following steps of weighing lead oxide, boron oxide, silicon dioxide, aluminum oxide, phosphorus pentoxide, antimony trioxide, germanium oxide or/and non-framework element oxide according to a certain mass ratio; mixing the ingredients in the pair by using a mixer; putting the mixed materials into a crucible for firing; quenching the fired material by using a double-roller machine; performing ball milling on the quenched material; drying the ball-milled glass powder; transferring the dried glass powder into a sand mill for fine grinding of the glass powder; drying the sanded glass powder by using freeze drying equipment; and (4) performing airflow dispersion on the dried powder by using airflow dispersion equipment to obtain a finished product of the nano glass powder. The conversion efficiency of the nano glass powder on the PERC back silver can be relatively improved by over 0.05 percent through the optimization of the components and the process, and good welding tension is ensured.

Description

Nano glass powder for PERC back silver and preparation method thereof
Technical Field
The invention relates to the technical field of preparation of nano glass powder, in particular to nano glass powder for PERC back silver and a preparation method thereof.
Background
The chemical and physical action performance of the powder can be greatly changed through the nanocrystallization of the powder, the amount of the glass powder after the nanocrystallization is more prone to be calculated by number rather than the traditional mass calculation, therefore, the amount of the glass powder can be remarkably reduced, the corrosion of the PERC back silver to a back passivation layer is lower, and the effect of finally improving the conversion efficiency of the battery is achieved. In addition, due to the determination of the basic preparation process of the glass powder, only the glass powder meeting certain specific conditions can be subjected to batch nano-production.
The defects and shortcomings of the prior art are as follows: the glass powder industry always belongs to a smaller industry, the effect of the formula is considered to be the core in the industry, the effect of the preparation process is rarely researched, the development of the process is slower than that of other powder industries, and a real nano preparation process technology is rarely provided.
Disclosure of Invention
In order to solve the technical problems, the invention provides a nano glass powder for PERC back silver and a preparation method thereof.
The invention provides the following technical scheme: a preparation method of nano glass powder for PERC back silver comprises the following steps:
s1, weighing ingredients: weighing lead oxide, boron oxide, silicon dioxide, aluminum oxide, phosphorus pentoxide, antimony trioxide, germanium oxide or/and non-framework element oxide according to a certain mass ratio;
s2, mixing materials: mixing the ingredients in the S1 by using a mixer;
s3, firing: putting the mixed material in the S2 into a crucible for firing;
s4 quenching: quenching the fired material in S3 by using a double-roller machine;
s5, ball milling: ball milling the quenched material in S4;
s6, drying I: drying the ball-milled glass powder;
s7, sanding: transferring the glass powder dried in the step S6 to a sand mill for fine grinding of the glass powder;
s8, drying II: drying the sanded glass powder by using freeze drying equipment;
s9, airflow milling: and (4) performing airflow dispersion on the dried powder in the S8 by using airflow dispersion equipment to obtain a nano glass powder finished product.
Further, in S1, the mass ratio of each substance is: 40-70 wt% of lead oxide, 5-40 wt% of boron oxide, 10-40 wt% of silicon dioxide, 0-20 wt% of aluminum oxide, 0-10 wt% of phosphorus pentoxide, 0-10 wt% of antimony trioxide, 0-10 wt% of germanium oxide and 0-20 wt% of non-framework element oxide.
Further, the non-framework element oxide includes bismuth oxide, copper oxide, manganese oxide, titanium dioxide or/and zinc oxide.
Further, in S2, the mixer may have a V-shape, a conical shape, or a double-conical shape.
Further, in S3, the melting temperature is 1100-1700 ℃, and the melting time is 1-3 h.
Further, in S5, a ball milling tank made of zirconia is used in combination with zirconia balls and deionized water for ball milling; the zirconia ball comprises the materials and water with the weight ratio of (1.5-3) to (1) (0.2-0.5), and zirconia balls with three particle sizes, namely phi 16 to phi 6 to phi 2, with the weight ratio of (0.3-0.6) to (1) (0.3-0.6); the volume of the zirconia balls, the materials and the water is limited in the range of 1/3-2/3 of the ball milling tank; the dispersant accounts for 0.05 to 0.5 weight percent of the material; the ball milling time is 2-6h, and the grain diameter D50 of the ball milled glass powder is controlled to be less than 2 mu m.
Further, the dispersant comprises a titanate coupling agent, an aluminate coupling agent or/and BYK 110.
Further, in S7, the medium is sanded by absolute ethyl alcohol, the weight ratio of the glass powder to the absolute ethyl alcohol is 1 (1-10), the sanding time is 12-24h, and the ratio after sanding is controlled to be 20m2More than g.
The nano glass powder is prepared according to the preparation method.
The invention relates to a nano glass powder for PERC back silver and a preparation method thereof, and the nano glass powder has the beneficial effects that: 1. not all the glass powder can be nano-sized, and the components of the glass powder are limited to ensure that the glass powder has good glass after being meltedThe state of chemical reaction, mainly consisting of oxides of elements capable of forming a glass skeleton, such as lead oxide, boron oxide, silicon dioxide, aluminum oxide, phosphorus pentoxide, antimony trioxide, germanium oxide; limiting the content of oxides of other elements not having a glass skeleton to be lower than 20% so as to reduce the generation of coarse crystals after glass quenching; the glass powder with more coarse crystals has poor nano effect; 2. through three core processes of ball milling, sand milling and air milling of the cores and fine control points, 20m is prepared2The nano glass powder subjected to surface treatment is more than g, so that the nano characteristic of the glass powder is ensured; the ball milling is preliminary thinning, so that the glass powder can reach the micron level; the glass powder can reach the nanometer level by sanding; the jet mill can disperse the glass powder, so that the nano-scale powder is not agglomerated and has the nano-characteristic; 3. the conversion efficiency of the nano glass powder on the PERC back silver can be relatively improved by more than 0.05% through the optimization of the components and the process, and good welding tension is ensured.
Detailed Description
The conception, the specific structure and the technical effects of the present invention will be clearly and completely described in the following with reference to the embodiments, so that the objects, the schemes and the effects of the present invention can be fully understood.
Example 1
S1, weighing ingredients: weighing 40 wt% of lead oxide, 20 wt% of boron oxide, 15 wt% of silicon dioxide, 5 wt% of phosphorus pentoxide, 5 wt% of antimony trioxide, 10 wt% of bismuth oxide and 5 wt% of titanium dioxide according to a certain mass ratio;
s2, mixing materials: mixing the ingredients in the S1 by using a V-shaped mixer;
s3, firing: putting the mixed material in the S2 into a crucible for firing; wherein the melting temperature is 1200 ℃, and the melting time is 1 h;
s4 quenching: quenching the fired material in S3 by using a double-roller machine;
s5, ball milling: ball milling the quenched material in S4; wherein, zirconia ball: materials: the specific gravity of water is 3:1:0.5, the weight ratio of zirconia balls with three particle sizes is phi 16: phi 6: phi 2 is 0.6:1:0.4, the total volume of the zirconia balls, materials and water is about 1/2 of a ball milling tank, a titanate coupling agent accounts for 0.3 wt% of the materials, and the ball milling time is 6 hours, so that the particle size of glass powder is 0.8 mu m;
s6, drying I: drying the ball-milled glass powder;
s7, sanding: transferring the glass powder dried in the step S6 to a sand mill for fine grinding of the glass powder; wherein the medium is sanded by absolute ethyl alcohol, the weight ratio of the glass powder to the absolute ethyl alcohol is 1:2, the sanding time is 24 hours, and the ratio after sanding is controlled to be 38-40 m2/g;
S8, drying II: drying the sanded glass powder by using freeze drying equipment;
s9, airflow milling: and (4) performing airflow dispersion on the dried powder in the S8 by using airflow dispersion equipment to obtain a nano glass powder finished product.
Taking the ball-milled glass powder and marking as A1; the glass powder after ball milling and sanding is marked as A2; the glass powder after ball milling, sand milling and air flow milling is marked as A3.
Table 1 the same formulation of PERC back silver was prepared using a1, a2, A3 glass frit, and the results of testing the conversion efficiency and the solder pull were as follows:
Figure BDA0003198756080000041
in the embodiment, when the usage amount of the nano glass powder in the PERC back silver is 0.5 wt%, the conversion efficiency of A3 can be improved by more than 0.05% compared with that of A1 or A2, and good welding tension is ensured.
Example 2
S1, weighing ingredients: weighing 60 wt% of lead oxide, 10 wt% of boron oxide, 20 wt% of silicon dioxide, 3 wt% of aluminum oxide, 2 wt% of germanium oxide, 2 wt% of zinc oxide and 3 wt% of copper oxide according to a certain mass ratio;
s2, mixing materials: mixing the ingredients in the S1 by using a V-shaped mixer;
s3, firing: putting the mixed material in the S2 into a crucible for firing; wherein the melting temperature is 1300 ℃, and the melting time is 1 h;
s4 quenching: quenching the fired material in S3 by using a double-roller machine;
s5, ball milling: ball milling the quenched material in S4; wherein, zirconia ball: materials: the specific gravity of water is 2:1:0.5, the weight ratio of zirconia balls with three particle sizes of phi 16: phi 6: phi 2 is 0.5:1:0.5, the total volume of the zirconia balls, materials and water is about 1/2 of a ball milling tank, a titanate coupling agent accounts for 0.2 wt% of the materials, and the ball milling time is 3 hours, so that the particle size of glass powder is 1.6 mu m;
s6, drying I: drying the ball-milled glass powder;
s7, sanding: transferring the glass powder dried in the step S6 to a sand mill for fine grinding of the glass powder; wherein the medium is sand-milled by absolute ethyl alcohol, the weight ratio of the glass powder to the absolute ethyl alcohol is 1:5, the sand-milling time is 16h, and the ratio after sand-milling is controlled to be 26-28 m2/g;
S8, drying II: drying the sanded glass powder by using freeze drying equipment;
s9, airflow milling: and (4) performing airflow dispersion on the dried powder in the S8 by using airflow dispersion equipment to obtain a nano glass powder finished product.
Table 2 the same formulation of PERC back silver was prepared using B1, B2, B3 glass frit, and the results of testing the conversion efficiency and the solder pull were as follows:
Figure BDA0003198756080000051
in the embodiment, when the usage amount of the nano glass powder in the PERC back silver is 0.5 wt%, the conversion efficiency of B3 can be improved by more than 0.05% compared with that of B1 or B2, and good welding tension is ensured.
Example 3
S1, weighing ingredients: weighing 70 wt% of lead oxide, 5 wt% of boron oxide, 10 wt% of silicon dioxide, 1 wt% of aluminum oxide, 8 wt% of germanium oxide and 6 wt% of manganese oxide according to a certain mass ratio;
s2, mixing materials: mixing the ingredients in the S1 by using a V-shaped mixer;
s3, firing: putting the mixed material in the S2 into a crucible for firing; wherein the melting temperature is 1100 ℃, and the melting time is 1 h;
s4 quenching: quenching the fired material in S3 by using a double-roller machine;
s5, ball milling: ball milling the quenched material in S4; wherein, zirconia ball: materials: the specific gravity of water is 1.5:1:0.5, the weight ratio of zirconia balls with three particle sizes is phi 16: phi 6: phi 2 is 0.4:1:0.6, the total volume of the zirconia balls, materials and water is about 1/2 of a ball milling tank, a titanate coupling agent accounts for 0.1 wt% of the materials, and the ball milling time is 2 hours, so that the particle size of glass powder is 1.8 mu m;
s6, drying I: drying the ball-milled glass powder;
s7, sanding: transferring the glass powder dried in the step S6 to a sand mill for fine grinding of the glass powder; wherein the medium is sand-milled by absolute ethyl alcohol, the weight ratio of the glass powder to the absolute ethyl alcohol is 1:10, the sand-milling time is 12h, and the ratio after sand-milling is controlled to be 22-24 m2/g;
S8, drying II: drying the sanded glass powder by using freeze drying equipment;
s9, airflow milling: and (4) performing airflow dispersion on the dried powder in the S8 by using airflow dispersion equipment to obtain a nano glass powder finished product.
Table 3 the same formulation of PERC back silver was prepared using C1, C2, C3 glass frits, and the results of testing the conversion efficiency and the solder pull were as follows:
Figure BDA0003198756080000061
in the embodiment, when the usage amount of the nano glass powder in the PERC back silver is 0.5 wt%, the conversion efficiency of C3 can be improved by more than 0.05% compared with that of C1 or C2, and good welding tension is ensured.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (9)

1. The preparation method of the nano glass powder for PERC back silver is characterized by comprising the following steps:
s1, weighing ingredients: weighing lead oxide, boron oxide, silicon dioxide, aluminum oxide, phosphorus pentoxide, antimony trioxide, germanium oxide or/and non-framework element oxide according to a certain mass ratio;
s2, mixing materials: mixing the ingredients in the S1 by using a mixer;
s3, firing: putting the mixed material in the S2 into a crucible for firing;
s4 quenching: quenching the fired material in S3 by using a double-roller machine;
s5, ball milling: ball milling the quenched material in S4;
s6, drying I: drying the ball-milled glass powder;
s7, sanding: transferring the glass powder dried in the step S6 to a sand mill for fine grinding of the glass powder;
s8, drying II: drying the sanded glass powder by using freeze drying equipment;
s9, airflow milling: and (4) performing airflow dispersion on the dried powder in the S8 by using airflow dispersion equipment to obtain a nano glass powder finished product.
2. The preparation method according to claim 1, wherein in S1, the mass ratio of each substance is as follows: 40-70 wt% of lead oxide, 5-40 wt% of boron oxide, 10-40 wt% of silicon dioxide, 0-20 wt% of aluminum oxide, 0-10 wt% of phosphorus pentoxide, 0-10 wt% of antimony trioxide, 0-10 wt% of germanium oxide and 0-20 wt% of non-framework element oxide.
3. The method of claim 2, wherein the non-framework element oxide comprises bismuth oxide, copper oxide, manganese oxide, titanium dioxide, or/and zinc oxide.
4. The method of claim 1, wherein in S2, the mixer has a V-shape, a conical shape or a double-conical shape.
5. The method as claimed in claim 1, wherein the melting temperature is 1100-1700 ℃ and the melting time is 1-3h in S3.
6. The method according to claim 1, wherein in S5, a zirconia ball mill pot is used with zirconia balls and deionized water for ball milling; the zirconia ball comprises the materials and water with the weight ratio of (1.5-3) to (1) (0.2-0.5), and zirconia balls with three particle sizes, namely phi 16 to phi 6 to phi 2, with the weight ratio of (0.3-0.6) to (1) (0.3-0.6); the volume of the zirconia balls, the materials and the water is limited in the range of 1/3-2/3 of the ball milling tank; the dispersant accounts for 0.05 to 0.5 weight percent of the material; the ball milling time is 2-6h, and the grain diameter D50 of the ball milled glass powder is controlled to be less than 2 mu m.
7. The method of claim 6, wherein the dispersant comprises a titanate coupling agent, an aluminate coupling agent, or/and BYK 110.
8. The preparation method according to claim 1, wherein in S7, the media is sand-milled by using absolute ethyl alcohol, the weight ratio of the glass powder to the absolute ethyl alcohol is 1 (1-10), the sand-milling time is 12-24h, and the ratio after sand-milling is controlled to be 20m2More than g.
9. A nano glass frit, characterized by being prepared by the preparation method according to any one of claims 1 to 8.
CN202110878473.1A 2021-08-05 2021-08-05 Nano glass powder for PERC back silver and preparation method thereof Pending CN113461338A (en)

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Application publication date: 20211001