CN104143370A - Calcium oxide and zirconia composite conductive silver paste and manufacturing method thereof - Google Patents
Calcium oxide and zirconia composite conductive silver paste and manufacturing method thereof Download PDFInfo
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- CN104143370A CN104143370A CN201410316478.5A CN201410316478A CN104143370A CN 104143370 A CN104143370 A CN 104143370A CN 201410316478 A CN201410316478 A CN 201410316478A CN 104143370 A CN104143370 A CN 104143370A
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Abstract
The invention discloses calcium oxide and zirconia composite conductive silver paste which is characterized by comprising the following raw materials of, by weight, 40-50 parts of silver powder, 2-4 parts of calcium oxide, 3-5 parts of zirconia, 0.2-0.5 part of methyltrimethoxysilane, 0.3-0.6 part of aluminium potassium sulfate, 1-3 parts of hydroxypropyl starch ether, 2.3-3.6 parts of iso-tridecanol polyoxyethylene ether phosphate, 2.4-4.5 parts of tetraethylortho silicate, 1.2-3.4 parts of polyurethane acrylic resin, 2.3-4.7 parts of normal butanol, 30-40 parts of additives and a proper amount of water. According to the paste, the calcium oxide and the zirconia are added to conductive silver paste, so that strength and conductivity of the conductive silver paste are improved; the polyurethane acrylic resin is added, so that thixotropy of the paste is enhanced, layering of the paste is reduced, and stability of silver powder particles in the paste is improved.
Description
Technical field
The present invention relates to conductive silver paste field, be specifically related to compound conductive silver paste of a kind of calcium oxide/zirconia and preparation method thereof.
Background technology
Conductive silver paste refers to and is printed on conduction stock, make it the silver slurry that there is conduction current and get rid of accumulate static charge ability, be to be generally imprinted on the non-conductive stocks such as plastics, glass, pottery or cardboard, it is made up of electroconductive stuffing, binder, solvent and additive.The characteristic that conductive silver paste need to possess has: conductivity (antistatic behaviour) is good, strong adhesion, printing adaptability are good and the excellent characteristic of solvent resistance, and existing conductive silver paste has a lot of shortcomings in the market, not only contain lead, cadmium etc. and poisonous, contaminated environment, and use conduction stock on time adhesive force low, soldering resistance is not good, sintering character is poor.
Summary of the invention
Object of the present invention is just to provide compound conductive silver paste of a kind of calcium oxide/zirconia and preparation method thereof, to overcome the deficiencies in the prior art.
The object of the present invention is achieved like this:
The conductive silver paste that a kind of calcium oxide/zirconia is compound, it is characterized in that, made by the raw material of following weight portion: silver powder 40-50, calcium oxide 2-4, zirconia 3-5, methyltrimethoxy silane 0.2-0.5, alum 0.3-0.6, hydroxypropyl starch ether 1-3, different tridecanol polyoxyethylene ether phosphate 2.3-3.6, tetraethoxysilane 2.4-4.5, polyurethane acrylic resin 1.2-3.4, n-butanol 2.3-4.7, auxiliary agent 30-40, suitable quantity of water.
Described auxiliary agent is made up of following raw materials in part by weight: silica 1-2, zinc oxide 3-4, celluloid 1.1-2.2, rilanit special 0.3-0.5, stearic acid 0.4-0.7, organosiloxane 0.1-0.3, turpentine alcohol 15-20, the molten acid anhydride acetic acid esters of butyl 10-15, its preparation method is silicon dioxide, zinc oxide to be put into calciner at 520-610 DEG C, calcine 1-2 hour, taking-up is cooled to room temperature, adds celluloid to grind 20-40 minute; Molten butyl acid anhydride acetic acid esters, turpentine alcohol, organosiloxane are stirred and evenly mixed, at 140-180 DEG C, react 2-3 hour, be cooled to 80-100 DEG C, add rilanit special, stearic acid, keep temperature to stir 3-4 hour; Above each product is mixed, grind and make 300-400 order slurry and get final product for 2-4 hour.
The preparation method of the compound conductive silver paste of described a kind of calcium oxide/zirconia, is characterized in that comprising the following steps:
(1) get hydroxypropyl starch ether and put into suitable quantity of water and stir into paste, be heated to gelatinization, put into zirconia, alum grinds and within 1-2 hour, makes 200-300 order slurry, spraying is dry, sends in calciner sintering 2-3 hour at 470-580 DEG C;
(2) getting n-butanol, tetraethoxysilane puts into reactor and is heated to 85-100 DEG C and stirs and evenly mixs, insulated and stirred 30-50 minute, add again different tridecanol polyoxyethylene ether phosphate, polyurethane acrylic resin, methyltrimethoxy silane stirring reaction 1-2 hour, be cooled to 40-50 DEG C and add calcium oxide to grind pulping;
(3) step (1), (2) reaction mass and other leftover materials are mixed, be warming up to 100-120 DEG C, stirring reaction 1-2 hour, cooling, grinding to form particle diameter is 10-20 μ m slurry grain, to obtain final product.
The present invention has following beneficial effect: the present invention by adding calcium oxide and zirconia in conductive silver paste, intensity and the conductivity of conductive silver paste are improved, add polyurethane acrylic resin, increase the thixotropy of slurry, reduce the layering of slurry, improved the stability of silver powder particles in slurry.
Embodiment
The described compound conductive silver paste of a kind of calcium oxide/zirconia, it is characterized in that, made by the raw material of following weight portion: silver powder 44, calcium oxide 4, zirconia 3, methyltrimethoxy silane 0.5, alum 0.3, hydroxypropyl starch ether 3, different tridecanol polyoxyethylene ether phosphate 2.7, tetraethoxysilane 3.5, polyurethane acrylic resin 3.4, n-butanol 2.3, auxiliary agent 33, suitable quantity of water.
Described auxiliary agent is made up of following raw materials in part by weight: silica 1 .5, zinc oxide 4, celluloid 1.9, rilanit special 0.3, stearic acid 0.4, organosiloxane 0.1, turpentine alcohol 16, the molten acid anhydride acetic acid esters 13 of butyl, its preparation method is silicon dioxide, zinc oxide to be put into calciner at 520-610 DEG C, calcine 1-2 hour, taking-up is cooled to room temperature, adds celluloid to grind 20-40 minute; Molten butyl acid anhydride acetic acid esters, turpentine alcohol, organosiloxane are stirred and evenly mixed, at 140-180 DEG C, react 2-3 hour, be cooled to 80-100 DEG C, add rilanit special, stearic acid, keep temperature to stir 3-4 hour; Above each product is mixed, grind and make 300-400 order slurry and get final product for 2-4 hour.
Manufacture method comprises the following steps:
(1) get hydroxypropyl starch ether and put into suitable quantity of water and stir into paste, be heated to gelatinization, put into zirconia, alum grinds and within 1-2 hour, makes 200-300 order slurry, spraying is dry, sends in calciner sintering 2-3 hour at 470-580 DEG C;
(2) getting n-butanol, tetraethoxysilane puts into reactor and is heated to 85-100 DEG C and stirs and evenly mixs, insulated and stirred 30-50 minute, add again different tridecanol polyoxyethylene ether phosphate, polyurethane acrylic resin, methyltrimethoxy silane stirring reaction 1-2 hour, be cooled to 40-50 DEG C and add calcium oxide to grind pulping;
(3) step (1), (2) reaction mass and other leftover materials are mixed, be warming up to 100-120 DEG C, stirring reaction 1-2 hour, cooling, grinding to form particle diameter is 10-20 μ m slurry grain, to obtain final product.
The technical indicator of processing the conductive silver paste obtaining by above-described embodiment is as follows:
(1) viscosity: 50-100PaS(Brookfield, 10RPM);
(2) sheet resistance: < 5m Ω/c;
(3) plumbous cadmium content: < 100ppm;
(4) solderability excellent, burnt in a heap easily separated, printing adaptability good and solvent resistance is excellent.
Claims (2)
1. the conductive silver paste that calcium oxide/zirconia is compound, it is characterized in that, made by the raw material of following weight portion: silver powder 40-50, calcium oxide 2-4, zirconia 3-5, methyltrimethoxy silane 0.2-0.5, alum 0.3-0.6, hydroxypropyl starch ether 1-3, different tridecanol polyoxyethylene ether phosphate 2.3-3.6, tetraethoxysilane 2.4-4.5, polyurethane acrylic resin 1.2-3.4, n-butanol 2.3-4.7, auxiliary agent 30-40, suitable quantity of water; Described auxiliary agent is made up of following raw materials in part by weight: silica 1-2, zinc oxide 3-4, celluloid 1.1-2.2, rilanit special 0.3-0.5, stearic acid 0.4-0.7, organosiloxane 0.1-0.3, turpentine alcohol 15-20, the molten acid anhydride acetic acid esters of butyl 10-15, its preparation method is silicon dioxide, zinc oxide to be put into calciner at 520-610 DEG C, calcine 1-2 hour, taking-up is cooled to room temperature, adds celluloid to grind 20-40 minute; Molten butyl acid anhydride acetic acid esters, turpentine alcohol, organosiloxane are stirred and evenly mixed, at 140-180 DEG C, react 2-3 hour, be cooled to 80-100 DEG C, add rilanit special, stearic acid, keep temperature to stir 3-4 hour; Above each product is mixed, grind and make 300-400 order slurry and get final product for 2-4 hour.
2. the manufacture method of the compound conductive silver paste of a kind of calcium oxide/zirconia according to claim 1, is characterized in that comprising the following steps:
(1) get hydroxypropyl starch ether and put into suitable quantity of water and stir into paste, be heated to gelatinization, put into zirconia, alum grinds and within 1-2 hour, makes 200-300 order slurry, spraying is dry, sends in calciner sintering 2-3 hour at 470-580 DEG C;
(2) getting n-butanol, tetraethoxysilane puts into reactor and is heated to 85-100 DEG C and stirs and evenly mixs, insulated and stirred 30-50 minute, add again different tridecanol polyoxyethylene ether phosphate, polyurethane acrylic resin, methyltrimethoxy silane stirring reaction 1-2 hour, be cooled to 40-50 DEG C and add calcium oxide to grind pulping;
(3) step (1), (2) reaction mass and other leftover materials are mixed, be warming up to 100-120 DEG C, stirring reaction 1-2 hour, cooling, grinding to form particle diameter is 10-20 μ m slurry grain, to obtain final product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410316478.5A CN104143370A (en) | 2014-07-05 | 2014-07-05 | Calcium oxide and zirconia composite conductive silver paste and manufacturing method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410316478.5A CN104143370A (en) | 2014-07-05 | 2014-07-05 | Calcium oxide and zirconia composite conductive silver paste and manufacturing method thereof |
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| CN104143370A true CN104143370A (en) | 2014-11-12 |
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| CN201410316478.5A Pending CN104143370A (en) | 2014-07-05 | 2014-07-05 | Calcium oxide and zirconia composite conductive silver paste and manufacturing method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104376894A (en) * | 2014-11-26 | 2015-02-25 | 江苏欧耐尔新型材料有限公司 | Solar cell conductive positive silver pulp |
-
2014
- 2014-07-05 CN CN201410316478.5A patent/CN104143370A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104376894A (en) * | 2014-11-26 | 2015-02-25 | 江苏欧耐尔新型材料有限公司 | Solar cell conductive positive silver pulp |
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| C06 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20141112 |
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| WD01 | Invention patent application deemed withdrawn after publication |