CN113658742B - Organic gold conductor slurry - Google Patents
Organic gold conductor slurry Download PDFInfo
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- CN113658742B CN113658742B CN202111223803.XA CN202111223803A CN113658742B CN 113658742 B CN113658742 B CN 113658742B CN 202111223803 A CN202111223803 A CN 202111223803A CN 113658742 B CN113658742 B CN 113658742B
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- 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
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41J—TYPEWRITERS; SELECTIVE PRINTING MECHANISMS, i.e. MECHANISMS PRINTING OTHERWISE THAN FROM A FORME; CORRECTION OF TYPOGRAPHICAL ERRORS
- B41J2/00—Typewriters or selective printing mechanisms characterised by the printing or marking process for which they are designed
- B41J2/315—Typewriters or selective printing mechanisms characterised by the printing or marking process for which they are designed characterised by selective application of heat to a heat sensitive printing or impression-transfer material
- B41J2/32—Typewriters or selective printing mechanisms characterised by the printing or marking process for which they are designed characterised by selective application of heat to a heat sensitive printing or impression-transfer material using thermal heads
- B41J2/335—Structure of thermal heads
- B41J2/3355—Structure of thermal heads characterised by materials
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- Spectroscopy & Molecular Physics (AREA)
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Abstract
The invention discloses organic gold conductor slurry which comprises the following components in percentage by mass: 40-60% of resin acid gold and metal organic2-10% of mixture, 30-50.9% of organic carrier and 1-4% of oily gold nano solution; wherein the resin acid gold is prepared by the reaction of sulfurized balsam and gold trichloride; the metal organic matter mixing agent is a mixture of lead octoate, 2-hexyl hexane bismuth, rhodium octoate, 2-ethyl silicon hexanoate, vanadium isooctanoate and trimethyl boron; the concentration of gold in the oily gold nano solution is 40-60 mug/mL, and the diameter is 5-40 nm. According to the invention, the sheet resistance of the conductor slurry is greatly reduced by adding the oily gold nano particles, the adhesive force and the scratch resistance are improved, meanwhile, the surface of the sintered film is compact, flat, low in roughness, acid-resistant and alkali-resistant, bright yellow and light-leak-free, the roughness Ra is lower than 0.05 mu m, the sheet resistance is about 20m omega/□, and the adhesive force reaches 64N/mm2As described above, the scratch resistance reached 3B.
Description
Technical Field
The invention belongs to the technical field of electronic paste, and particularly relates to organic gold conductor paste with a compact and smooth surface, acid and alkali resistance, low sheet resistance, high adhesion and strong scratch resistance of a sintered film.
Background
Along with the rapid development of related industries of intellectualization and informatization, electronic components and the like in an upstream industrial chain rapidly grow, the market scale is continuously expanded, wherein the global scale of the thermal printer market in 2019 reaches $ 409 billion, and the thermal printer market is not influenced by new global crown epidemic situations and keeps a rapid growth trend.
The thermal printing head is one of key materials of thermal printing equipment, enterprises such as Japanese Sekio (Sekio) and Fujitsu (FUJITSU) occupy most of global markets, belong to technical leaders, and related enterprises such as Shandonghua Ling and Hunan Kaitong of domestic enterprises are pursuing enthusiasm, but the organic gold paste conductor slurry of the most key material in the product is monopolized by the American and Japanese enterprises all the time, and the global trade friction conflict is normalized, so that the organic gold conductor slurry with independent intellectual property and high performance is developed, the preparation technical blockade of foreign organic gold paste electronic slurry products is favorably broken through, and the safety of the industrial chain of the thermal printing machine market in China is ensured.
The current mainstream organic gold paste conductor paste product has the defects of higher sheet resistance, low adhesive force and low scratch resistance. Chinese patent CN 112652418A discloses an organic gold conductor slurry and a preparation method thereof, wherein the slurry comprises, by mass: 55-75% of resin gold, 2.5-9.5% of metal organic mixture, 0.3-0.8% of additive and 28-42% of organic carrier; the resin gold is prepared by the reaction of vulcanized resin and gold trichloride, the metallorganic mixing agent is prepared by the reaction of technical salt and vulcanized resin, metal in the metallorganic mixing agent is selected from one or more of Tm, Yb, Rh, Pr, Nb, Sb, Bi, Cr, Pd and Pt, and the additive is selected from one or more of viscosity reducer, polymeric dispersant, polyester plasticizer and polyvinylpyrrolidone. The organic gold conductor slurry has good adhesive force and electrical conductivity under the combined action of the components with the content, and the sintered slurry has the advantages of smooth surface, uniform thickness, high compactness, good acid and alkali resistance, good metal glossiness and excellent ductility. But the conductivity, adhesion and scratch resistance need to be further improved so as to better meet the development requirements of application products.
Disclosure of Invention
The invention aims to provide the organic gold conductor slurry, which further improves the adhesion and scratch resistance after sintering, and simultaneously reduces the sheet resistance of products, so that the requirements of updating and iterating products such as a thermal printing head, a capacitive sensor and the like can be better met.
Aiming at the purposes, the organic gold conductor slurry adopted by the invention comprises the following components in percentage by mass: 40-60% of resin acid gold, 2-10% of metal organic matter mixing agent, 30-50.9% of organic carrier and 1-4% of oily gold nano solution.
The resin acid gold is prepared by the reaction of sulfurized balsam and gold trichloride.
The metal organic matter mixing agent is a mixture of lead octoate, 2-hexyl hexane bismuth, rhodium octoate, 2-ethyl silicon hexanoate, vanadium isooctanoate and trimethyl boron. Preferably, in the metal organic compound mixture, the addition amounts of lead octoate, 2-hexyl hexane bismuth, rhodium octoate, 2-ethyl silicon hexanoate, vanadium isooctanoate and trimethyl boron sequentially account for 0.2-2.0%, 0.08-0.5%, 0.2-2.0%, 0.1-2.0% and 0.5-2.0% of the weight of the organic gold conductor slurry.
The solvent of the oily gold nano solution is dimethylbenzene, the concentration of gold is 40-60 mug/mL, and the diameter of gold is 5-40 nm.
The organic carrier comprises the following components in percentage by weight: 10-20% of resin and 80-90% of organic solvent; wherein the resin is at least one of epoxy resin, polyester resin and acrylic resin, and the organic solvent is at least one of diethylene glycol monobutyl ether, terpineol, turpentine and dodecyl glycol ester.
The invention has the following beneficial effects:
according to the invention, the sheet resistance of the conductor slurry is greatly reduced by adding the oily gold nanoparticles, the adhesive force and the scratch resistance are obviously improved, and meanwhile, the surface of the sintered film is compact, flat, low in roughness, acid-resistant and alkali-resistant, and bright yellow and has no light leakage. Wherein the roughness Ra is lower than 0.05 mu m; the sheet resistance is about 20m omega/□; the adhesive force reaches 64N/mm2The above; the scratch resistance reaches 3B.
Detailed Description
The present invention will be described in further detail with reference to examples, but the scope of the present invention is not limited to these examples.
The oily gold nanoparticle solutions used in the following examples were prepared using XFJ 857440-57-5 (diameter 5nm, solvent xylene, concentration 50. mu.g/mL) and XFJ 85-57440-57-5 (diameter 40nm, solvent xylene, concentration 50. mu.g/mL) produced by Pioneer nano.
Preparation of organic vehicle: mixing 80g of terpineol and 20g of epoxy resin NPEL-127 together, heating to 80 ℃ in a water bath, continuously stirring until the terpineol and the epoxy resin NPEL-127 are completely dissolved and are in a uniform state, and stopping heating; and cooling at room temperature for 24h, and storing for use.
And (3) synthesis of gold resinate: dissolving gold trichloride with acidity of 8% in isopropanol to obtain a solution with gold trichloride content (weight ratio) of 30%, pouring sulfurated balsam with sulfur content of 10% into the solution to obtain a solution with gold-sulfur molar ratio of 1: 0.1, stirring the solution at 80 ℃ for reaction for 8 hours, cleaning the solution with isopropanol after the reaction, crystallizing and separating out, decompressing to 0.8 atmosphere, distilling and drying for 1.5 hours to obtain a black brown pasty sulfurated balsam gold compound, namely resin acid gold, and storing for later use.
Comparative example 1
40g of gold resinate, 1g of lead octoate, 2g of 2-hexyl hexane bismuth, 0.1g of rhodium octoate, 2g of 2-ethyl silicon hexanoate, 1g of vanadium isooctanoate, 2g of trimethyl boron and 51.9g of organic carrier are stirred by a high-speed dispersion machine, sufficiently dispersed by three rollers and defoamed in vacuum to obtain the organic gold conductor slurry.
Example 1
Taking 40g of resin acid gold, 1g of lead octoate, 2g of 2-hexyl hexane bismuth, 0.1g of rhodium octoate, 2g of 2-ethyl silicon hexanoate, 1g of vanadium isooctanoate, 2g of trimethyl boron, 50.9g of organic carrier and 1g of oily gold nano solution (diameter is 5 nm), stirring by adopting a high-speed dispersion machine, fully dispersing by three rollers, and defoaming in vacuum to obtain the organic gold conductor slurry.
Example 2
40g of gold resinate, 1g of lead octoate, 2g of 2-hexyl hexane bismuth, 0.1g of rhodium octoate, 2g of 2-ethyl silicon hexanoate, 1g of vanadium isooctanoate, 2g of trimethyl boron, 49.4g of organic carrier and 2.5g of oily gold nano solution (diameter is 5 nm) are stirred by a high-speed dispersion machine, fully dispersed by three rollers and defoamed in vacuum to obtain the organic gold conductor slurry.
Example 3
40g of gold resinate, 1g of lead octoate, 2g of 2-hexyl hexane bismuth, 0.1g of rhodium octoate, 2g of 2-ethyl silicon hexanoate, 1g of vanadium isooctanoate, 2g of trimethyl boron, 47.9g of organic carrier and 4g of oily gold nano solution (diameter of 5 nm) are stirred by a high-speed dispersion machine, fully dispersed by three rollers and defoamed in vacuum to obtain the organic gold conductor slurry.
Example 4
60g of gold resinate, 1g of lead octoate, 2g of 2-hexyl hexane bismuth, 0.1g of rhodium octoate, 2g of 2-ethyl silicon hexanoate, 1g of vanadium isooctanoate, 2g of trimethyl boron, 29.4g of organic carrier and 2.5g of oily gold nano solution (diameter is 5 nm) are stirred by a high-speed dispersion machine, fully dispersed by three rollers and defoamed in vacuum to obtain the organic gold conductor slurry.
Example 5
Taking 40g of resin gold, 1g of lead octoate, 2g of 2-hexyl hexane bismuth, 0.1g of rhodium octoate, 2g of 2-ethyl silicon adipate, 1g of vanadium isooctanoate, 2g of trimethyl boron, 49.4g of organic carrier and 2.5g of oily gold nano solution (the diameter is 40 nm), stirring by adopting a high-speed dispersion machine, fully dispersing by three rollers, and defoaming in vacuum to obtain the organic gold conductor slurry.
Example 6
60g of gold resinate, 1g of lead octoate, 2g of 2-hexyl hexane bismuth, 0.1g of rhodium octoate, 2g of 2-ethyl silicon hexanoate, 1g of vanadium isooctanoate, 2g of trimethyl boron, 29.4g of organic carrier and 2.5g of oily gold nano solution (diameter of 40 nm) are stirred by a high-speed dispersion machine, fully dispersed by three rollers and defoamed in vacuum to obtain the organic gold conductor slurry.
And finishing printing, drying and sintering; the third step: the sample wafer was tested for acid and alkali resistance, backlight, roughness, sheet resistance, adhesion, etc., and the test data are shown in table 1.
The organic gold conductor slurry obtained in the above examples 1-6 and comparative example 1 is printed on a 230 × 60mm glazed substrate by using a 325-mesh stainless steel wire net, leveled, dried at 150 ℃ for 10-11 min, and sintered by using a mesh belt sintering furnace according to a sintering curve of 850 + -0.5 ℃ for 9.5-10.5 min, 20-25 min for temperature rise and 30-35 min for temperature decrease to obtain a sample wafer. The sample wafer is tested for acid and alkali resistance, backlight, roughness, sheet resistance, adhesion and the like, the specific test method is as follows, and the test data are shown in table 1.
(1) The test method of acid resistance comprises the following steps: and (3) adding sulfuric acid and deionized water into a clean beaker until the pH value of the solution is 3-5. Putting a sample wafer into the solution, soaking for 2 hours, taking out the sample wafer, sucking water on the surface of the sample wafer, and observing whether the sample wafer has the phenomena of color change, bubbling, falling off and the like;
(2) alkali resistance test method: and adding sodium carbonate and deionized water into a clean beaker until the pH value of the solution is 11-12. Putting a sample wafer into the solution, soaking for 2 hours, taking out the sample wafer, sucking water on the surface of the sample wafer, and observing whether the sample wafer has the phenomena of color change, bubbling, falling off and the like;
(3) and (3) gold film adhesion: printing the slurry on a glass glaze according to the size of 10cm by 10cm, drying and sintering, scraping by using a blade or dust-free paper, and observing the stripping condition of the gold film, wherein the standard is reached if the gold film is not stripped;
(4) square resistance: measuring by using a four-probe sheet resistance instrument, horizontally placing a sample on a measuring table, and vertically pressing four probes of the instrument to contact the surface of the sample so as to obtain a sheet resistance value;
(5) and (3) roughness testing: adopting a German Bruk step profiler Dektak XT;
(6) backlight test: irradiating the back surface of the sample wafer by a light source, and observing whether the sample wafer has a light transmission phenomenon or not after the front surface of the sample wafer is amplified by 200-500 times;
(7) the adhesion test adopts the method in GB/T5210-.
Table 1 performance test data
As can be seen from Table 1, the organic gold conductor slurry prepared by adding the oily gold nano solution has the advantages of compact and flat surface, good acid and alkali resistance, strong adhesive force, good conductivity and low sheet resistance after the slurry is sintered. The experimental results show that: the sintered surface is smooth and compact, the roughness Ra is lower than 0.05 mu m, and the sintered surface is bright yellow and has no light leakage; the sheet resistance is about 20m omega/□; after being soaked in acid and alkaline solutions for 2 hours, the metal layer does not fall off, discolor or foam; the adhesive force reaches 64N/mm2The above; the scratch resistance reaches 3B.
Claims (4)
1. An organic gold conductor paste, characterized in that: the composite material comprises the following components in percentage by mass: 40-60% of resin acid gold, 2-10% of metal organic matter mixing agent, 30-50.9% of organic carrier and 1-4% of oily gold nano solution;
the resin acid gold is prepared by the reaction of sulfurized balsam and gold trichloride;
the metal organic matter mixing agent is a mixture of lead octoate, 2-hexyl hexane bismuth, rhodium octoate, 2-ethyl silicon hexanoate, vanadium isooctanoate and trimethyl boron.
2. The organic gold conductive paste according to claim 1, wherein: the solvent of the oily gold nano solution is dimethylbenzene, the concentration of gold is 40-60 mug/mL, and the diameter of gold is 5-40 nm.
3. The organic gold conductive paste according to claim 1, wherein: in the metal organic compound mixing agent, the addition amounts of lead octoate, 2-hexyl hexane bismuth, rhodium octoate, 2-ethyl silicon hexanoate, vanadium isooctanoate and trimethyl boron sequentially account for 0.2-2.0 percent, 0.08-0.5 percent, 0.2-2.0 percent, 0.1-2.0 percent and 0.5-2.0 percent of the weight of the organic gold conductor slurry.
4. The organic gold conductive paste according to claim 1, wherein: the organic carrier comprises the following components in percentage by weight: 10-20% of resin and 80-90% of organic solvent; the resin is at least one of epoxy resin, polyester resin and acrylic resin, and the organic solvent is at least one of diethylene glycol monobutyl ether, terpineol, turpentine and dodecyl glycol ester.
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| CN113921165B (en) * | 2021-12-14 | 2022-03-29 | 西安宏星电子浆料科技股份有限公司 | Organic gold slurry |
| CN114023493B (en) * | 2021-12-28 | 2022-04-19 | 西安宏星电子浆料科技股份有限公司 | Scratch-resistant organic gold conductor slurry |
| CN114530275B (en) * | 2022-04-22 | 2022-07-08 | 西安宏星电子浆料科技股份有限公司 | Environment-friendly organic gold conductor slurry |
| CN114639501B (en) * | 2022-05-17 | 2022-09-30 | 西安宏星电子浆料科技股份有限公司 | Low-cost organic gold slurry |
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| JPS61256657A (en) * | 1985-05-08 | 1986-11-14 | Mitsubishi Electric Corp | Method of forming thick film |
| US4849284A (en) * | 1987-02-17 | 1989-07-18 | Rogers Corporation | Electrical substrate material |
| CN1414568A (en) * | 2001-10-26 | 2003-04-30 | 倪传流 | Organic gold conductive paste |
| JP2004285106A (en) * | 2003-03-19 | 2004-10-14 | Toppan Forms Co Ltd | Coating liquid and sheet containing metal nanoparticle |
| CN104637568B (en) * | 2015-02-02 | 2017-02-01 | 南通天盛新能源股份有限公司 | Aluminum paste for all-aluminum back surface field crystalline silicon solar cell and preparation method thereof |
| JP2017082297A (en) * | 2015-10-29 | 2017-05-18 | 三菱マテリアル株式会社 | Method for forming metal film on surface of copper-containing base material |
| CN110453203A (en) * | 2019-08-13 | 2019-11-15 | 北京科技大学 | A kind of organic chemistry additive and its application method for gold paste material |
| CN112331379B (en) * | 2020-10-26 | 2022-02-11 | 潮州三环（集团）股份有限公司 | Organic gold conductor slurry |
| CN112652418B (en) * | 2020-12-04 | 2022-06-21 | 湖南利德电子浆料股份有限公司 | Organic gold conductor slurry and preparation method thereof |
| CN112735631B (en) * | 2020-12-21 | 2022-10-21 | 有研工程技术研究院有限公司 | Low-viscosity organic gold paste capable of being sintered on surface of circuit board substrate at low temperature |
| CN113257458B (en) * | 2021-06-16 | 2021-10-08 | 西安宏星电子浆料科技股份有限公司 | Conductor paste for chip resistor electrode |
| CN113314252B (en) * | 2021-08-02 | 2021-10-22 | 西安宏星电子浆料科技股份有限公司 | Resin gold conductor slurry |
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