CN112652418B - Organic gold conductor slurry and preparation method thereof - Google Patents

Organic gold conductor slurry and preparation method thereof Download PDF

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CN112652418B
CN112652418B CN202011412195.2A CN202011412195A CN112652418B CN 112652418 B CN112652418 B CN 112652418B CN 202011412195 A CN202011412195 A CN 202011412195A CN 112652418 B CN112652418 B CN 112652418B
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gold
organic
resin
metal
reaction
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CN112652418A (en
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刘飘
宁天翔
宁文敏
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Hunan Leed Electronic Ink Co ltd
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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
    • 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
    • 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

Abstract

The invention provides organic gold conductor slurry and a preparation method thereof, wherein the slurry comprises the following components in percentage 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 metal-organic matter mixing agent is prepared by the reaction of metal salt and vulcanized resin; the metal in the metal-organic compound is selected from one or more of Tm, Yb, Rh, Pr, Nb, Sb, Bi, Cr, Pd and Pt; the additive is selected from one or more of a viscosity reducer, a high molecular dispersant, a polyester plasticizer and polyvinylpyrrolidone. The organic gold conductor paste has better adhesive force and electrical conductivity under the combined action of the components with the contents. The slurry has smooth surface, uniform thickness, high compactness, good acid and alkali resistance after being sintered; high scratch resistance, good luster of the gold surface and excellent ductility.

Description

Organic gold conductor slurry and preparation method thereof
Technical Field
The invention belongs to the technical field of slurry, and particularly relates to organic gold conductor slurry and a preparation method thereof.
Background
With the improvement of electronic informatization and automation degree and the development of bar code identification technology, the application range of novel ceramic circuit elements is continuously expanded, and the ceramic circuit elements are rapidly expanded from traditional office and home fax documents to emerging professional application fields such as commercial retail, industrial manufacturing, transportation, logistics, finance, lottery and medical treatment. The new ceramic circuit component growth area derives from global mPOS market and payment terminal market scale growth, and global Internet financial POS, E-commerce logistics, and smartphone-related color photo printing market. The market size of new ceramic circuit component applications (including printers and related consumables) has increased from $ 328 million in 2014 to $ 393 million in 2018, to $ 409 million in 2019 in the global market for thermal printers, with a annual composite growth rate of 4.3%.
The thermal printing head is one of key materials of thermal printing equipment, the market is mainly occupied by enterprises such as Japanese Sekio (SEKIO), Epson (EPSON), Fujitsu (FUJITSU) and the like at present, and domestic enterprises need to make a breakthrough in technology, so that the thermal printing head is caught up, the sintered gold paste for the thermal printing head is one of key materials for producing the product, and the gold paste in the market is mainly supplied by American and Japanese enterprises, so that the sintered gold paste for the thermal printing head with independent intellectual property rights and high performance is developed, and the long-term market monopoly abroad is broken. Meanwhile, the product performance of the domestic thermal printing head can be improved to replace the import at foreign countries.
Therefore, the sintered gold paste for the thermal printing head piece has the key common technical problems of matching performance of the sintered gold paste for the thermal printing head piece with a substrate, conductive paste and the like, develops the sintered gold paste product for the thermal printing head piece with independent intellectual property, high performance (the technical performance reaches the international advanced level) and low price (the price is estimated to be about 60 percent of the similar foreign products), breaks through the long-term market monopoly abroad, and improves the competitiveness of manufacturing enterprises such as domestic thermal printing heads and the like.
Disclosure of Invention
In view of the above, the present invention is directed to an organic gold conductive paste and a method for preparing the same, wherein the paste has good adhesion and electrical conductivity.
The invention provides organic gold conductor slurry which comprises the following components in parts 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 metal-organic matter mixing agent is prepared by the reaction of metal salt and vulcanized resin; the metal in the metal-organic compound is selected from one or more of Tm, Yb, Rh, Pr, Nb, Sb, Bi, Cr, Pd and Pt;
the additive is selected from one or more of viscosity reducer, polymer dispersant, polyester plasticizer and polyvinylpyrrolidone.
Preferably, the metal organic compound mixture comprises 0-2% of Tm, 2-4% of Yb, 0-1.5% of Pr, 2-4% of Nb, 0-1% of Sb, 0-0.5% of Pd, 0.5-1.5% of Pt and 88-93% of vulcanized resin.
Preferably, the organic carrier comprises the following components in a mass ratio of 80-85: 15-20 parts of an organic solvent and an organic resin;
the organic solvent is selected from one or more of terpineol, diethylene glycol ethyl ether acetate, isobornyl acetate, C12 alkane solvent, span 85 and decaglycol ester;
the organic resin is selected from one or more of ethyl cellulose, furfuryl alcohol phenolic aldehyde modified resin, modified epoxy resin and polyurethane resin.
Preferably, the vulcanized resin is prepared by vulcanization reaction of sulfur powder, butyl carbitol acetate, modified rosin resin and acrylic resin;
the mass ratio of the sulfur powder to the butyl carbitol acetate to the modified rosin resin to the acrylic resin is 10-14: 35-45: 8-12: 15-20: 16-24.
Preferably, the temperature of the vulcanization reaction is 160-220 ℃, and the time is 60-120 min.
Preferably, the gold trichloride participates in the reaction in the form of an ethanol solution of gold trichloride; the gold trichloride is characterized in that the content of gold in an ethanol solution of gold trichloride is 10-30%;
the mass ratio of the ethanol solution of gold trichloride to the vulcanized resin is 1: 2.0 to 3.5.
Preferably, the temperature of the reaction between the vulcanized resin and the gold trichloride is 40-80 ℃, and the time is 180-240 min.
The invention provides a preparation method of organic gold conductor slurry, which comprises the following steps:
and mixing the resin gold, the metal organic matter mixing agent, the additive and the organic carrier, and stirring for 80-180 min at 40-60 ℃ to obtain the organic gold conductor slurry.
The invention provides organic gold conductor slurry which comprises the following components in parts 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 metal-organic matter mixing agent is prepared by the reaction of metal salt and vulcanized resin; the metal in the metal-organic compound is selected from one or more of Tm, Yb, Rh, Pr, Nb, Sb, Bi, Cr, Pd and Pt; the additive is selected from one or more of viscosity reducer, polymer dispersant, polyester plasticizer and polyvinylpyrrolidone. The organic gold conductor paste provided by the invention is arranged onThe components with the contents have better adhesive force and electrical conductivity under the combined action. The slurry has smooth surface, uniform thickness, high compactness, good acid and alkali resistance after being sintered; high scratch resistance, good luster of the gold surface and excellent ductility. The experimental results show that: the scratch resistance is 4B-5B; the sintered surface is smooth and fine, has no black spots and is bright golden; the adhesive force is 33-45N/mm2(ii) a The sheet resistance is 0.136-0.194 m omega/□; after being soaked in acid and alkaline solution for 2 hours, the metal layer does not fall off and does not change color.
Drawings
FIG. 1 is an electron micrograph of resinated gold prepared according to formulation A2 of the present invention;
FIG. 2 is a surface electron microscope image of a gold layer prepared from the organic gold conductive paste No. 3 according to the present invention.
Detailed Description
The invention provides organic gold conductor slurry which comprises the following components in parts 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 metal-organic matter mixing agent is prepared by the reaction of metal salt and vulcanized resin; the metal in the metal-organic compound is selected from one or more of Tm, Yb, Rh, Pr, Nb, Sb, Bi, Cr, Pd and Pt;
the additive is selected from one or more of viscosity reducer, polymer dispersant, polyester plasticizer and polyvinylpyrrolidone.
The organic gold conductor slurry provided by the invention comprises 55-75% of resin gold. In specific embodiments, the percentage of resin gold is 55%, 60%, 65%, 70%, or 75%. In the invention, the resin gold is prepared by the reaction of vulcanized resin and gold trichloride; the vulcanized resin is prepared by carrying out vulcanization reaction on sulfur powder, butyl carbitol acetate, modified rosin resin and acrylic resin. The content of organic gold in the resin gold is 30-75%.
In the invention, the mass ratio of the sulfur powder, the butyl carbitol acetate, the modified rosin resin and the acrylic resin is preferably 10-14: 35-45: 8-12: 15-20: 16-24, more preferably 12: 40: 10: 18: 20. the temperature of the vulcanization reaction of the vulcanized resin, namely sulfur powder, butyl carbitol acetate, the modified rosin resin and the acrylic resin is preferably 160-220 ℃, and the time is 60-120 min. The viscosity of the vulcanized resin is preferably 2 to 10 pas.
The gold trichloride preferably participates in the reaction in the form of an ethanol solution of gold trichloride, and the mass content of gold in the ethanol solution of gold trichloride is 10-30%. The mass ratio of the ethanol solution of gold trichloride to the vulcanized resin is 1: 2.0 to 3.5. The temperature of the reaction between the vulcanized resin and the gold trichloride is 40-80 ℃, and the time is 180-240 min.
The organic gold conductor slurry provided by the invention comprises 2.5-9.5% of metal organic mixture. The metal-organic matter mixing agent is prepared by the reaction of metal salt and vulcanized resin; the metal in the metal-organic compound is selected from one or more of Tm, Yb, Rh, Pr, Nb, Sb, Bi, Cr, Pd and Pt. In specific examples, the proportion of the metal-organic mixture is 9.5%, 8.0%, 6.5%, 4.5%, or 2.5%. The metal in the metal salt is selected from one or more of Tm (thulium), Yb (ytterbium), Rh (rhodium), Pr (praseodymium), Nb (niobium), Sb (antimony), Bi (bismuth), Cr (chromium), Pd (palladium) and Pt (platinum). Preferably, the metal organic mixture comprises, by mass, 0-2% of Tm, 2-4% of Yb, 0-1.5% of Pr, 2-4% of Nb, 0-1% of Sb, 0-0.5% of Pd, 0.5-1.5% of Pt and 88-93% of a vulcanized resin. The reaction temperature of the vulcanized resin and the metal salt is preferably 40-80 ℃, and more preferably 50-70 ℃; the reaction time is preferably 60-180 min.
The organic gold conductor slurry provided by the invention comprises 0.3-0.8% of additive. In particular embodiments, the additive is present in an amount of 0.8%, 0.7%, 0.55%, 0.45%, or 0.3%. The additive is selected from one or more of viscosity reducer, polymer dispersant, polyester plasticizer and polyvinylpyrrolidone.
The organic gold conductor slurry provided by the invention comprises 28-42% of an organic carrier; in particular embodiments, the organic vehicle is present at 34.7%, 31.3%, 27.95%, 25.05%, or 22.2%. The organic carrier comprises the following components in a mass ratio of 80-85: 15-20 parts of an organic solvent and an organic resin; the organic solvent is preferably selected from one or more of terpineol, diethylene glycol ethyl ether acetate, isobornyl acetate, C12 alkane solvent, span 85 and decaglycol ester; the organic resin is preferably selected from one or more of ethyl cellulose, furfuryl alcohol phenolic modified resin, modified epoxy resin and polyurethane resin. The organic carrier is preferably prepared according to the following method: dissolving organic resin in an organic solvent, and homogenizing to obtain an organic carrier; the temperature of the organic resin solvent in the organic solvent is preferably 50-95 ℃ for 200-360 min.
The invention provides a preparation method of organic gold conductor slurry, which comprises the following steps:
and mixing the resin gold, the metal organic matter mixing agent, the additive and the organic carrier, and stirring for 80-180 min at 40-60 ℃ to obtain the organic gold conductor slurry.
The stirring speed is preferably 550-650 rpm, and more preferably 580-620 rpm; in a specific embodiment, the stirring rate is 600 rpm.
In the invention, the viscosity of the organic gold conductor slurry is 38-45 Pa.s.
In order to further illustrate the present invention, the following will describe an organic gold conductive paste and a method for preparing the same in detail with reference to the examples, which should not be construed as limiting the scope of the present invention.
Example 1
1. Preparation of resinated gold
(1) Preparation of the vulcanized resin: according to the weight percentage, 12 percent of sulfur powder is mixed with 40 percent of butyl carbitol, 10 percent of butyl carbitol acetate, 18 percent of modified rosin resin and 20 percent of acrylic resin, the mixture is heated for 80min at 180 ℃, the mixture is heated and decocted, after the sulfur powder and the terpineol are fully mixed, organic binder with the viscosity of 6 Pa.s, namely vulcanized resin is generated, and the mixture is cooled for standby application.
(2) Mixing 10-30% of molten gold with vulcanized resin, heating and stirring at 65 ℃ for 185min to generate resin molten gold, and cooling for later use.
TABLE 1 raw Material composition of resin gold
Figure GDA0003619505000000051
(3) And adding absolute ethyl alcohol into the cooled resin gold water for dilution, performing high-speed centrifugal sedimentation, adding an extracting agent, filtering, removing coarse particles and the like, and obtaining the resin gold with the organic gold content of 30-75%. (wherein, the resin gold is obtained by the following calculation method that a certain amount of extracted resin gold is weighed and recorded, the weight of the resin gold is sintered at high temperature, the residual weight is weighed, and the organic gold content is obtained by using the residual weight/the initial weight multiplied by 100%).
2. Preparing a metal organic compound mixture:
(1) preparation of raw materials:
according to the weight percentage, Tm (0-2%) -Yb (2-4%) -Pr (0-1.5%) -Nb (2-4%) -Sb (0-1%) -Pd (0-0.5%) -Pt (0.5-1.5%) -vulcanized resin (88-93%) is weighed according to the proportion in a table 2, 3 formulas of B1, B2 and B3 are respectively prepared, and the three formulas are respectively added into a glass container, the temperature is 65 ℃, the heating and stirring are carried out, and the time is 140 min. Respectively storing 3 metal organic compounds in containers for later use until the metal organic compounds are completely dissolved or uniformly mixed;
TABLE 2 raw Material composition of Metal-organic mixtures
Figure GDA0003619505000000061
(2) Preparing organic gold conductor slurry:
the resin gold content is 60%; b2 is selected as the organic mixture, and the content is set as 6.5%; the additive is a macromolecular dispersant with the content of 0.55 percent; the content of the organic vehicle was 32.95%, weighed in proportion, heated and stirred by a stirred tank until the components were mixed thoroughly, and then vacuum defoamed, whereby an organic gold conductor paste 1, an organic gold conductor paste 2, an organic gold conductor paste 3 and an organic gold conductor paste 4 were prepared according to the paste formulation of table 3:
TABLE 3 formulation composition of the organo-gold conductor paste
Figure GDA0003619505000000062
Figure GDA0003619505000000071
Performance evaluation method
The resin gold, the metal organic matter mixing agent, the additive and the organic carrier are heated and stirred uniformly, viscosity and fineness detection is carried out, the two detections are qualified, and the slurry is defoamed in vacuum. Printing the slurry on the ceramic chip, drying for 5min at 200 ℃, and sintering by a belt sintering furnace under the process conditions of 450-. At this time, the surface quality, scratch resistance, adhesion, sheet resistance and other properties were tested.
The test method of acid resistance comprises the following steps:
preparing 1 container, adding purified water, proportionally adding sulfuric acid to prepare acidic solution with pH value of 3-5. And (3) putting the sample into the solution, soaking for 2 hours, taking out the sample, sucking to remove water on the surface of the sample, and observing whether the sample has the phenomena of color change, bubbling, falling and the like.
Alkali resistance test method:
preparing 1 container, adding purified water, and proportionally adding sodium carbonate to prepare alkaline solution with pH value of 11-12. And (3) putting the 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 and the like.
As can be seen from the experimental results in Table 2, the results of the slurries prepared from different matched resinoid gold show that the performance of the slurry prepared from A2 resinoid gold is the best and meets or exceeds the set standard.
In order to further improve various performances of the organic gold conductor slurry, the invention adopts a resin gold formula A2 with better performance, adjusts the formula of an organic mixture agent and the types of additives in the formula, keeps the proportion of the resin gold and the organic carrier in the slurry unchanged, prepares a plurality of organic mixture agent formulas and a plurality of additives, and then evaluates the influence of different organic mixture agent formulas and additives on the performance of the slurry:
TABLE 4 slurry formulations of different metal-organic compounds and additives in the organo-gold conductor slurries
Figure GDA0003619505000000072
Figure GDA0003619505000000081
The performance of the slurry prepared in the table 4 is detected, and the result is shown in the table 5:
TABLE 5 Performance test results for Organogold conductor pastes of different formulations
Figure GDA0003619505000000082
Figure GDA0003619505000000091
As can be seen in table 5: after different organic matter mixing agents and additives are added, the performance change of the organic gold conductor slurry after being matched with a substrate is small, and all performance detection results reach or exceed the design standard of a formula.
The resin gold formula A2, the organic matter mixing agent B2 and the additive polyester plasticizer are adopted to prepare the slurry with various proportions, and then the influence of the resin gold, the organic matter mixing agent and the additive with different contents on the performance of the slurry is evaluated.
TABLE 6 slurry formula with different proportions of components in organic gold conductor slurry and performance test results
Figure GDA0003619505000000092
Figure GDA0003619505000000101
As can be seen from table 6: the performance of the organic gold conductor slurry prepared from different components is measured after being matched with the substrate, and the result shows that the performance change of the slurry prepared from different component proportions after being matched with the substrate is small, and the performance detection results all reach the design standard of the formula.
The paste number 3 in the table 6 is printed by screen printing, dried at 200 ℃ for 5min and then sintered at 850-900 ℃ for 10min to prepare the gold layer. FIG. 2 is a surface electron microscope image of a gold layer prepared from the organic gold conductive paste No. 3 according to the present invention.
The viscosity of the organic gold conductor slurry provided by the invention is 10-45 Pa.s; drying the slurry at 200 ℃ for 5min, and sintering at 850 ℃ for 20min to obtain a gold layer with a smooth and fine surface, no black spots and bright gold color; scratch resistance is more than or equal to 4B, and adhesive force is more than or equal to 30N/mm2(ii) a The sheet resistance is less than or equal to 0.2m omega/□; the gold layer is not stripped and discolored completely after being soaked in acid and alkaline solutions for 2 hours.
The organic gold conductor slurry provided by the invention is matched with the expansion coefficient of the base material, and has the advantages of wide matching range, good conductivity, high adhesion and high sintering density.
From the above embodiments, the invention provides an organic gold conductor paste, which comprises the following components in parts 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 metal-organic matter mixing agent is prepared by the reaction of metal salt and vulcanized resin; the metal in the metal-organic compound is selected from one or more of Tm, Yb, Rh, Pr, Nb, Sb, Bi, Cr, Pd and Pt; the additive is selected from one or more of viscosity reducer, polymer dispersant, polyester plasticizer and polyvinylpyrrolidone. The organic matter provided by the inventionThe gold conductor paste has better adhesive force and electrical conductivity under the combined action of the components with the contents. The slurry has smooth surface, uniform thickness, high compactness, good acid and alkali resistance after being sintered; high scratch resistance, good luster of the gold surface and excellent ductility. The experimental results show that: the scratch resistance is 4B-5B; the sintered surface is smooth and fine, has no black spots and is bright golden; the adhesive force is 33-45N/mm2(ii) a The sheet resistance is 0.136-0.194 m omega/□; after being soaked in acid and alkaline solution for 2 hours, the metal layer does not fall off and does not change color.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (5)

1. An organic gold conductor paste comprises the following components in percentage 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 metal-organic matter mixing agent is prepared by the reaction of metal salt and vulcanized resin; the metal organic matter mixing agent comprises 0-2% of Tm, 2-4% of Yb, 0-1.5% of Pr, 2-4% of Nb, 0-1% of Sb, 0-0.5% of Pd, 0.5-1.5% of Pt and 88-93% of vulcanized resin;
the vulcanized resin is prepared by carrying out vulcanization reaction on sulfur powder, butyl carbitol acetate, modified rosin resin and acrylic resin;
the mass ratio of the sulfur powder to the butyl carbitol acetate to the modified rosin resin to the acrylic resin is 10-14: 35-45: 8-12: 15-20: 16-24;
the additive is selected from one or more of viscosity reducer, polymer dispersant, polyester plasticizer and polyvinylpyrrolidone;
the organic carrier comprises the following components in a mass ratio of 80-85: 15-20 parts of an organic solvent and an organic resin;
the organic solvent is selected from one or more of terpineol, diethylene glycol ethyl ether acetate, isobornyl acetate, C12 alkane solvent, span 85 and decaglycol ester;
the organic resin is selected from one or more of ethyl cellulose, furfuryl alcohol phenolic aldehyde modified resin, modified epoxy resin and polyurethane resin.
2. The organic gold conductor paste according to claim 1, wherein the temperature of the sulfidation reaction is 160 to 220 ℃ and the time is 60 to 120 min.
3. The organic gold conductor paste according to claim 1, wherein the gold trichloride is reacted in the form of an ethanol solution of gold trichloride; the gold trichloride is characterized in that the content of gold in an ethanol solution of gold trichloride is 10-30%;
the mass ratio of the ethanol solution of gold trichloride to the vulcanized resin is 1: 2.0 to 3.5.
4. The organic gold conductor paste according to claim 1, wherein the temperature of the reaction between the sulfide resin and the gold trichloride is 40 to 80 ℃ and the time is 180 to 240 min.
5. A method for preparing the organic gold conductor paste of any one of claims 1 to 4, comprising the steps of:
and mixing the resin gold, the metal organic matter mixing agent, the additive and the organic carrier, and stirring for 80-180 min at 40-60 ℃ to obtain the organic gold conductor slurry.
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Denomination of invention: An organic gold conductor slurry and its preparation method

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