CN112735631B - Low-viscosity organic gold paste capable of being sintered on surface of circuit board substrate at low temperature - Google Patents
Low-viscosity organic gold paste capable of being sintered on surface of circuit board substrate at low temperature Download PDFInfo
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- CN112735631B CN112735631B CN202011520326.9A CN202011520326A CN112735631B CN 112735631 B CN112735631 B CN 112735631B CN 202011520326 A CN202011520326 A CN 202011520326A CN 112735631 B CN112735631 B CN 112735631B
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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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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K1/00—Printed circuits
- H05K1/02—Details
- H05K1/09—Use of materials for the conductive, e.g. metallic pattern
- H05K1/092—Dispersed materials, e.g. conductive pastes or inks
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K2201/00—Indexing scheme relating to printed circuits covered by H05K1/00
- H05K2201/03—Conductive materials
- H05K2201/032—Materials
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Abstract
The present invention belongs to the field of electronic paste technology for integrated circuit manufactureThe invention relates to a low-viscosity organic gold paste which can be sintered on the surface of a circuit board substrate at low temperature: 39.0 to 49.5 percent of gold-containing organic precursor; 50.0 to 60.0 percent of organic carrier (organic solvent, plasticizer, casting control agent, etc.); 0.5-1.8% of bismuth-containing and chromium-containing organic resinate additive. The slurry can be sintered to form a film at a lower temperature (450 ℃), the residual amount of organic matters after sintering is low, the components do not contain lead, the volatility of the slurry is small at normal temperature, and the slurry is relatively friendly to human bodies and environment. After sintering, the gold-based conductive film can be uniformly adhered to the surface of a target substrate, the film and the substrate have strong bonding force, good conductivity, compactness and difficult shedding, and the viscosity of the paste can be far lower than that of common thick film gold paste by more than 4-5 orders of magnitude (up to 10) ‑2 Pa · s) can be printed, spin coated, spray coated, and directly painted on a specific portion of the target substrate.
Description
Technical Field
The invention belongs to the technical field of electronic paste for integrated circuit manufacturing industry, and particularly relates to low-viscosity organic gold paste capable of being sintered on the surface of a circuit board substrate at low temperature.
Background
Gold is second only to silver and copper in electrical conductivity, but gold has a higher chemical stability and ability to work in harsh environments than silver migration and copper corrosion phenomena, which are generally difficult to overcome. Therefore, gold conductor pastes are increasingly being used more widely in the field of electronics, particularly in multilayer wiring circuits, PCB circuits and semiconductor packages in integrated circuit technology. Different from the traditional thick film gold conductor paste, the organic gold paste is not a suspension liquid for solid-liquid separation of solid gold particles and an organic binder, but becomes a homogeneous liquid system, the surface of the sintered conductive film is smooth, the conductivity is good, the film layer is compact and is not easy to fall off, the thickness is only one percent (about 0.1 mu m) of the thickness of the film layer of the sintered common thick film gold paste, and the gold amount and the cost for film formation can be greatly reduced. Particularly, the viscosity of the gold paste can be far lower than that of common thick film gold paste by more than 4-5 orders of magnitude (up to 10) -2 Pa · s order) can be conveniently printed, spun, sprayed, and directly painted onto a specific location on the target substrate.
The research and application conditions of gold-containing vulcanized resinate are reported in foreign countries at the beginning of the last century (U.S. Pat. No. 2,682310 and document J.Prakt.chem.,1927,117). Some domestic companies and research institutions have been following the steps of foreign development, some imitation and improvement are carried out on the organic gold slurry, and the sintering temperature of the organic gold slurry is increased to 850 ℃ through a high-temperature additive in the patent CN 01134072. X; patent CN 200910107301.3 provides some noble metal preparation or gloss preparation formulas for prolonging effective use time of metal organic slurry; patent CN 201610668957.2 provides a precious metal slurry formulation with long quality guarantee period, good adhesion, crack resistance and good rheological property, and in general, the invention mostly researches the gold organic slurry as a decorative coating, and does not consider the conductivity of the sintered film and related applications. Later researchers found that the circuit formed by sintering the coating can also be used for a thermal printing head, a conductor of a high-density circuit and the like, and a sintered film layer is thin and has high linear resolution, so that the coating has certain functional extension in the electronic circuit manufacturing industry by supplementing and developing the thick-film gold paste process (precious metals 2001,22 (2): 9 and electronic components and materials 1997,16 (5): 27), but the component design of the organic gold paste is not disclosed, and the reduction of the sintering temperature of the organic gold paste due to the temperature resistance of a circuit board substrate is not considered.
Disclosure of Invention
Technical problem to be solved by the invention
The invention aims to provide organic gold slurry which can be sintered on the surfaces of certain circuit boards at a lower temperature to form film current channels.
Means for solving the technical problem
Aiming at the problems, the invention provides an organic gold paste which can be coated on the surface of a circuit board substrate and sintered into a conductive film, and the organic gold paste comprises the following components in percentage by mass: 39.0 to 49.5 percent of gold-containing organic precursor; 50.0 to 60.0 percent of organic carrier; the total amount of the bismuth-containing and chromium-containing organic resinate additive is 0.5-1.8%, and the organic carrier comprises an organic solvent, a plasticizer and a casting control agent.
In a preferred embodiment, the substrate can withstand a 450 ℃ sintering for 1h without failing the solid insulating medium.
In a preferred embodiment, the gold-containing organic precursor is prepared as follows:
firstly, preparing gold trichloride into an aqueous solution with the mass concentration of gold of 50-200 g/L;
secondly, preparing turpentine oil distilled at 140-160 ℃ into vulcanized balsam organic solution with the sulfur content of 10-12%;
thirdly, continuously dropwise adding the sulfurized balsam solution prepared in the second step into the gold trichloride aqueous solution prepared in the first step according to the mass ratio of gold to sulfurized balsam =1: 3-1, reacting for 3-4 h after 0.5-1.5 h, and separating the reactant by using a decantation method to obtain a brown colloidal mixture;
fourthly, centrifugally washing the brown colloidal mixture prepared in the third step by using absolute ethyl alcohol until the brown colloidal mixture is powdery solid, and drying the obtained solid powder at 40 ℃ in vacuum;
fifthly, dissolving the resin acid gold solid powder prepared in the fourth step into gold-containing organic precursor by using nitrogen methyl pyrrolidone, wherein the gold content is not lower than 30%.
In a preferred embodiment, the mass percentages of the components of the organic carrier are as follows: 35-45% of dibutyl phthalate, 15-25% of turpentine, 10-20% of linalool, 10-15% of eucalyptol, 5-8% of modified phenolic resin, 2-5% of hydrogenated castor oil and 1-3% of nonylphenol polyoxyethylene ether.
In a preferred embodiment, the bismuth-containing, chromium-containing organic resinate is prepared in a similar manner to the gold-containing organic precursor described above, but the first synthesis reaction is carried out in an aqueous solution instead of in absolute ethanol.
The invention has the advantages of
The organic gold paste can be used similar to thick-film gold paste, can be sintered on the surface of a substrate of a certain circuit board to form a film layer current path, has lower sintering temperature (only 450 ℃), and has smooth surface and good conductivity after being sintered into a film, and the film layer is thin in thickness, compact and not easy to fall off.
The organic gold paste has lower use cost compared with a thick-film gold paste process, and the low viscosity characteristic of the paste increases the variety and operability of paste coating modes, and can be more flexibly coated on a target substrate through printing, spin coating, spray coating, direct drawing and other modes.
Further features of the present invention will become apparent from the following description of exemplary embodiments.
Detailed Description
One embodiment of the present disclosure will be specifically described below, but the present disclosure is not limited thereto.
In order to realize the purpose, the technical scheme adopted by the invention is as follows: the gold resinate precursor is prepared by reacting gold trichloride aqueous solution with sulfurated balsam, the gold precursor is dissolved by designing low-boiling-point organic carrier component to form low-viscosity organic slurry, and finally, a proper amount of bismuth-containing and chromium-containing organic resinate is added into the organic slurry to improve the film forming property and the electrical property of a sintered gold film.
The substrate is a PCB board, a hybrid circuit board, or the like including a glass fiber board, an alumina ceramic board, or the like, but is not limited to the above-listed two types of substrates.
The technical scheme of the invention comprises the following specific implementation steps:
firstly, preparing gold trichloride into an aqueous solution with the mass concentration of gold of 50-200 g/L;
secondly, preparing turpentine oil distilled at 140-160 ℃ into vulcanized balsam organic solution (with the sulfur content of 10-12%);
thirdly, continuously dropwise adding the aqueous solution of the gold trichloride prepared in the first step into the balsam sulfide solution prepared in the second step according to the mass ratio (gold: balsam sulfide =1: 3-1: 3.5) (after the addition of 0.5-1.5 h, the reaction lasts for 3-4 h), and separating the reactant by using a decantation method to obtain a brown colloidal mixture;
fourthly, centrifugally washing the brown colloidal mixture prepared in the third step by using absolute ethyl alcohol to obtain powdery solid, and drying the obtained solid powder at 40 ℃ in vacuum;
fifthly, dissolving the resin acid gold solid powder prepared in the fourth step into gold-containing organic precursor (the gold content is not less than 30%) by using azomethylpyrrolidone;
sixthly, preparing the organic carrier, wherein the organic carrier comprises the following components in percentage by weight: 35-45% of dibutyl phthalate, 15-25% of turpentine, 10-20% of linalool, 10-15% of eucalyptol, 5-8% of modified phenolic resin, 2-5% of hydrogenated castor oil and 1-3% of nonylphenol polyoxyethylene ether;
seventhly, the preparation of the organic resinate containing bismuth and chromium is carried out in absolute ethyl alcohol instead of aqueous solution according to a similar method for preparing an organic precursor containing gold;
and eighthly, mixing and stirring the gold-containing organic precursor prepared in the fifth step, the organic carrier solution prepared in the sixth step and the bismuth-containing and chromium-containing organic resinate (total) prepared in the seventh step according to the weight ratio of 39.0-49.5%, 50.0-60.0% and 0.5-1.8%, and aging for one week to obtain the organic gold slurry.
Examples
The present invention is described in more detail by way of examples, but the present invention is not limited to the following examples.
The following 3 sets of organic gold paste formulations (see table 1) are used to further detail the preferred embodiments of the present invention, but the invention itself is not limited to these embodiments, and all technical routes derived from equivalent substitutions or equivalent transformations of the present invention are within the scope of the present invention.
TABLE 1
(example 1 #)
Gold trichloride (analytically pure) is used as a raw material, and a 250mL volumetric flask is used for preparing a gold trichloride solution with the Au mass concentration of 50g/L for later use.
Distilling and purifying the turpentine oil by a distilling device under normal pressure, and only collecting fractions at the temperature of 140-160 ℃ for later use. 270g of distilled turpentine oil is weighed in a 1L three-neck flask, 30g of sublimed sulfur powder is added, and the mixture is heated to 160-165 ℃ under the reaction conditions of continuous stirring and cooling reflux for reaction for 4 hours to obtain dark brown vulcanized balsam solution.
200mL of the prepared gold trichloride solution was taken out of a 500mL beaker, heated and stirred in a boiling water bath, 35g of balsam sulfide was added dropwise over about 1h by a peristaltic pump, and then allowed to react sufficiently for 3h, and after cooling, the residual liquid separated therefrom was poured out to obtain a brown viscous colloidal mixture. And (2) centrifugally washing the colloidal mixture by using absolute ethyl alcohol to obtain powdery solid, placing the obtained resin acid gold solid powder at 40 ℃ for vacuum drying, dissolving the powder in 15g of nitrogen methyl pyrrolidone, fully stirring and dissolving the powder by using a planetary gravity stirring machine to form a gold-containing organic precursor of organic gold slurry for later use, and measuring the content of Au in the precursor to be 32.5% after sintering the precursor at 600 ℃.
Similarly, respectively dropwise adding sulfurated balsam solution into prepared anhydrous ethanol solution of bismuth trichloride and chromium nitrate in which Bi and Cr are dissolved with the mass concentration of 20g/L for full reaction for 3.5h, cooling, separating and pouring out respective viscous colloidal mixtures, respectively cleaning and drying to obtain powdery solids, and using the powdery solids as resinate additives for later use.
Adding 3g of modified phenolic resin into a 100mL conical flask, dissolving with 12g of turpentine, heating and stirring, supplementing the volatile amount of the turpentine after dissolving, and then sequentially adding 21g of dibutyl phthalate, 12g of linalool, 9g of eucalyptol, 1.8g of hydrogenated castor oil and 1.2g of nonylphenol polyoxyethylene ether to prepare a gold paste organic carrier for later use.
And (2) weighing 19.5g of the prepared gold-containing organic precursor in a stirring cup, sequentially adding 0.4g of bismuth resinate, 0.1g of chromium resinate and 30g of gold paste organic carrier solution, mixing, fully stirring by using a planetary gravity stirrer, and aging for one week to obtain the No. 1 organic gold paste. The viscosity of the No. 1 organic gold slurry is measured to be 0.028 Pa.s, the slurry is coated on a glass fiber board and sintered for 1h at 450 ℃, the obtained gold film is bright golden yellow, and the conductivity of the film layer is 2520S/m.
(example 2 #)
Gold trichloride solution with the Au mass concentration of 100g/L is prepared by using gold powder (with the purity of 99.99%) as a raw material and dissolving the gold trichloride solution with the Au mass concentration of 50mL to 200mL in a beaker for later use.
Distilling and purifying the turpentine oil by a distilling device under normal pressure, and only collecting fractions at the temperature of 140-160 ℃ for later use. 264g of distilled turpentine oil is weighed in a 1L three-neck flask, 36g of sublimed sulfur powder is added, and the mixture is heated to 160-165 ℃ under the reaction conditions of continuous stirring and cooling reflux for reaction for 4 hours to obtain dark brown vulcanized balsam solution for later use.
Heating and stirring the gold trichloride solution for standby in a boiling water bath, dropwise adding 15g of the prepared balsam sulfide solution by using a peristaltic pump for 0.5h, then fully reacting for 3.5h, and pouring out residual liquid which can be separated after cooling to obtain a brown viscous colloidal mixture. And (2) centrifugally washing the colloidal mixture by using absolute ethyl alcohol to obtain powdery solid, placing the obtained resin acid gold solid powder at 40 ℃ for vacuum drying, dissolving the powder in 8g of nitrogen methyl pyrrolidone, and fully stirring and dissolving the powder by using a planetary gravity stirring machine to form a gold-containing organic precursor of organic gold slurry for later use, wherein the Au content of the precursor is determined to be 31.2% after the precursor is sintered at 600 ℃.
And in the same way, respectively dropwise adding sulfuration balsam solution into prepared bismuth trichloride and chromium nitrate absolute ethyl alcohol solution in which the mass concentrations of Bi and Cr are both 50g/L for full reaction for 4h, cooling, separating and pouring out respective sticky colloidal mixtures, respectively cleaning and drying to obtain powdery solids, and using the powdery solids as resinate additives for later use.
Adding 8g of modified phenolic resin into a 200mL conical flask, dissolving with 15g of turpentine, heating and stirring, supplementing the volatile amount of the turpentine after dissolving, and then sequentially adding 40g of dibutyl phthalate, 15g of linalool, 14g of eucalyptol, 5g of hydrogenated castor oil and 3g of nonylphenol polyoxyethylene ether to prepare a gold paste organic carrier for later use.
Weighing 12g of prepared gold-containing organic precursor in a stirring cup, sequentially adding 0.3g of bismuth resinate, 0.2g of chromium resinate and 15g of gold paste organic carrier solution, mixing, fully stirring by using a planetary gravity stirrer, and aging for one week to obtain the 2# organic gold paste. The viscosity of the 2# organic gold paste is measured to be 0.065 Pa.s, the 2# organic gold paste is coated on a glass fiber board and sintered for 1h at the temperature of 450 ℃, the obtained gold film is golden yellow, the color is darker than that of the gold film sintered by the 1# organic gold paste, and the conductivity of the film layer is 3150S/m.
(example 3 #)
Gold trichloride (analytically pure) is used as a raw material, and a gold trichloride solution with the Au mass concentration of 200g/L is prepared by using a 100mL volumetric flask for later use.
Distilling and purifying the turpentine oil by a distilling device under normal pressure, and only collecting fractions at the temperature of 140-160 ℃ for later use. 267g of distilled turpentine oil is weighed in a 1L three-neck flask, 33g of sublimed sulfur powder is added, and the mixture is heated to 160-165 ℃ under the reaction conditions of continuous stirring and cooling reflux for reaction for 4 hours to obtain dark brown vulcanized balsam solution.
100mL of the prepared gold trichloride solution is poured into a 500mL beaker, the beaker is heated and stirred in a boiling water bath, 65g of balsam sulfide is dropwise added in about 1.5h by a peristaltic pump, then the mixture is allowed to react for 4h fully, and the residual liquid separated from the mixture is poured out after cooling to obtain a brown viscous colloidal mixture. And (2) centrifugally washing the colloidal mixture by using absolute ethyl alcohol to obtain powdery solid, placing the obtained resin acid gold solid powder at 40 ℃ for vacuum drying, dissolving the powder in 28g of N-methyl pyrrolidone, fully stirring and dissolving the powder by using a planetary gravity stirrer to form a gold-containing organic precursor of organic gold slurry for later use, and measuring the content of Au in the precursor to be 30.3% after sintering at 600 ℃.
Similarly, respectively dropwise adding sulfurated balsam solution into prepared anhydrous ethanol solution of bismuth trichloride and chromium nitrate in which Bi and Cr are dissolved with the mass concentration of 20g/L for full reaction for 3.5h, cooling, separating and pouring out respective viscous colloidal mixtures, respectively cleaning and drying to obtain powdery solids, and using the powdery solids as resinate additives for later use.
Adding 7g of modified phenolic resin into a 200mL conical flask, dissolving with 25g of turpentine, heating and stirring, supplementing the volatile amount of the turpentine after dissolving, and then sequentially adding 45g of dibutyl phthalate, 10g of linalool, 10g of eucalyptol, 2g of hydrogenated castor oil and 1g of nonylphenol polyoxyethylene ether to prepare a gold paste organic carrier for later use.
49.5g of prepared gold-containing organic precursor is weighed in a stirring cup, 0.4g of bismuth resinate, 0.1g of chromium resinate and 50g of gold paste organic carrier solution are sequentially added, mixed and fully stirred by a planetary gravity stirrer, and aged for one week to obtain 3# organic gold paste. The viscosity of 3# organic gold paste is measured to be 0.129 Pa.s, the paste is coated on a glass fiber board and sintered for 1h at 450 ℃, the obtained gold film is bright golden yellow, the color of the gold film is similar to that of 1# organic gold paste, but the film layer is thicker, and the conductivity of the film layer is 5300S/m.
In examples 1#, 2#, and 3#, if the step of distilling and purifying turpentine oil by a distillation device under normal pressure is omitted, or resin acid gold solid powder prepared by dissolving azomethyl pyrrolidone is not used, it is difficult to obtain gold-containing organic precursor with Au content of 30% or more, and even if the rest of the method and steps are not changed, the prepared organic gold slurry cannot easily reach the viscosity described in the examples; or the gold paste is coated on a glass fiber board and sintered for 1 hour at 450 ℃, even if the rest method and steps are not changed, the prepared gold paste is difficult to compact and continuous, and cannot be used.
Industrial applicability
The slurry can be sintered at a lower temperature (450 ℃) to form a film, the residual amount of organic matters after sintering is low, the components do not contain lead, the volatility of the slurry is small at normal temperature, and the slurry is relatively friendly to human bodies and environment. The slurry can enable the gold-based conductive film to be uniformly attached to the surface of a target substrate after being sintered, and the film has strong bonding force with the substrate, good conductivity, compactness and difficult shedding. Particularly, the viscosity of the paste can be far lower than that of common thick-film gold paste by more than 4-5 orders of magnitude (up to 10) -2 Pa · s) can be printed, spin coated, spray coated, and directly painted on a specific portion of the target substrate.
The present invention is not limited to the above embodiments, and any changes or substitutions that can be easily made by those skilled in the art within the technical scope of the present invention are also within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (2)
1. The organic gold slurry capable of being coated on the surface of a circuit board substrate and sintered into a conductive film is characterized by comprising the following components in percentage by mass: 39.0 to 49.5 percent of gold-containing organic precursor; 50.0 to 60.0 percent of organic carrier; 0.5 to 1.8 percent of bismuth-containing and chromium-containing organic resinate additive, wherein the organic carrier comprises an organic solvent, a plasticizer and a tape casting control agent;
the preparation method of the gold-containing organic precursor comprises the following steps:
firstly, preparing gold trichloride into an aqueous solution with the gold mass concentration of 50-200g/L;
the second step is to carry out the steps of 140 to 160 o C, preparing the distilled turpentine into an organic vulcanized balsam solution with the sulfur content of 10 to 12 percent;
thirdly, continuously dropwise adding the aqueous solution of the gold trichloride prepared in the first step into the aqueous solution of the gold trichloride according to the mass ratio of gold to balsam sulfide =1 to 3.5, reacting for 3 to 4 hours after 0.5 to 1.5 hours, and separating the reactant by decantation to obtain a brown colloidal mixture;
fourthly, centrifugally washing the brown colloidal mixture prepared in the third step by using absolute ethyl alcohol until the brown colloidal mixture is powdery solid, and drying the obtained solid powder at 40 ℃ in vacuum;
fifthly, preparing the resin acid gold solid powder prepared in the fourth step into a gold-containing organic precursor by using N-methyl pyrrolidone, wherein the gold content is not lower than 30%;
the organic carrier comprises the following components in percentage by mass: 35-45% of dibutyl phthalate, 15-25% of turpentine, 10-20% of linalool, 10-15% of eucalyptol, 5-8% of modified phenolic resin, 2-5% of hydrogenated castor oil and 1-3% of nonylphenol polyoxyethylene ether.
2. The organic gold paste capable of being coated on the surface of a circuit board substrate and sintered into a conductive film according to claim 1, wherein the organic gold paste comprises the following components in percentage by weight: the substrate can bear 450 o C sintered for 1h without failure of the solid insulating medium.
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| 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 |
| CN113658742B (en) * | 2021-10-21 | 2022-03-08 | 西安宏星电子浆料科技股份有限公司 | Organic gold conductor slurry |
| CN113909738B (en) * | 2021-11-09 | 2023-08-15 | 佛山市摩陶新材料科技有限公司 | Preparation method and application of ceramic soldering tin head surface treatment coating |
| 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 |
| CN116199822B (en) * | 2023-04-24 | 2023-08-15 | 有研工程技术研究院有限公司 | Carboxyl-containing gold resinate and negative-tone photo-etching organic gold slurry and preparation method thereof |
| CN116199817B (en) * | 2023-04-25 | 2023-08-15 | 有研工程技术研究院有限公司 | Boc-containing gold resinate and positive photo-etching organic gold slurry and preparation method thereof |
| CN116199811B (en) * | 2023-04-25 | 2023-08-15 | 有研工程技术研究院有限公司 | Polymer thioether-based gold resinate and organic gold slurry and preparation method thereof |
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