CN102760934A - Conductive paste for thick film circuit, thick film circuit board employing same and manufacturing method thereof - Google Patents
Conductive paste for thick film circuit, thick film circuit board employing same and manufacturing method thereof Download PDFInfo
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- CN102760934A CN102760934A CN2012102606799A CN201210260679A CN102760934A CN 102760934 A CN102760934 A CN 102760934A CN 2012102606799 A CN2012102606799 A CN 2012102606799A CN 201210260679 A CN201210260679 A CN 201210260679A CN 102760934 A CN102760934 A CN 102760934A
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Abstract
A conductive paste for a thick film circuit, a thick film circuit board employing the same and a manufacturing method thereof relate to the field of thick film circuits. One of the purposes of the invention is to provide a conductive paste for a thick film circuit, which can replace a silver paste and low cost and high security. The conductive paste comprises the following components by mass percent: 72-77 percent of copper powder, 8-10 percent of inorganic adhesive, 4-6 percent of organic adhesive, 5-12 percent of organic solvent and 1-5 percent of additive. Another purpose of the invention is to provide a thick film circuit board employing the paste and adopting toughened glass as a baseplate. The third purpose of the invention is to provide a manufacturing method of the thick film circuit board. The manufacturing method comprises the steps of preparation of the conductive paste, a encapsulating paste and the baseplate, as well as the printing, encapsulating, sintering, performance test and packaging of a circuit diagram. The thick film circuit board has favorable sintering characteristic and aesthetic appearance, and can be widely used in the manufacturing field of electronic components.
Description
Technical field
The present invention relates to the thick film circuit field, be specifically related to thick film circuit with conductor paste, the thick film circuit board of using this slurry and manufacturing approach thereof.
Background technology
Thick film circuit is a kind of of integrated circuit, be meant with resistance, inductance, electric capacity, semiconductor element and interconnecting lead through printing, burn till and operation such as welding the circuit unit of on substrate, processing with certain function.
In thick film circuit; Conduction connection between each function element need be used conductor paste, and mostly existing conductor paste is the silver slurry, and the silver slurry is at aspect excellent performances such as conductivity, solderability, adhesive force, stability; But because the ore reserve of whole world silver are limited; Add excessive exploitation in recent years, caused the price surge of noble metal silver, the cost of enterprise production product is high.And silver is under the Dc bias effect, and generation is moved and caused short circuit easily, reduces the coefficient of safety of using greatly.So, need to seek a kind of cheap and metal good conductivity and replace argent.
At present; Adopt the protective devices of clear glasses more in the photovoltaic solar field, and electric current is derived, still through electric wire as solar panel; This kind mode has caused circuit intensive various and profile is wordy attractive in appearance, and how to address the above problem becomes the new challenge of pendulum in face of the technical staff.
Summary of the invention
An object of the present invention is to provide a kind of thick film circuit cheap, safe, the silver-colored slurry of instead and use conductor paste.
For realizing above-mentioned purpose; The invention provides a kind of thick film circuit and use conductor paste, it is characterized in that: said conductor paste comprises the component of following quality percentage composition: copper powder 72% ~ 77%, inorganic bond 8% ~ 10%, organic bond 4% ~ 6%, organic solvent 5% ~ 12%, auxiliary agent 1% ~ 5%; Said inorganic bond is the lead free and cadmium free glasses powder; Said organic bond comprises organic resin; The quality percentage composition that said organic resin occupies the machine adhesive is 15%; Said organic solvent is one or more the mixture in terpinol, diethylene glycol butyl ether and the dibutyl phthalate, and said auxiliary agent is silane coupler, Bi
2O
3, one or more the mixture among lecithin and the Si Ban.
Preferably, said copper powder is made up of copper powder A and copper powder B, and said copper powder A and said copper powder B are spherical copper powder; Said copper powder A particle size distribution is 0.5 ~ 2 μ m, and purity is 99.90%, and said copper powder B particle size distribution is 1 ~ 3 μ m; Purity is 99.90%, and the mass ratio of copper powder A and copper powder B is 5 ~ 7:3 ~ 5.
Preferably, the softening point temperature of said lead free and cadmium free glasses powder is 400 ℃ ~ 600 ℃, and particle size distribution is 1 ~ 5 μ m.
Preferably, said organic bond also comprises terpinol, and said organic resin is an ethyl cellulose.
Preferably, said silane coupler is KH-550.
Another object of the present invention provides a kind of cheap, safe, thick film circuit board of burning till the good and good looking appearance of characteristic performance; Comprise the encapsulated layer that conductor layer that substrate, conductor paste lay and packaging slurry lay; It is characterized in that: said substrate is a toughened glass, and said conductor paste is above-mentioned conductor paste.
Preferably, said packaging slurry comprises the component of following quality percentage composition: pigment 5% ~ 8%, lead-free glass powder 75% ~ 80%, organic bond 5% ~ 6%, organic solvent 7% ~ 13%, organic additive 1% ~ 2%; Said organic bond comprises organic resin; The quality percentage composition that said organic resin occupies the machine adhesive is 15%; Said organic solvent is one or both in terpinol and the diethylene glycol butyl ether, and said organic additive is one or both in silicone defoaming agent and the wetting dispersing agent.
Preferably, said pigment is high temperature resistant inorganic pigment, and particle size distribution is 1 ~ 3 μ m.
Preferably, said lead-free glass powder is a microcrystalline glass powder, and softening point temperature is 450 ℃ ~ 600 ℃, and particle size distribution is 1 ~ 5 μ m.
Preferably, said organic bond also comprises the diethylene glycol butyl ether, and said organic resin is an ethyl cellulose.
Preferably, said silicone defoaming agent is Airex980.
Preferably, said wetting dispersing agent is Dispers710.
The 3rd purpose of the present invention provides a kind of method of making above-mentioned thick film circuit board, may further comprise the steps:
The preparation of a, conductor paste: the component in will filling a prescription except that organic solvent is mixed to join in the three-high mill, on one side rolling slurry add the organic solvent in the prescription on one side, regulate viscosity; After grinding 20 ~ 40min; Be dispersed into and have the homodisperse slurry of certain fineness, it is 20 ~ 70pas/25 ℃ that slurry satisfies viscosity, and fineness is 10 ~ 20 μ m; Copper content is 70% ~ 85%, and it is subsequent use to bottle;
The preparation of b, packaging slurry: the component in will filling a prescription except that organic solvent is mixed to join in the three-high mill, on one side rolling slurry add the organic solvent in the prescription on one side, regulate viscosity; After grinding 20 ~ 40min; Be dispersed into and have the homodisperse slurry of certain fineness, it is 10 ~ 50pas/25 ℃ that slurry satisfies viscosity, and fineness is 10 ~ 20 μ m; Solids content is 75% ~ 90%, and it is subsequent use to bottle;
The preparation of c, substrate: ordinary plate glass is put into glass tempering furnace carry out the tempering processing;
The printing of d, circuit diagram: adopting thick film screen printing technology is that raw material is printed on circuit design drawing on the substrate of step c with the conductor paste of step a, puts into IR bake at 100 ~ 150 ℃ of drying 2 ~ 5min, cooling after drying finishes;
E, seal: the packaging slurry with step b is the surface printing encapsulated layer of raw material at foregoing circuit figure, and whole conductor layer only exposes the part of welding pin, puts into IR bake then at 100 ~ 150 ℃ of drying 2 ~ 5min;
F, sintering: the circuit board that finishes printing is put into the nitrogen continuous tunnel furnace carry out sintering, belt speed is 160mm/min, and peak temperature is 500 ℃ ~ 580 ℃/5 ~ 15min, and total duration is 50 ~ 60min;
After g, sintering finish, test performance, packing.
Beneficial effect:
Compared with prior art, the present invention has the following advantages:
1, conductor paste provided by the invention is conductive powder body with the copper powder, and metallic copper has good electrical conductivity, and the specific insulation of copper is 1.70 * 10-6 Ω cm; The specific insulation (1.62 * 10-6 Ω cm) that is only second to silver; And metallic copper is cheap than the argent wide material sources, under the Dc bias effect, can not move; Safe; Through detecting, have excellent square resistance, solderability, adhesive force, drought tolerance and resolution behind the copper slurry sintering provided by the invention, can replace existing silver slurry fully;
2, thick film circuit board provided by the invention adopts toughened glass as substrate; Have excellent intensity, stability and transparency; Can make its electronic device of protecting avoid extraneous and corrode, based on this, this circuit board can be used for protective device and the electric current let-off gear(stand) of photovoltaic solar field as solar panel; It has replaced traditional electric wire; Conductor is integrated on the toughened glass, makes that circuit level is high, profile is succinctly attractive in appearance, when solar panel is played protection, do not influence its daylighting property rate again;
3, the used packaging slurry of the present invention is starched with no lead bronze, toughened glass sintering matching is good, and entrapped copper conductor change in resistance is little behind the sintering, and the smooth densification of glaze, anti-UV and yellow property are good;
4, used conductor paste and packaging slurry all meets the RoHS standard in the thick film circuit board provided by the invention;
5, thick film circuit board provided by the invention is through detecting the equal National standard of each item performance index.
Embodiment
Below in conjunction with specific embodiment the present invention is done further detailed description, following examples are that the present invention is not limited to following examples to the explanation of invention.
Embodiment 1
The prescription of conductor paste: copper powder A45g, copper powder B27g, lead free and cadmium free glasses powder 8.4g, the organic bond 4g, terpinol 10g, dibutyl phthalate 1.6g, KH-5502g, the Bi that form by ethyl cellulose and terpinol
2O
33g
The prescription of packaging slurry: Cr
2O
3Pigment 6g, microcrystalline glass powder 75g, the organic bond 5g, terpinol 13g, Airex9800.5g, the Dispers7100.5g that form by ethyl cellulose and diethylene glycol butyl ether
The manufacturing of thick film circuit board:
The preparation of a, conductor paste: the component in will filling a prescription except that terpinol and dibutyl phthalate is mixed to join in the three-high mill, on one side rolling slurry add the terpinol dibutyl phthalate on one side, regulate viscosity; After grinding 40min; Be dispersed into and have the homodisperse slurry of certain fineness, slurry viscosity is 30pas/25 ℃, and fineness is 20 μ m; Copper content is 72%, and it is subsequent use to bottle;
The preparation of b, packaging slurry: the component in will filling a prescription except that terpinol is mixed to join in the three-high mill, on one side rolling slurry add terpinol on one side, regulate viscosity; After grinding 30min; Be dispersed into and have the homodisperse slurry of certain fineness, it is 20pas/25 ℃ that slurry satisfies viscosity, and fineness is 15 μ m; Solids content is 85%, and it is subsequent use to bottle.
The preparation of c, substrate: the ordinary plate glass of 50cm * 50cm is put into glass tempering furnace, plate glass is carried out tempering handle.
The printing of d, circuit diagram: adopting thick film screen printing technology is that raw material is printed on circuit design drawing on the substrate of step c with the conductor paste of step a, puts into IR bake at 120 ℃ of dry 4min, cooling after drying finishes;
E, seal: the packaging slurry with step b is the surface printing encapsulated layer of raw material at foregoing circuit figure, and whole conductor layer only exposes the part of welding pin, puts into IR bake then at 120 ℃ of dry 3min;
F, sintering: the circuit board that finishes printing is put into the nitrogen continuous tunnel furnace carry out sintering, belt speed is 160mm/min, and peak temperature is 560 ℃/10min, and total duration is 60min;
After g, sintering finish, test performance, packing.
Embodiment 2
The prescription of conductor paste: copper powder A45g, copper powder B30g, lead free and cadmium free glasses powder 8.8g, the organic bond 4.3g, terpinol 2g, diethylene glycol butyl ether 4g, dibutyl phthalate 1.6, lecithin 1g, the Bi that form by ethyl cellulose and terpinol
2O
33.3g
The prescription of packaging slurry: Cr
2O
3Pigment 6g, microcrystalline glass powder 78g, the organic bond 5.2g, terpinol 4.8g, diethylene glycol butyl ether 5g, Airex9800.5g, the Dispers7100.5g that form by ethyl cellulose and diethylene glycol butyl ether
The manufacturing of thick film circuit board:
The preparation of a, conductor paste: the copper powder A in will filling a prescription, copper powder B, lead free and cadmium free glasses powder, organic bond, lecithin and Bi
2O
3Be mixed to join in the three-high mill, on one side rolling slurry add terpinol, diethylene glycol butyl ether and dibutyl phthalate on one side, regulate viscosity; After grinding 40min; Be dispersed into and have the homodisperse slurry of certain fineness, slurry viscosity is 32pas/25 ℃, and fineness is 20 μ m; Copper content is 75%, and it is subsequent use to bottle;
The preparation of b, packaging slurry: the component in will filling a prescription except that terpinol and diethylene glycol butyl ether is mixed to join in the three-high mill, on one side rolling slurry add terpinol and diethylene glycol butyl ether on one side, the adjusting viscosity; After grinding 30min; Be dispersed into and have the homodisperse slurry of certain fineness, it is 23pas/25 ℃ that slurry satisfies viscosity, and fineness is 15 μ m; Solids content is 84%, and it is subsequent use to bottle.
The preparation of c, substrate: the ordinary plate glass of 50cm * 50cm is put into glass tempering furnace, plate glass is carried out tempering handle.
The printing of d, circuit diagram: adopting thick film screen printing technology is that raw material is printed on circuit design drawing on the substrate of step c with the conductor paste of step a, puts into IR bake at 120 ℃ of dry 4min, cooling after drying finishes;
E, seal: the packaging slurry with step b is the surface printing encapsulated layer of raw material at foregoing circuit figure, and whole conductor layer only exposes the part of welding pin, puts into IR bake then at 120 ℃ of dry 3min;
F, sintering: the circuit board that finishes printing is put into the nitrogen continuous tunnel furnace carry out sintering, belt speed is 160mm/min, and peak temperature is 560 ℃/10min, and total duration is 60min;
After g, sintering finish, test performance, packing.
Embodiment 3
The prescription of conductor paste: copper powder A45g, copper powder B32g, lead free and cadmium free glasses powder 9g, the organic bond 4.5g, diethylene glycol butyl ether 4g, dibutyl phthalate 1.5g, 80 1g of class of department, the Bi that form by ethyl cellulose and terpinol
2O
33g
The prescription of packaging slurry: Cr
2O
3Pigment 6g, microcrystalline glass powder 80g, the organic bond 5.4g, diethylene glycol butyl ether 7.6g, Airex9800.5g, the Dispers7100.5g that form by ethyl cellulose and diethylene glycol butyl ether
The manufacturing of thick film circuit board:
The preparation of a, conductor paste: the component in will filling a prescription except that diethylene glycol butyl ether and dibutyl phthalate is mixed to join in the three-high mill, on one side rolling slurry add diethylene glycol butyl ether and dibutyl phthalate on one side, regulate viscosity; After grinding 40min; Be dispersed into and have the homodisperse slurry of certain fineness, slurry viscosity is 35pas/25 ℃, and fineness is 20 μ m; Copper content is 77%, and it is subsequent use to bottle;
The preparation of b, packaging slurry: the component in will filling a prescription except that the diethylene glycol butyl ether is mixed to join in the three-high mill, on one side rolling slurry add the diethylene glycol butyl ether on one side, regulate viscosity; After grinding 30min; Be dispersed into and have the homodisperse slurry of certain fineness, it is 25pas/25 ℃ that slurry satisfies viscosity, and fineness is 15 μ m; Solids content is 86%, and it is subsequent use to bottle.
The preparation of c, substrate: the ordinary plate glass of 50cm * 50cm is put into glass tempering furnace, plate glass is carried out tempering handle.
The printing of d, circuit diagram: adopting thick film screen printing technology is that raw material is printed on circuit design drawing on the substrate of step c with the conductor paste of step a, puts into IR bake at 120 ℃ of dry 4min, cooling after drying finishes;
E, seal: the packaging slurry with step b is the surface printing encapsulated layer of raw material at foregoing circuit figure, and whole conductor layer only exposes the part of welding pin, puts into IR bake then at 120 ℃ of dry 3min;
F, sintering: the circuit board that finishes printing is put into the nitrogen continuous tunnel furnace carry out sintering, belt speed is 160mm/min, and peak temperature is 560 ℃/10min, and total duration is 60min;
After g, sintering finish, test performance, packing.
Performance test:
According to the regulation in the relative national standards conductor paste among the embodiment 1 to 3 and thick film circuit board are carried out performance test, test result is seen table 1 and table 2:
Table 1
| Side's resistance test 1* | The adhesive force test 2* | The solderability test 3* | The soldering resistance test 4* | Resolution test 5* | |
| Embodiment 1 | 5.5mΩ/□ | 2.1kgf/2×2mm 2 | ＞9/10 | ＞9/10 | 0.3mm |
| Embodiment 2 | 5.0mΩ/□ | 2.5kgf/2×2mm 2 | ＞9/10 | ＞9/10 | 0.3mm |
| Embodiment 3 | 4.8mΩ/□ | 2.5kgf/2×2mm 2 | ＞9/10 | ＞9/10 | 0.3mm |
1*Side's resistance test is according to GB/T17473.3-2008
2*The adhesive force test is according to GB/T17473.4-2008
3*4*Solderability, soldering resistance are tested according to GB/T17473.7-2008
5*Resolution test is according to GB/T17473.6-2008
Table 2
1*Side's resistance changes test according to GB/T15654-1995
2*The insulating properties test is according to GB/T1410-2006
3*The aging test is according to GB/T1865-2009
4*The acid resistance test is according to YS/T610-2006
Claims (10)
1. a thick film circuit is used conductor paste, it is characterized in that: said conductor paste comprises the component of following quality percentage composition: copper powder 72% ~ 77%, inorganic bond 8% ~ 10%, organic bond 4% ~ 6%, organic solvent 5% ~ 12%, auxiliary agent 1% ~ 5%; Said inorganic bond is the lead free and cadmium free glasses powder; Said organic bond comprises organic resin; The quality percentage composition that said organic resin occupies the machine adhesive is 15%; Said organic solvent is one or more the mixture in terpinol, diethylene glycol butyl ether and the dibutyl phthalate, and said auxiliary agent is silane coupler, Bi
2O
3, one or more the mixture among lecithin and the Si Ban.
2. conductor paste according to claim 1; It is characterized in that: said copper powder is made up of copper powder A and copper powder B, and said copper powder A and said copper powder B are spherical copper powder, and said copper powder A particle size distribution is 0.5 ~ 2 μ m; Purity is 99.90%; Said copper powder B particle size distribution is 1 ~ 3 μ m, and purity is 99.90%, and the mass ratio of copper powder A and copper powder B is 5 ~ 7:3 ~ 5.
3. conductor paste according to claim 1 is characterized in that: the softening point temperature of said lead free and cadmium free glasses powder is 400 ℃ ~ 600 ℃, and particle size distribution is 1 ~ 5 μ m.
4. conductor paste according to claim 1 is characterized in that: said organic bond also comprises terpinol, and said organic resin is an ethyl cellulose.
5. thick film circuit board comprises the encapsulated layer that conductor layer that substrate, conductor paste lay and packaging slurry lay, and it is characterized in that: said substrate is a toughened glass, and said conductor paste is any described conductor paste of claim 1 to 4.
6. thick film circuit board according to claim 5 is characterized in that: said packaging slurry comprises the component of following quality percentage composition: pigment 5% ~ 8%, lead-free glass powder 75% ~ 80%, organic bond 5% ~ 6%, organic solvent 7% ~ 13%, organic additive 1% ~ 2%; Said organic bond comprises organic resin; The quality percentage composition that said organic resin occupies the machine adhesive is 15%; Said organic solvent is one or both in terpinol and the diethylene glycol butyl ether, and said organic additive is one or both in silicone defoaming agent and the wetting dispersing agent.
7. thick film circuit board according to claim 6 is characterized in that: said pigment is high temperature resistant inorganic pigment, and particle size distribution is 1 ~ 3 μ m.
8. thick film circuit board according to claim 6 is characterized in that: said lead-free glass powder is a microcrystalline glass powder, and softening point temperature is 450 ℃ ~ 600 ℃, and particle size distribution is 1 ~ 5 μ m.
9. thick film circuit board according to claim 6 is characterized in that: said organic bond also comprises the diethylene glycol butyl ether, and said organic resin is an ethyl cellulose.
10. method of making any described thick film circuit board of claim 5 to 9 may further comprise the steps:
The preparation of a, conductor paste: the component in will filling a prescription except that organic solvent is mixed to join in the three-high mill, on one side rolling slurry add the organic solvent in the prescription on one side, regulate viscosity; After grinding 20 ~ 40min; Be dispersed into and have the homodisperse slurry of certain fineness, it is 20 ~ 70pas/25 ℃ that slurry satisfies viscosity, and fineness is 10 ~ 20 μ m; Copper content is 70% ~ 85%, and it is subsequent use to bottle;
The preparation of b, packaging slurry: the component in will filling a prescription except that organic solvent is mixed to join in the three-high mill, on one side rolling slurry add the organic solvent in the prescription on one side, regulate viscosity; After grinding 20 ~ 40min; Be dispersed into and have the homodisperse slurry of certain fineness, it is 10 ~ 50pas/25 ℃ that slurry satisfies viscosity, and fineness is 10 ~ 20 μ m; Solids content is 75% ~ 90%, and it is subsequent use to bottle;
The preparation of c, substrate: ordinary plate glass is put into glass tempering furnace carry out the tempering processing;
The printing of d, circuit diagram: adopting thick film screen printing technology is that raw material is printed on circuit design drawing on the substrate of step c with the conductor paste of step a, puts into IR bake at 100 ~ 150 ℃ of drying 2 ~ 5min, cooling after drying finishes;
E, seal: the packaging slurry with step b is the surface printing encapsulated layer of raw material at foregoing circuit figure, and whole conductor layer only exposes the part of welding pin, puts into IR bake then at 100 ~ 150 ℃ of drying 2 ~ 5min;
F, sintering: the circuit board that finishes printing is put into the nitrogen continuous tunnel furnace carry out sintering, belt speed is 160mm/min, and peak temperature is 500 ℃ ~ 580 ℃/5 ~ 15min, and total duration is 50 ~ 60min;
After g, sintering finish, test performance, packing.
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|---|---|---|---|
| CN201210260679.9A CN102760934B (en) | 2012-07-26 | 2012-07-26 | Thick film circuit conductor paste, the thick film circuit board applying this slurry and manufacture method thereof |
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|---|---|---|---|
| CN201210260679.9A CN102760934B (en) | 2012-07-26 | 2012-07-26 | Thick film circuit conductor paste, the thick film circuit board applying this slurry and manufacture method thereof |
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|---|---|
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| CN102760934B CN102760934B (en) | 2015-08-05 |
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| CN105321593A (en) * | 2014-11-13 | 2016-02-10 | 珠海罗西尼表业有限公司 | Medium printing sizing agent and preparation method therefor, and thick film circuit board using sizing agent |
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| CN105682346A (en) * | 2016-02-03 | 2016-06-15 | 武汉华尚绿能科技股份有限公司 | Manufacturing method for high-conduction transparent glass-based circuit board |
| CN106252272A (en) * | 2016-10-13 | 2016-12-21 | 珠海市华晶微电子有限公司 | The connecting process of laminate patch multilayer thick film circuit |
| CN106252272B (en) * | 2016-10-13 | 2019-01-15 | 珠海市华晶微电子有限公司 | The connecting process of laminate patch multilayer thick film circuit |
| CN109524310A (en) * | 2018-10-11 | 2019-03-26 | 中国电子科技集团公司第四十三研究所 | A kind of ltcc substrate cofiring welding resistance layer manufacturing method thereof |
| CN110335701A (en) * | 2019-03-25 | 2019-10-15 | 绍兴文理学院元培学院 | A kind of thick-film resistor paste for aluminium oxide ceramics pressure sensor |
| CN112435774A (en) * | 2020-10-21 | 2021-03-02 | 中国电子科技集团公司第十三研究所 | Copper conductor slurry suitable for ceramic packaging shell and preparation method thereof |
| CN112735631A (en) * | 2020-12-21 | 2021-04-30 | 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 |
| 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 |
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