CN101217067B - A lead free aluminum electrode slurry of PTC thermo-sensitive resistor and preparation method - Google Patents
A lead free aluminum electrode slurry of PTC thermo-sensitive resistor and preparation method Download PDFInfo
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- CN101217067B CN101217067B CN2007100329396A CN200710032939A CN101217067B CN 101217067 B CN101217067 B CN 101217067B CN 2007100329396 A CN2007100329396 A CN 2007100329396A CN 200710032939 A CN200710032939 A CN 200710032939A CN 101217067 B CN101217067 B CN 101217067B
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Abstract
The invention discloses a lead-free aluminum electrode paste for a PTC thermistor and the preparation method, the electrode paste is composed of the raw materials with the following parts by weight: 55 to 70 parts of aluminum powder, 10 to 20 parts of inorganic binder, 15 to 25 parts of organic binder and 2 to 4 parts of auxiliary; wherein, the organic binder is composed of 2 to 5 parts by weightof ethyl cellulose, 3 to 6 parts by weight of butyl carbitol, 15 to 23 parts by weight of butyl carbitol acetate, 2 to 4 parts by weight of benzyl alcohol, 60 to 70 parts by weight of terpineol, 0.5 to2 parts by weight of phenolic resin and 1 to 4 parts by weight of castor oil; and the auxiliary is composed of 30 to 50 parts by weight of Bi2O3 and 50 to 70 parts by weight of phosphorus red. The el ectrode paste can prepare the aluminum conductive paste by rolling, an aluminum electrode can be formed by screen printing and sintering on a doped barium titanate semiconductor substrate within therange of 630 plus or minus 20 DEG C, the electrode and the substrate form good ohmic contact, the adhesion is good, the aluminum membrane dose not shed, and the long-term placement of the electrode has no oxidation.
Description
Technical field
The present invention relates to the resistor electric slurry, particularly relate to a kind of lead free aluminum electrode slurry and preparation method thereof.
Background technology
The PTC ceramic thermistor is one of widely used electrode component in recent years, in it is made, annually all will consume a large amount of noble metal silver and makes slurry electrode.Because economy and the technology such as the expensive and silver ion migration of silver cause many producers to adopt combination electrode to improve.Be coated with silver, chemical nickel plating and electrotinning electrode such as chemical nickel plating, so both increased the technological operation difficulty, be easy to again cause electrode surface quality to descend, a large amount of slice, thin pieces are scrapped.More external producers adopt the means such as electric arc spraying, swallow plating, sputter at PTC substrate preparation aluminum conductive electric slurry electrode recently.The general lead tolerance of the used glass dust of known aluminum conductive electric slurry electrode is very high, and slurry can cause bigger pollution to environment in making and using.
In order to reduce electronic product pollution to environment in making use, ohm on February 13rd, 2003 Official Journal in issued " waste electronic andelectrical equipment decree " (WEEE) and " about in electronic electric equipment, banning use of some harmful substance decree " (ROHS decree) two decrees be converted into formal law on August 13rd, 2004, the content of lead, mercury, Cr VI, Polybrominated biphenyl and Poly Brominated Diphenyl Ethers must not be above 0.1 part in the ROHS instruction regulation electronic product in 2005, and the content of cadmium must not be above 0.01 part.Except that European Union, global harmful substance control is all in constantly advancing.Japan, the U.S. also have been that legislation is used in the restriction of harmful substance.China Ministry of Information Industry has issued " electronics and IT products pollution control management way " and in enforcement on July 1 in 2006.Therefore it is inevitable to look for a kind of crown glass to replace having lead glass to become.
The application people discloses a kind of PTC pottery environmental-friendly lead-free silver slurry and preparation method thereof for the Chinese patent CN 1870180A of Hefei Shengda Industrial Corp, Huadong Microelectronic Technology Inst., mainly formed by micro silver powder, lead-free glass powder, organic carrier, mainly contain Bi in the lead-free glass powder
2O
2, B
2O
3, ZnO, SiO
2, Al
2O
3, the compositions such as CuO adopt newly-designed B-Bi-Zn glass system, replace usually used B-Pb-Si system frit, have realized the unleaded of product.The parts by weight of raw materials of its unorganic glass powder is: Bi
2O
3: 15-45 part, B
2O
3: 8-35 part, ZnO1-30 part, SiO
2: 1-15 part, Al
3O
3: 0-5 part, CuO:0-5 part, fusing point is lower than 470 ℃, simultaneously chemical stability, all very superior with wellability and the electrical property of PTC ceramic matrix.
The application people is the Chinese patent of the refined application of Tan Fu, publication number CN 1925070A, its invention has related to a kind of composition and preparation method of aluminum conductive electric slurry for positive temperature coefficient heat-variable resistor, the composition of its slurry comprises the aluminium powder of mass parts 45-65 part, the inorganic adhesive of 20-35 part, the organic adhesive of 15-30 part.Inorganic adhesive is flint glass powder or lead-free glass powder; Organic adhesive is a rosin ethyl cellulose organic adhesive.Its crown glass is by mass parts MgO 1-10 part, CaO 0.5-5 part, B
2O
310-20 part, SiO
25-15 part, Al
2O
31-5 part, V
2O
50.5-5 part, Bi
2O
340-75 part prescription.Its rolling aluminum conductive electric slurry through silk screen printing, sintering on the barium titanate doping semiconductor chip, the PTC themistor of formation, electrode forms good Ohmic contact with substrate, adheres to well, resistance change rate is little, the electrode non-oxidation, the aluminium film does not have obscission.Sintering temperature is at 650 ± 5 ℃.
Also there are a lot of problems in known lead free aluminum electrode slurry, at its aspect of performance not if any lead glass.The subject matter of its existence is: (1) is unqualified for the lead content of lead free aluminum electrode slurry.(2) ohmic contact is bad, with In-Ga electrode comparison resistance rate of change greater than 10 parts.(3) sintering range is narrow, and sintering range has only ± and 5 ℃, high temperature sintering can come off, and is difficult to satisfy the needs of explained hereafter.
Summary of the invention
One of purpose of the present invention provides a kind of PTC themistor lead free aluminum electrode slurry, this electrode slurry is through the rolling aluminum conductive electric slurry that gets, sintering forms the aluminium electrode on the barium titanate doping semiconductor chip in silk screen printing, 630 ± 20 ℃ of scopes, electrode forms good ohmic with substrate and contacts, adhesive force is good, the aluminium film does not come off, and places the electrode non-oxidation for a long time.
The technical scheme that realizes above-mentioned purpose is as follows:
A kind of PTC themistor lead free aluminum electrode slurry, its raw material by following mass parts is formed: the aluminium powder of 55-70 part, the inorganic bond of 10-20 part, the organic bond of 15-25 part, the auxiliary agent of 2-4 part;
Wherein, aluminium powder is particle mean size 3.0-5.0 μ m, and purity is greater than 99.80%, span 1.4-1.6, apparent density 0.45-0.6g/cm
3Ball aluminum powder; Described inorganic bond is lead-free glass powder, by pressing mass parts SiO
21-3 part, B
2O
315-30 part, Al
2O
31-3 part, Bi
2O
345-65 part and ZnO10-20 part form; Described organic bond is by by ethyl cellulose 2-5 part of mass parts, BC 3-6 part, and BC acetate 15-23 part, phenmethylol 2-4 part, terpinol 60-70 part, phenolic resins 0.5-2 part, castor oil 1-4 part forms; Described auxiliary agent is by the Bi by mass parts
2O
330-50 part, red phosphorus 50-70 part forms.
Preferably, described organic bond is by 3 parts of the ethyl celluloses of pressing mass parts, 5 parts of BCs, 19 parts of BC acetates, 4 parts of phenmethylols, 65 parts of terpinols, 1 part in phenolic resins, 3 parts of compositions of castor oil; Described inorganic bond is lead-free glass powder, by pressing mass parts SiO
22 parts, B
2O
322 parts, Al
2O
31 part, Bi
2O
363 parts and ZnO12 part; Described auxiliary agent is Bi
2O
335 parts, 65 parts of compositions of red phosphorus.
Another object of the present invention provides the preparation method of above-mentioned PTC themistor with lead free aluminum electrode slurry.
The described PTC themistor of a kind of preparation claim 1 lead free aluminum electrode slurry method may further comprise the steps:
1) raw material that will form organic bond dissolves under 80-120 ℃ of temperature, obtains the adhesive that transparent primary raw material is an ethyl cellulose;
2) raw material that will form inorganic bond mixes in batch mixer, in the porcelain crucible of packing into, in baking oven behind 140-160 ℃ of dry 2-4h, put into high temperature furnace, 850-950 ℃ of melting 0.5-1.5h, below oven dry ball milling to the 10 μ m, oven dry obtains lead-free glass powder after the shrend;
3) with described aluminium powder 55-70 part, inorganic bond 10-20 part, organic bond 15-25 part, auxiliary agent 2-4 part mixes the back and is rolled to below the fineness 22.5 μ m with three rod milling trains, and viscosity 60000-80000mPaS obtains the aluminum conductive electric slurry product.
The present invention forms by the proportioning that inorganic bond is new by the proportioning different proportion,, thus made softening point at 500-550 ℃ lead-less glasses material, and can effectively replace has lead glass.Add with Bi simultaneously
2O
3With the auxiliary agent that red phosphorus forms, when having realized aluminum conductive electric slurry unleaded (lead content＜0.1 part), also have very wide sintering range (630 ℃ ± 20 ℃ of sintering temperatures), the aluminium film can not come off behind the sintering.
Embodiment
Embodiment 1
1 preparation lead-free glass powder
By mass parts SiO
22 parts, B
2O
320 parts, Al
2O
32 parts, Bi
2O
360 parts, ZnO16 part mixes with batch mixer, in the porcelain crucible of packing into, behind 150 ℃ of dry 3h, puts into high temperature furnace in baking oven, and 900 ℃ of melting 1h are below shrend post-drying ball milling to the 10 μ m.
2 preparation organic bonds
By 3 parts of mass parts ethyl celluloses, 5 parts of butyl carbitol, 19 parts of butyl carbitol acetates, 4 parts of phenmethylols, 65 parts of terpinols, 1 part in phenolic resins, castor oil 3, above material mix the back and add at 80-120 ℃ and be hot melt to clear solution, obtain required organic bond.
3 aluminium powders: be 99.82 parts of commercially available purity, average grain diameter 3.2 μ m, aluminium powder span 1.52, apparent density 0.52g/cm
3Ball aluminum powder.
4 auxiliary agents: Bi
2O
350 parts, 50 parts in red phosphorus.
5 preparation lead free aluminum electrode slurries
By 55 parts of mass parts aluminium powders, 16 parts of lead-free glass powders, primary raw material are 25 parts in the adhesive of ethyl cellulose, add 4 parts of auxiliary agents, after mixing, are rolled to fineness 20 μ m, the lead free aluminum electrode slurry of viscosity 70000mPaS with three rod milling trains.Slurry is passed through 200 order silk screen printings on the one side of barium titanate doping semiconductor chip, 250 ℃ of oven dry are after 15 minutes, the 250 ℃ of oven dry 15 minutes again of printing order one side, put into the continuous tunnel furnace sintering, 630 ± 20 ℃ of sintering peak temperatures, 5 minutes peak temperature time, make PTC ceramic thermistor electrode.The PTC pottery heat-sensor electrode that lead free aluminum electrode slurry is made is done performance test, and transferring electrode (In: Ga=1: 1)) with indium, to compare rate of change be 0.6 part, proves that itself and ceramics ohmic contact are good.The PTC ceramic thermistor that makes at alternating current 220V, was switched on 72 hours, and the resistance increment rate is 26.8 parts; At 250 ℃, high temperature ageing 72 hours, the resistance increment rate is 31.3 parts; 97 parts of relative humidity, under 40 ℃ of the temperature, aging 72 hours, electrode non-oxidation obscission; Firmly scraping electrode can not come off.
Embodiment 2
1 preparation lead-free glass powder
By mass parts SiO
22 parts, B
2O
322 parts, Al
2O
31 part, Bi
2O
363 parts and ZnO12 part mix with batch mixer, in the porcelain crucible of packing into, behind 150 ℃ of dry 3h, put into high temperature furnace in baking oven, and 900 ℃ of melting 1h are below shrend post-drying ball milling to the 10 μ m.
2 preparation organic bonds
By 3.5 parts of mass parts ethyl celluloses, 5 parts of butyl carbitol, 20 parts of butyl carbitol acetates, 3 parts of phenmethylols, 64.5 parts of terpinols, 1 part in phenolic resins, 3 parts of castor oil, above material mix the back and add at 80-120 ℃ and be hot melt to clear solution, obtain required organic bond.
3 aluminium powders are identical with embodiment 1.
4 auxiliary agents: Bi
2O
345 parts, 55 parts in red phosphorus
5 preparation lead free aluminum electrode slurries
By 63 parts of mass parts aluminium powders, 14 parts of lead-free glass powders, 20 parts of ethyl cellulose organic bonds add 3 parts of auxiliary agents, after mixing, are rolled to fineness 20 μ m, the lead free aluminum electrode slurry of viscosity 70000mPaS with three rod milling trains.
The PTC pottery heat-sensor electrode that above-mentioned lead free aluminum electrode slurry is made is done performance test, and transferring electrode (In: Ga=1: 1)) with indium, to compare rate of change be 0.3 part, proves that itself and ceramics ohmic contact are good.The PTC ceramic thermistor that makes at alternating current 220V, was switched on 72 hours, and the resistance increment rate is 30.2 parts; At 250 ℃, high temperature ageing 72 hours, the resistance increment rate is 29.3 parts; 97 parts of relative humidity, under 40 ℃ of the temperature, aging 72 hours, electrode non-oxidation obscission; Firmly scraping electrode can not come off.
Embodiment 3
1 preparation lead-free glass powder
By mass parts SiO
21 part, B
2O
320 parts, Al
2O
31 part, Bi
2O
363 parts and ZnO20 part mix with batch mixer, in the porcelain crucible of packing into, behind 150 ℃ of dry 3h, put into high temperature furnace in baking oven, and 900 ℃ of melting 1h are below shrend post-drying ball milling to the 10 μ m.
2 preparation organic bonds
By 5 parts of mass parts ethyl celluloses, 4 parts of butyl carbitol, 23 parts of butyl carbitol acetates, 2 parts of phenmethylols, 62 parts of terpinols, 1 part in phenolic resins, 3 parts of castor oil, above material mix the back and add at 80-120 ℃ and be hot melt to clear solution, obtain required organic bond.
3 aluminium powders are identical with embodiment 1.
4 auxiliary agents: Bi
2O
335 parts, 65 parts in red phosphorus.
5 preparation lead free aluminum electrode slurries
By 70 parts of mass parts aluminium powders, 13 parts of lead-free glass powders, primary raw material are 15 parts in the adhesive of ethyl cellulose, add 2 parts of auxiliary agents, after mixing, are rolled to fineness 20 μ m, the lead free aluminum electrode slurry of viscosity 70000mPaS with three rod milling trains.
The PTC pottery heat-sensor electrode that above-mentioned lead free aluminum electrode slurry is made is done performance test, and transferring electrode (In: Ga=1: 1)) with indium, to compare rate of change be 0.9 part, proves that itself and ceramics ohmic contact are good.The PTC ceramic thermistor that makes at alternating current 220V, was switched on 72 hours, and the resistance increment rate is 26.8 parts; At 250 ℃, high temperature ageing 72 hours, the resistance increment rate is 32.4 parts; 97 parts of relative humidity, under 40 ℃ of the temperature, aging 72 hours, electrode non-oxidation obscission; Firmly scraping electrode can not come off.
Claims (8)
1. a PTC themistor lead free aluminum electrode slurry is characterized in that, its raw material by following mass parts is formed: the aluminium powder of 55-70 part, the inorganic bond of 10-20 part, the organic bond of 15-25 part, the auxiliary agent of 2-4 part;
Wherein, aluminium powder is spherical, particle mean size 3.0-5.0 μ m, and purity is greater than 99.80%, span 1.4-1.6, apparent density 0.45-0.6g/cm
3Described inorganic bond is lead-free glass powder, by pressing mass parts SiO
21-3 part, B
2O
315-30 part, Al
2O
31-3 part, Bi
2O
345-65 part and ZnO 10-20 part form; Described organic bond is by by ethyl cellulose 2-5 part of mass parts, BC 3-6 part, and BC acetate 15-23 part, phenmethylol 2-4 part, terpinol 60-70 part, phenolic resins 0.5-2 part, castor oil 1-4 part forms; Described auxiliary agent is by the Bi by mass parts
2O
330-50 part, red phosphorus 50-70 part forms.
2. PTC themistor lead free aluminum electrode slurry according to claim 1, it is characterized in that, described organic bond is by 3 parts of the ethyl celluloses of pressing mass parts, 5 parts of butyl carbitol, 19 parts of butyl carbitol acetates, 4 parts of phenmethylols, 65 parts of terpinols, 1 part in phenolic resins, 3 parts of compositions of castor oil.
3. PTC themistor lead free aluminum electrode slurry according to claim 1 is characterized in that, described inorganic bond is lead-free glass powder, by pressing mass parts SiO
22 parts, B
2O
322 parts, Al
2O
31 part, Bi
2O
363 parts and ZnO12 part composition.
4. according to each described PTC themistor lead free aluminum electrode slurry of claim 1-3, it is characterized in that described auxiliary agent is by the Bi by mass parts
2O
335 parts, 65 parts of compositions of red phosphorus.
5. one kind prepares the described PTC themistor of claim 1 lead free aluminum electrode slurry method, it is characterized in that, may further comprise the steps:
1) raw material that will form organic bond dissolves under 80-120 ℃ of temperature, obtains the adhesive that transparent primary raw material is an ethyl cellulose;
2) raw material that will form inorganic bond mixes in batch mixer, in the porcelain crucible of packing into, in baking oven behind 140-160 ℃ of dry 2-4h, put into high temperature furnace, 850-950 ℃ of melting 0.5-1.5h, below oven dry ball milling to the 10 μ m, oven dry obtains lead-free glass powder after the shrend;
3) with described aluminium powder 55-70 part, inorganic bond 10-20 part, organic bond 15-25 part, auxiliary agent 2-4 part mixes the back and is rolled to below the fineness 22.5 μ m with three rod milling trains, and viscosity 60000-80000mPaS obtains the aluminum conductive electric slurry product.
6. the PTC themistor according to claim 5 preparation method of lead free aluminum electrode slurry, it is characterized in that, described organic bond is by 3 parts of the ethyl celluloses of pressing mass parts, 5 parts of butyl carbitol, 19 parts of butyl carbitol acetates, 4 parts of phenmethylols, 65 parts of terpinols, 1 part in phenolic resins, 3 parts of compositions of castor oil.
7. PTC themistor according to claim 5 lead free aluminum electrode slurry preparation method is characterized in that, described inorganic bond is lead-free glass powder, by pressing mass parts SiO
22 parts, B
2O
322 parts, Al
2O
31 part, Bi
2O
363 parts and ZnO12 part composition.
8. PTC themistor according to claim 5 lead free aluminum electrode slurry preparation method is characterized in that, described auxiliary agent is by the Bi by mass parts
2O
335 parts, 65 parts of compositions of red phosphorus.
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| CN101217067B true CN101217067B (en) | 2010-04-07 |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101555388B (en) * | 2009-05-19 | 2012-09-05 | 无锡市儒兴科技开发有限公司 | Inorganic adhesive for aluminum paste of silicon solar cells and preparation method thereof |
| CN101714607B (en) * | 2009-09-22 | 2011-06-22 | 华南理工大学 | Piezoelectric ceramic element of metal aluminium electrode and preparation method thereof |
| WO2011066294A1 (en) * | 2009-11-25 | 2011-06-03 | E. I. Du Pont De Nemours And Company | Aluminum pastes and use thereof in the production of passivated emitter and rear contact silicon solar cells |
| CN101774758B (en) * | 2010-02-05 | 2011-12-28 | 北京科技大学 | Unleaded glass adhesives for unleaded metal electrode sizing agent and preparing method thereof |
| CN106098140A (en) * | 2016-05-23 | 2016-11-09 | 东莞珂洛赫慕电子材料科技有限公司 | A kind of PTC thermistor slurry based on stainless steel substrate and preparation method thereof |
| CN106560489A (en) * | 2016-07-14 | 2017-04-12 | 西安英诺维特新材料有限公司 | Organic secondary encapsulation slurry for sheet-type resistors, and preparation method thereof |
| CN107068237B (en) * | 2016-12-30 | 2019-05-28 | 彩虹集团新能源股份有限公司 | The preparation method of lower Tc PTC heat sensitive electronic component electrode thick liquid without lead and silver |
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| US7018864B2 (en) * | 2001-09-20 | 2006-03-28 | Murata Manufacturing Co., Ltd. | Conductive paste for terminal electrodes of monolithic ceramic electronic component, method for making monolithic ceramic electronic component, and monolithic ceramic electronic component |
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| CN1925070A (en) * | 2006-09-19 | 2007-03-07 | 谭富彬 | Composition and preparation of aluminum conductive electric slurry for positive temperature coefficient heat-variable resistor |
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2007
- 2007-12-27 CN CN2007100329396A patent/CN101217067B/en not_active Expired - Fee Related
Patent Citations (3)
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| US7018864B2 (en) * | 2001-09-20 | 2006-03-28 | Murata Manufacturing Co., Ltd. | Conductive paste for terminal electrodes of monolithic ceramic electronic component, method for making monolithic ceramic electronic component, and monolithic ceramic electronic component |
| CN1870180A (en) * | 2006-06-28 | 2006-11-29 | 华东微电子技术研究所合肥圣达实业公司 | Environment pretection leadless surface silver coating for PTC ceramic and its preparation method |
| CN1925070A (en) * | 2006-09-19 | 2007-03-07 | 谭富彬 | Composition and preparation of aluminum conductive electric slurry for positive temperature coefficient heat-variable resistor |
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