CN106825559A - resistor copper electrode sintering process - Google Patents

resistor copper electrode sintering process Download PDF

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Publication number
CN106825559A
CN106825559A CN201710011587.XA CN201710011587A CN106825559A CN 106825559 A CN106825559 A CN 106825559A CN 201710011587 A CN201710011587 A CN 201710011587A CN 106825559 A CN106825559 A CN 106825559A
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China
Prior art keywords
copper electrode
sintering
sintering furnace
resistor copper
resistor
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CN201710011587.XA
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CN106825559B (en
Inventor
尧巍华
张凯
宋秀鹏
杜军
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Dongguan E-Leo Electronics Co Ltd
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Dongguan E-Leo Electronics Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10Sintering only
    • B22F3/1017Multiple heating or additional steps
    • B22F3/1021Removal of binder or filler
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/22Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01CRESISTORS
    • H01C17/00Apparatus or processes specially adapted for manufacturing resistors
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2999/00Aspects linked to processes or compositions used in powder metallurgy

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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Mechanical Engineering (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Apparatuses And Processes For Manufacturing Resistors (AREA)
  • Powder Metallurgy (AREA)

Abstract

The invention discloses a kind of resistor copper electrode sintering process, it comprises the following steps:Resistor copper electrode product is placed on the guipure of meshbeltfurnace, resistor copper electrode product carries out dumping operation with the transmission of guipure in meshbeltfurnace;By through the resistor copper electrode product cooling after guipure stove heat to room temperature;Resistor copper electrode product after cooling is delivered in sintering furnace, organic matter is placed in sintering furnace;Fire door of sintering furnace is closed, to being vacuumized in sintering furnace and leads to nitrogen to normal pressure, open the circulation pump cycle sintering furnace gas starts sintering;Opening sintering furnace fire door, opening sintering furnace internal fan is by greenhouse cooling in sintering furnace to room temperature.The present invention produces weakly reducing atmosphere by placing quantitative organic matter in sintering furnace; oxygen is aoxidized with protective resistor copper electrode in inflated with nitrogen discharge sintering furnace; cycle sintering furnace gas; simplify the sintering process of resistor copper electrode; ensure that the stability of sintering; the cost of sintering has been saved, it is practical, can more meet industrial process conditions.

Description

Resistor copper electrode sintering process
Technical field
The present invention relates to a kind of high temperature sintering technique field, more particularly, to a kind of resistor copper electrode sintering process.
Background technology
Electric slurry is a kind of new material, is widely used in solar cell, space flight and aviation, sensing element, resistance The technical fields such as network, display, copper electric slurry is only second to heat of the gold, silver as electric slurry by its inexpensive and electric conductivity Door, but because the oxidation of its easy-sintering process without being developed well.
By conductive phase, organic phase, bonding phase composition, conductive phase is metal powder to electric slurry, and organic phase is organic adhesive, Binder Phase is glass dust, and the electrode of printing need to could form the good electricity of solderable electric conductivity by two processes of dumping and sintering Pole.For copper electrode, dumping process is easy to aoxidize copper electrode, and dumping does not become conductive network again, and sintering process is needed Oxygen free condition is wanted, otherwise copper is oxidizable, this contradiction causes that the sintering engineering of copper electrode becomes difficult.
The sintering process conditions of absolute anaerobic are extremely difficult to, and the sealing property for body of heater is harsh, the control to furnace gas System is also what is be difficult, and these problems hamper the extensive utilization of copper electrode, especially on strontium titanate pressure-sensitive resistor electrode, copper Cheap, electric conductivity is only second to silver, will not be shunk during welding migration etc. the advantages of, with copper electrode replace silver electrode idea one Directly have, but technology is immature, and sintering process not enough optimizes, and causes sintering cost to improve, and practicality is not strong, plant produced difficulty Greatly.
The content of the invention
Based on this, it is necessary in view of the shortcomings of the prior art, there is provided there is one kind high conduction performance to be not easy to oxidation simultaneously Resistor copper electrode sintering process, reduce copper electrode sintering circuit complexity, effectively reduce sintering cost.
In order to solve the above technical problems, the technical solution adopted in the present invention is:A kind of resistor copper electrode sintering process, It comprises the following steps:
(1), dumping:Resistor copper electrode product is placed on the guipure of meshbeltfurnace, resistor copper electrode product is with net The transmission of band carries out dumping operation in meshbeltfurnace;
(2), cool down:By through the resistor copper electrode product cooling after guipure stove heat to room temperature;
(3), shift:Resistor copper electrode product after cooling is delivered in sintering furnace, organic matter is placed in sintering furnace;
(4), sinter:Fire door of sintering furnace is closed, to being vacuumized in sintering furnace and leads to nitrogen to normal pressure, ON cycle pump circulation Sintering furnace gas, starts sintering, obtains final product semi-finished product resistor copper electrode;
(5), lower the temperature:Opening sintering furnace fire door, opening sintering furnace internal fan to room temperature, obtains final product greenhouse cooling in sintering furnace Resistor copper electrode finished product.
Wherein in one embodiment, the electrode one of resistor copper electrode product faces up setting in the step (1).
Wherein in one embodiment, the dump temperature in the step (1) in meshbeltfurnace is 250~280 DEG C, dumping work The sequence time is 10~20min.
Wherein in one embodiment, resistor copper electrode product is to be printed through screen process press in the step (1) Resistor copper electrode.
Wherein in one embodiment, the weight of organic matter is resistor copper electrode product after cooling in the step (3) The 1 of gross weight~5 ‰.
Wherein in one embodiment, in the step (3) organic matter including carbon dust that percentage by weight is 5~15%, 60~80% ethyl cellulose and 5~15% epoxy resin.
Wherein in one embodiment, the heating rate in the step (4) in sintering furnace is 10~15 DEG C/min, sintering Sintering temperature in stove is 500~600 DEG C, and soaking time is 10~20min.
To time for being vacuumized in sintering furnace it is 10min in the step (4) wherein in one embodiment.
To being vacuumized in sintering furnace and lead to nitrogen to normal pressure and preset wherein in one embodiment, in the step (4) Number of times is 2 times.
Wherein in one embodiment, in the step (5) opening sintering furnace internal fan by greenhouse cooling in sintering furnace extremely The temperature fall time of room temperature is not higher than 10min.
In sum, resistor copper electrode sintering process of the present invention is produced weak by the quantitative organic matter of placement in sintering furnace Reducing atmosphere, oxygen is aoxidized with protective resistor copper electrode in inflated with nitrogen discharge sintering furnace, and cycle sintering furnace gas is simplified The sintering process of resistor copper electrode, it is ensured that the stability of sintering, has saved the cost of sintering, practical, can more meet Industrial process conditions.
Specific embodiment
It is specific purposes, the function that can further appreciate that feature of the invention, technological means and reached, with reference to Specific embodiment is described in further detail to the present invention.
Resistor copper electrode sintering process of the present invention comprises the following steps:
(1), dumping:Resistor copper electrode product is laid on the guipure of meshbeltfurnace, wherein, resistor copper electrode product Electrode one face up setting, resistor copper electrode product carries out dumping operation with the transmission of guipure in meshbeltfurnace, sets Dump temperature in meshbeltfurnace is 250~280 DEG C, and dumping activity time is 10~20min;Wherein, resistor copper electrode product It is the resistor copper electrode printed through screen process press;
(2), cool down:By through the resistor copper electrode product cooling after guipure stove heat to room temperature;
(3), shift:Resistor copper electrode product after cooling is delivered in sintering furnace, places a certain amount of in sintering furnace Organic matter, wherein, the organic matter is placed in crucible, and the crucible is placed in sintering furnace, the weight of the organic matter It is 1~5 ‰ of resistor copper electrode product gross weight after cooling, the organic matter includes carbon that percentage by weight is 5~15% Powder, 60~80% ethyl cellulose and 5~15% epoxy resin;
(4), sinter:Fire door of sintering furnace is closed, to being vacuumized in sintering furnace and leads to nitrogen to normal pressure, ON cycle pump circulation Sintering furnace gas, starts sintering, and the heating rate in sintering furnace is 10~15 DEG C/min, and the sintering temperature in sintering furnace is 500~600 DEG C, soaking time is 10~20min, obtains final product semi-finished product resistor copper electrode;
Wherein in one embodiment, the time to being vacuumized in sintering furnace is 10min, to vacuumizing and leading in sintering furnace Nitrogen to the preset times of normal pressure are 2 times;
Specifically, quantitative organic matter is placed in sintering furnace and produces weakly reducing atmosphere, oxygen in inflated with nitrogen discharge sintering furnace Aoxidized with protective resistor copper electrode, cycle sintering furnace gas, it is not necessary to continuously logical nitrogen protection gas and hydrogen, an oxidation The also Primordial Qi such as carbon, the organic matter placed in sintering furnace consumes oxygen, the opposing party in faint oxygen environment further aspect imperfect combustion Face generates the weakly reducing atmosphere environment of carbon monoxide, moreover it is possible to reduces already oxidised copper electrode surface, simplifies resistor copper electrode Sintering process, it is ensured that the stability of sintering, saved sintering cost, it is practical, can more meet industrial process conditions.
(5), lower the temperature:Opening sintering furnace fire door, opening sintering furnace internal fan lowers the temperature greenhouse cooling in sintering furnace to room temperature Time is not higher than 10min, obtains final product resistor copper electrode finished product.
Resistor copper electrode after sintered stove sintering is in glassy yellow, its performance has been carried out electric conductivity, tensile strength, can Weldering performance, metallographic pattern, air inoxidizability dependence test, as a result show:Resistor copper electrode product is in two electrodes, three electrodes The film layer that surface is formed, each performance indications are all good, reach industrial application requirement, and specific embodiment is as follows:
Embodiment one
The strontium titanate pressure-sensitive resistor copper electrode printed through screen process press carries out dumping on the guipure of meshbeltfurnace, row Glue temperature is 250 DEG C, dumping activity time 10min;Then move into sintering furnace, place 0.1g organic matters, organic matter includes 0.01g carbon dusts, 0.08g ethyl celluloses, 0.01g epoxy resin;Fire door of sintering furnace is closed, 10min is vacuumized, inflated with nitrogen is to normal Pressure, repeats 2 times, opens circulating pump cycle sintering furnace gas, starts sintering, 10 DEG C/min of heating rate, sintering temperature 500 DEG C are warming up to, 10min is incubated;Heat up and be incubated after terminating, opening sintering furnace internal fan 10min is cooled to room temperature, take out electricity Resistance device copper electrode Product checking, the results are shown in Table one.
Embodiment two
The strontium titanate pressure-sensitive resistor copper electrode printed through screen process press carries out dumping on the guipure of meshbeltfurnace, row 250 DEG C of glue temperature, dumping activity time 10min;Then move into sintering furnace, place 0.1g organic matters, organic matter includes 0.01g Carbon dust, 0.08g ethyl celluloses, 0.01g epoxy resin;Fire door of sintering furnace is closed, 10min, inflated with nitrogen to normal pressure, weight is vacuumized It is multiple 2 times, circulating pump cycle sintering furnace gas is opened, start sintering, 15 DEG C/min of heating rate, sintering temperature is warming up to 500 DEG C, it is incubated 10min;Heat up and be incubated after terminating, opening sintering furnace internal fan 10min is cooled to room temperature, take out resistor copper electricity Pole Product checking, the results are shown in Table one.
Embodiment three
The strontium titanate pressure-sensitive resistor copper electrode printed through screen process press carries out dumping on the guipure of meshbeltfurnace, row 250 DEG C of glue temperature, dumping activity time 15min;Then move into sintering furnace, place 0.1g organic matters, organic matter includes 0.01g Carbon dust, 0.08g ethyl celluloses, 0.01g epoxy resin;Fire door of sintering furnace is closed, 10min, inflated with nitrogen to normal pressure, weight is vacuumized It is multiple 2 times, circulating pump cycle sintering furnace gas is opened, start sintering, 10 DEG C/min of heating rate, sintering temperature is warming up to 500 DEG C, it is incubated 10min;Heat up and be incubated after terminating, opening sintering furnace internal fan 10min is cooled to room temperature, take out resistor copper electricity Pole Product checking, the results are shown in Table one.
Example IV
The strontium titanate pressure-sensitive resistor copper electrode printed through screen process press carries out dumping on the guipure of meshbeltfurnace, row 250 DEG C of glue temperature, dumping activity time 10min;Then move into sintering furnace, place 1g organic matters, organic matter includes 0.01g carbon Powder, 0.08g ethyl celluloses, 0.01g epoxy resin;Fire door of sintering furnace is closed, 10min is vacuumized, inflated with nitrogen to normal pressure is repeated 2 times, circulating pump cycle sintering furnace gas is opened, starts sintering, 10 DEG C/min of heating rate, sintering temperature is warming up to 500 DEG C, Insulation 15min;Heat up and be incubated after terminating, opening sintering furnace internal fan 10min is cooled to room temperature, take out resistor copper electrode and produce Product examine is surveyed, and the results are shown in Table one.
Embodiment five
The strontium titanate pressure-sensitive resistor copper electrode printed through screen process press carries out dumping on the guipure of meshbeltfurnace, row 250 DEG C of glue temperature, dumping activity time 10min;Then move into sintering furnace, place 1g organic matters, organic matter includes 0.15g carbon Powder, 0.8g ethyl celluloses, 0.05g epoxy resin;Fire door of sintering furnace is closed, 10min is vacuumized, inflated with nitrogen to normal pressure repeats 2 It is secondary, circulating pump cycle sintering furnace gas is opened, start sintering, 10 DEG C/min of heating rate, sintering temperature is warming up to 500 DEG C, Insulation 10min;Heat up and be incubated after terminating, opening sintering furnace internal fan 10min is cooled to room temperature, take out resistor copper electrode and produce Product examine is surveyed, and the results are shown in Table one.
The film layer that the resistor copper electrode product of table one is formed in three electrode surfaces
Wherein, E10 is the magnitude of voltage that logical 10V voltages reflect on three electrodes, the good standard model of electric conductivity Enclose for:Higher limit 6.60V, lower limit 4.00V.
In sum, resistor copper electrode sintering process of the present invention is produced weak by the quantitative organic matter of placement in sintering furnace Reducing atmosphere, oxygen is aoxidized with protective resistor copper electrode in inflated with nitrogen discharge sintering furnace, and cycle sintering furnace gas is simplified The sintering process of resistor copper electrode, it is ensured that the stability of sintering, has saved the cost of sintering, practical, can more meet Industrial process conditions.
Embodiment described above only expresses several embodiments of the invention, and its description is more specific and detailed, but simultaneously Therefore limitation of the scope of the invention can not be interpreted as.It should be pointed out that for the person of ordinary skill of the art, Without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection model of the invention Enclose.Therefore, protection scope of the present invention should be determined by the appended claims.

Claims (10)

1. a kind of resistor copper electrode sintering process, it is characterised in that comprise the following steps:
(1), dumping:Resistor copper electrode product is placed on the guipure of meshbeltfurnace, resistor copper electrode product is with guipure Transmission carries out dumping operation in meshbeltfurnace;
(2), cool down:By through the resistor copper electrode product cooling after guipure stove heat to room temperature;
(3), shift:Resistor copper electrode product after cooling is delivered in sintering furnace, organic matter is placed in sintering furnace;
(4), sinter:Fire door of sintering furnace is closed, to being vacuumized in sintering furnace and leads to nitrogen to normal pressure, open the circulation pump cycle sintering Furnace gas, starts sintering, obtains final product semi-finished product resistor copper electrode;
(5), lower the temperature:Greenhouse cooling in sintering furnace to room temperature, is obtained final product resistance by opening sintering furnace fire door, opening sintering furnace internal fan Device copper electrode finished product.
2. a kind of resistor copper electrode sintering process as claimed in claim 1, it is characterised in that:Resistance in the step (1) The electrode one of device copper electrode product faces up setting.
3. a kind of resistor copper electrode sintering process as claimed in claim 1, it is characterised in that:Guipure in the step (1) Dump temperature in stove is 250~280 DEG C, and dumping activity time is 10~20min.
4. a kind of resistor copper electrode sintering process as claimed in claim 1, it is characterised in that:Resistance in the step (1) Device copper electrode product is the resistor copper electrode printed through screen process press.
5. a kind of resistor copper electrode sintering process as claimed in claim 1, it is characterised in that:It is organic in the step (3) The weight of thing is 1~5 ‰ of resistor copper electrode product gross weight after cooling down.
6. a kind of resistor copper electrode sintering process as claimed in claim 1, it is characterised in that:It is organic in the step (3) Thing includes carbon dust, 60~80% ethyl cellulose and 5~15% epoxy resin that percentage by weight is 5~15%.
7. a kind of resistor copper electrode sintering process as claimed in claim 1, it is characterised in that:Sintering in the step (4) Heating rate in stove is 10~15 DEG C/min, and the sintering temperature in sintering furnace is 500~600 DEG C, soaking time is 10~ 20min。
8. a kind of resistor copper electrode sintering process as claimed in claim 1, it is characterised in that:To burning in the step (4) The time vacuumized in freezing of a furnace is 10min.
9. a kind of resistor copper electrode sintering process as claimed in claim 1, it is characterised in that:To burning in the step (4) It is 2 times that nitrogen to the preset times of normal pressure are vacuumized and led in freezing of a furnace.
10. a kind of resistor copper electrode sintering process as claimed in claim 1, it is characterised in that:Opened in the step (5) The temperature fall time of greenhouse cooling in sintering furnace to room temperature is not higher than 10min by sintering furnace internal fan.
CN201710011587.XA 2017-01-07 2017-01-07 Resistor copper electrode sintering process Active CN106825559B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111489865A (en) * 2020-03-31 2020-08-04 昆明理工大学 Preparation method of self-promoting antioxidant copper electrode
CN112216457A (en) * 2020-09-24 2021-01-12 深圳顺络电子股份有限公司 Preparation method of copper electrode and piezoresistor

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0339402A (en) * 1989-07-07 1991-02-20 Mitsubishi Heavy Ind Ltd Manufacture of metal powder sintered body
JPH04333501A (en) * 1991-01-18 1992-11-20 Janome Sewing Mach Co Ltd Production of metal sintered body
CN1629986A (en) * 2003-12-18 2005-06-22 广东风华高新科技集团有限公司 Copper electrode strontium titanate annular piezoresistor and method for making same
CN102881388A (en) * 2012-09-07 2013-01-16 广州新莱福磁电有限公司 Barium strontium calcium titanate annular piezoresistor with copper alloy electrodes and preparation method thereof
CN103915248A (en) * 2014-03-27 2014-07-09 深圳振华富电子有限公司 Manufacturing method of base metal terminal electrode inductor

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0339402A (en) * 1989-07-07 1991-02-20 Mitsubishi Heavy Ind Ltd Manufacture of metal powder sintered body
JPH04333501A (en) * 1991-01-18 1992-11-20 Janome Sewing Mach Co Ltd Production of metal sintered body
CN1629986A (en) * 2003-12-18 2005-06-22 广东风华高新科技集团有限公司 Copper electrode strontium titanate annular piezoresistor and method for making same
CN102881388A (en) * 2012-09-07 2013-01-16 广州新莱福磁电有限公司 Barium strontium calcium titanate annular piezoresistor with copper alloy electrodes and preparation method thereof
CN103915248A (en) * 2014-03-27 2014-07-09 深圳振华富电子有限公司 Manufacturing method of base metal terminal electrode inductor

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111489865A (en) * 2020-03-31 2020-08-04 昆明理工大学 Preparation method of self-promoting antioxidant copper electrode
CN111489865B (en) * 2020-03-31 2021-07-30 昆明理工大学 Preparation method of self-promoting antioxidant copper electrode
CN112216457A (en) * 2020-09-24 2021-01-12 深圳顺络电子股份有限公司 Preparation method of copper electrode and piezoresistor

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