CN107723691A - A kind of chemically plating for copper electrode negative tempperature coefficient thermistor method - Google Patents
A kind of chemically plating for copper electrode negative tempperature coefficient thermistor method Download PDFInfo
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- CN107723691A CN107723691A CN201710872855.7A CN201710872855A CN107723691A CN 107723691 A CN107723691 A CN 107723691A CN 201710872855 A CN201710872855 A CN 201710872855A CN 107723691 A CN107723691 A CN 107723691A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
- C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
- C23C18/36—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents using hypophosphites
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
- C23C18/1646—Characteristics of the product obtained
- C23C18/165—Multilayered product
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/1851—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material
- C23C18/1872—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material by chemical pretreatment
- C23C18/1886—Multistep pretreatment
- C23C18/1893—Multistep pretreatment with use of organic or inorganic compounds other than metals, first
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/38—Coating with copper
- C23C18/40—Coating with copper using reducing agents
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- Chemical & Material Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Thermistors And Varistors (AREA)
Abstract
The present invention discloses a kind of method of chemically plating for copper electrode negative tempperature coefficient thermistor, comprises the following steps：(1) to thermistor ceramic matrix surface preparation；(2) using stannous chloride solution as sensitizing solution, using palladium chloride solution as activating solution, sensitization activation process is carried out to ceramic matrix surface；(3) actived slurry is printed onto to the position that need to be metallized, re-dry and high-temperature activation；(4) by thermistor ceramic matrix of the step (3) through high-temperature activation, it is placed in chemical nickel-plating liquid, Ni P transition zones is deposited under the conditions of 65 80 DEG C；(5) thermistor of step (4) is quickly transferred in chemical bronze plating liquid, deposition forms copper electrode under conditions of 60 70 DEG C；(6) dried after thermistor is rinsed well；(7) glass paste is formed on copper electrode surface by way of silk-screen printing in electrode surface, sintering forms glassivation.The application preparation method is simple, it is easy to accomplish, it is easy to enterprise scale to produce.
Description
Technical field
The invention belongs to thermistor technology field, and in particular to a kind of chemically plating is for copper electrode negative temperature coefficient heat-sensitive
The method of resistance.
Background technology
Negative temperature coefficient (NTC) thermistor refer to when temperature declines resistance value can elevated a kind of temperature sensor,
All it is used widely in fields such as industrial automation, instrument and meter, medical electronics, household electrical appliance, Aero-Space.
NTC thermistor typically uses silver electrode or gold electrode, main using the method re-sintered after printing or coating
Prepare.There is scholar's research to be investigated application of the ag paste electrode in NTC thermistor, the thickness of primary study ag paste electrode,
The influence [Tan Wei, University of Electronic Science and Technology, 2012] of sintering temperature and time to resistive performance.But your gold silver and gold belong to
Category, production cost is higher, therefore numerous manufacturers and researcher attempt low-pricedization by electrode, to accomplish scale production.
Application number CN2012100624701 Chinese patent application replaces Ag to make silver paste, but AgO whole generations with AgO
For Ag powder, actual silver content in slurry can be caused to reduce, silver layer function thickness does not reach requirement.
The content of the invention
For the deficiency of existing issue, it is an object of the invention to provide a kind of chemically plating for copper electrode negative temperature coefficient heat
The method of quick resistance, thermistor preparation method provided by the invention are simple, it is easy to accomplish, it is easy to enterprise scale to produce, and
Cost is cheap.
To achieve the above object, the technical solution adopted by the present invention is：
A kind of chemically plating comprises the following steps for the method for copper electrode negative tempperature coefficient thermistor：
(1) thermistor ceramic matrix surface is polished, then ceramic matrix surface is cleaned, dried after cleaning；
(2) thermistor ceramic matrix surface is carried out being sensitized-activation process, using stannous chloride as sensitizer, with chlorination
Palladium is activator, and 3-5min is sensitized in 30-50 DEG C of stannous chloride solution；3- is activated in 40-60 DEG C of palladium chloride solution
5min；
(3) by the thermistor ceramic matrix through sensitization activation in step (2), it is placed in chemical nickel-plating liquid, at 65-80 DEG C
Under the conditions of deposit Ni-P transition zones, using nickel sulfate and nickel acetate as nickel salt in chemical nickel-plating liquid, the two mass ratio 4：1, with secondary Asia
Phosphoric acid sodium is reducing agent, and using sodium citrate as complexing agent, the mass ratio of wherein nickel salt, sodium hypophosphite and sodium citrate is
20-25：15-21：30-40；
(4) thermistor of step (3) is quickly transferred in chemical bronze plating liquid, shape is deposited under conditions of 60-70 DEG C
Into one layer of copper electrode；
(5) thermistor in step (4) is rinsed well, after acetone is dehydrated,；
(6) step (5) surface electrode drying after, electrode surface by way of silk-screen printing in copper electrode surface shape
Into one layer of glass paste, sintering forms fine and close glassivation.
As a kind of optimal technical scheme of the application, in the step (1), cleaning way is first to clean 3-5 with acetone
Time, then with alcohol rinse 2-4 times, then rinsed well with deionized water.
As a kind of optimal technical scheme of the application, the chemical-copper-plating process of the step (4), copper plating bath includes as follows
Component：Copper sulphate, sodium potassium tartrate tetrahydrate, hydrazine, stabilizer and binding agent, the copper sulphate, sodium potassium tartrate tetrahydrate, hydrazine, stabilizer and viscous
It is 6-16 to tie agent mass ratio：8-28：15-28：0.05-1.5：0.05-0.8.
Preferably, stabilizer is any one or more of Phen, potassium ferrocyanide or sodium thiosulfate.
Preferably, binding agent is any one or more of cellulose ether, cellulose ether derivative.
Beneficial effect
Thermistor heat transfer rate provided by the invention is fast, and material is slim and graceful；Preparation method is simple simultaneously, it is easy to accomplish, just
Produced in enterprise scale, cost is cheap.
Embodiment
The present invention is described in further details with reference to embodiments.Agents useful for same or the unreceipted production of instrument and equipment
Manufacturer, it is accordingly to be regarded as the conventional products that can be bought by market.
A kind of chemically plating comprises the following steps for the method for copper electrode negative tempperature coefficient thermistor：
(1) thermistor ceramic matrix surface is polished, then ceramic matrix surface is cleaned, dried after cleaning；Institute
State in step (1), cleaning way is first to clean 3-5 times with acetone, then with alcohol rinse 2-4 times, then uses deionized water rinsing
Totally；
(2) thermistor ceramic matrix surface is carried out being sensitized-activation process, with stannous chloride (SnCl2) it is sensitizer,
With palladium bichloride (PdCl2) it is activator, it is sensitized 3-5min in 30-50 DEG C of stannous chloride solution；In 40-60 DEG C of palladium bichloride
3-5min is activated in solution；
(3) by the thermistor ceramic matrix through sensitization activation in step (2), it is placed in chemical nickel-plating liquid, at 65-80 DEG C
Under the conditions of deposit Ni-P transition zones, using nickel sulfate and nickel acetate as nickel salt in chemical nickel-plating liquid, the two mass ratio 4：1, with secondary Asia
Phosphoric acid sodium is reducing agent, and using sodium citrate as complexing agent, the mass ratio of wherein nickel salt, sodium hypophosphite and sodium citrate is
20-25：15-21：30-40；
(4) thermistor of step (3) is quickly transferred in chemical bronze plating liquid, shape is deposited under conditions of 60-70 DEG C
Into one layer of copper electrode；
The chemical-copper-plating process of the step (5), copper plating bath include following component：It is copper sulphate, sodium potassium tartrate tetrahydrate, hydrazine, steady
Determine agent and binding agent, the copper sulphate, sodium potassium tartrate tetrahydrate, hydrazine, stabilizer and binding agent mass ratio are 6-16：8-28：15-28：
0.05-1.5：0.05-0.8, wherein stabilizer be Phen, potassium ferrocyanide or sodium thiosulfate any one or it is more
Kind, binding agent is any one or more of cellulose ether, cellulose ether derivative.
(5) thermistor in step (4) is rinsed well, after acetone is dehydrated, 30- is dried under the conditions of 105 ± 5 DEG C
50min；
(6) step (5) surface electrode drying after, electrode surface by way of silk-screen printing in copper electrode surface shape
Into one layer of glass paste, sintering forms fine and close glassivation.
Embodiment 1
A kind of chemically plating comprises the following steps for the method for copper electrode negative tempperature coefficient thermistor：
(1) thermistor ceramic matrix surface is polished, is first cleaned 3 times with acetone after polishing, then rushed with alcohol
Wash 2 times, then rinsed well with deionized water, dried；
(2) ceramic matrix surface sensitizing-activation process, 50 DEG C are sensitized 3min in stannous chloride solution, molten in palladium bichloride
40 DEG C of activation 5min in liquid；
(3) by the thermistor ceramic matrix through sensitization activation in step (2), it is placed in chemical nickel-plating liquid, in 65 DEG C of bars
Ni-P transition zones are deposited under part, wherein chemical nickel-plating liquid process for preparation is as follows, weighs nickel sulfate 16g, nickel acetate 4g, adds solvent
In be well mixed, then thereto add sodium hypophosphite 15g, sodium citrate 30g, be well mixed；
(4) thermistor of step (3) is quickly transferred in chemical bronze plating liquid, deposition forms one under conditions of 60 DEG C
Layer copper electrode；Wherein every liter of copper plating bath includes following component：Copper sulphate 6g, sodium potassium tartrate tetrahydrate 8g, hydrazine 15g, Phen
0.05g, cellulose ether 0.05g.
(5) thermistor in step (4) is rinsed well, after acetone is dehydrated, dried under the conditions of 105 ± 5 DEG C
30min；
(6) step (5) surface electrode drying after, electrode surface by way of silk-screen printing in copper electrode surface shape
Into one layer of glass paste, sintering forms fine and close glassivation.
(25 DEG C) of the resistance value of the thermistor of embodiment 1 is 20.112 Ω, within ± 1% qualification rate 99.2%,
1000h agings rate of change is 0.23%.
Embodiment 2
A kind of chemically plating comprises the following steps for the method for copper electrode negative tempperature coefficient thermistor：
(1) thermistor ceramic matrix surface is polished, first cleaned 4 times with acetone after polishing, then with alcohol rinse 3
Time, finally rinsed well, dried with deionized water；
(2) ceramic matrix surface sensitizing-activation process, 50 DEG C are sensitized 4min in stannous chloride solution, molten in palladium bichloride
40 DEG C of activation 4min in liquid；
(3) by the thermistor ceramic matrix through sensitization activation in step (2), it is placed in chemical nickel-plating liquid, in 73 DEG C of bars
Ni-P transition zones are deposited under part, wherein chemical nickel-plating liquid process for preparation is as follows, weighs nickel sulfate 17.6g, nickel acetate 4.4g, adds
It is well mixed in solvent, then adds sodium hypophosphite 18g, sodium citrate 35g thereto, is well mixed；
(4) thermistor of step (3) is quickly transferred in chemical bronze plating liquid, deposition forms one under conditions of 65 DEG C
Layer copper electrode；Wherein every liter of copper plating bath includes following component：Copper sulphate 10g, sodium potassium tartrate tetrahydrate 15g, hydrazine 20g, potassium ferrocyanide
1g, cellulose ether 0.5g.
(5) thermistor in step (4) is rinsed well, after acetone is dehydrated, dried under the conditions of 105 ± 5 DEG C
40min；
(6) step (5) surface electrode drying after, electrode surface by way of silk-screen printing in copper electrode surface shape
Into one layer of glass paste, sintering forms fine and close glassivation.
(25 DEG C) of the resistance value of the thermistor of embodiment 2 is 19.998 Ω, within ± 1% qualification rate 99.5%,
1000h agings rate of change is 0.21%.
Embodiment 3
A kind of chemically plating comprises the following steps for the method for copper electrode negative tempperature coefficient thermistor：
(1) thermistor ceramic matrix surface is polished, first cleaned 5 times with acetone after polishing, then with alcohol rinse 3
Time, finally rinsed well, dried with deionized water；
(2) ceramic matrix surface sensitizing-activation process, 50 DEG C are sensitized 5min in stannous chloride solution, molten in palladium bichloride
40 DEG C of activation 3min in liquid；
(3) by the thermistor ceramic matrix through sensitization activation in step (2), it is placed in chemical nickel-plating liquid, in 73 DEG C of bars
Ni-P transition zones are deposited under part, wherein chemical nickel-plating liquid process for preparation is as follows, weighs nickel sulfate 20g, nickel acetate 5g, adds solvent
In be well mixed, then thereto add sodium hypophosphite 21g, sodium citrate 40g, be well mixed；
(4) thermistor of step (3) is quickly transferred in chemical bronze plating liquid, deposition forms one under conditions of 70 DEG C
Layer copper electrode；Wherein every liter of copper plating bath includes following component：Copper sulphate 16g, sodium potassium tartrate tetrahydrate 28g, hydrazine 28g, potassium ferrocyanide
1.5g, cellulose ether 0.8g.
(5) thermistor in step (4) is rinsed well, after acetone is dehydrated, dried under the conditions of 105 ± 5 DEG C
50min；
(6) step (5) surface electrode drying after, electrode surface by way of silk-screen printing in copper electrode surface shape
Into one layer of glass paste, sintering forms fine and close glassivation.
(25 DEG C) of the resistance value of the thermistor of embodiment 3 is 19.827 Ω, within ± 1% qualification rate 99.0%,
1000h agings rate of change is 0.30%.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (5)
1. a kind of chemically plating is for the method for copper electrode negative tempperature coefficient thermistor, it is characterised in that comprises the following steps：
(1) thermistor ceramic matrix surface is polished, then ceramic matrix surface is cleaned, dried after cleaning；
(2) thermistor ceramic matrix surface is carried out being sensitized-activation process, using stannous chloride as sensitizer, using palladium bichloride as
Activator, 3-5min is sensitized in 30-50 DEG C of stannous chloride solution；3-5min is activated in 40-60 DEG C of palladium chloride solution；
(3) by the thermistor ceramic matrix through sensitization activation in step (2), it is placed in chemical nickel-plating liquid, in 65-80 DEG C of condition
Lower deposition Ni-P transition zones, using nickel sulfate and nickel acetate as nickel salt in chemical nickel-plating liquid, the two mass ratio 4：1, with ortho phosphorous acid
Sour sodium is reducing agent, and using sodium citrate as complexing agent, wherein the mass ratio of nickel salt, sodium hypophosphite and sodium citrate is 20-25：
15-21：30-40；
(4) thermistor of step (3) is quickly transferred in chemical bronze plating liquid, deposition forms one under conditions of 60-70 DEG C
Layer copper electrode；
(5) thermistor in step (4) is rinsed well, after acetone is dehydrated, 30- is dried under the conditions of 105 ± 5 DEG C
50min；
(6) after the drying of step (5) surface electrode, one is formed on copper electrode surface by way of silk-screen printing in electrode surface
Layer glass paste, sintering form fine and close glassivation.
2. chemically plating according to claim 1 is for the method for copper electrode negative tempperature coefficient thermistor, it is characterised in that
In the step (1), cleaning way is first to clean 3-5 times with acetone, then with alcohol rinse 2-4 times, then is rushed with deionized water
Wash clean.
3. chemically plating according to claim 1 is for the method for copper electrode negative tempperature coefficient thermistor, it is characterised in that
The chemical-copper-plating process of the step (4), copper plating bath include following component：Copper sulphate, sodium potassium tartrate tetrahydrate, hydrazine, stabilizer and viscous
Agent is tied, the copper sulphate, sodium potassium tartrate tetrahydrate, hydrazine, stabilizer and binding agent mass ratio are 6-16：8-28：15-28：0.05-1.5：
0.05-0.8。
4. chemically plating according to claim 4 is for the method for copper electrode negative tempperature coefficient thermistor, it is characterised in that
Stabilizer is any one or more of Phen, potassium ferrocyanide or sodium thiosulfate.
5. chemically plating according to claim 4 is for the method for copper electrode negative tempperature coefficient thermistor, it is characterised in that
Binding agent is any one or more of cellulose ether, cellulose ether derivative.
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Cited By (2)
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| CN109627863A (en) * | 2018-11-15 | 2019-04-16 | 安徽兆拓新能源科技有限公司 | A kind of plate solar collector heat-absorbing paint |
| CN110014146A (en) * | 2019-05-22 | 2019-07-16 | 中国矿业大学 | A kind of nickel-molybdenum iron chromium-diamond alloy composite powder and its preparation method and application |
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| CN109627863A (en) * | 2018-11-15 | 2019-04-16 | 安徽兆拓新能源科技有限公司 | A kind of plate solar collector heat-absorbing paint |
| CN110014146A (en) * | 2019-05-22 | 2019-07-16 | 中国矿业大学 | A kind of nickel-molybdenum iron chromium-diamond alloy composite powder and its preparation method and application |
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