CN103762049A - Method for removing nickel electrode outer edge in chemical nickel plating of semiconductor ceramic - Google Patents
Method for removing nickel electrode outer edge in chemical nickel plating of semiconductor ceramic Download PDFInfo
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- CN103762049A CN103762049A CN201310530834.9A CN201310530834A CN103762049A CN 103762049 A CN103762049 A CN 103762049A CN 201310530834 A CN201310530834 A CN 201310530834A CN 103762049 A CN103762049 A CN 103762049A
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- nickel
- chip
- barium titanate
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Abstract
The invention discloses a method for removing a nickel electrode outer edge in chemical nickel plating of semiconductor ceramics. The method comprises the following steps: 1, preparing a barium titanate based PTC powder; 2, preparing a barium titanate based semiconductor ceramic chip; 3, conducting chemical nickel plating; 4, forming a chemical anti-etching protective layer: printing a layer of etching-resist ink on the circular surface of a resistor chip covered with nickel layer on a screen printing machine, and after light curing, printing a layer of etching-resist ink on the other surface; 5, etching the nickel layer to be removed; and 6, neutralizing the etched resistor chip with alkali lye, rinsing with clean water and drying to obtain the nickel electrode resistor chip. Compared with the prior art, the method for removing the nickel electrode outer edge in chemical nickel plating of semiconductor ceramic provided by the invention does not employ mechanical grinding, and can effectively prepare the nickel electrode on the resistor chip without breaking the chip.
Description
Technical field
The present invention relates to the method that remove a kind of semiconductive ceramic chemical nickel plating nickel electrode outer, particularly there is barium titanate (BaTiO3) based semiconductor ceramics of positive temperature coefficient, especially use this ceramic material such as electronic devices and components such as PTC thermistors.
Background technology
BaTiO
3pottery is a kind of typical ferroelectric ceramic, by the micro-rare earth element that adulterates, as Y, Nb etc., can make its resistivity at room temperature be down to below 102, shows PTC(Positive Temperature Coefficient simultaneously) effect.When temperature, surpass the Curie temperature of ceramics, ceramics resistance value is rise phenomenon sharply with the rising of temperature.This ceramic thermal resistance with positive temperature coefficient is widely used in the various aspects such as heater, overflow protecting element, degaussing component, motor starting, temp probe.Along with the development of China's household electrical appliances, communication, automobile industry, the application of PTC thermistor is more and more general.
With ceramic making electronic component, must there is electrode.Usually electrode slurry is applied to the upper and lower surface of ceramics, then through high temperature burning infiltration technique, on ceramics, forms silvery white conductive layer, for the use of energising.Yet PTC semiconductor and general dielectric porcelain are different, contact resistance in the middle of can producing between metal electrode and PTC semiconductor, its large I reaches kilo-ohm, therefore, adopts the method for conventionally preparing electrode not just to be suitable for semiconductive ceramic.Why occurring the middle contact resistance of this class, is because after N-shaped semiconductor surface adsorb oxygen molecule, electron production chemisorbed in oxygen molecule and semiconductor superficial layer, these electronics that serve as charge carrier are captured by oxygen, carrier concentration is reduced, produce positive space charge district, form resistive formation.If at semiconductor surface obliterating In-Ga alloy, because In-Ga captures oxygen, sruface charge is neutralized, therefore reduce contact berrier, make between metal electrode and semiconductor contact resistance minimum, be called ohmic contact.If make electrode with noble metal, owing to being difficult for reacting with oxygen, thereby can not discharge the electronics of being captured by oxygen, thereby contact resistance is very large, is referred to as non-ohmic contact.
If can prepare the PTC thermistor Ohm contact electrode that is applicable to suitability for industrialized production under stable process conditions, Jiang Wei China brings very large economic benefit and social benefit.The method of preparing this class electrode is a lot, as chemical nickel plating, burning infiltration Ag-Zn, A1 slurry and Ag electrode etc.Because the conductive capability of Ag is strong, antioxygenic property is good, and the direct weld metal on Ag surface, so general electronic ceramic adopts the burning infiltration of silver slurry to prepare electrode conventionally.But because Ag and semiconductor element can not form ohmic contact, thus can not be directly with the electrode of silver slurry preparation PTC thermistor.Need in silver paste, introduce the metal that reproducibility is strong, as Zn, Fe, Al, Ni etc., can make semiconductive ceramic surface depletion layer disappear and reduce contact resistance, this silver slurry is called ohm silver slurry.Old first-class has been carried out " research of the easy welding electrode slurry of silver-colored aluminium tin ohmic contact " (< < electronic component and material > > 1997,16 (6): 37-40), find that aluminium electrode shows low contact resistance.Yet, the people such as Zhan Yizeng (< < modern technologies pottery > > 2003,97 (3): 12-15) find that burning infiltration aluminium electrode exists shock-resistant electric current little, ageing-resistant moist characteristic is poor, burning infiltration temperature is narrow, and finished product storage capacity is poor etc.Burning infiltration aluminium electrode can not be applied in requiring high product.Professors Zhou Dongxiang etc. have reported (Sensors and Actuators A 101 (2002): the Ni-P alloy (through heat treatment) that 123) chemically coated nickel method forms forms good ohmic contact electrode with PTC semiconductive ceramic.Stability is good, and is widely used as PTC semiconductive ceramic Ohm contact electrode (plating and covering with paint, 2004,23 (1): 28).Its metal deposition adopts traditional sensitization-activation method; then in chemical nickel plating pond, deposit one deck 0.5-0.7 μ m Ni-P alloy; (nitrogen protection) heat treatment 90 minutes under the condition of 300 ℃ again; with coreless grinding machine, grind off after nickel dam around, at the top layer of nickel coating electrode, pass through to be formed by silver-colored burning infiltration method the silver electrode of one deck (2 μ m).The method can meet metal electrode and PTC semiconductive ceramic forms good ohmic contact problem.
The pattern of expectation or image are etched into a suprabasil method of knowing, comprise first the ink printing that is called as etching resisting ink to substrate, be printed onto in not etched those base part, to protect or to shelter those regions away from etching media.The substrate of sheltering with etching resisting ink is exposed to etching media subsequently, for example, acid solution, the basal region of not sheltered by ink is etched.After etching step, this etching resisting ink for example by rinsing and removed from substrate in alkali.The method is widely used in the manufacture of printed circuit board, wherein Multiple depositions, shelter with etching step and be used to set up complicated structure.In the manufacture process of solar cell and steel embossed tape, etching resisting ink is also used in etching.
The same with etching, etching resisting ink has application in plating.In this kind of situation, the region at the bottom of etching resisting ink masked radical is away from electroplating medium and therefore preventing the deposition on those regions.The method is used in the production of some solar cells.
Silk screen printing is used to etching resisting ink to be applied in substrate widely.This technical costs is low and reliable.
The ink using in the silk screen printing of resist is often photocuring, and therefore, after it is printed in substrate, this ink can be cured into dura mater immediately.Such silk-screen ink typically comprises the alkali soluble resins that can reach 40%, to give cured printing ink layer alkali solubility, therefore, they can utilize aqueous alkali to be washed off from substrate.
At present, the preparation of thermistor Ohmic electrode, generally first adopts the method for chemical nickel plating at circular resistance chip surface plating one deck nickel, then adopts mechanical grinding that the nickel dam of chip edge is ground off.But easy damage resistance chip during grinding, produces a large amount of noise pollutions simultaneously, and when chip form is irregular, then adopt the method for grinding, production efficiency is low, is unfavorable for large-scale production.
Summary of the invention
The method that provides a kind of semiconductive ceramic chemical nickel plating nickel electrode outer to remove is just provided object of the present invention, the method that remove this semiconductive ceramic chemical nickel plating nickel electrode outer does not adopt mechanical grinding, can, not destroying under the prerequisite of chip, effectively on resistance chip, prepare nickel electrode.
Technical scheme of the present invention is: the method that remove a kind of semiconductive ceramic chemical nickel plating nickel electrode outer, and the method comprises the following steps:
1. barium titanate-based PTC powder is produced: ball milling form slurry after barium phthalate base raw material is mixed, and pre-burning after drying, ball milling after pre-burning, then enters spray tower granulation and obtains barium titanate-based PTC powder;
2. barium titanate-based semiconductor ceramics chip is produced: utilize rotation press to carry out moulding process, barium titanate-based PTC pressed by powder is become to put into sintering furnace after ceramic green and obtain barium titanate-based semiconductor ceramics chip;
3. chemical nickel plating: barium titanate-based semiconductor ceramics chip obtains the resistance chip of surface coverage nickel dam through cleaning, sensitization, activation, nickel plating;
4. chemical anti-etch protection layer forms: on screen process press, to the resistance chip circular surface printing one deck etching resisting ink that covers nickel dam, after photocuring, turn-over is to another circular surface printing one deck etching resisting ink;
5. the nickel dam that eating away need remove: the resistance chip of the covering nickel dam with chemical anti-etch protection layer is put into acid solution and etch away the nickel dam that need remove;
6. by the resistance chip after etching with in alkali lye and rinse post-drying with clear water and obtain nickel electrode resistance chip afterwards.
As preferably, described acid solution is 15% hydrochloric acid, and etch period is 5-10min.
As preferably, the NaOH that described alkali lye is 5%, in and the time be 5-10min.
As preferably, described oven dry is dried in baking oven, and temperature is 100 ℃, and the time is 20min.
Compared with prior art, beneficial effect of the present invention is:
(1) can effectively for resistance chip, prepare nickel electrode, avoid the damage of mechanical grinding to chip simultaneously, and also can carry out large-scale production for chip in irregular shape.
(2) compare with adopting the method for mechanical grinding, more cost-saving, while noise-less pollution, and also electrical property is constant.
(3) in chip size design, can not consider by the part of mechanical grinding, save raw material.
Accompanying drawing explanation
Fig. 1 is for removing the resistance chip generalized section before the nickel dam that need remove;
Fig. 2 is for removing the chip profile schematic diagram after the nickel dam that need remove;
In Fig. 1, Fig. 2: 1-resistance chip; The anti-etch protection layer of 2-chemistry; The nickel dam that 3-need retain; The nickel dam of 4-etching.
Embodiment
Below in conjunction with accompanying drawing, the invention will be further described.
Embodiment 1
1) by BaCO
3, TiO
2, Y
2o
3, CaCO
3according to BaCO
378, TiO
2101, Y
2o
30.4, CaCO
315 molar constituent, than mixing, obtains mixed slurry for 4 hours with 400 revs/min of ball millings.Mixed slurry is dried, with the speed of 200 ℃/h, be raised to 1200 ℃ of insulations and within 2 hours, carry out pre-burning, powder after pre-burning after 4 hours, is entered to the barium titanate-based PTC powder that spray tower granulation obtains with 400 revs/min of ball millings;
(2) utilize rotation press to carry out moulding process, PTC pressed by powder is become to diameter 10mm, the ceramic green of thickness 3.5mm, puts into sintering furnace by ceramic green and carries out 1 hour sintering processes of 1300 ℃ of insulations, obtains barium titanate-based semiconductor ceramics chip;
(3) adopt the method for chemical nickel plating, first ceramic chip is cleaned, then in sensitizing solution, soak 10min, then washing enters activation procedure.Chip takes out place 5min in activating solution after, and clear water enters nickel plating process after rinsing.Chip soaks in nickel-plating liquid, take out after stirring 10min, then through clear water or hot water shower, then in baking oven 250-280 ℃ of heat treatment 25min, obtain the resistance chip of surface coverage nickel dam;
(4) on screen process press, give resistance chip circular surface printing one deck etching resisting ink, after photocuring, turn-over, to another circular surface printing one deck etching resisting ink, is put into 15% hydrochloric acid solution by the chip printing and is stirred 5-10min, etches away the nickel dam on circumference;
(5) the resistance chip after etching in (4) is put into 5% sodium hydroxide solution, and stir after 5-10min, with clear water, rinse chip, put into 100 ℃ of baking oven 20min and dry moisture, complete nickel electrode preparation, recording this resistor core sheet resistivity is 45 Ω mm.
Resistance chip before the nickel dam that removal need be removed is shown in Fig. 1, and the resistance chip after the nickel dam that removal need be removed is shown in Fig. 2.
Comparative example 1
(1) by BaCO
3, TiO
2, Y
2o
3, CaCO
3according to BaCO
378, TiO
2101, Y
2o
30.4, CaCO
315 molar constituent, than mixing, obtains mixed slurry for 4 hours with 400 revs/min of ball millings.Mixed slurry is dried, with the speed of 200 ℃/h, be raised to 1200 ℃ of insulations and within 2 hours, carry out pre-burning, powder after pre-burning after 4 hours, is entered to the barium titanate-based PTC powder that spray tower granulation obtains with 400 revs/min of ball millings;
(2) utilize rotation press to carry out moulding process, PTC pressed by powder is become to diameter 10mm, the ceramic green of thickness 3.5mm, puts into sintering furnace by ceramic green and carries out 1 hour sintering processes of 1300 ℃ of insulations, obtains barium titanate-based semiconductor ceramics chip;
(3) adopt the method for chemical nickel plating, first ceramic chip is cleaned, then in sensitizing solution, soak 10min, then washing enters activation procedure.Chip takes out place 5min in activating solution after, and clear water enters nickel plating process after rinsing.Chip soaks in nickel-plating liquid, take out after stirring 10min, then through clear water or hot water shower, then in baking oven 250-280 ℃ of heat treatment 25min, obtain the resistance chip of surface coverage nickel dam;
(4) adopt coreless grinding machine, the nickel dam on resistance chip circumference is ground off, with clear water, rinse chip, put into 100 ℃ of baking oven 20min and dry moisture, complete nickel electrode preparation, recording this resistor core sheet resistivity is 45 Ω mm;
Resistance chip before the nickel dam that removal need be removed is shown in Fig. 1, and the resistance chip after the nickel dam that removal need be removed is shown in Fig. 2.
From above-described embodiment, can find out, adopt coated surface is carried out to diaphragm coating, and after etching finishes, the method for this protective film removal be prepared to nickel electrode, the nickel electrode electrical property of preparing with the method for traditional mechanical grinding is consistent.
Claims (4)
1. the method that remove semiconductive ceramic chemical nickel plating nickel electrode outer, the method comprises the following steps:
1. barium titanate-based PTC powder is produced: ball milling form slurry after barium phthalate base raw material is mixed, and pre-burning after drying, ball milling after pre-burning, then enters spray tower granulation and obtains barium titanate-based PTC powder;
2. barium titanate-based semiconductor ceramics chip is produced: utilize rotation press to carry out moulding process, barium titanate-based PTC pressed by powder is become to put into sintering furnace after ceramic green and obtain barium titanate-based semiconductor ceramics chip;
3. chemical nickel plating: barium titanate-based semiconductor ceramics chip obtains the resistance chip of surface coverage nickel dam through cleaning, sensitization, activation, nickel plating;
4. chemical anti-etch protection layer forms: on screen process press, to the resistance chip circular surface printing one deck etching resisting ink that covers nickel dam, after photocuring, turn-over is to another circular surface printing one deck etching resisting ink;
5. the nickel dam that eating away need remove: the resistance chip of the covering nickel dam with chemical anti-etch protection layer is put into acid solution and etch away the nickel dam that need remove;
6. by the resistance chip after etching with in alkali lye and rinse post-drying with clear water and obtain nickel electrode resistance chip afterwards.
2. the method that remove semiconductive ceramic chemical nickel plating nickel electrode according to claim 1 outer, is characterized in that: described acid solution is 15% hydrochloric acid, etch period is 5-10min.
3. the method that remove semiconductive ceramic chemical nickel plating nickel electrode according to claim 1 outer, is characterized in that: the NaOH that described alkali lye is 5%, in and the time be 5-10min.
4. the method that remove semiconductive ceramic chemical nickel plating nickel electrode according to claim 3 outer, is characterized in that: described oven dry is dried in baking oven, temperature is 100 ℃, and the time is 20min.
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| CN201310530834.9A CN103762049A (en) | 2013-11-01 | 2013-11-01 | Method for removing nickel electrode outer edge in chemical nickel plating of semiconductor ceramic |
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| CN201310530834.9A CN103762049A (en) | 2013-11-01 | 2013-11-01 | Method for removing nickel electrode outer edge in chemical nickel plating of semiconductor ceramic |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107602158A (en) * | 2017-09-25 | 2018-01-19 | 江苏时瑞电子科技有限公司 | A kind of preparation method of thermistor copper electrode |
| CN112670046A (en) * | 2020-12-11 | 2021-04-16 | 成都顺康三森电子有限责任公司 | Method for manufacturing low-resistance high-voltage-resistance PTC thermistor |
Citations (4)
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| CN1624816A (en) * | 2004-12-21 | 2005-06-08 | 上海维安热电材料股份有限公司 | Method for manufacturing chip ceramic matrix electronic element |
| CN1630917A (en) * | 2002-02-11 | 2005-06-22 | 尼科原料美国公司 | Etching solution for forming an embedded resistor |
| CN1694934A (en) * | 2002-09-20 | 2005-11-09 | 艾夫西亚有限公司 | Process and ink for making electronic devices |
| KR100841142B1 (en) * | 2007-02-16 | 2008-06-24 | 엘에스전선 주식회사 | Ptc-device with improved safety and manufacturing method thereof |
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2013
- 2013-11-01 CN CN201310530834.9A patent/CN103762049A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1630917A (en) * | 2002-02-11 | 2005-06-22 | 尼科原料美国公司 | Etching solution for forming an embedded resistor |
| CN1694934A (en) * | 2002-09-20 | 2005-11-09 | 艾夫西亚有限公司 | Process and ink for making electronic devices |
| CN1624816A (en) * | 2004-12-21 | 2005-06-08 | 上海维安热电材料股份有限公司 | Method for manufacturing chip ceramic matrix electronic element |
| KR100841142B1 (en) * | 2007-02-16 | 2008-06-24 | 엘에스전선 주식회사 | Ptc-device with improved safety and manufacturing method thereof |
Non-Patent Citations (1)
| Title |
|---|
| DAOLI ZHANG等: ""The ac electrical failure behaviors and mechanisms of current limiting BaCO3-based positive-temperature-coefficient (PTC) ceramic thermistors coated with electroless nickel-phosphorous electrode"", 《SENSORS AND ACTUATORS A》, vol. 101, no. 12, 30 September 2002 (2002-09-30), pages 123 - 131, XP004380159, DOI: doi:10.1016/S0924-4247(02)00189-9 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107602158A (en) * | 2017-09-25 | 2018-01-19 | 江苏时瑞电子科技有限公司 | A kind of preparation method of thermistor copper electrode |
| CN112670046A (en) * | 2020-12-11 | 2021-04-16 | 成都顺康三森电子有限责任公司 | Method for manufacturing low-resistance high-voltage-resistance PTC thermistor |
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Application publication date: 20140430 |