CN101333662A - Surface treating method of copper or copper ally - Google Patents
Surface treating method of copper or copper ally Download PDFInfo
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- CN101333662A CN101333662A CNA2008101268271A CN200810126827A CN101333662A CN 101333662 A CN101333662 A CN 101333662A CN A2008101268271 A CNA2008101268271 A CN A2008101268271A CN 200810126827 A CN200810126827 A CN 200810126827A CN 101333662 A CN101333662 A CN 101333662A
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- treatment agent
- copper alloy
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Abstract
The invention provides a surface processing method for forming an antirust film on Cu or Cu alloy by using a surface treating agent containing imidazole compound. The method includes steps of forming a resin layer with an opening on the surface of Cu or Cu alloy, and contacting the surface treating agent being mist particles with particle size less than 100 mum with the surface of Cu or Cu alloy in the opening.
Description
Technical field
The surface treatment agent that the present invention relates to a kind of copper that will contain imidazolium compounds or copper alloy is evenly coated copper or the copper of copper alloy surface or the surface treatment method of copper alloy in the path hole particularly.
Background technology
For example for antirust, improve weldability etc., use surface treatment agent form antirust epithelium so that form at printed base plate on the surface of the copper of distribution or copper alloy.As such surface treatment agent, the known in the past surface treatment agent that contains the imidazolium compounds of the main component that becomes formed antirust epithelium.Open in the flat 4-99285 communique the spy, disclose use 2-alkyl benzimidazole and organic acid, under 20～60 ℃, will be made as duration of contact 1 second～several minutes, as method can for the dipping and the spraying in any.In special public table 10-511431 communique, the method for dipping or spraying organic acid and triazole pyridines etc. is disclosed under 20～60 ℃, duration of contact are 30 seconds～2 minutes condition.For handle copper or copper alloy surface with these surface treatment agents for,, in order to form certain a certain amount of above antirust epithelium, generally carry out dip treating with flooding transporter etc. though can be coated with by spraying or dip treating.
But, the diameter of the peristome of the solder mask (solderresist) in such, the copper packing portion that uses in base plate for packaging etc. is under the situation of the substrate below the 400 μ m, because solder mask is usually applied is thickness about 20～35 μ m, thereby the ratio (coating thickness/opening footpath) in the coating thickness of solder mask and solder mask opening footpath becomes big.Following problem is consequently arranged: the displacement variation of air and surface treatment agent, surface treatment agent can not enter copper packing inside well in the dipping transporter, can not form antirust epithelium.
As the technology that is used to be formed uniformly epithelium, open the such technology of 2001-345544 communique: liquid is sprayed the method for handling to substrate on one side Yi Bian atomizer in the liquid is loaded in the steeping vat just like the spy.That is, atomizer in the liquid is set in the dip treating groove, forms the method for uniform epithelium.But, even atomizer in such liquid also is difficult to be formed uniformly antirust epithelium in the copper packing of such as mentioned above minor diameter.
In addition, when carrying out dip treating, be necessary in treatment trough, to store in advance liquid, and since the amount of liquid of in this treatment trough, storing in advance be generally about 1000L, very many, thereby use up at short notice just to throw away cost is uprised, be a difficulty.Therefore, the liquid management that needs the supply epithelium to become to grade, but this liquid management is very miscellaneous.And then, even common atomizer spray also is difficult to be formed uniformly antirust epithelium in the copper packing of such as mentioned above minor diameter.In addition, similarly, in communicating pores, on the such thin of via, form antirust epithelium, can have any problem with dip treating.
Summary of the invention
The present invention finishes in order to solve above-mentioned problem in the past, its objective is provides the following copper or the surface treatment method of copper alloy: even can form uniform antirust epithelium in fine part, do not need liquid management, the usage quantity of treatment agent gets final product on a small quantity, can handle with low cost.
The surface treatment method of copper of the present invention or copper alloy (below, also abbreviate " surface treatment method " as), by the surface treatment agent that contains imidazolium compounds is contacted with copper or copper alloy surface, on this copper or copper alloy, form antirust epithelium, it is characterized in that, comprise following operation: form the operation of the resin layer with peristome on the surface of described copper or copper alloy, making described surface treatment agent is the operation that the surface of copper in vaporific particle and the described peristome below the 100 μ m or copper alloy contacts as particle diameter.
Because the present invention makes particle diameter tiny vaporific (particle diameter is the following vaporific particles of 100 μ m) with surface treatment agent to contact, thereby even can be in the copper packing of minor diameter, fine parts such as the liquid communicating pores that is difficult to enter, via form uniform antirust epithelium.In addition, by handling with atomizer, need not be in steeping vat treatment agent storage, do not need liquid management.And then, promptly use dip treating, the usage quantity of treatment agent also gets final product on a small quantity, can handle with low cost.Particularly when using two fluid spray devices, on one side since on one side mixing air and treatment agent spray, thereby can suppress the usage quantity of liquid with evenly being coated with on a small quantity especially.
Description of drawings
Fig. 1: the side illustration figure of the spraying handler of Shi Yonging in an embodiment.
Fig. 2: the front explanatory view of observing preimpregnation handling part shown in Figure 1 from the transporter downstream side.
Embodiment
Below, the embodiment of surface treatment method of the present invention is elaborated.
(1) atomizer
The atomizer that uses in surface treatment method of the present invention as long as can spray particle diameter be the following tiny vaporific particles of 100 μ m, just can use any form, but preferred especially second fluid nozzle atomizer (two fluid spray devices).
The second fluid nozzle atomizer, owing in nozzle, spray after the two fluids mixing with air and liquid, thereby can under low pressure spray as fine particles, be suitable for surface treatment method of the present invention.In addition, the treatment solution of use gets final product on a small quantity, thereby the advantage that can suppress processing cost is arranged.
As the particle of being sprayed, wish that median size is below the 100 μ m, is preferably below the 70 μ m, more preferably below the 50 μ m, because this can make antirust epithelium also adhere to equably in fine copper packing.Above-mentioned median size can be measured with commercially available size-grade distribution meter.For example, can use the particle size distribution device that adopts the laser diffraction and scattering method etc. to measure.
Spray time can be according to the spray amount of the kind of surface treatment agent, atomizer, want the antirust epithelium amount that forms etc. suitably to adjust, for example, when using spray amount, preferably carry out the spraying about 5～60 seconds as the atomiser nozzle of 0.01L/ minute～0.1L/ minute.In addition, can before and after spray area, setting contain the sponge roller that is soaked with surface treatment agent, contact the auxiliary epithelium that replenishes to form with the surface of copper or copper alloy by making this sponge roller.
If with the sponge roller surface treatment agent is coated the surface of copper or copper alloy so in advance, then can form the epithelium of adequate thickness at short notice.
(2) surface treatment agent of copper or copper alloy
Surface treatment agent as the copper that uses among the present invention or copper alloy (below be also referred to as " copper/copper alloy ") so long as form the surface treatment agent that contains imidazolium compounds of antirust epithelium on the surface of copper/copper alloy, just can use any form.In surface treatment method of the present invention, spray after with atomizer surface treatment agent being made the fine particle shape, be difficult owing at high temperature handle, therefore, preferably can and form the treatment agent of antirust epithelium in the short period of time at low temperature.Particularly, preferably under duration of contact, adhere to the treatment agent of the above epithelium amount of 0.13 μ m at the liquid about 20～30 ℃, 20 seconds.
Example as the imidazolium compounds that can use in the present invention, following material: 2-(1 '-ethyl propyl) benzoglyoxaline is arranged, 2-(2 '-carboxyl phenyl) benzoglyoxaline, 2-(2 '-hydroxy phenyl) benzoglyoxaline, 2-(1-naphthyl methyl) benzoglyoxaline, 2-(2 '-chloro-phenyl-) benzoglyoxaline, 2-(2 '-aminomethyl phenyl) benzoglyoxaline, 2-(1 '-aminophenyl) benzoglyoxaline, 2-(1 '-ethyl pentyl group) benzoglyoxaline, 2-nonyl benzoglyoxaline, 2-(5 '-tolyl) pentylidene benzoglyoxaline, 1,4-bisbenzimidazole butane, 2-decyl benzoglyoxaline, 2-(5 '-xylyl) pentylidene benzoglyoxaline, 2-undecyl benzoglyoxaline, 2-dodecyl benzo imidazoles, 2-tridecyl benzo imidazoles, 5-chloro-2-octyl group benzoglyoxaline, 2-tetradecyl benzoglyoxaline.They can use separately, also can mix more than 2 kinds and use.
Above-mentioned imidazolium compounds preferably uses as the aqueous solution, and in this case, the concentration of imidazolium compounds is preferably 0.03～3 weight %.
(3) surface of copper/copper alloy
As the surface of the copper/copper alloy that is suitable for handling with surface treatment method of the present invention, for example can enumerate: be not used as the copper packing part that solder mask covered of resin layer, it is the conductive surface that forms on printed base plate.
Such copper packing, minor diameterization particularly is below the 400 μ m in base plate for packaging in recent years, also has little of the peristome that only is the minor diameter about 150 μ m～80 μ m.
When in such minor diameter copper packing, forming antirust epithelium, even dipping copper packing part in surface treatment agent, because to compare the peristome diameter little with the thickness of solder mask, thereby surface treatment agent can not enter in the copper packing well, can not be formed uniformly antirust epithelium.
In surface treatment method of the present invention, because the fine vaporific surface treatment agent of spraying, thereby in so fine copper packing, also can fully form antirust epithelium.
The diameter of copper packing and surface treatment agent though to enter easiness also relevant with the thickness of solder mask, but the thickness of solder mask is applied usually is about 20～35 μ m, thereby, if particularly become the following opening footpath of 250 μ m, then in common dip treating, liquid enter variation.
In addition, in the present invention, being not limited to circle in the shape of the surperficial formed peristome of copper or copper alloy, can be oval, rectangle (square, rectangle), unsetting, other shapes arbitrarily.In addition, in this manual, so-called " diameter of peristome ", under the situation of the peristome of circle, be meant the inside diameter of this peristome, under the situation of oval-shaped peristome, be meant the short-and-medium diameter of inside diameter of this peristome, under rectangle or unsetting etc. situation, be meant circle that the inboard with peristome joins or an oval less side's diameter.
In order to remove dirt, can also can implement microetch and handle with the surface of acid or alkaline solution processing copper/copper alloy.These acid/alkaline purifications, microetch handle or subsequent handling in clean in, also can use with the present invention in the same atomizer of atomizer that uses.
[embodiment]
Below, the embodiment of surface treatment method of the present invention is described, just not only be defined in described embodiment but the present invention is original.
" experiment 1 "
(making of substrate)
Prepare (trade(brand)name in advance at GEA-67N, Hitachi Chemical Co., Ltd.'s system epoxy glass (glass epoxy) base material, thickness: it is the sticking copper plywood in two sides that the Copper Foil of 18 μ m forms that two sides 1.6mm) is stained with thickness, and prepares 4 and cut into vertical: the plywood of 11.0cm, horizontal stroke: 8.5cm is as testing substrate.
On each test substrate, print the thick PSR-4000AUS703 (trade(brand)name of 15～30 μ m, Taiyo Ink Manufacturing Co., Ltd's system solder resist), expose, develop, form opening respectively and directly be each 100 of the copper packings of 8 kinds of circles of 80 μ m, 100 μ m, 150 μ m, 200 μ m, 250 μ m, 300 μ m, 350 μ m and 400 μ m.
(embodiment 1)
When transporting aforesaid substrate,, transporting the upper and lower settings nozzle of face for the top of substrate with followingly handle simultaneously with transporter.The position of nozzle is arranged on the position that distance is transported face 10cm.Second fluid nozzle uses BIMV8002S (trade(brand)name, Ikeuchi Corp.'s system second fluid nozzle).
Surface treatment agent uses MECSEAL CL-5018S (trade(brand)name, Mitsuku K.K.'s control surface treatment agent).Spray time was made as 20 seconds.
(embodiment 2)
Embodiment 2, and except spray time was made as 5 seconds, other are handled similarly to Example 1.
(embodiment 3)
(embodiment 4)
Embodiment 4, and except spray time was made as 5 seconds, other are handled similarly to Example 3.
(embodiment 5)
One fluid nozzle uses KB80071 (trade(brand)name, Ikeuchi Corp.'s system one fluid nozzle).Surface treatment agent uses the MECSEAL CL-5018S identical with embodiment 1.Spray time was made as 20 seconds.
(embodiment 6)
(comparative example 1)
Comparative example 1 in the spraying handler identical with embodiment 5, uses other a fluid nozzle (the system VP9030 (trade(brand)name) of Ikeuchi Corp.).Spray condition is: air pressure 0.2MPa, 20～35 ℃ of fluid temperatures, spray time 20 seconds.Surface treatment agent uses the MECSEAL CL-5018S identical with embodiment 1.
(comparative example 2)
As a comparative example 2, the test substrate in 1 liter dip treating groove, is carried out dip treating under 30 ℃, 1 minute condition.Surface treatment agent uses the MECSEAL CL-5018S identical with embodiment 1.
Respectively test substrate after handling with the microscopic examination visual valuation.Evaluation method is: if the whole face in copper packing is formed with epithelium, color changes, then be qualified; Even the part (part that epithelium does not adhere to) that has a small amount of color not change then is defective.Acceptance number in whole copper packings is made as qualification rate (%).The results are shown in the table 1.
[table 1]
As shown in Table 1, embodiments of the invention 1～6, owing to contact after surface treatment agent made tiny vaporific of particle diameter, thereby even can be in the copper packing of minor diameter, fine parts such as liquid communicating pores difficult to get access, via form uniform antirust epithelium.In addition, handle by atomizer, need not be in steeping vat treatment agent storage, do not need liquid management.And then, to compare with the dip treating of comparative example 2, the usage quantity of treatment agent gets final product on a small quantity, can handle with low cost.Particularly when using the two fluid spray devices of embodiment 1～4, on one side since on one side mixing air and treatment agent spray, thereby can be coated with particularly equably, can suppress the usage quantity of treatment agent.
" experiment 2 "
In experiment 2, measure the epithelium amount of adhering in each copper packing.
Prepare and test 1 same test substrate, on this test substrate, print the thick PSR-4000AUS703 (trade(brand)name of 15～30 μ m, Taiyo Ink Manufacturing Co., Ltd's system solder resist), expose, develop, form opening respectively and directly be each 100 of the copper packings of 6 kinds of circles of 80 μ m, 100 μ m, 200 μ m, 300 μ m, 400 μ m, 1000 μ m.
And then, use the copper surface treatment agent same, and two fluid spray machines, a fluid spray machine with experimental example 1, handle each embodiment, comparative example.
The second fluid nozzle of embodiment 7 and embodiment 8 uses the BIMV8002S (trade(brand)name) of Ikeuchi Corp.'s system, and embodiment 9 and 10 second fluid nozzle use the BIMV8075S (trade(brand)name) of Ikeuchi Corp.'s system.In addition, embodiment 11 and a fluid nozzle of 12 use the KB80071 (trade(brand)name) of Ikeuchi Corp.'s system.
The spray time of embodiment all is with the processing of spraying in 5 seconds, but in embodiment 8,10 and 12, uses in the front of spraying the spraying handler handled, is provided with the device of the preimpregnation handling part shown in Fig. 1～2.
Device shown in Figure 1, with atomizer to the substrate 2 spraying aqueous surface treatment agent of mounting on transporter 1.The spraying handler 3 of spraying and handling comprises air compressor portion 4, copper surface treatment agent reservoir 5 and spraying handling part 6, and spraying handling part 6 has second fluid nozzle.In embodiment 5 grades, replace second fluid nozzle and adopt a fluid nozzle, at this moment, do not need air compressor portion 4, replace and adopt pump (not shown).
Upstream side at spraying handler 3 is equipped with preimpregnation handling part 7.This preimpregnation handling part 7 comprises: clamping transporter 1 and be disposed at this transporter about in the of 1 a pair of upstream side sponge roller 8 and only leave in the downstream side of this upstream side sponge roller 8 that predetermined distance disposes, clamping transporter 1 and be disposed at a pair of downstream side sponge roller 9 of this transporter about in the of 1.In upstream side sponge roller 8 and the downstream side sponge roller 9, be disposed at the below part of each sponge roller of transporter 1 below, impregnated in the aqueous copper surface treatment agent that is contained in the dipping 10.
In addition, be configured in each sponge roller above the transporter 1 above, slightly be equipped with the shower 11 that is formed with squit hole with appropriate intervals abreast with each sponge roller.Like this, the sponge roller of upside is wetting by the aqueous copper surface treatment agent that the squit hole from shower 11 drips, and on the other hand, the aqueous copper surface treatment agent that the sponge roller of downside is accommodated in the dipping ware 10 is wetting.When substrate 2 passed through between the described sponge roller 8,9, the copper surface treatment agent that penetrates in this sponge roller 8,9 was wetting with substrate 2.Because sponge has elasticity, therefore have aqueous copper surface treatment agent is also clamp-oned (being coated with) effect in the tiny pad.The thickness of the sponge part of sponge roller 8,9 is necessary for about 5mm, and thickness is thicker, can obtain bigger treatment agent and clamp-on effect.
Comparative example 3 is similarly handled with comparative example 2, but use with the front of the same 1 liter of dip treating machine of comparative example 2, be provided with the device of preimpregnation handling part.
Then, measure the epithelium amount (leather film thickness) of adhering in each copper packing with following method.
[leather film thickness measuring method]
Utilize EDS (energy dispersive X-ray optical spectroscopy) to measure leather film thickness.
At first, the sticking copper plywood (identical with experiment 1) to 4cm * 4cm obtains the epithelium amount with the UV method.In this UV method, make particular area (32cm
2) the copper surface on the epithelium that adheres to be dissolved in the solution of 35% hydrochloric acid/methyl alcohol (1 grade of reagent)=0.5/99.5 (weight ratio), be in the quartzy cuvette of 10mm with its light path amplitude of packing into, measure near the ultraviolet absorbancy the wavelength 277nm.The meltage of the imidazolium compounds in absorbancy and the epithelium, that is, the adhesion amount of epithelium is proportional.
Then, to identical sample, measure the carbon counting with EDS.That is, using JSM-6390LA (trade(brand)name, the analysis scanning electronic microscope of Jeol Ltd.'s system), mensuration acceleration voltage is that 15kv, spot size (spot size) are 60, the counting of the carbon when counting rate was 6300 counting/seconds.
The epithelium amount that to measure with the UV method 1/4 as leather film thickness, make calibration curve with this leather film thickness and the carbon counting of measuring with EDS.
Then,, measure the carbon counting, obtain leather film thickness by above-mentioned calibration curve with EDS to the minor diameter pad of measuring.
Show the result in the table 2.
[table 2]
As shown in table 2, in using the processing of short period of time, leather film thickness has the tendency of attenuation, if but carry out preimpregnation and handle, then leather film thickness also can thickening.
In addition, when spraying processing, can guarantee enough leather film thickness in the minor diameter copper packing, but under the big situation of area, leather film thickness there is the situation of attenuation with fine particle.But, under the situation of carrying out the preimpregnation processing, even also can form the epithelium of adequate thickness in the large-area copper packing.
Therefore, even under the situation of printed base plate etc., minor diameter pad and the partially mixed existence of large-area copper, also can form the epithelium of adequate thickness.
Claims (5)
1. the surface treatment method of copper or copper alloy contacts with copper or copper alloy surface by making the surface treatment agent that contains imidazolium compounds, forms antirust epithelium on this copper or copper alloy, it is characterized in that, comprises following operation:
Form the operation of resin layer with peristome on the surface of described copper or copper alloy,
Making described surface treatment agent is the operation that the surface of copper in vaporific particle and the described peristome below the 100 μ m or copper alloy contacts as particle diameter.
2. the surface treatment method of copper according to claim 1 or copper alloy is characterized in that, described peristome is the path hole of maximum diameter below 400 μ m.
3. the surface treatment method of copper according to claim 1 and 2 or copper alloy is characterized in that, with the two fluid spray devices described surface treatment agent of spraying.
4. the surface treatment method of copper according to claim 3 or copper alloy is characterized in that, below the spray diameter average out to 70 μ m that formed by described two fluid spray devices.
5. the surface treatment method of copper according to claim 1 and 2 or copper alloy, it is characterized in that, with after impregnation has the sponge roller of described surface treatment agent to contact, described surface treatment agent is contacted with this surface as vaporific particle the surface of copper in the described peristome or copper alloy.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2007168035 | 2007-06-26 | ||
| JP2007168035 | 2007-06-26 | ||
| JP2007176381 | 2007-07-04 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101333662A true CN101333662A (en) | 2008-12-31 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2008101268271A Pending CN101333662A (en) | 2007-06-26 | 2008-06-24 | Surface treating method of copper or copper ally |
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| Country | Link |
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| CN (1) | CN101333662A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103668225A (en) * | 2013-12-03 | 2014-03-26 | 福州金锻工业有限公司 | Spray rust resistant machine for forged workpiece and rust resistant method therefor |
| CN111954729A (en) * | 2018-01-03 | 2020-11-17 | 埃科莱布美国股份有限公司 | Process and method for reducing corrosion of metals in water |
-
2008
- 2008-06-24 CN CNA2008101268271A patent/CN101333662A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103668225A (en) * | 2013-12-03 | 2014-03-26 | 福州金锻工业有限公司 | Spray rust resistant machine for forged workpiece and rust resistant method therefor |
| CN103668225B (en) * | 2013-12-03 | 2015-11-04 | 福州金锻工业有限公司 | Forging workpiece spraying antirust device and rust-proofing method thereof |
| CN111954729A (en) * | 2018-01-03 | 2020-11-17 | 埃科莱布美国股份有限公司 | Process and method for reducing corrosion of metals in water |
| CN111954729B (en) * | 2018-01-03 | 2023-05-23 | 埃科莱布美国股份有限公司 | Process and method for reducing corrosion of metals in water |
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