CN101982288A - Organic copper solderability preservative having selective film forming function and use method thereof - Google Patents
Organic copper solderability preservative having selective film forming function and use method thereof Download PDFInfo
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- CN101982288A CN101982288A CN2010105025064A CN201010502506A CN101982288A CN 101982288 A CN101982288 A CN 101982288A CN 2010105025064 A CN2010105025064 A CN 2010105025064A CN 201010502506 A CN201010502506 A CN 201010502506A CN 101982288 A CN101982288 A CN 101982288A
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Abstract
The invention discloses an organic copper solderability preservative having a selective film forming function and a use method thereof. The organic copper solderability preservative is a composite solution prepared from 10-100ML/L of formic acid, 100-500ML/L of acetic acid, 1-8g/L of imidazole organic matter, 1-6g/L of thiourea, 2-8g/L of zinc acetate, 1-10ml/L of ethanolamine, and 5-20g/L of citric acid. The use method has the following steps: performing oil removal and mircoetching on printed circuit boards (PCBs) and then carrying out film forming on the PCBs in the organic copper solderability preservative for 90-120s and controlling film thickness within 0.15-0.25mu m. The organic copper solderability preservative of the invention can be directly utilized to manufacture C support plates and chemically selective plates; in addition, gold surfaces of the two kinds of plates do not discolour, can maintain initial property and are free from influence of the organic copper solderability preservative; the organic film can resist high temperature for 5 times and features good weldability, fast production efficiency, low cost, simple and environment-friendly preparation, easy treatment of waste water and fine solderability.
Description
[technical field]
The present invention relates to the print circuit board surface treatment technology, relate to a kind of naked copper or copper/golden mixed printing PCB surface of realizing specifically under copper and the common situation about existing of gold, organic film can not be deposited on Jin Mianshang, but selectively be deposited on organic copper solderability preservative that a kind of on the copper face have a selectivity film forming with and using method.
[background technology]
At present, electronic product is towards gently, and is thin, short, miniaturization, multifunction development, simultaneously printed wiring board is also towards high precision, slimming, multiple stratification, the aperture direction develops, the especially fast development of SMT, thus make SMT use the high density thin plate (as IC-card, mobile phone, notebook computer, printed boards such as tuner) constantly development, and in the SMT processing procedure, what have only copper and tin is the most firm in conjunction with formed IMC, makes more and more incompatibility above-mentioned requirements of hot air leveling technology.The Sn-Pb scolder of hot air leveling technology use does not simultaneously meet environmental requirement yet, formal enforcement along with the RoHS of European Union instruction on July 1st, 2006, industry is badly in need of seeking the unleaded alternative of PCB surface-treated, the most organic solder resistant (OSP), and it possesses following advantage:
1, heat endurance, with the FLUX that is similarly surface conditioning agent relatively the time, find 235 ℃ of OSP post bake after, surperficial non-oxidation phenomenon, diaphragm is not destroyed.Get two in the sample of the sample of OSP and FLUX respectively, put into 60 ℃ simultaneously, in 90% the climatic chamber, after the week, the sample of OSP does not have significant change, and yellow point appears in the sample surface of FULX, promptly is heated rear oxidation.
2, management simplicity, the technology of OSP is fairly simple, also operation easily, client can use any welding manner that it is processed, and does not need specially treated; When circuit is produced, needn't consider the problem of surface uniformity, also needn't worry, simply and easily the operational method of way to manage ， Kuai Qian for the concentration of its soup.
3, low cost because of itself and naked copper partly react, forms inviscid, thin and uniform diaphragm, so every square metre cost is lower than other surface conditioning agent, can be described as in all surface treatment process, and is lower-cost a kind of.
4, reduce pollution, do not contain the direct harmful substance that influences environment among the OSP, as: lead and lead compound, bromine and bromine compounds etc., on automatic assembly line, working environment is good, and equipment is less demanding.
5, ease of assembly adopts OSP to carry out surface treatment, and surfacing when print solder paste or stickup SMD element, reduces the skew of part, reduces the probability of the empty weldering of SMD solder joint simultaneously.
OSP is exactly on the naked copper surface of cleaning; method with chemistry forms a kind of organic epithelium; that this layer epithelium has is anti-oxidation, heat shock resistance, moisture-proof; in normal environment, no longer continue oxidized in order to the protection copper face; but in follow-up high-temperature soldering process; this diaphragm must be easy to again be dissolved rapidly by scaling powder; make in the extremely short time scolding tin with fusion be combined at once to lead solid solder joint to expose clean copper face; and leadless process is had higher requirement to the high temperature resistant impact of OSP film, generally requires the high temperature of minimum ability more than three times.When production mixed golden plate, golden face can variable color in addition.When at present producing gold finger plate, solution is to stick blue glue at Jin Mianshang earlier, and having served as and having torn blue glue behind the OSP again is time-consumingly to require great effort again to reach protective money face nondiscolouring purpose, to do like this, and has had a strong impact on production efficiency.And rubberizing only is fit to do the mixed golden plate of golden finger, and as IC support plate (BGA), choosingization plate (copper/gold mix) is unworkable at all with rubberizing, has only by gold-plated and does surface treatment, has increased cost greatly.The defective value of described prior art must improve.
[summary of the invention]
The objective of the invention is at above-mentioned technological deficiency, a kind of organic copper solderability preservative with selectivity film forming is provided, and this is a kind of to have organic copper solderability preservative of selectivity film forming in order to be applicable to leadless process, gold face variable color when preventing OSP, enhance productivity, reduce production costs.
Technical scheme of the present invention is as described below: a kind of organic copper solderability preservative with selectivity film forming, it is characterized in that: it is the composition solution that is prepared into by formic acid, acetate, imidazoles organic matter, thiocarbamide, zinc acetate, monoethanolamine, citric acid, and wherein the quality proportioning of each component is:
Formic acid 10-100ML/L acetate 100-500ML/L imidazoles organic matter 1-8g/L
Thiocarbamide 1-6g/L zinc acetate 2-8g/L monoethanolamine 1-10ml/L
Citric acid 5-20g/L.
A kind of organic copper solderability preservative with selectivity film forming according to above-mentioned is characterized in that the imidazoles organic matter is preferably the aryl phenyl imidazoles, and wherein the quality proportioning of each component is:
Formic acid 10-100ML/L acetate 100-500ML/L aryl phenyl imidazoles 1-8g/L
Thiocarbamide 1-6g/L zinc acetate 2-8g/L monoethanolamine 1-10ml/L
Citric acid 5-20g/L.
According to above-mentioned a kind of organic copper solderability preservative with selectivity film forming, its feature is that also the imidazoles organic matter is preferably the alkylbenzene imidazoles, and wherein the quality proportioning of each component is:
Formic acid 10-100ML/L acetate 100-500ML/L alkylbenzene imidazoles 1-4g/L
Thiocarbamide 1-6g/L zinc acetate 2-8g/L monoethanolamine 1-10ml/L
Citric acid 5-20g/L
According to above-mentioned a kind of organic copper solderability preservative with selectivity film forming, its feature also is: the imidazoles organic matter is preferably alkyl imidazole, and wherein the quality proportioning of each component is:
Formic acid 10-100ML/L acetate 100-500ML/L alkyl imidazole 1-6g/L
Thiocarbamide 1-6g/L zinc acetate 2-8g/L monoethanolamine 1-10ml/L
Citric acid 5-20g/L
According to above-mentioned a kind of organic copper solderability preservative with selectivity film forming, its feature is that also each constituent mass proportioning is:
Formic acid 25-40ML/L acetate 180-300ML/L aryl phenyl imidazoles 1-6g/L
Thiocarbamide 1-6g/L zinc acetate 2-6g/L monoethanolamine 1-6ml/L
Citric acid 5-18g/L
A kind of as above-mentioned a kind of using method with organic copper solderability preservative of selectivity film forming, it is characterized in that this method comprises the steps:
A, with the pcb board oil removing
1) material is prepared,
Preparing concentration is the sulfuric acid of 5ml/L, and concentration is that the APES of 0.1ml/L is stand-by, and environment temperature is controlled at 33～37 ℃,
2) 100L builds bath:
1. the pure water of 2/3 volume is put into groove,
2. add 500ml sulfuric acid while stirring, the 10ml APES,
3. add pure water and stir to 100L,
B, with the pcb board microetch
1) material is prepared
Preparing concentration is the sulfuric acid of 5ml/L, and concentration is that the hydrogen peroxide of 60ml/L is stand-by, and environment temperature is controlled at 28 ℃-32 ℃,
2) the immersion microetch time is controlled at 60-90S, or the spray-type microetch time be controlled at 30-60S,
C, pcb board is put into as film forming in above-mentioned a kind of organic copper solderability preservative with selectivity film forming
1) thorough cleaning equipment,
2) stoste that adds 100% final volume in groove is opened cylinder,
3) detect pH value, pH value transferred to 3.9 ± 0.2 with ammoniacal liquor,
4) ON cycle pump is heated to 42 ℃ ± 1 ℃ with solution.
According to as above-mentioned a kind of using method with organic copper solderability preservative of selectivity film forming, it is characterized in that the time of described step a oil removing is controlled at 30-60S, the time of step c film forming is controlled at 90-120S.
According to as above-mentioned a kind of using method with organic copper solderability preservative of selectivity film forming, it is characterized in that, between step b and step c, also comprise a water-washing step, adopt DI water during washing, and its pH value is controlled between the 3.9-4.1.
According to as above-mentioned a kind of using method with organic copper solderability preservative of selectivity film forming, it is characterized in that, behind step c, also comprise a water-washing step, adopt DI water during washing, and pH value is controlled between the 3.9-4.1.
According to as above-mentioned a kind of using method, it is characterized in that the film thickness of step c film forming is controlled between the 0.15-0.25um with organic copper solderability preservative of selectivity film forming.
According to above-mentioned the present invention, its beneficial effect is: the present invention can directly produce the IC support plate, choosingization plate, and golden face nondiscolouring, can keep original characteristic, be not subjected to the influence of OSP liquid medicine, and five high temperature of organic film ability, good solderability had, and production efficiency is fast, cost is low, and the simple environmental protection of processing procedure, wastewater treatment are easily and have a good solderability.
[specific embodiment]
Below in conjunction with embodiment the present invention is further described:
A kind of organic copper solderability preservative with selectivity film forming is characterized in that it is the composition solution that is prepared into by formic acid, acetate, imidazoles organic matter, thiocarbamide, zinc acetate, monoethanolamine, citric acid, and wherein the quality proportioning of each component is:
Formic acid 10-100ML/L acetate 100-500ML/L imidazoles organic matter 1-8g/L
Thiocarbamide 1-6g/L zinc acetate 2-8g/L monoethanolamine 1-10ml/L
Citric acid 5-20g/L.
Embodiment 1
A kind of organic copper solderability preservative with selectivity film forming, by the quality proportioning, its composition is: aryl phenyl imidazoles 1g/L, formic acid 10ml/L, acetate 100ml/L, thiocarbamide 1g/L, zinc acetate 2g/L, monoethanolamine 1ml/L, citric acid 5g/L.
A kind of organic copper solderability preservative with selectivity film forming that said ratio obtains is 42 ° of C in operating temperature, and pH value is under 4.0 the situation, last film time 90S, and thickness is 0.15um, and it is even that outward appearance presents film, and golden face does not have variable color.
Embodiment 2
A kind of organic copper solderability preservative with selectivity film forming, by the quality proportioning, its composition is: aryl phenyl imidazoles 4g/L, formic acid 20ml/L, acetate 200ml/L, thiocarbamide 2g/L, zinc acetate 4g/L, monoethanolamine 3ml/L, citric acid 12g/L.
A kind of organic copper solderability preservative with selectivity film forming that said ratio obtains is 42 ° of C in operating temperature, and pH value is under 4.0 the situation, last film time 90S, and thickness is 0.2um, and it is even that outward appearance presents film, and golden face does not have variable color.
Embodiment 3
A kind of organic copper solderability preservative with selectivity film forming, by the quality proportioning, its composition is: aryl phenyl imidazoles 8g/L, formic acid 100ml/L, acetate 500ml/L, thiocarbamide 4g/L, zinc acetate 6g/L, monoethanolamine 6ml/L, citric acid 18g/L.
A kind of organic copper solderability preservative with selectivity film forming that said ratio obtains is 42 ° of C in operating temperature, and pH value is under 4.0 the situation, last film time 90S, and thickness is 0.25um, and it is even that outward appearance presents film, and golden face does not have variable color.
According to above-mentioned a kind of organic copper solderability preservative with selectivity film forming, its feature is that also each constituent mass proportioning is:
Formic acid 25-40ML/L acetate 180-300ML/L aryl phenyl imidazoles 1-6g/L
Thiocarbamide 1-6g/L zinc acetate 2-6g/L monoethanolamine 1-6ml/L
Citric acid 5-18g/L.
Embodiment 4
A kind of organic copper solderability preservative with selectivity film forming, by the quality proportioning, its composition is: alkylbenzene imidazoles 1g/L, formic acid 12ml/L, acetate 110ml/L, thiocarbamide 1.5g/L, zinc acetate 2.2g/L, monoethanolamine 1.8ml/L, citric acid 6.3g/L.
A kind of organic copper solderability preservative with selectivity film forming that said ratio obtains is 42 ° of C in operating temperature, and pH value is under 4.0 the situation, last film time 90S, and thickness is 0.22um, and it is even that outward appearance presents film, and golden face does not have variable color.
Embodiment 5
A kind of organic copper solderability preservative with selectivity film forming, by the quality proportioning, its composition is: alkylbenzene imidazoles 2g/L, formic acid 13.5ml/L, acetate 118ml/L, thiocarbamide 2.3g/L, zinc acetate 2.6g/L, monoethanolamine 2.0ml/L, citric acid 7.1g/L.
A kind of organic copper solderability preservative with selectivity film forming that said ratio obtains is 42 ° of C in operating temperature, and pH value is under 4.0 the situation, last film time 90S, and thickness is 0.17um, and it is even that outward appearance presents film, and golden face does not have variable color.
Embodiment 6
A kind of organic copper solderability preservative with selectivity film forming, by the quality proportioning, its composition is: alkylbenzene imidazoles 4g/L, formic acid 17.8ml/L, acetate 182ml/L, thiocarbamide 2.3g/L, zinc acetate 4.8g/L, monoethanolamine 3.8ml/L, citric acid 12.9g/L.
A kind of organic copper solderability preservative with selectivity film forming that said ratio obtains is 42 ° of C in operating temperature, and pH value is under 4.0 the situation, last film time 90S, and thickness is 0.24um, and it is even that outward appearance presents film, and golden face does not have variable color.
Embodiment 7
A kind of organic copper solderability preservative with selectivity film forming, by the quality proportioning, its composition is: alkyl imidazole 1g/L, formic acid 10.5ml/L, acetate 102ml/L, thiocarbamide 5.8g/L, zinc acetate 7.2g/L, monoethanolamine 8.3ml/L, citric acid 16.6g/L.
A kind of organic copper solderability preservative with selectivity film forming that said ratio obtains is 42 ° of C in operating temperature, and pH value is under 4.0 the situation, last film time 90S, and thickness is 0.19um, and it is even that outward appearance presents film, and golden face does not have variable color.
Embodiment 8
A kind of organic copper solderability preservative with selectivity film forming, by the quality proportioning, its composition is: alkyl imidazole 3g/L, formic acid 90ml/L, acetate 450ml/L, thiocarbamide 6g/L, zinc acetate 5.2g/L, monoethanolamine 10ml/L, citric acid 10.6g/L.
A kind of organic copper solderability preservative with selectivity film forming that said ratio obtains is 42 ° of C in operating temperature, and pH value is under 4.0 the situation, last film time 90S, and thickness is 0.18um, and it is even that outward appearance presents film, and golden face does not have variable color.
Embodiment 9
A kind of organic copper solderability preservative with selectivity film forming, by the quality proportioning, its composition is: alkyl imidazole 6g/L, formic acid 16ml/L, acetate 158ml/L, thiocarbamide 2.8g/L, zinc acetate 6.2g/L, monoethanolamine 9.5ml/L, citric acid 11.5g/L.
A kind of organic copper solderability preservative with selectivity film forming that said ratio obtains is 42 ° of C in operating temperature, and pH value is under 4.0 the situation, last film time 90S, and thickness is 0.23um, and it is even that outward appearance presents film, and golden face does not have variable color.
A kind of as above-mentioned a kind of using method with organic copper solderability preservative of selectivity film forming, it is characterized in that this method comprises the steps:
A, with the pcb board oil removing
1) material is prepared,
Preparing concentration is the sulfuric acid of 5ml/L, and concentration is that the APES of 0.1ml/L is stand-by, and environment temperature is controlled at 33～37 ℃,
2) 100L builds bath:
1. the pure water of 2/3 volume is put into groove,
2. add 500ml sulfuric acid while stirring, the 10ml APES,
3. add pure water and stir to 100L,
B, with the pcb board microetch
1) material is prepared
Preparing concentration is the sulfuric acid of 5ml/L, and concentration is that the hydrogen peroxide of 60ml/L is stand-by, and environment temperature is controlled at 28 ℃-32 ℃,
2) the immersion microetch time is controlled at 60-90S, or the spray-type microetch time be controlled at 30-60S,
C, pcb board is put into as claim 1-5 as described in arbitrary film forming in a kind of organic copper solderability preservative with selectivity film forming
1) thorough cleaning equipment,
2) stoste that adds 100% final volume in groove is opened cylinder,
3) detect pH value, pH value transferred to 3.9 ± 0.2 with ammoniacal liquor,
4) ON cycle pump is heated to 42 ℃ ± 1 ℃ with solution.
The time of described step a oil removing is controlled at 30-60S, and the time of step c film forming is controlled at 90-120S.
Between step b and step c, also comprise a water-washing step, adopt DI water during washing, and its pH value is controlled between the 3.9-4.1.
Behind step c, also comprise a water-washing step, adopt DI water during washing, and its pH value is controlled between the 3.9-4.1.
The film thickness of step c film forming is controlled between the 0.15-0.25um.
Put into film forming key in a kind of organic copper solderability preservative with selectivity film forming and be and control the thickness of oxygen-proof film well.Film is too thin, and heat-resistant impact ability is poor, and when crossing Reflow Soldering, rete is anti-not toward high temperature (190-200 ℃), finally influences welding performance.Film is too thick, and on the electronic assemblies line, film can not well be dissolved by scaling powder, influences welding performance.
Though the present invention describes with reference to the above embodiments; but those of ordinary skill in the art can recognize very clearly that fully above embodiment is used to illustrate the present invention; wherein can make variations and modifications and not break away from the present invention in a broad sense; so be not as limitation of the invention; as long as in connotation scope of the present invention, all will fall within the protection domain that the present invention requires variation, the distortion of above-described embodiment.
Claims (10)
1. organic copper solderability preservative with selectivity film forming, it is characterized in that: it is the composition solution that is prepared into by formic acid, acetate, imidazoles organic matter, thiocarbamide, zinc acetate, monoethanolamine, citric acid, and wherein the quality proportioning of each component is:
Formic acid 10-100ML/L acetate 100-500ML/L imidazoles organic matter 1-8g/L
Thiocarbamide 1-6g/L zinc acetate 2-8g/L monoethanolamine 1-10ml/L
Citric acid 5-20g/L.
2. a kind of organic copper solderability preservative according to claim 1 with selectivity film forming, its feature also is: the imidazoles organic matter is preferably the aryl phenyl imidazoles, and the quality proportioning of its each component is:
Formic acid 10-100ML/L acetate 100-500ML/L aryl phenyl imidazoles 1-8g/L
Thiocarbamide 1-6g/L zinc acetate 2-8g/L monoethanolamine 1-10ml/L
Citric acid 5-20g/L.
3. a kind of organic copper solderability preservative according to claim 1 with selectivity film forming, its feature also is: the imidazoles organic matter is preferably the alkylbenzene imidazoles, and the quality proportioning of its each component is:
Formic acid 10-100ML/L acetate 100-500ML/L alkylbenzene imidazoles 1-4g/L
Thiocarbamide 1-6g/L zinc acetate 2-8g/L monoethanolamine 1-10ml/L
Citric acid 5-20g/L.
4. a kind of organic copper solderability preservative according to claim 1 with selectivity film forming, its feature also is: the imidazoles organic matter is preferably alkyl imidazole, and the quality proportioning of its each component is:
Formic acid 10-100ML/L acetate 100-500ML/L alkyl imidazole 1-6g/L
Thiocarbamide 1-6g/L zinc acetate 2-8g/L monoethanolamine 1-10ml/L
Citric acid 5-20g/L.
5. a kind of organic copper solderability preservative according to claim 2 with selectivity film forming, its feature is that also each constituent mass proportioning is:
Formic acid 25-40ML/L acetate 180-300ML/L aryl phenyl imidazoles 1-6g/L
Thiocarbamide 1-6g/L zinc acetate 2-6g/L monoethanolamine 1-6ml/L
Citric acid 5-18g/L.
6. one kind as a kind of using method with organic copper solderability preservative of selectivity film forming as described in arbitrary among the claim 1-5, it is characterized in that this method comprises the steps:
A, with the pcb board oil removing
1) material is prepared,
Preparing concentration is the sulfuric acid of 5ml/L, and concentration is that the APES of 0.1ml/L is stand-by, and environment temperature is controlled at 33～37 ℃,
2) 100L builds bath:
1. the pure water of 2/3 volume is put into groove,
2. add 500ml sulfuric acid while stirring, the 10ml APES,
3. add pure water and stir to 100L,
B, with the pcb board microetch
1) material is prepared
Preparing concentration is the sulfuric acid of 5ml/L, and concentration is that the hydrogen peroxide of 60ml/L is stand-by, and environment temperature is controlled at 28 ℃-32 ℃,
2) the immersion microetch time is controlled at 60-90S, or the spray-type microetch time be controlled at 30-60S,
C, pcb board is put into as claim 1-5 as described in arbitrary film forming in a kind of organic copper solderability preservative with selectivity film forming
1) thorough cleaning equipment,
2) stoste that adds 100% final volume in groove is opened cylinder,
3) detect pH value, pH value transferred to 3.9 ± 0.2 with ammoniacal liquor,
4) ON cycle pump is heated to 42 ℃ ± 1 ℃ with solution.
7. a kind of using method according to claim 6 with organic copper solderability preservative of selectivity film forming, it is characterized in that: the time of described step a oil removing is controlled at 30-60S, and the time of step c film forming is controlled at 90-120S.
8. a kind of using method with organic copper solderability preservative of selectivity film forming according to claim 6 is characterized in that: also comprise a water-washing step between step b and step c, adopt DI water during washing, and its pH value is controlled between the 3.9-4.1.
9. a kind of using method with organic copper solderability preservative of selectivity film forming according to claim 6 is characterized in that: also comprise a water-washing step behind step c, adopt DI water during washing, and its pH value is controlled between the 3.9-4.1.
10. the method that a kind of organic copper solderability preservative with selectivity film forming according to claim 6 uses, it is characterized in that: the film thickness of step c film forming is controlled between the 0.15-0.25um.
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| CN105081614A (en) * | 2015-09-07 | 2015-11-25 | 东莞市富默克化工有限公司 | OSP (organic solderability preservative) preimpregnation agent |
| CN105916312A (en) * | 2016-05-27 | 2016-08-31 | 建业科技电子（惠州）有限公司 | Blue glue production process for printed circuit boards |
| CN108012438A (en) * | 2017-11-24 | 2018-05-08 | 江门市奔力达电路有限公司 | A kind of pcb board ink cleaning |
| CN109735838A (en) * | 2019-03-14 | 2019-05-10 | 广东省石油与精细化工研究院 | A kind of copper face selectivity organic weldable protective agent |
| CN110881249A (en) * | 2019-10-21 | 2020-03-13 | 信丰福昌发电子有限公司 | FQC back-pass surface treatment method for double-sided circuit board |
| CN110896598A (en) * | 2019-10-10 | 2020-03-20 | 信丰福昌发电子有限公司 | Multilayer circuit board processing technology |
| CN110913599A (en) * | 2019-10-21 | 2020-03-24 | 信丰福昌发电子有限公司 | Processing technology of stepped circuit board with gold-surface copper-plating mixed surface technology |
| CN110933863A (en) * | 2019-10-10 | 2020-03-27 | 信丰福昌发电子有限公司 | Preparation method of organic solder mask on surface of HDI circuit board |
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