CN102766874A - Organic solderability preservative (OSP) protective agent for copper surfaces - Google Patents

Organic solderability preservative (OSP) protective agent for copper surfaces Download PDF

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CN102766874A
CN102766874A CN2012102960938A CN201210296093A CN102766874A CN 102766874 A CN102766874 A CN 102766874A CN 2012102960938 A CN2012102960938 A CN 2012102960938A CN 201210296093 A CN201210296093 A CN 201210296093A CN 102766874 A CN102766874 A CN 102766874A
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osp
acid
copper surface
surface protecting
protecting agent
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朱虹
张毅
邵磊
孙颖睿
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HEFEI AOFU SURFACE TREATMENT TECHNOLOGY Co Ltd
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HEFEI AOFU SURFACE TREATMENT TECHNOLOGY Co Ltd
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Abstract

The invention discloses an OSP protective agent for copper surfaces. The protective agent comprises long chain alkyl benzimidazole, aryl benzimidazole and water. The weight ratio of the long chain alkyl benzimidazole and the aryl benzimidazole is (1:2)-(2:1), and the total weight of the long chain alkyl benzimidazole and the aryl benzimidazole accounts for 0.01-10% of the total weight of the protective agent. According to the OSP, two benzimidazole derivatives are adopted to prepare an OSP aqueous solution for processing copper surfaces, high temperature resistance of produced copper surface OSP films can be remarkably improved, therefore the copper surfaces are effectively protected, and the solderability is improved.

Description

The OSP copper surface protecting agent
Technical field
The present invention relates to a kind of OSP copper surface protecting agent.
Background technology
Electroplate and electronics manufacturing at five metals, copper face often need carry out anti-oxidation processing to its surface as the base material and the line material of widespread use, to satisfy the requirement of later welded or processing.
In electronics manufacturing, in printed circuit board (PCB) components and parts when welding,, the thermotolerance that the protection metal is avoided oxidation and strengthened it is necessary.Usually, many circuit cards that contain copper are when electronic devices and components weld, because surface oxidation or stain, solder joint is unreliable, cause components and parts in the process of using, to burn easily.Generally speaking, PCB can adopt process of surface treatment that copper face is processed before welding, makes it possess oxidation-resistance and thermotolerance.The process of surface treatment of PCB has a lot, such as OSP, chemical nickel and gold, electronickelling gold, chemistry silver, chemical tin, hot air leveling etc.Wherein OSP technology receives much concern, and is used widely owing to low cost, simple operation and other advantages.OSP technology is to adopt the organism of benzoglyoxaline or phenylimidazole, is configured to the Organic Solderability copper surface protecting agent, makes copper surface and its reaction generate organic copper complex, be revealed as one deck homogeneous, as thin as a wafer, transparent organic coat film.This tunic can effectively protect copper face to receive the erosion of extraneous corrodibility or oxidizing atmosphere, reaches anti-oxidation effect.This manufacturing process is simple, with low cost, dependable performance, has been widely used in the surface treatment of copper face in five metals plating and the printed circuit board production.
No matter be printed circuit board or Communication Equipment element; Its OSP technology all is through the naked copper zone of element surface is immersed in a kind of aqueous solution; Form the organic protective film of the hydrophobic nature of a layer thickness 0.2-0.5 μ m on the copper surface through chemical reaction; This tunic can protect the copper surface to avoid oxidation, helps the weldering function, also can bear thermal shocking more than three times to various scolders are compatible.This process characteristic: 1) surface is evenly smooth, and thickness 0.2-0.5 μ m is suitable for the SMT dress and pastes thin wire, the manufacturing of the lead printed board of thin space; 2) aqueous solution operation, service temperature can not cause substrate warp below 80 ℃; 3) not crisp, the easy weldering of rete also can be born the thermal shocking more than three times with any scolder is compatible; 4) avoided the high temperature, noise and the fire alarm hidden danger that produce in the production process; 5) running cost is than the low 25-50% of hot blast levelling process; 6) preservation period can reach 1 year, and is easy to reprocess.
The core of OSP technical recipe is the aqueous solution that is disposed, and this solution can form the organic protective film of the hydrophobic nature of a layer thickness 0.2-0.5 μ m through chemical reaction on copper surface, plays anti-oxidation and the effect that helps weldering.OSP supplier adopts imidazole derivative to be dissolved in the acidic aqueous solution at present, makes it in certain temperature and pH value scope, act on copper face, generates the organic copper complex film, plays a protective role.This shows the quality of OSP film forming properties; The imidazoles kind of selecting for use with the OSP aqueous solution has much relations; The surface treatment worker of various countries has done number of research projects on the used imidazoles of OSP for a long time, develops different imidazole derivatives and is applied in the OSP treatment process.
The OSP prescription has all adopted the functional group with a kind of structure, 1,3 two pyrolle (being imidazoles) at present; The nfrastructure of this 5-member heterocyclic ring containing nitrogen Chang Zuowei OSP composition; Can further carry out multiviscosisty or replacement on this basis, generate multi-form verivate, become the primary structure of OSP prescription.As follows.
Change in Japanese four countries in the US5173130 patent of people's applications such as the Kinoshita of company, the nfrastructure of OSP prescription is following (1), and this is a kind of fused heterocycle structure, and R1 is the alkyl that contains 3 carbon atoms at least.On this basis, this structure further development for the form of (2), as the general formula of OSP formulation composition, R2 wherein, R3 and R4 are respectively alkyl, nitrogen-atoms and the Wasserstoffatomss of low-carbon (LC).(3) then be optimum two kinds of structures of OSP prescription that patent is recommended.
Figure 2012102960938100002DEST_PATH_IMAGE002
Figure 2012102960938100002DEST_PATH_IMAGE003
(1) (2) (3)
In the US5362334 patent of people such as the american wheat dolantin William of company application, the OSP formulation composition general formula that is proposed is as follows.
Figure 2012102960938100002DEST_PATH_IMAGE005
They point out in this general structure; R2; R3, R4 and R5 can be from Wasserstoffatomss, select in halogen atom, nitrogen-atoms and the low alkane chain; And select halogenated aromatic yl group in the locational R1 of benzoglyoxaline 2 functional group ordinary priority, for example halogenated phenyl, halogenated phenmethyl or halogenated ethylphenyl.And this structure has solved and has selected the high temperature resistance and the water-soluble incompatible problem that cause behind the long alkane chain on 2 positions of benzoglyoxaline.This OSP compound formula is generally with a kind of solution dissolving in organic acid, mineral acid or the organic acid metal complex compound.
In the US5376189 patent of people such as the Peter of Mai Demei company application in the same year, preferred following general structure is as optimum formula:
Figure 2012102960938100002DEST_PATH_IMAGE006
Wherein R1 replaces or unsubstituted long-chain or aromatic group, and R2 then selects in carboxylic acid group COOH and sulfonic group SO3H.This prescription adopts sodium hydroxide, Pottasium Hydroxide or carbonate to regulate between the pH value 7-11.High temperature weldability, stability of solution base solubility that copper face represents after this prescription is handled are all more outstanding, and are higher than the acid prescription of OSP in early stage.
The above patent of analysis-by-synthesis is found; Though the imidazole derivative structure that the various countries investigator adopts is different, in the OSP solution of configuration, all be to use a kind of imidazole derivative, the effect of copper face protection is not ideal enough; And along with the direction of global manufacturing to green production develops; Issuing of the Rohs of European Union instruction, pb-free solder technology replaces traditional leaded weldprocedure basically, and this moment, the temperature of copper face welding had very big raising.And adopt traditional OSP technology, though the organic complex film that forms can play anti-oxidation effect, under the welding temperature of pb-free solder, be easy to decomposition vapor away; Can not effectively protect copper face, thereby cause the copper face weldability to worsen, wettability is bad; Solder joint comes off, and components and parts lost efficacy.In this case, need to optimize OSP technology, adopt novel imidazolium compounds, to improve the resistance to elevated temperatures of OSP film.
Summary of the invention
The object of the present invention is to provide a kind of strong film forming high temperature resistant and anti-aging capability of copper face that has, more can adapt to the current OSP copper surface protecting agent that requires more harsh pb-free solder processing procedure to require to resistance to elevated temperatures.
OSP copper surface protecting agent of the present invention; It includes chain alkyl benzo imidazoles, aromatic base benzoglyoxaline and water; The weight ratio of said chain alkyl benzo imidazoles and aromatic base benzoglyoxaline is 1:2-2:1; The gross weight of said chain alkyl benzo imidazoles and aromatic base benzoglyoxaline accounts for the 0.01-10% of protective material gross weight, and the gross weight of preferred chain alkyl benzo imidazoles and aromatic base benzoglyoxaline accounts for the 0.1-5% of protective material gross weight.
Preferably; Said chain alkyl benzo imidazoles is the 2-alkyl benzimidazole of C5-C12; Comprise 2-hexyl benzoglyoxaline, 2-amyl group benzoglyoxaline etc.; Said aromatic base benzoglyoxaline comprises that the C1-C5 alkyl replaces or halogen replaces or nitro replaces or the 2-Phenylbenzimidazole of unsubstituted, comprises 2-chloro-phenyl-benzoglyoxaline, 2,4 dichloro benzene base benzoglyoxaline, 2-bromophenyl benzoglyoxaline, 2; 4-dibromo phenyl benzoglyoxaline, 2-ethylphenyl benzoglyoxaline, 2,4-3,5-dimethylphenyl benzoglyoxaline, 4-nitrophenyl benzoglyoxaline, 2-Phenylbenzimidazole etc.
Preferably; OSP copper surface protecting agent of the present invention also can comprise organic acid or the mineral acid that accounts for protective material gross weight 0.1-50%; Preferred organic acid or inorganic acid constitutes protective material gross weight 0.1-10%, said organic acid are at least a in the following component: the saturated or undersaturated aliphatics monocarboxylic acid of C1-C12; Saturated or the unsaturated aliphatic di-carboxylic acid of C2-C6; The aromatic carboxylic acid of C7-C8; The aromatic sulphonic acid of C6-C8; TNP;
Preferred organic acid is the saturated or undersaturated aliphatics monocarboxylic acid of C1-C12, most preferably
Organic acid is formic acid, acetate, propionic acid or lactic acid.
As preferably, OSP copper surface protecting agent of the present invention also can comprise the solubilizing agent that accounts for protective material gross weight 0.1-50%, and preferred solubilizing agent consumption accounts for protective material gross weight 0.1-10%.
Lower alcohol, acetone, the N of said solubilizing agent for dissolving each other with water, at least a in dinethylformamide, gylcol ether and the terepthaloyl moietie.
Preferred OSP copper surface protecting agent of the present invention also can comprise the membrane-forming agent that accounts for protective material gross weight 0.01-10%; Be preferably film and account for protective material gross weight 0.05-5%, said membrane-forming agent is at least a in cuprous chloride, cupric chloride, cuprous bromide, cupric bromide, cupric iodide, neutralized verdigris, cupric phosphate, copper sulfate, cupric nitrate and the verditer.
Also can comprise the buffer reagent that accounts for protective material gross weight 0.001-10% as preferred OSP copper surface protecting agent of the present invention; Preferred reducing accounts for protective material gross weight 0.05-5%, and said buffer reagent is the oxyhydroxide of ammonia, organic amine, alkali-metal oxyhydroxide or earth alkali metal.
Two kinds of imidazoles that the present invention adds are respectively chain alkyl benzo imidazoles and aromatic base benzoglyoxaline, and its general structure is distinguished as follows:
Figure DEST_PATH_IMAGE007
The imidazoles of these two kinds of general structures is dissolved in the aqueous solution of the about 2.0-5.0 of pH value with mineral acid and organic acid, aid in other pharmaceutical chemicalss as solubilizing agent, increase film, buffer reagent, composite together in final Organic Solderability copper surface protecting agent.After this copper surface protecting agent was handled, copper face can generate the protective membrane of the colourless even light of one deck, has splendid hydrophobicity, effectively prevents copper face oxidation corrosion.
The OSP aqueous solution with imidazolium compounds configuration of the present invention can be applicable to the copper metal, also can be used for copper alloy, the wire line of more representational processing sample such as printed circuit board, encapsulation IC support plate wire line, the heat conduction conducting surface of Communication Equipment.When handling such sample, processing mode comprises modes such as submergence, spray, and the treatment solution temperature is generally about 10-70 ℃, is preferably 20-50 ℃, copper face and about 1 second-10 minutes duration of contact of the OSP aqueous solution, is preferably 10 seconds-5 minutes.After the OSP aqueous solution was handled copper face, sample also must pass through washing, drying, gets into later welded technology subsequently.
After the present invention adopted the OSP aqueous solution of two kinds of benzimidizole derivatives configurations that copper face is handled, the resistance to elevated temperatures of the copper face OSP film of its generation can significantly improve.In the face of current pb-free solder technology, the copper face of handling with the present invention can still keep good weldability in the Reflow Soldering more than three times, and this performance is the single imidazole components of numerous employings, comprises that the OSP aqueous solution of benzoglyoxaline or phenylimidazole is not available.
Copper face after the present invention handles is through the high temperature reflux welder preface of five pb-free solder settings, and its temperature and time is as shown in the table.
Figure 2012102960938100002DEST_PATH_IMAGE008
After these five reflow operations, by the apparent light discolouration of copper face that the present invention handles, the No oxidation corrosion sign is again through pb-free solder wetting balance test, the equal Pass of weldability.And the copper face of the OSP solution-treated that is provided by supplier on the market is after three reflow operations; Apparent obvious variable color; The oxidation corrosion sign is serious, and pb-free solder wetting balance test all is difficult to complete Pass (sample segment fail through, weldability is bad).
Embodiment
Embodiment 1
Choose 2-amyl group benzoglyoxaline (meeting chain alkyl benzo imidazoles general formula) and 2 with the ratio of weight ratio 1:2; Two kinds of imidazoles of 4-dichlorophenyl benzoglyoxaline (meeting aromatic base benzoglyoxaline general formula); Auxiliary buffer reagent, solubilizing agent, increase film, the buffer reagent configuration OSP aqueous solution, shown in concrete consumption sees the following form.
Component Consumption Kind and effect
2-amyl group benzoglyoxaline 1g/L Film forming host
2,4 dichloro benzene base benzoglyoxaline 2g/L Film forming host
Formic acid 5g/L Solvent, the dissolving imidazoles
Acetate 3g/L Solvent, the dissolving imidazoles
EGME 10ml/L Solubilizing agent promotes the imidazoles dissolving
Cupric chloride 1.0g/l Film forming master's salt promotes film forming
Thanomin 5ml/L Buffer reagent is kept the pH value of solution value stabilization.
The OSP solution-treated copper face of the component configuration in more than showing, treating processes is according to oil removing → washing → little erosion → washing → OSP → washing → air-dry several steps that waits, and the OSP treatment temp is between 40 ℃, and the treatment time is 90 seconds.The organic membrane that the surperficial formation light of the back copper of finishing dealing with is smooth and hydrophobicity is preferable.
Behind dilute hydrochloric acid solution dissolving copper face OSP film, test lysate absorbing wavelength under the UV ultraviolet spectrophotometer, conversion obtains the OSP thickness between 0.2-0.4 μ m, meets OSP film required thickness.
OSP is handled the high temperature reflux welder preface that the back copper face carries out five pb-free solder settings, and its temperature and time is as shown in the table.
Figure DEST_PATH_IMAGE009
After five reflow operations, by the apparent light discolouration of copper face that the present invention handles, the No oxidation corrosion sign is again through pb-free solder wetting balance test, the equal Pass of weldability.
Embodiment 2
Choose 2-hexyl benzoglyoxaline and 2-chloro-phenyl-benzoglyoxaline two kinds of film forming imidazoles as OSP solution, weight ratio is set at 1:1, and each component concentration is as shown in the table.
Component Consumption Kind and effect
2-hexyl benzoglyoxaline 2g/L Film forming host
2-chloro-phenyl-benzoglyoxaline 2g/L Film forming host
Acetate 10g/L Solvent, the dissolving imidazoles
EGME 10ml/L Solubilizing agent promotes the imidazoles dissolving
Cupric bromide 1g/l Film forming master's salt promotes film forming
Ammoniacal liquor 10ml/L Buffer reagent is kept the pH value of solution value stabilization.
The OSP solution-treated copper face of the component configuration in more than showing, treating processes is according to oil removing → washing → little erosion → washing → OSP → washing → air-dry several steps that waits, and the OSP treatment temp is between 40 ℃, and the treatment time is 120 seconds.The organic membrane that the surperficial formation light of the back copper of finishing dealing with is smooth and hydrophobicity is preferable.Measuring its thickness with embodiment 1 same method is between the 0.3-0.5 μ m, meets OSP film required thickness.OSP handles the back sample again through five pb-free solder Reflow Soldering operations, and temperature and time is identical with embodiment 1.The copper face variable color is not obvious equally, the No oxidation corrosion sign, and through wetting balance test, weldability all satisfies the pb-free solder requirement.
Embodiment 3
Choose 2-amyl group benzoglyoxaline (meeting chain alkyl benzo imidazoles general formula) and 2 with the ratio of weight ratio 2:1; Two kinds of imidazoles of 4-dibromo phenyl benzoglyoxaline (meeting aromatic base benzoglyoxaline general formula); Auxiliary buffer reagent, solubilizing agent, increase film, the buffer reagent configuration OSP aqueous solution, shown in concrete consumption sees the following form.
Component Consumption Kind and effect
2-amyl group benzoglyoxaline 2g/L Film forming host
2,4-dibromo phenyl benzoglyoxaline 1g/L Film forming host
Lactic acid 1g/L Solvent, the dissolving imidazoles
Acetate 1g/L Solvent, the dissolving imidazoles
Ethanol 10ml/L Solubilizing agent promotes the imidazoles dissolving
Cuprous chloride 0.5g/l Film forming master's salt promotes film forming
Ammoniacal liquor 0.5ml/L Buffer reagent is kept the pH value of solution value stabilization.
The OSP solution-treated copper face of the component configuration in more than showing, treating processes is according to oil removing → washing → little erosion → washing → OSP → washing → air-dry several steps that waits, and the OSP treatment temp is between 40 ℃, and the treatment time is 90 seconds.The organic membrane that the surperficial formation light of the back copper of finishing dealing with is smooth and hydrophobicity is preferable.Measuring its thickness with embodiment 1 same method is between the 0.2-0.4 μ m, meets OSP film required thickness.OSP handles the back sample again through five pb-free solder Reflow Soldering operations, and temperature and time is identical with embodiment 1.The copper face variable color is not obvious equally, the No oxidation corrosion sign, and through wetting balance test, weldability all satisfies the pb-free solder requirement.
Embodiment 4
Choose 2-hexyl benzoglyoxaline and 2-nitrophenyl benzoglyoxaline two kinds of film forming imidazoles as OSP solution, weight ratio is set at 1:1, and each component concentration is as shown in the table.
Component Consumption Kind and effect
2-hexyl benzoglyoxaline 25g/L Film forming host
2-nitrophenyl benzoglyoxaline 25g/L Film forming host
TNP 50g/L Solvent, the dissolving imidazoles
Acetone 80ml/L Solubilizing agent promotes the imidazoles dissolving
Copper sulfate 1g/l Film forming master's salt promotes film forming
Sodium hydroxide 20ml/L Buffer reagent is kept the pH value of solution value stabilization.
The OSP solution-treated copper face of the component configuration in more than showing, treating processes is according to oil removing → washing → little erosion → washing → OSP → washing → air-dry several steps that waits, and the OSP treatment temp is between 40 ℃, and the treatment time is 120 seconds.The organic membrane that the surperficial formation light of the back copper of finishing dealing with is smooth and hydrophobicity is preferable.Measuring its thickness with embodiment 1 same method is between the 0.3-0.5 μ m, meets OSP film required thickness.OSP handles the back sample again through five pb-free solder Reflow Soldering operations, and temperature and time is identical with embodiment 1.The copper face variable color is not obvious equally, the No oxidation corrosion sign, and through wetting balance test, weldability all satisfies the pb-free solder requirement.
Embodiment 5
Choose 2-decyl benzoglyoxaline (meeting chain alkyl benzo imidazoles general formula) and two kinds of imidazoles of 2-aminomethyl phenyl benzoglyoxaline (meeting aromatic base benzoglyoxaline general formula) with the ratio of weight ratio 2:1; Auxiliary buffer reagent, solubilizing agent, increase film, the buffer reagent configuration OSP aqueous solution, shown in concrete consumption sees the following form.
Component Consumption Kind and effect
2-decyl benzoglyoxaline 2g/L Film forming host
2-aminomethyl phenyl benzoglyoxaline 1g/L Film forming host
Phenylsulfonic acid 1g/L Solvent, the dissolving imidazoles
Acetate 1g/L Solvent, the dissolving imidazoles
N, dinethylformamide 10ml/L Solubilizing agent promotes the imidazoles dissolving
Cuprous chloride 0.5g/l Film forming master's salt promotes film forming
Ammoniacal liquor 0.5ml/L Buffer reagent is kept the pH value of solution value stabilization.
The OSP solution-treated copper face of the component configuration in more than showing, treating processes is according to oil removing → washing → little erosion → washing → OSP → washing → air-dry several steps that waits, and the OSP treatment temp is between 40 ℃, and the treatment time is 90 seconds.The organic membrane that the surperficial formation light of the back copper of finishing dealing with is smooth and hydrophobicity is preferable.Measuring its thickness with embodiment 1 same method is between the 0.2-0.4 μ m, meets OSP film required thickness.OSP handles the back sample again through five pb-free solder Reflow Soldering operations, and temperature and time is identical with embodiment 1.The copper face variable color is not obvious equally, the No oxidation corrosion sign, and through wetting balance test, weldability all satisfies the pb-free solder requirement.
Comparative example 1
For the OSP solution film forming performance that is disposed with this patent compares, the elite film forming imidazoles of getting this a kind of imidazoles of 2,4 dichloro benzene base benzoglyoxaline as OSP solution, the OSP solution of configuration comparative example 1.Each component concentration is as shown in the table.
Component Consumption Kind and effect
2,4 dichloro benzene base benzoglyoxaline 3g/L Film forming host
Formic acid 5g/L Solvent, the dissolving imidazoles
Acetate 3g/L Solvent, the dissolving imidazoles
EGME 10ml/L Solubilizing agent promotes the imidazoles dissolving
Cupric chloride 1.0g/l Film forming master's salt promotes film forming
Thanomin 5ml/L Buffer reagent is kept the pH value of solution value stabilization.
Visible by last table, each component concentration is except that the film forming imidazoles in the OSP solution of comparative example 1 configuration, and other is all identical with embodiment 1.Adopt this OSP solution-treated copper face, treating processes accordings to oil removing → washing → little erosion → washing → OSP → washing → air-dry several steps that waits equally, and the OSP treatment temp is between 40 ℃, and the treatment time is 90 seconds.The copper surface also forms the organic membrane that light is smooth and hydrophobicity is preferable after finishing dealing with.Color and glossiness and embodiment 1 do not have significant difference.
Measuring its thickness with embodiment 1 same method is between the 0.2-0.5 μ m, meets OSP film required thickness.Subsequently again will be through the sample after the OSP of comparative example 1 solution-treated through five pb-free solder Reflow Soldering operations, temperature and time is identical with embodiment 1.This moment, the copper face variable color was obvious, and apparent turning white, and the oxidation corrosion sign is serious, and through wetting balance test, weldability all can not be passed through the pb-free solder requirement.
Comparative example 2
For the OSP solution film forming performance that is disposed with this patent compares, the elite film forming imidazoles of getting this a kind of imidazoles of 2-hexyl benzoglyoxaline as OSP solution, the OSP solution of configuration comparative example 2.Each component concentration is as shown in the table.
Component Consumption Kind and effect
2-hexyl benzoglyoxaline 2g/L Film forming host
Acetate 10g/L Solvent, the dissolving imidazoles
EGME 10ml/L Solubilizing agent promotes the imidazoles dissolving
Cupric bromide 1g/l Film forming master's salt promotes film forming
Ammoniacal liquor 10ml/L Buffer reagent is kept the pH value of solution value stabilization.
Visible by last table, each component concentration is except that the film forming imidazoles in the OSP solution of comparative example 2 configurations, and other is all identical with embodiment 2.Adopt this OSP solution-treated copper face, treating processes accordings to oil removing → washing → little erosion → washing → OSP → washing → air-dry several steps that waits equally, and the OSP treatment temp is between 40 ℃, and the treatment time is 120 seconds.The copper surface also forms the organic membrane that light is smooth and hydrophobicity is preferable after finishing dealing with.Color and glossiness and embodiment 2 do not have significant difference.
Measuring its thickness with embodiment 1 same method is between the 0.2-0.5 μ m, meets OSP film required thickness.Subsequently again will be through the sample after the OSP of comparative example 2 solution-treated through five pb-free solder Reflow Soldering operations, temperature and time is identical with embodiment 1.This moment, the copper face variable color was obvious, and apparent turning white, and the oxidation corrosion sign is serious, and through wetting balance test, weldability all can not be passed through the pb-free solder requirement.
Comprehensive embodiment 1,2 and comparative example 1,2 can be known; When adopting two kinds of benzoglyoxalines; Join in the OSP solution with a certain proportion of mode; Can effectively improve OSP solution in the film forming high temperature resistant and anti-aging capability of copper face, more can adapt to the current pb-free solder processing procedure requirement more harsh the resistance to elevated temperatures requirement.
The invention discloses a kind of OSP copper surface protecting agent; It comprises chain alkyl benzo imidazoles, aromatic base benzoglyoxaline and water; The weight ratio of said chain alkyl benzo imidazoles and aromatic base benzoglyoxaline is 1:2-2:1, and the gross weight of said chain alkyl benzo imidazoles and aromatic base benzoglyoxaline accounts for the 0.01-10% of protective material gross weight.The present invention adopts two kinds of benzimidizole derivatives to make the OSP aqueous solution, and after using it copper face being handled, the resistance to elevated temperatures of the copper face OSP film of its generation can significantly improve, thereby has effectively protected copper face, has improved its weldability.

Claims (9)

1. OSP copper surface protecting agent; It includes chain alkyl benzo imidazoles, aromatic base benzoglyoxaline and water; The weight ratio of said chain alkyl benzo imidazoles and aromatic base benzoglyoxaline is 1:2-2:1, and the gross weight of said chain alkyl benzo imidazoles and aromatic base benzoglyoxaline accounts for the 0.01-10% of protective material gross weight.
2. OSP copper surface protecting agent as claimed in claim 1; It is characterized in that: said chain alkyl benzo imidazoles is the 2-alkyl benzimidazole of C5-C12, and said aromatic base benzoglyoxaline comprises that the C1-C5 alkyl replaces or halogen replaces or nitro replaces or the 2-Phenylbenzimidazole of unsubstituted.
3. OSP copper surface protecting agent as claimed in claim 1; It is characterized in that: also comprise the organic acid or the mineral acid that account for protective material gross weight 0.1-50%, said organic acid is at least a in the following component: the saturated or undersaturated aliphatics monocarboxylic acid of C1-C12; Saturated or the unsaturated aliphatic di-carboxylic acid of C2-C6; The aromatic carboxylic acid of C7-C8; The aromatic sulphonic acid of C6-C8; TNP.
4. OSP copper surface protecting agent as claimed in claim 3 is characterized in that: said organic acid is the saturated or undersaturated aliphatics monocarboxylic acid of C1-C12.
5. OSP copper surface protecting agent as claimed in claim 4 is characterized in that: said organic acid is formic acid, acetate, propionic acid or lactic acid.
6. OSP copper surface protecting agent as claimed in claim 3 is characterized in that: also comprise the solubilizing agent that accounts for protective material gross weight 0.1-50%.
7. OSP copper surface protecting agent as claimed in claim 6 is characterized in that: lower alcohol, acetone, the N of said solubilizing agent for dissolving each other with water, at least a in dinethylformamide, gylcol ether and the terepthaloyl moietie.
8. OSP copper surface protecting agent as claimed in claim 6; It is characterized in that: also comprise the membrane-forming agent that accounts for protective material gross weight 0.01-10%, said membrane-forming agent is at least a in cuprous chloride, cupric chloride, cuprous bromide, cupric bromide, cupric iodide, neutralized verdigris, cupric phosphate, copper sulfate, cupric nitrate and the verditer.
9. OSP copper surface protecting agent as claimed in claim 8 is characterized in that: also comprise the buffer reagent that accounts for protective material gross weight 0.001-10%, said buffer reagent is the oxyhydroxide of ammonia, organic amine, alkali-metal oxyhydroxide or earth alkali metal.
CN2012102960938A 2012-08-20 2012-08-20 Organic solderability preservative (OSP) protective agent for copper surfaces Pending CN102766874A (en)

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Cited By (9)

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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
CN105772989A (en) * 2016-04-04 2016-07-20 广东工业大学 Copper surface organic solder preservative and application thereof
CN106903455A (en) * 2016-12-26 2017-06-30 长沙理工大学 A kind of high temperature resistant organic solderability preservative and apply usage
CN108281359A (en) * 2018-01-11 2018-07-13 广东禾木科技有限公司 A kind of organic anti-oxidation method of bonding wire
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
CN111266568A (en) * 2020-02-18 2020-06-12 深圳第三代半导体研究院 Imidazole group modified micro-nano granular paste and preparation method thereof
CN111269555A (en) * 2020-03-31 2020-06-12 浙江益弹新材料科技有限公司 Thermoplastic polyurethane elastomer composition and preparation method thereof
CN111527593A (en) * 2017-12-25 2020-08-11 住友电木株式会社 Method for manufacturing electronic device
CN111673078A (en) * 2020-05-14 2020-09-18 深圳第三代半导体研究院 Anti-oxidation treatment method for micro-nano copper material

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CN101560656A (en) * 2009-04-14 2009-10-21 东莞市中实焊锡有限公司 Lead-free printed circuit board copper surface protecting agent and preparation method thereof

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CN101228000A (en) * 2005-05-24 2008-07-23 四国化成工业株式会社 Water-soluble preflux and use thereof
CN101560656A (en) * 2009-04-14 2009-10-21 东莞市中实焊锡有限公司 Lead-free printed circuit board copper surface protecting agent and preparation method thereof

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN105772989A (en) * 2016-04-04 2016-07-20 广东工业大学 Copper surface organic solder preservative and application thereof
CN105772989B (en) * 2016-04-04 2018-02-23 广东工业大学 A kind of copper face organic solderability preservative and its application
CN106903455A (en) * 2016-12-26 2017-06-30 长沙理工大学 A kind of high temperature resistant organic solderability preservative and apply usage
CN111527593A (en) * 2017-12-25 2020-08-11 住友电木株式会社 Method for manufacturing electronic device
CN111527593B (en) * 2017-12-25 2021-05-04 住友电木株式会社 Method for manufacturing electronic device
CN108281359A (en) * 2018-01-11 2018-07-13 广东禾木科技有限公司 A kind of organic anti-oxidation method of bonding wire
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
CN111266568A (en) * 2020-02-18 2020-06-12 深圳第三代半导体研究院 Imidazole group modified micro-nano granular paste and preparation method thereof
CN111269555A (en) * 2020-03-31 2020-06-12 浙江益弹新材料科技有限公司 Thermoplastic polyurethane elastomer composition and preparation method thereof
CN111673078A (en) * 2020-05-14 2020-09-18 深圳第三代半导体研究院 Anti-oxidation treatment method for micro-nano copper material

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Application publication date: 20121107