CN104195604A - Iridium plating solution for inhibiting crack generation and plating method thereof, and coated substance - Google Patents
Iridium plating solution for inhibiting crack generation and plating method thereof, and coated substance Download PDFInfo
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- CN104195604A CN104195604A CN201410474992.1A CN201410474992A CN104195604A CN 104195604 A CN104195604 A CN 104195604A CN 201410474992 A CN201410474992 A CN 201410474992A CN 104195604 A CN104195604 A CN 104195604A
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Abstract
The invention relates to an iridium plating solution for inhibiting the crack generation and a plating method thereof, and a coated substance. The iridium plating solution comprises iridium (III) complex salt taking halogen as an anion composition, soluble alkali metal salt or soluble alkaline earth metal salt, a compound selected from more than one of saturated monocarboxylic acid, saturated monocarboxylic acid salt, unsaturated dicarboxylic acid, unsaturated dicarboxylic acid salt, saturated hydroxy carboxylic acid, saturated hydroxy carboxylic acid salt, amide and urea and a pH regulating agent. According to the invention, the good effect of inhibiting the coating crack generation can be obtained only in need ofthe lower soluble alkali metal salt or the lower soluble alkaline earth metal salt, so that the production cost is obviously reduced; moreover, the pollution caused by the soluble alkali metal salt or the soluble alkaline earth metal salt to the environment is obviously lower than that caused by Fe, Co, Ni, Cu and the like; the same effect as that of the prior art can be obtained only in need of soluble alkali metal salt or soluble alkaline earth metal salt with the amount 1/100-1/10 of that in the prior art.
Description
Technical field
The present invention relates to electroplating technology field, relate in particular to a kind of iridium electroplate liquid and electro-plating method and plated film thing that crack produces that suppress.
Background technology
Iridium is to have high rigidity, for the acid of high density and chloroazotic acid or halogen, also demonstrates the metal of good erosion resistance simultaneously.And its range of application not only comprises ornament, also comprise solidifying agent or the catalyzer of specific metal, and at the industrial material that is widely used as anticorrosive and contact etc.
Iridium electroplate liquid during as this iridium of use, known have a following iridium electroplate liquid: in the iridium that is halogen to anionic component (III) complex salt, add be selected from saturated mono carboxylic acid, saturated mono carboxylate salt, saturated dicarboxylic acid, saturated dicarboxylic acid salt, saturated hydroxy carboxylic acid, saturated hydroxy carboxylate salt, acid amides, urea more than one compound and stir, the material of gained is used as iridic compound.This iridium electroplate liquid is difficult for decomposing, having the practicality iridium electroplate liquid of high current efficiency and high electroplating velocity effectively as stablizing.
But such iridium electroplate liquid also has the problem of electroplating as follows proterties about it.For example, be used in as in the situation for the electronic devices and components that are electrically connected to such as pin, can produce that iridium electroplates that crack appears in tunicle and the phenomenon that cannot fully meet electrical characteristic.For this as electronic devices and components such as pins, conventionally adopt and on the rhodium of substrate, carry out the method that iridium is electroplated coating, but along with as surging in the price of the rare metals such as rhodium, study the rhodium that reduces substrate and the counte-rplan of carrying out electroplating processes with thicker iridium plating tunicle.Form so thicker iridium and electroplate in the situation of tunicle, the crack of iridium electroplate liquid in the past generates and becomes remarkable especially, and generation cannot meet the situation of electrical characteristic.
CN 102400190 A disclose a kind of iridium electroplate liquid and electro-plating method thereof, described iridium electroplate liquid, be use in iridium (III) complex salt from halogen to anionic component that be, add be selected from saturated mono carboxylic acid, saturated mono carboxylate salt, saturated dicarboxylic acid, saturated dicarboxylic acid salt, saturated hydroxy carboxylic acid, saturated hydroxy carboxylate salt, acid amides, urea more than one compound and stir the iridium electroplate liquid of the iridic compound obtaining, more than comprising at least one in Fe, Co, Ni, Cu.Although this iridium electroplate liquid can solve the problem that crack produces, the large usage quantity of Fe, Co, Ni, Cu etc., not only brings the problem that cost is high, and can weighting ring environment pollution.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of iridium electroplate liquid and electro-plating method and plated film thing that crack produces that suppress.Described iridium electroplate liquid not only can effectively suppress plated film crack and produce, and the consumption of metal-salt is low, and then reduces costs and alleviate environmental pollution.
For realizing object of the present invention, by the following technical solutions:
In first aspect, the invention provides a kind of iridium electroplate liquid that crack produces that suppresses, it is characterized in that, described iridium electroplate liquid comprises:
Anionic component is iridium (III) complex salt of halogen;
Soluble alkali metal salts or soluble alkaline earth salt;
Be selected from more than one the compound in saturated mono carboxylic acid, saturated mono carboxylate salt, saturated dicarboxylic acid, saturated dicarboxylic acid salt, saturated hydroxy carboxylic acid, saturated hydroxy carboxylate salt, acid amides and urea; With
PH adjusting agent.
As the preferred technical solution of the present invention, the content of described soluble alkali metal salts or soluble alkaline earth salt is 0.1mg/L～1mg/L.
As the preferred technical solution of the present invention, described soluble alkali metal salts is selected from soluble potassium salt, sodium salt or lithium salts; Described soluble alkaline earth salt is selected from solubility magnesium salts, calcium salt or barium salt.
As the preferred technical solution of the present invention, the iridium that described anionic component is halogen (III) complex salt is selected from chlordene iridium (III) hydrochlorate, hexabromo iridium (III) hydrochlorate or hexafluoro iridium (III) hydrochlorate.
As the preferred technical solution of the present invention, the concentration of the iridium that described anionic component is halogen (III) complex salt comprises 1～200g/L iridium with metal iridium densitometer, preferably with metal iridium densitometer, comprises 10～20g/L iridium.
As the preferred technical solution of the present invention, described more than one the concentration of compound being selected from saturated mono carboxylic acid, saturated mono carboxylate salt, saturated dicarboxylic acid, saturated dicarboxylic acid salt, saturated hydroxy carboxylic acid, saturated hydroxy carboxylate salt, acid amides and urea is 0.001～1.0mol/L, is preferably 0.01～0.2mol/L.
As the preferred technical solution of the present invention, described pH adjusting agent is selected from boric acid or thionamic acid.
In second aspect, the invention provides a kind of iridium electro-plating method, the iridium electroplate liquid that described method is used the inhibition crack described in first aspect to produce, in pH1～8,50～98 ℃ of temperature, current density 0.01～3.0A/dm
2condition electroplate.
As the preferred technical solution of the present invention, in pH4～6,80～90 ℃ of temperature, current density 0.1～0.8A/dm
2condition electroplate.
In the third aspect, the invention provides a kind of plated film thing, described plated film thing obtains by the iridium electro-plating method described in second aspect.
Beneficial effect of the present invention is: the present invention only needs lower soluble alkali metal salts or soluble alkaline earth salt can obtain the effect that good inhibition plated film crack produces, significantly reduce production costs, and the pollution of soluble alkali metal salts of the present invention or soluble alkaline earth salt pair environment is starkly lower than Fe, Co, Ni, Cu etc.The present invention only needs in prior art 1/100 to 1/10 soluble alkali metal salts or soluble alkaline earth salt can obtain the effect that prior art is identical.
Embodiment
Iridium electroplate liquid of the present invention comprises: the iridium that anionic component is halogen (III) complex salt; Soluble alkali metal salts or soluble alkaline earth salt; Be selected from more than one the compound in saturated mono carboxylic acid, saturated mono carboxylate salt, saturated dicarboxylic acid, saturated dicarboxylic acid salt, saturated hydroxy carboxylic acid, saturated hydroxy carboxylate salt, acid amides and urea; And pH adjusting agent.By make in soluble alkali metal salts or soluble alkaline earth salt at least any one is present in electroplate liquid, the generation that iridium is electroplated the crack in tunicle is effectively suppressed.
Iridium electroplate liquid of the present invention is better that the content of soluble alkali metal salts or soluble alkaline earth salt is 0.1mg/L～1mg/L.If lower than 0.1mg/L, easily produce crack; If higher than 1mg/L, crystalline growth becomes unstable.Described soluble alkali metal salts is selected from soluble potassium salt, sodium salt or lithium salts; Described soluble alkaline earth salt is selected from solubility magnesium salts, calcium salt or barium salt.
Iridium electroplate liquid of the present invention is better to comprise 1～200g/L iridium with metal iridium densitometer, is more preferably 10～20g/L.If iridium concentration is lower than 1g/L, the upper limit of current density diminishes, and is difficult to for actual; If higher than 200g/L, saturated and iridium cannot dissolve, and cost raises, and practicality is not good.As iridium (III) complex salt, can adopt chlordene iridium (III) hydrochlorate, hexabromo iridium (III) hydrochlorate, hexafluoro iridium (III) hydrochlorate, be better the sour sodium of hexabromo iridium (III), the sour sodium of chlordene iridium (III) etc.In addition, more than one the addition of compound that is selected from saturated mono carboxylic acid, saturated mono carboxylate salt, saturated dicarboxylic acid, saturated dicarboxylic acid salt, saturated hydroxy carboxylic acid, saturated hydroxy carboxylate salt, acid amides, urea is better 0.001～1.0mol/L, is more preferably 0.01～0.2mol/L.In addition, as this compound, can adopt such as acetic acid, propanedioic acid disodium, oxalic acid etc., be better propanedioic acid disodium.In addition, the reason that its addition is made as to 0.001～1.0mol/L is: if lower than 0.001mol/L, can manifest the effect that interpolation produces hardly; If higher than 1.0mol/L, can hinder and separate out.
Iridium electroplate liquid of the present invention can comprise the buffer reagent of adjusting for pH, such as boric acid, thionamic acid etc. as required.
In iridium electro-plating method of the present invention, condition is made as to pH1～8,50～98 ℃ of temperature, current density 0.01～3.0A/dm
2, be better with pH4～6,80～90 ℃ of temperature, current density 0.1～0.8A/dm
2operational condition use.The reason that is made as pH1～8 is: if pH lower than 1, the upper limit of current density diminishes, practicality is not good; If pH, higher than 8, generates oxyhydroxide, produce precipitation.In addition, if temperature lower than 50 ℃, is extremely difficult for separating out; If temperature is higher than 98 ℃, evaporation of water is violent, and practicality is not good.In addition, current density is lower than 0.01A/dm
2time, speed of separating out is extremely slow; Current density is higher than 3.0A/dm
2time, produce hydrogen and do not separate out precipitate.
If employing the present invention, the iridium that the generation that can form crack obtains significantly suppressing is electroplated tunicle.
Below in conjunction with embodiment, embodiment of the present invention are described in detail.It will be understood to those of skill in the art that following examples are only the preferred embodiments of the present invention, so that understand better the present invention, thereby should not be considered as limiting scope of the present invention.
Embodiment 1:
In this embodiment 1, to add the situation of K in iridium electroplate liquid, describe.The electroplate liquid of this embodiment 1 is composed as follows:
In embodiment 1, as iridic compound, adopt the compound obtaining as follows: in the sour sodium of above-mentioned hexabromo iridium (III), add the propanedioic acid disodium as " dicarboxylate ", when being kept at 85 ℃ with heating bath, with magnetic stirrer, stirring 1 hour and obtain.In this iridium electroplate liquid, add Repone K, make the K that comprises 0.01g/L in electroplate liquid.
Then, the brass test film of 2cm * 2cm is carried out to golden strike plating processing, after the gold-plated processing of thick 1.0 μ m, the iridium that forms thick 3.0 μ m is electroplated tunicle.Electroplating processes condition is made as pH3.5～4.0,80～85 ℃ of temperature of electroplating solution, current density 0.5A/dm
2.
Iridium for institute's coating is electroplated tunicle, uses metalloscope (400 times) to observe coating proterties.In addition, in order to compare, by not adding the iridium electroplate liquid of any blank in soluble alkali metal salts or soluble alkaline earth salt, make the test film that is formed with iridium plating tunicle.The plating condition of this blank is identical when comprising K.Confirmation produces a large amount of cracks by not containing the test film of the iridium electroplate liquid coating of K on surface.On the other hand, in the situation of the iridium electroplate liquid that comprises K, almost do not confirm crack.
In addition, make the content of K become 0.05mg/L, 0.1mg/L, 0.5mg/L, 5mg/L, 10mg/L, confirmed the generation state in its crack, result confirms the generation in crack when 0.05mg/L, the generation to crack unconfirmed when 0.1mg/L is above.
Embodiment 2:
In this embodiment 2, to add the situation of Li in iridium electroplate liquid, describe.The electroplate liquid of this embodiment 2 is composed as follows:
In embodiment 2, as iridic compound, adopt the compound obtaining as follows: in the sour sodium of above-mentioned hexabromo iridium (III), add the disodium citrate as " hydroxycarboxylate ", when being kept at 85 ℃ with heating bath, with magnetic stirrer, stirring 1 hour and obtain.In this iridium electroplate liquid, add lithium chloride, make the Li that comprises 0.5mg/L in electroplate liquid.
Then, the brass test film of 2cm * 2cm is carried out to golden strike plating processing, after the gold-plated processing of thick 1.0 μ m, the iridium that forms thick 3.0 μ m is electroplated tunicle.Electroplating processes condition is made as pH3.5～4.0,80～85 ℃ of temperature of electroplating solution, current density 0.5A/dm
2.
Iridium for institute's coating is electroplated tunicle, uses metalloscope (400 times) to observe coating proterties.In the situation of the iridium electroplate liquid that comprises Li, almost do not confirm crack.
In addition, make the content of Li become 0.05mg/L, 0.1mg/L, 0.5mg/L, 5mg/L, 10mg/L, confirmed the generation state in its crack, result confirms the generation in crack when 0.05mg/L, the generation to crack unconfirmed when 0.1mg/L is above.
Embodiment 3:
In this embodiment 3, to add the situation of Na in iridium electroplate liquid, describe.The electroplate liquid of this embodiment 3 is composed as follows:
In embodiment 3, as iridic compound, adopt the compound obtaining as follows: in the sour sodium of above-mentioned hexabromo iridium (III), add the oxalic acid as " dicarboxylic acid ", when being kept at 85 ℃ with heating bath, with magnetic stirrer, stirring 1 hour and obtain.In this iridium electroplate liquid, add sodium-chlor, make the Na that comprises 0.5mg/L in electroplate liquid.
Then, the brass test film of 2cm * 2cm is carried out to golden strike plating processing, after the gold-plated processing of thick 1.0 μ m, the iridium that forms thick 3.0 μ m is electroplated tunicle.Electroplating processes condition is made as pH3.5～4.0,80～85 ℃ of temperature of electroplating solution, current density 0.5A/dm
2.
Iridium for institute's coating is electroplated tunicle, uses metalloscope (400 times) to observe coating proterties.In the situation of the iridium electroplate liquid that comprises Na, almost do not confirm crack.
In addition, make the content of Na become 0.05mg/L, 0.1mg/L, 0.5mg/L, 5mg/L, 10mg/L, confirmed the generation state in its crack, result confirms the generation in crack when 0.05mg/L, the generation to crack unconfirmed when 0.1mg/L is above.
In addition, the content of Na is made as to 20mg/L, uses metalloscope (400 times) to observe coating proterties.When the content of Na is made as 20mg/L, fails to obtain and separate out normally.
Embodiment 4:
In this embodiment 4, to add the situation of Mg in iridium electroplate liquid, describe.The electroplate liquid of this embodiment 4 is composed as follows:
In embodiment 4, as iridic compound, adopt the compound obtaining as follows: in the sour sodium of above-mentioned hexabromo iridium (III), add the acetic acid as " monocarboxylic acid ", when being kept at 85 ℃ with heating bath, with magnetic stirrer, stirring 1 hour and obtain.In this iridium electroplate liquid, add magnesium chloride, make the Mg that comprises 0.1mg/L in electroplate liquid.
Then, the brass test film of 2cm * 2cm is carried out to golden strike plating processing, after the gold-plated processing of thick 1.0 μ m, the iridium that forms thick 3.0 μ m is electroplated tunicle.Electroplating processes condition is made as pH3.5～4.0,80～85 ℃ of temperature of electroplating solution, current density 0.5A/dm
2.
Iridium for institute's coating is electroplated tunicle, uses metalloscope (400 times) to observe coating proterties.In the situation of the iridium electroplate liquid that comprises Mg, almost do not confirm crack.
In addition, make the content of Mg become 0.05mg/L, 0.1mg/L, 0.5mg/L, 5mg/L, 10mg/L, confirmed the generation state in its crack, result confirms the generation in crack when 0.05mg/L, the generation to crack unconfirmed when 0.1mg/L is above.
Embodiment 5:
In this embodiment 5, to add the situation of Ca in iridium electroplate liquid, describe.The electroplate liquid of this embodiment 5 is composed as follows:
In embodiment 5, as iridic compound, adopt the compound obtaining as follows: in the sour sodium of above-mentioned chlordene iridium (III), add the propanedioic acid disodium as dicarboxylate, when being kept at 85 ℃ with heating bath, with magnetic stirrer, stirring 1 hour and obtain.In this iridium electroplate liquid, add calcium chloride, make the Ca that comprises 5mg/L in electroplate liquid.
Then, the brass test film of 2cm * 2cm is carried out to golden strike plating processing, after the gold-plated processing of thick 1.0 μ m, the iridium that forms thick 3.0 μ m is electroplated tunicle.Electroplating processes condition is made as pH3.5～4.0,80～85 ℃ of temperature of electroplating solution, current density 0.2A/dm
2.
Iridium for institute's coating is electroplated tunicle, uses metalloscope (400 times) to observe coating proterties.In the situation of the iridium electroplate liquid that comprises Ca, almost do not confirm crack.
Embodiment 6:
In this embodiment 6, the situation of adding Ba and changing plating condition in iridium electroplate liquid is described.The electroplate liquid of this embodiment 6 is composed as follows:
In embodiment 6, as iridic compound, adopt the compound obtaining as follows: in the sour sodium of above-mentioned hexabromo iridium (III), add the oxalic acid as dicarboxylic acid, when being kept at 85 ℃ with heating bath, with magnetic stirrer, stirring 1 hour and obtain.In this iridium electroplate liquid, add bariumchloride, make the Ba that comprises 0.5mg/L in electroplate liquid.
Then, the brass test film of 2cm * 2cm is carried out to golden strike plating processing, after the gold-plated processing of thick 1.0 μ m, the iridium that forms thick 3.0 μ m is electroplated tunicle, measures precipitation efficiency.Electroplating processes condition is made as pH2.0～8.5,40～95 ℃ of temperature of electroplating solution, current density 0.01～2.0A/dm
2.
Mensuration is made as 85 ℃ of temperature of electroplating solution, current density 0.5A/dm
2and the precipitation efficiency while changing pH.
During pH0.5, precipitation efficiency is 0%, does not separate out.During pH3.0, precipitation efficiency is 85%, unconfirmed to crack.PH4.0～7.0 o'clock, precipitation efficiency is 95%～100%, unconfirmed to crack.In addition, during pH8.5, produce the precipitation of oxyhydroxide.
Then, measure and be made as current density 0.5A/dm
2, pH3.5 the precipitation efficiency while change bathing temperature.
While bathing warm 40 ℃, precipitation efficiency is 0%, does not separate out.While bathing warm 50 ℃, precipitation efficiency is 35%, confirms crack.While bathing warm 60 ℃～70 ℃, precipitation efficiency is 40%～60%, unconfirmed to crack.While bathing warm 80 ℃～95 ℃, precipitation efficiency is 90%～100%, unconfirmed to crack.In addition, when bath temperature is risen to 99 ℃, water becomes acutely from the evaporation of plating bath, is difficult to carry out stable electroplating processes.
Then, measure the precipitation efficiency being made as when bathing 85 ℃ of temperature, pH3.5 and changing current density.Current density 0.01A/dm
2time, precipitation efficiency is 50%, unconfirmed to crack.Current density 0.02A/dm
2～1.0A/dm
2time, precipitation efficiency is 90～100%, unconfirmed to crack.Current density 1.5A/dm
2time, precipitation efficiency is 60%, unconfirmed to crack.Current density 3.0A/dm
2time, precipitation efficiency is 20%, confirms crack.In addition, current density is risen to 3.5A/dm
2time, produce hydrogen, do not obtain and separate out normally.
Applicant's statement, the present invention illustrates detailed features of the present invention and detailed method by above-described embodiment, but the present invention is not limited to above-mentioned detailed features and detailed method, do not mean that the present invention must rely on above-mentioned detailed features and detailed method could be implemented.Person of ordinary skill in the field should understand, any improvement in the present invention is selected the selection of the equivalence replacement of component and the interpolation of ancillary component, concrete mode etc., within all dropping on protection scope of the present invention and open scope to the present invention.
Claims (10)
1. suppress the iridium electroplate liquid that crack produces, it is characterized in that, described iridium electroplate liquid comprises:
Anionic component is iridium (III) complex salt of halogen;
Soluble alkali metal salts or soluble alkaline earth salt;
Be selected from more than one the compound in saturated mono carboxylic acid, saturated mono carboxylate salt, saturated dicarboxylic acid, saturated dicarboxylic acid salt, saturated hydroxy carboxylic acid, saturated hydroxy carboxylate salt, acid amides and urea; With
PH adjusting agent.
2. the iridium electroplate liquid that inhibition according to claim 1 crack produces, is characterized in that, the content of described soluble alkali metal salts or soluble alkaline earth salt is 0.1mg/L～1mg/L.
3. the iridium electroplate liquid that inhibition according to claim 1 and 2 crack produces, is characterized in that, described soluble alkali metal salts is selected from soluble potassium salt, sodium salt or lithium salts; Described soluble alkaline earth salt is selected from solubility magnesium salts, calcium salt or barium salt.
4. the iridium electroplate liquid producing according to the inhibition crack described in claim 1-3 any one, it is characterized in that, the iridium that described anionic component is halogen (III) complex salt is selected from chlordene iridium (III) hydrochlorate, hexabromo iridium (III) hydrochlorate or hexafluoro iridium (III) hydrochlorate.
5. the iridium electroplate liquid producing according to the inhibition crack described in claim 1-4 any one, it is characterized in that, described anionic component is that the concentration of iridium (III) complex salt of halogen comprises 1～200g/L iridium with metal iridium densitometer, preferably with metal iridium densitometer, comprises 10～20g/L iridium.
6. the iridium electroplate liquid producing according to the inhibition crack described in claim 1-5 any one, it is characterized in that, described more than one the concentration of compound being selected from saturated mono carboxylic acid, saturated mono carboxylate salt, saturated dicarboxylic acid, saturated dicarboxylic acid salt, saturated hydroxy carboxylic acid, saturated hydroxy carboxylate salt, acid amides and urea is 0.001～1.0mol/L, is preferably 0.01～0.2mol/L.
7. the iridium electroplate liquid producing according to the inhibition crack described in claim 1-6 any one, is characterized in that, described pH adjusting agent is selected from boric acid or thionamic acid.
8. an iridium electro-plating method, is characterized in that, the iridium electroplate liquid that described method right to use requires the inhibition crack described in 1-7 any one to produce, in pH1～8,50～98 ℃ of temperature, current density 0.01～3.0A/dm
2condition electroplate.
9. iridium electro-plating method according to claim 8, is characterized in that, in pH4～6,80～90 ℃ of temperature, current density 0.1～0.8A/dm
2condition electroplate.
10. a plated film thing, is characterized in that, described plated film thing obtains by the iridium electro-plating method described in claim 8 or 9.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109234757A (en) * | 2018-10-18 | 2019-01-18 | 任杰 | A kind of preparation method and application of uniform and stable ruthenium iridium bimetal-doped Ti electrode |
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