CN102400190A - Iridium plating solution and electroplate method thereof - Google Patents
Iridium plating solution and electroplate method thereof Download PDFInfo
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- CN102400190A CN102400190A CN2010102900158A CN201010290015A CN102400190A CN 102400190 A CN102400190 A CN 102400190A CN 2010102900158 A CN2010102900158 A CN 2010102900158A CN 201010290015 A CN201010290015 A CN 201010290015A CN 102400190 A CN102400190 A CN 102400190A
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- 229910052741 iridium Inorganic materials 0.000 title claims abstract description 89
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 238000000034 method Methods 0.000 title claims abstract description 17
- 238000007747 plating Methods 0.000 title abstract description 16
- 150000001875 compounds Chemical class 0.000 claims abstract description 21
- 229920006395 saturated elastomer Polymers 0.000 claims abstract description 12
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical class OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052742 iron Inorganic materials 0.000 claims abstract description 10
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 8
- MILUBEOXRNEUHS-UHFFFAOYSA-N iridium(3+) Chemical compound [Ir+3] MILUBEOXRNEUHS-UHFFFAOYSA-N 0.000 claims abstract description 7
- 150000003839 salts Chemical class 0.000 claims abstract description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 5
- 150000001408 amides Chemical class 0.000 claims abstract description 5
- 239000004202 carbamide Substances 0.000 claims abstract description 5
- 229910052736 halogen Inorganic materials 0.000 claims abstract description 5
- 150000002367 halogens Chemical class 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims abstract description 4
- 239000007788 liquid Substances 0.000 claims description 50
- 238000009713 electroplating Methods 0.000 claims description 22
- -1 carboxylate salt Chemical class 0.000 claims description 10
- 150000002763 monocarboxylic acids Chemical class 0.000 claims description 5
- 125000000129 anionic group Chemical group 0.000 claims description 3
- 150000001991 dicarboxylic acids Chemical class 0.000 claims 2
- 150000001990 dicarboxylic acid derivatives Chemical class 0.000 abstract description 7
- 229910052802 copper Inorganic materials 0.000 abstract description 2
- 150000001450 anions Chemical class 0.000 abstract 1
- 150000002504 iridium compounds Chemical class 0.000 abstract 1
- 150000002762 monocarboxylic acid derivatives Chemical class 0.000 abstract 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 16
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 15
- 239000011248 coating agent Substances 0.000 description 15
- 238000000576 coating method Methods 0.000 description 15
- 239000002184 metal Substances 0.000 description 15
- 229910052751 metal Inorganic materials 0.000 description 15
- 238000001556 precipitation Methods 0.000 description 15
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 14
- 229910052708 sodium Inorganic materials 0.000 description 14
- 239000011734 sodium Substances 0.000 description 14
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 13
- BKLCQTJLGBIHJV-UHFFFAOYSA-H Br[Ir](Br)(Br)(Br)(Br)Br Chemical compound Br[Ir](Br)(Br)(Br)(Br)Br BKLCQTJLGBIHJV-UHFFFAOYSA-H 0.000 description 11
- 239000010949 copper Substances 0.000 description 10
- 150000002503 iridium Chemical class 0.000 description 9
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 7
- 239000004327 boric acid Substances 0.000 description 7
- 229910001369 Brass Inorganic materials 0.000 description 6
- 238000003287 bathing Methods 0.000 description 6
- 239000010951 brass Substances 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- SXJCWCGNPYHALZ-UHFFFAOYSA-N propanedioic acid;sodium Chemical compound [Na].[Na].OC(=O)CC(O)=O SXJCWCGNPYHALZ-UHFFFAOYSA-N 0.000 description 6
- 235000006408 oxalic acid Nutrition 0.000 description 5
- 241000220317 Rosa Species 0.000 description 4
- XCJXQCUJXDUNDN-UHFFFAOYSA-N chlordene Chemical compound C12C=CCC2C2(Cl)C(Cl)=C(Cl)C1(Cl)C2(Cl)Cl XCJXQCUJXDUNDN-UHFFFAOYSA-N 0.000 description 4
- 229940116202 nickel sulfate hexahydrate Drugs 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 3
- 230000005764 inhibitory process Effects 0.000 description 3
- 229910052703 rhodium Inorganic materials 0.000 description 3
- 239000010948 rhodium Substances 0.000 description 3
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 3
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- JZCCFEFSEZPSOG-UHFFFAOYSA-L copper(II) sulfate pentahydrate Chemical compound O.O.O.O.O.[Cu+2].[O-]S([O-])(=O)=O JZCCFEFSEZPSOG-UHFFFAOYSA-L 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 235000019262 disodium citrate Nutrition 0.000 description 2
- 239000002526 disodium citrate Substances 0.000 description 2
- CEYULKASIQJZGP-UHFFFAOYSA-L disodium;2-(carboxymethyl)-2-hydroxybutanedioate Chemical compound [Na+].[Na+].[O-]C(=O)CC(O)(C(=O)O)CC([O-])=O CEYULKASIQJZGP-UHFFFAOYSA-L 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 150000004688 heptahydrates Chemical class 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- XNCMOUSLNOHBKY-UHFFFAOYSA-H iron(3+);trisulfate;heptahydrate Chemical compound O.O.O.O.O.O.O.[Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O XNCMOUSLNOHBKY-UHFFFAOYSA-H 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- NICDRCVJGXLKSF-UHFFFAOYSA-N nitric acid;trihydrochloride Chemical compound Cl.Cl.Cl.O[N+]([O-])=O NICDRCVJGXLKSF-UHFFFAOYSA-N 0.000 description 1
- 238000010979 pH adjustment Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
Images
Abstract
The invention discloses an iridium plating solution capable of forming an iridium electroplate film easily to intensively inhibit generation of cracks, and an electroplate method thereof. An iridium compound iridium plating solution employed by the invention is obtained by adding more than one compound selected from saturated monocarboxylic acid, saturated monocarboxylate, saturated dicarboxylic acid, saturated dicarboxylate, saturated hydroxy carboxylic acid, saturated hydroxy-carboxylate, amide and urea into an iridium (III) complex salt containing halogen as anions and stirring well. The iridium plating solution is characterized by comprising at least one selected from Fe, Co, Ni and Cu.
Description
Technical field
The present invention relates to iridium electroplate liquid and electro-plating method thereof.
Background technology
Iridium is to have high firmness, also demonstrates simultaneously the metal of good anti-corrosion for the acid of high density and chloroazotic acid or halogen.And its range of application not only comprises ornamental, also comprises the solidifying agent or the catalyzer of specific metal, and in industry, is widely used as the material of anticorrosive and contact etc.
Iridium electroplate liquid during as this iridium of use; Known following iridium electroplate liquid: to anionic component be add in iridium (III) complex salt of halogen 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 (with reference to patent documentation 1) as iridic compound.
This iridium electroplate liquid is by the practicality iridium electroplate liquid that is difficult for as stablizing effectively decomposing, having high current efficiency and high electroplating velocity.
Yet outstanding like this iridium electroplate liquid has also been pointed out the following problem about its plating proterties.For example, be used under the situation of the electronic devices and components that are used to be electrically connected like pin etc. (with reference to patent documentation 2), produce sometimes that iridium electroplates that the crack appears in tunicle and the phenomenon that can't fully satisfy electrical characteristic.For this like electronic devices and components such as pins; Usually be employed in the method for carrying out iridium plating lining on the rhodium of substrate; But, studying the rhodium that reduces substrate and electroplating the counte-rplan that tunicle carries out electroplating processes with thicker iridium along with surging like the price of rare metals such as rhodium.Form thicker iridium like this and electroplate under the situation of tunicle, the crack of iridium electroplate liquid in the past generates and becomes remarkable especially, and generation can't be satisfied the situation of electrical characteristic.
Patent documentation 1: japanese patent laid-open 6-316786 communique
Patent documentation 2: japanese patent laid-open 7-21867 communique
Summary of the invention
The present invention is the invention of accomplishing in aforesaid situation, and its purpose is to provide the iridium that can easily form the inhibition that fissured generation obtains doing one's utmost to electroplate the iridium electroplate liquid and the electro-plating method thereof of tunicle.
The present invention be to use to anionic component be add in iridium (III) complex salt of halogen 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 that gets; It is characterized in that, comprise more than at least a among Fe, Co, Ni, the Cu.Through any one metal at least among Fe, Co, Ni, the Cu is present in the electroplate liquid, the fissured generation that iridium is electroplated in the tunicle is effectively suppressed.
Iridium electroplate liquid of the present invention better is that at least a above content among Fe, Co, Ni, the Cu is 0.01g/L～10g/L.If be lower than 0.01g/L, then be easy to generate the crack; If be higher than 10g/L, then crystalline growth becomes unstable.
Any one metal among this Fe, Co, Ni, the Cu better is that the form with soluble metallic salt is contained in the electroplate liquid.
Iridium electroplate liquid of the present invention better is to comprise 1～200g/L iridium with metal iridium densitometer, is more preferably 10～20g/L.If iridium concentration is lower than 1g/L, then the upper limit of current density diminishes, and is difficult to supply actual use; If be higher than 200g/L, then saturated and iridium can't 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, better be 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 better is 0.001～1.0mol/L, is more preferably 0.01～0.2mol/L.In addition, as this compound, can adopt for example acetate, propanedioic acid disodium, oxalic acid etc., better be the propanedioic acid disodium.In addition, the reason that its addition is made as 0.001～1.0mol/L is: if be lower than 0.001mol/L, then can manifest the effect that interpolation produces hardly; If be higher than 1.0mol/L, then can hinder and separate out.
Iridium electroplate liquid of the present invention can comprise the buffer reagent that is used for the pH adjustment, for example boric acid, thionamic acid etc. as required.
In the iridium electro-plating method of the present invention, condition is made as pH1～8,50～98 ℃ of temperature, current density 0.01～3.0A/dm
2, better be 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 is lower than 1, then the upper limit of current density diminishes, and practicality is not good; If pH is higher than 8, then generate oxyhydroxide, produce deposition.In addition, if temperature is lower than 50 ℃, then extremely be difficult for separating out; If temperature is higher than 98 ℃, then evaporation of water is violent, and practicality is not good.In addition, current density is lower than 0.01A/dm
2The time, speed of separating out is extremely slow; Current density is higher than 3.0A/dm
2The time, produce hydrogen and do not separate out precipitate.
If employing the present invention, the iridium that then can form the inhibition that fissured generation obtains doing one's utmost is electroplated tunicle.
Description of drawings
Fig. 1 is that the coating surface of embodiment 1 is observed photo.
Fig. 2 is that the coating surface when not adding metal is observed photo.
Fig. 3 is that the coating surface of embodiment 2 is observed photo.
Fig. 4 is that the coating surface of the Co content 20.0g/L of embodiment 2 is observed photo.
Fig. 5 is that the coating surface of embodiment 3 is observed photo.
Fig. 6 is that the coating surface of the Ni content 15.0g/L of embodiment 3 is observed photo.
Fig. 7 is that the coating surface of embodiment 4 is observed photo.
Fig. 8 is that the coating surface of embodiment 5 is observed photo.
Embodiment
Below, with reference to embodiment embodiment of the present invention is elaborated.
Embodiment 1:
Among this embodiment 1, the situation of in the iridium electroplate liquid, adding Fe is described.The electroplate liquid of this embodiment 1 is formed as follows:
The sour sodium of hexabromo iridium (III)
15g/L (being scaled metal iridium)
Boric acid 40g/L
Propanedioic acid disodium 0.02mol/L
Ferric sulfate heptahydrate 0.01g/L (being scaled metallic iron)
Among the embodiment 1,, adopt the compound that obtains as follows: in the sour sodium of above-mentioned hexabromo iridium (III), add propanedioic acid disodium, stirred 1 hour and got with magnetic stirrer when being kept at 85 ℃ with heating bath as " dicarboxylate " as iridic compound.In this iridium electroplate liquid, add the ferric sulfate heptahydrate, make the Fe that comprises 0.01g/L in the electroplate liquid.
Then, the brass test film of 2cm * 2cm is carried out golden strike plating handle, after the gold-plated processing of thick 1.0 μ m, the iridium that forms thick 3.0 μ m is electroplated tunicle.The electroplating processes condition is made as pH3.5～4.0,80～85 ℃ of temperature of electroplating solution, current density 0.5A/dm
2
Electroplate tunicle for the iridium that is covered, use metalloscope (400 times) to observe the coating proterties.Its result is shown in Fig. 1.
In addition, in order to compare, through not adding the iridium electroplate liquid of any blank among Fe, Co, Ni, the Cu, process the test film that is formed with iridium plating tunicle.The plating condition of this blank is identical when comprising Fe.Its result is shown in Fig. 2.
As shown in Figure 2, confirm to produce a large amount of cracks on the surface through the test film that the iridium electroplate liquid that does not contain Fe is covered.On the other hand, as shown in Figure 1, comprise under the situation of iridium electroplate liquid of Fe, almost do not confirm the crack.
In addition, make the content of Fe become 0.005g/L, 0.01g/L, 0.5g/L, 5.0g/L, 10g/L, confirmed its fissured generation state, the result confirms fissured generation when 0.005g/L, and is unconfirmed to fissured generation when 0.01g/L is above.
Embodiment 2:
Among this embodiment 2, the situation of in the iridium electroplate liquid, adding Co is described.The electroplate liquid of this embodiment 2 is formed as follows:
The sour sodium of hexabromo iridium (III)
15g/L (being scaled metal iridium)
Boric acid 40g/L
Disodium citrate 0.05mol/L
Rose vitriol heptahydrate 0.5g/L (being scaled cobalt metal)
Among the embodiment 2,, adopt the compound that obtains as follows: in the sour sodium of above-mentioned hexabromo iridium (III), add disodium citrate, stirred 1 hour and got with magnetic stirrer when being kept at 85 ℃ with heating bath as " hydroxycarboxylate " as iridic compound.In this iridium electroplate liquid, add rose vitriol, make the Co that comprises 0.5g/L in the electroplate liquid.
Then, the brass test film of 2cm * 2cm is carried out golden strike plating handle, after the gold-plated processing of thick 1.0 μ m, the iridium that forms thick 3.0 μ m is electroplated tunicle.The electroplating processes condition is made as pH3.5～4.0,80～85 ℃ of temperature of electroplating solution, current density 0.5A/dm
2
Electroplate tunicle for the iridium that is covered, use metalloscope (400 times) to observe the coating proterties.Its result is shown in Fig. 3.
As shown in Figure 3, comprise under the situation of iridium electroplate liquid of Co, almost do not confirm the crack.
In addition, make the content of Co become 0.005g/L, 0.01g/L, 0.5g/L, 5.0g/L, 10g/L, confirmed its fissured generation state, the result confirms fissured generation when 0.005g/L, and is unconfirmed to fissured generation when 0.01g/L is above.
In addition, the content of Co is made as 20.0g/L, uses metalloscope (400 times) to observe the coating proterties.Its result is shown in Fig. 4.When the content of Co is made as 20.0g/L, fail to obtain to separate out normally.
Embodiment 3:
Among this embodiment 3, the situation of in the iridium electroplate liquid, adding Ni is described.The electroplate liquid of this embodiment 3 is formed as follows:
The sour sodium of hexabromo iridium (III)
15g/L (being scaled metal iridium)
Boric acid 40g/L
Oxalic acid 0.05mol/L
Nickel sulfate hexahydrate compound 0.5g/L (being scaled metallic nickel)
Among the embodiment 3,, adopt the compound that obtains as follows: in the sour sodium of above-mentioned hexabromo iridium (III), add oxalic acid, stirred 1 hour and got with magnetic stirrer when being kept at 85 ℃ with heating bath as " dicarboxylicacid " as iridic compound.In this iridium electroplate liquid, add the nickel sulfate hexahydrate compound, make the Ni that comprises 0.5g/L in the electroplate liquid.
Then, the brass test film of 2cm * 2cm is carried out golden strike plating handle, after the gold-plated processing of thick 1.0 μ m, the iridium that forms thick 3.0 μ m is electroplated tunicle.The electroplating processes condition is made as pH3.5～4.0,80～85 ℃ of temperature of electroplating solution, current density 0.5A/dm
2
Electroplate tunicle for the iridium that is covered, use metalloscope (400 times) to observe the coating proterties.Its result is shown in Fig. 5.
As shown in Figure 5, comprise under the situation of iridium electroplate liquid of Ni, almost do not confirm the crack.
In addition, make the content of Ni become 0.005g/L, 0.01g/L, 0.5g/L, 5.0g/L, 10g/L, confirmed its fissured generation state, the result confirms fissured generation when 0.005g/L, and is unconfirmed to fissured generation when 0.01g/L is above.
In addition, the content of Ni is made as 15.0g/L, uses metalloscope (400 times) to observe the coating proterties.Its result is shown in Fig. 6.When the content of Ni is made as 15.0g/L, fail to obtain to separate out normally.
Embodiment 4:
Among this embodiment 4, the situation of in the iridium electroplate liquid, adding Cu is described.The electroplate liquid of this embodiment 4 is formed as follows:
The sour sodium of hexabromo iridium (III)
15g/L (being scaled metal iridium)
Boric acid 40g/L
Acetate 0.02mol/L
Copper sulfate pentahydrate 0.01g/L (being scaled metallic copper)
Among the embodiment 4,, adopt the compound that obtains as follows: in the sour sodium of above-mentioned hexabromo iridium (III), add acetate, stirred 1 hour and got with magnetic stirrer when being kept at 85 ℃ with heating bath as " monocarboxylic acid " as iridic compound.In this iridium electroplate liquid, add copper sulfate pentahydrate, make the Cu that comprises 0.01g/L in the electroplate liquid.
Then, the brass test film of 2cm * 2cm is carried out golden strike plating handle, after the gold-plated processing of thick 1.0 μ m, the iridium that forms thick 3.0 μ m is electroplated tunicle.The electroplating processes condition is made as pH3.5～4.0,80～85 ℃ of temperature of electroplating solution, current density 0.5A/dm
2
Electroplate tunicle for the iridium that is covered, use metalloscope (400 times) to observe the coating proterties.Its result is shown in Fig. 7.
As shown in Figure 7, comprise under the situation of iridium electroplate liquid of Cu, almost do not confirm the crack.
In addition, make the content of Cu become 0.005g/L, 0.01g/L, 0.5g/L, 1.0g/L, confirmed its fissured generation state, the result confirms fissured generation when 0.005g/L, and is unconfirmed to fissured generation when 0.01g/L is above.
Embodiment 5:
Among this embodiment 5, the situation of in the iridium electroplate liquid, adding Co is described.The electroplate liquid of this embodiment 5 is formed as follows:
The sour sodium of chlordene iridium (III)
5g/L (being scaled metal iridium)
Boric acid 20g/L
Propanedioic acid disodium 0.10mol/L
Rose vitriol heptahydrate 0.5g/L (being scaled cobalt metal)
Among the embodiment 5,, adopt the compound that obtains as follows: in the sour sodium of above-mentioned chlordene iridium (III), add propanedioic acid disodium, stirred 1 hour and got with magnetic stirrer when being kept at 85 ℃ with heating bath as dicarboxylate as iridic compound.In this iridium electroplate liquid, add rose vitriol, make the Co that comprises 0.5g/L in the electroplate liquid.
Then, the brass test film of 2cm * 2cm is carried out golden strike plating handle, after the gold-plated processing of thick 1.0 μ m, the iridium that forms thick 3.0 μ m is electroplated tunicle.The electroplating processes condition is made as pH3.5～4.0,80～85 ℃ of temperature of electroplating solution, current density 0.2A/dm
2
Electroplate tunicle for the iridium that is covered, use metalloscope (400 times) to observe the coating proterties.Its result is shown in Fig. 8.
As shown in Figure 8, comprise under the situation of iridium electroplate liquid of Co, almost do not confirm the crack.
Embodiment 6:
Among this embodiment 6, the situation of in the iridium electroplate liquid, adding Ni and changing the plating condition is described.The electroplate liquid of this embodiment 6 is formed as follows:
The sour sodium of hexabromo iridium (III)
10g/L (being scaled metal iridium)
Boric acid 30g/L
Oxalic acid 0.05mol/L
Nickel sulfate hexahydrate compound 0.5g/L (being scaled metallic nickel)
Among the embodiment 6,, adopt the compound that obtains as follows: in the sour sodium of above-mentioned hexabromo iridium (III), add oxalic acid, stirred 1 hour and got with magnetic stirrer when being kept at 85 ℃ with heating bath as dicarboxylicacid as iridic compound.In this iridium electroplate liquid, add the nickel sulfate hexahydrate compound, make the Ni that comprises 0.5g/L in the electroplate liquid.
Then, the brass test film of 2cm * 2cm is carried out golden strike plating handle, 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.The 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 when changing pH.
During pH0.5, precipitation efficiency is 0%, does not separate out.During pH3.0, precipitation efficiency is 85%, and is unconfirmed to the crack.PH4.0～7.0 o'clock, precipitation efficiency is 95%～100%, and is unconfirmed to the crack.In addition, during pH8.5, produce the deposition of oxyhydroxide.
Then, mensuration is made as current density 0.5A/dm
2, pH3.5 and the precipitation efficiency when change bathing temperature.
When bathing warm 40 ℃, precipitation efficiency is 0%, does not separate out.When bathing warm 50 ℃, precipitation efficiency is 35%, confirms the crack.When bathing warm 60 ℃～70 ℃, precipitation efficiency is 40%～60%, and is unconfirmed to the crack.When bathing warm 80 ℃～95 ℃, precipitation efficiency is 90%～100%, and is unconfirmed to the crack.In addition, will bathe temperature when rising to 99 ℃, water becomes acutely from the evaporation of plating bath, is difficult to carry out stable electroplating processes.
Then, measure the precipitation efficiency that is made as when bathing 85 ℃ of temperature, pH3.5 and changing current density.Current density 0.01A/dm
2The time, precipitation efficiency is 50%, and is unconfirmed to the crack.Current density 0.02A/dm
2～1.0A/dm
2The time, precipitation efficiency is 90～100%, and is unconfirmed to the crack.Current density 1.5A/dm
2The time, precipitation efficiency is 60%, and is unconfirmed to the crack.Current density 3.0A/dm
2The time, precipitation efficiency is 20%, confirms the crack.In addition, current density is risen to 3.5A/dm
2The time, produce hydrogen, do not obtain to separate out normally.
The possibility of utilizing on the industry
The iridium that can easily form the inhibition that fissured generation obtains doing one's utmost is electroplated tunicle.
Claims (3)
1. iridium electroplate liquid; It is to use to anionic component be add in iridium (III) complex salt of halogen 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 that gets; It is characterized in that
Comprise more than at least a among Fe, Co, Ni, the Cu.
2. iridium electroplate liquid as claimed in claim 1 is characterized in that, at least a above content among Fe, Co, Ni, the Cu is 0.01g/L～10g/L.
3. an iridium electro-plating method is characterized in that, uses claim 1 or 2 described electroplate liquids, with pH1～8,50～98 ℃ of temperature, current density 0.01～3.0A/dm
2Condition electroplate.
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| CN2010102900158A CN102400190A (en) | 2010-09-17 | 2010-09-17 | Iridium plating solution and electroplate method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104195604A (en) * | 2014-09-17 | 2014-12-10 | 朱忠良 | Iridium plating solution for inhibiting crack generation and plating method thereof, and coated substance |
| CN104611744A (en) * | 2014-12-15 | 2015-05-13 | 常州大学 | Method for low temperature aqueous solution electrochemical codeposition of nickel iridium alloy |
| 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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| JPH06316786A (en) * | 1993-04-30 | 1994-11-15 | Electroplating Eng Of Japan Co | Water-soluble iridium plating bath and plating method using the same |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104195604A (en) * | 2014-09-17 | 2014-12-10 | 朱忠良 | Iridium plating solution for inhibiting crack generation and plating method thereof, and coated substance |
| CN104611744A (en) * | 2014-12-15 | 2015-05-13 | 常州大学 | Method for low temperature aqueous solution electrochemical codeposition of nickel iridium alloy |
| CN104611744B (en) * | 2014-12-15 | 2017-06-06 | 常州大学 | A kind of method of low-temperature aqueous solution electrochemical co-deposition nickel iridium alloy |
| 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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