CN102776537B - Method for preparing Ir layer on Pt matrix in chloride fused salt system through electrolytic deposition - Google Patents
Method for preparing Ir layer on Pt matrix in chloride fused salt system through electrolytic deposition Download PDFInfo
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- CN102776537B CN102776537B CN201210247725.1A CN201210247725A CN102776537B CN 102776537 B CN102776537 B CN 102776537B CN 201210247725 A CN201210247725 A CN 201210247725A CN 102776537 B CN102776537 B CN 102776537B
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Abstract
The invention discloses a method for preparing Ir layer on Pt matrix in a chloride fused salt system through electrolytic deposition. The method comprises the steps: depositing an Ir layer in the chloride fused salt system by setting different electrolytic deposition parameters, wherein a constant current mode is adopted in the electrolytic deposition; and mixing sodium chloride and potassium chloride at a molar ratio of 1:1 under high-temperature environment to obtain a mixture, and adding Ir salt at high temperature to form electrolytic deposition liquid. With the method, the Ir layer prepared on the Pt matrix in the chloride fused salt system through electrolytic deposition has the advantages of being convenient to operate, excellent in performance, suitable for deposition on parts with complicated shapes and the like.
Description
Technical field
The present invention relates to a kind of electro-deposition preparation method, more particularly, refer to that one adopts constant current process to prepare the method for iridium (Ir) layer at platinum (Pt) matrix substrates in Chlorides molten salts.
Background technology
The fusing point of metal iridium (Ir) is up to 2400 DEG C, and unreactiveness is very strong, very low consumption rate can be kept below 2100 DEG C, be also difficult to react below the eutectoid point of 2280 DEG C with carbon, and be insoluble to all mineral acids, can resist the erosion of much melting reagent and high temperature silicon hydrochlorate, these are all not available for other metal.Due to the anti-oxidant and corrosion resistance nature that Ir is at high temperature excellent, therefore, Ir is usually deposited over the surface needing resistant to elevated temperatures vital part, as the surface of rocket chamber inwall, turbine engine, thermoelectric generator, automotive industry and other special construction part, be with a wide range of applications in resistance to high temperature oxidation field.But Ir is but a kind of friable metal without ductility, and time many, Ir can show obvious work hardening phenomenon after overheated or cold shaping manufacturing procedure, and therefore, the shaping of Ir is a technical problem urgently to be resolved hurrily.
At present, the technology preparing Ir layer has: Ir layer is prepared in chemical vapour deposition, sputtering physical vapor deposition prepares Ir layer, plasma spraying is prepared galvanic deposit in Ir layer and molten salt system and prepared Ir layer etc.As a kind of high-temperature electric deposition method, compared with other many technology preparing Ir, there is unique advantage in fused salt electro-deposition techniques.Owing to not having water in fused salt, its electrochemical window is wider, thus can prepare the refractory metal being difficult to galvanic deposit in aqueous in molten salt system.At present, domesticly yet there are no the bibliographical information preparing Ir layer about utilizing fused salt technology to carry out galvanic deposit.
Summary of the invention
The object of the invention is to propose one in Chlorides molten salts, Pt matrix adopts the method for continuous current carry out galvanic deposit and prepare Ir layer.
In a kind of Chlorides molten salts of the present invention, Pt matrix substrates prepares the method for Ir layer, and it adopts the continuous current mode under hot environment to carry out galvanic deposit, and the Chlorides molten salts described in application carries out the step that galvanic deposit prepares Ir layer on negative electrode to be had:
Step one: preparation electrodeposit liquid
101st step: by being that the sodium chloride nacl that takes of 1 ︰ 1 and potassium chloride (KCl) carry out being mixed to get mixture in molar ratio, then described mixture is joined in electrolyzer (7), good seal electrolyzer (7) subsequently;
102nd step: vacuumized electrolyzer (7) by vacuum orifice (21), makes electrolyzer (7) interior vacuum tightness reach 2 × 10
-5pa ~ 4 × 10
-5pa;
103rd step: regulate well formula resistance furnace (5), and be 3 ~ 10 DEG C/min with temperature rise rate, be warming up to 300 DEG C, after keeping 300 DEG C to dewater 2 ~ 5 hours, vacuumizes while be filled with argon gas by argon filling gas port (22) in electrolyzer (7);
104th step: add iridium salt by charging opening (23) in electrolyzer (7) after continuing to be warmed up to working temperature 790 DEG C ~ 890 DEG C, leaves standstill 5min ~ 10min at keeping working temperature 790 DEG C ~ 890 DEG C, obtains galvanic deposit tank liquor;
Consumption: be first that 1 ︰ 1 carries out being mixed to get mixture by NaCl and KCl with mol ratio; The iridium salt of 2g ~ 15g is added in the described mixture of 100g;
Described iridium salt can be iridous chloride IrCl
3, borontrifluoride iridium IrF
3, tribromide iridium IrBr
3in one;
Step 2: select electrode
Anode (1): the one in graphite, platinum or iridium;
Negative electrode (3): negative electrode selects Pt;
Step 3: galvanostatic conditions galvanic deposit
301st step: the negative electrode chosen (3) and anode (1) are assembled with electrolyzer (7) and DC current regulator power supply respectively;
302nd step: the cathode current density arranging DC current regulator power supply output is 5mA/cm
2~ 50mA/cm
2;
303rd step: arranging well formula resistance furnace (5) working temperature is that at 790 DEG C ~ 890 DEG C, electrodeposition time is 0.5h ~ 5h; After galvanic deposit terminates, take out negative electrode (3), namely obtain the first sample;
304th step: the first sample is placed in the ultrasonic cleaning pond that dehydrated alcohol is housed, the ultrasonic frequency regulating ultrasonic cleaning instrument is 20kHz ~ 50kHz, and ultrasonic cleaning time 2min ~ 10min, obtains the second sample after cleaning;
305th step: the second sample is placed in the ultrasonic cleaning pond that deionized water is housed, the ultrasonic frequency regulating ultrasonic cleaning instrument is 20kHz ~ 50kHz, and ultrasonic cleaning time 2min ~ 10min, obtains the 3rd sample after cleaning;
306th step: the 3rd sample after standing and drying, is obtained deposition iridium layer sample at temperature is 15 DEG C ~ 35 DEG C;
In described deposition iridium layer sample, the thickness of iridium deposition iridium layer is 0.01mm ~ 0.2mm.
The advantage of preparation method of the present invention: the Ir layer utilizing the inventive method galvanic deposit in Chlorides molten salts to prepare has easy to operate, excellent property, and be applicable to being deposited on the first-class advantage of complex-shaped component.
Accompanying drawing explanation
Fig. 1 is the equipment schematic diagram that the present invention carries out galvanic deposit.
Fig. 2 is the SEM shape appearance figure of Pt matrix surface of the present invention deposition Ir layer.
Fig. 3 is the XRD figure spectrum of Pt matrix surface of the present invention deposition Ir layer.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in further detail.
Shown in Figure 1, a kind ofly prepare in the device systems of Ir layer of the present invention in Chlorides molten salts in the galvanic deposit of Pt matrix, include the DC current regulator power supply for providing continuous current to carry out galvanic deposit, for filling the electrolyzer 7 of molten chloride 6, for providing the well formula resistance furnace 5 of heating environment, for testing the thermopair 4 of molten chloride 6 temperature in electrolyzer 7, DC current regulator power supply is connected with anode 1 and negative electrode 3 respectively, electrolyzer 7 is sealed structure, electrolyzer 7 is at least provided with vacuum orifice 21 and argon filling gas port 22.
In the present invention, the model that described DC current regulator power supply selects Beijing Dahua Radio Instruments Factory to produce is the DC current regulator power supply of DH1719A-2.
In the present invention, the model that well formula resistance furnace 5 selects Beijing Lu Ye company limited of Xiang Long Tontru to produce is the well formula resistance furnace of RJ2-120-9.
The present invention adopts the continuous current mode under hot environment to carry out galvanic deposit, applies Chlorides molten salts of the present invention and on negative electrode, carries out the step that galvanic deposit prepares iridium Ir layer have:
Step one: preparation electrodeposit liquid
101st step: by being that the sodium chloride nacl (analytical pure) that takes of 1 ︰ 1 and potassium chloride (KCl) (analytical pure) carry out being mixed to get mixture in molar ratio, then described mixture is joined in electrolyzer 7, subsequently good seal electrolyzer 7;
102nd step: vacuumized by vacuum orifice 21 pairs of electrolyzers 7, makes vacuum tightness in electrolyzer 7 reach 2 × 10
-5pa ~ 4 × 10
-5pa;
103rd step: regulate well formula resistance furnace 5, and be 3 ~ 10 DEG C/min with temperature rise rate, be warming up to 300 DEG C, after keeping 300 DEG C to dewater 2 ~ 5 hours, vacuumize while be filled with argon gas (mass percent concentration of high-purity argon gas is 99.99%) by argon filling gas port 22 in electrolyzer 7;
104th step: add iridium salt by charging opening 23 in electrolyzer 7 after continuing to be warmed up to working temperature 790 DEG C ~ 890 DEG C, leaves standstill 5min ~ 10min at keeping working temperature 790 DEG C ~ 890 DEG C, obtains molten chloride 6(and galvanic deposit tank liquor);
Consumption: be first that 1 ︰ 1 carries out being mixed to get mixture by NaCl and KCl with mol ratio; The iridium salt of 2g ~ 15g is added in the described mixture of 100g;
Described iridium salt can be iridous chloride IrCl
3, borontrifluoride iridium IrF
3, tribromide iridium IrBr
3in one;
Step 2: select electrode
Anode 1: the one in graphite, platinum or iridium;
Negative electrode 3: negative electrode selects Pt;
Step 3: galvanostatic conditions galvanic deposit
301st step: the negative electrode 3 chosen and anode 1 are assembled with electrolyzer 7 and DC current regulator power supply respectively;
302nd step: the cathode current density arranging DC current regulator power supply output is 5mA/cm
2~ 50mA/cm
2;
303rd step: arranging well formula resistance furnace 5 working temperature is that at 790 DEG C ~ 890 DEG C, the working hour (electrodeposition time) is 0.5h ~ 5h; After galvanic deposit terminates, take out negative electrode 3, namely obtain the first sample;
304th step: the first sample is placed in the ultrasonic cleaning pond that dehydrated alcohol is housed, the ultrasonic frequency regulating ultrasonic cleaning instrument is 20kHz ~ 50kHz, and ultrasonic cleaning time 2min ~ 10min, obtains the second sample after cleaning;
305th step: the second sample is placed in the ultrasonic cleaning pond that deionized water is housed, the ultrasonic frequency regulating ultrasonic cleaning instrument is 20kHz ~ 50kHz, and ultrasonic cleaning time 2min ~ 10min, obtains the 3rd sample after cleaning;
In the present invention, the negative electrode 3 after completing galvanic deposit uses dehydrated alcohol, deionized water ultrasonic cleaning successively, is the muriate in order to remove in galvanic deposit Ir layer.
306th step: the 3rd sample after standing and drying, is obtained the 4th sample at temperature is 15 DEG C ~ 35 DEG C; Described 4th sample is the sample that deposited iridium layer at cathode surface, also referred to as deposition iridium layer sample.
In described deposition iridium layer sample, the thickness of iridium deposition iridium layer is 0.01mm ~ 0.2mm.
embodiment 1
Step one: preparation electrodeposit liquid
101st step: by being that the sodium chloride nacl (analytical pure) that takes of 1 ︰ 1 and potassium chloride (KCl) (analytical pure) carry out being mixed to get mixture in molar ratio, then described mixture is joined in electrolyzer 7, subsequently good seal electrolyzer 7;
102nd step: vacuumized by vacuum orifice 21 pairs of electrolyzers 7, makes vacuum tightness in electrolyzer 7 reach 3 × 10
-5pa;
103rd step: regulate well formula resistance furnace 5, and be 7 DEG C/min with temperature rise rate, be warming up to 300 DEG C, after keeping 300 DEG C to dewater 2 hours, vacuumize while be filled with argon gas (mass percent concentration of high-purity argon gas is 99.99%) by argon filling gas port 22 in electrolyzer 7;
104th step: add iridous chloride IrCl by charging opening 23 in electrolyzer 7 after continuing to be warmed up to working temperature 840 DEG C
3, leave standstill 10min at keeping working temperature 840 DEG C, obtain molten chloride 6(and galvanic deposit tank liquor);
Consumption: be first that 1 ︰ 1 carries out being mixed to get mixture by NaCl and KCl with mol ratio; The iridous chloride IrCl of 9.4g is added in the described mixture of 100g
3;
Step 2: select electrode
Anode 1: graphite (Φ 3mm, spectroscopically pure);
Negative electrode 3: negative electrode selects Pt(size 2mm × 8mm);
Step 3: galvanostatic conditions galvanic deposit
301st step: the negative electrode 3 chosen and anode 1 are assembled with electrolyzer 7 and DC current regulator power supply respectively; Space D between anode 1 and negative electrode 3 is 30mm;
302nd step: the cathode current density arranging DC current regulator power supply output is 30mA/cm
2;
303rd step: arranging well formula resistance furnace 5 working temperature is at 840 DEG C, and the working hour (electrodeposition time) is 3h; After galvanic deposit terminates, take out negative electrode 3, namely obtain the first sample;
304th step: the first sample is placed in the ultrasonic cleaning pond that dehydrated alcohol is housed, the ultrasonic frequency regulating ultrasonic cleaning instrument is 32kHz, and ultrasonic cleaning time 5min, obtains the second sample after cleaning;
305th step: the second sample is placed in the ultrasonic cleaning pond that deionized water is housed, the ultrasonic frequency regulating ultrasonic cleaning instrument is 32kHz, and ultrasonic cleaning time 5min, obtains the 3rd sample after cleaning;
306th step: the 3rd sample after standing and drying, is obtained the 4th sample at temperature is 25 DEG C; Described 4th sample is the sample that deposited iridium layer at cathode surface, also referred to as deposition iridium layer sample.
In described deposition iridium layer sample, the thickness of iridium deposition iridium layer is 0.06mm.
In the present invention, the model that galvanic deposit power supply selects Beijing Dahua Radio Instruments Factory to produce is the DC current regulator power supply of DH1719A-2.
In the present invention, the ultrasonic model selecting Kunshan Ultrasonic Instruments Co., Ltd. to produce is the ultrasonic cleaning instrument of KQ5200B.
The deposition iridium layer sample obtained to embodiment 1 utilizes HIT S-530 scanning electron microscope (SEM) to observe, and its pattern as shown in Figure 2.In Fig. 2, have densification, even, flawless settled layer at Pt matrix surface.
The deposition iridium layer sample obtained to embodiment 1 utilizes Japanese Shimadzu business administration (China) company limited XRD-7000S/L type X-ray diffractometer to carry out thing and characterizes mutually, as shown in Figure 3, in Fig. 3, result shows that in the deposition iridium layer sample obtained, settled layer is Ir simple substance.
embodiment 2
Step one: preparation electrodeposit liquid
101st step: by being that the sodium chloride nacl (analytical pure) that takes of 1 ︰ 1 and potassium chloride (KCl) (analytical pure) carry out being mixed to get mixture in molar ratio, then described mixture is joined in electrolyzer 7, subsequently good seal electrolyzer 7;
102nd step: vacuumized by vacuum orifice 21 pairs of electrolyzers 7, makes vacuum tightness in electrolyzer 7 reach 2 × 10
-5pa;
103rd step: regulate well formula resistance furnace 5, and be 4 DEG C/min with temperature rise rate, be warming up to 300 DEG C, after keeping 300 DEG C to dewater 5 hours, vacuumize while be filled with argon gas (mass percent concentration of high-purity argon gas is 99.99%) by argon filling gas port 22 in electrolyzer 7;
104th step: add borontrifluoride iridium IrF by charging opening 23 in electrolyzer 7 after continuing to be warmed up to working temperature 790 DEG C
3, leave standstill 5min at keeping working temperature 790 DEG C, obtain molten chloride 6(and galvanic deposit tank liquor);
Consumption: be first that 1 ︰ 1 carries out being mixed to get mixture by NaCl and KCl with mol ratio; The borontrifluoride iridium IrF of 14.5g is added in the described mixture of 100g
3;
Step 2: select electrode
Anode 1: iridium (Φ 3mm);
Negative electrode 3: negative electrode selects Pt(size 2mm × 8mm);
Step 3: galvanostatic conditions galvanic deposit
301st step: the negative electrode 3 chosen and anode 1 are assembled with electrolyzer 7 and DC current regulator power supply respectively; Space D between anode 1 and negative electrode 3 is 30mm;
302nd step: the cathode current density arranging DC current regulator power supply output is 10mA/cm
2;
303rd step: arranging well formula resistance furnace 5 working temperature is at 790 DEG C, and the working hour (electrodeposition time) is 5h; After galvanic deposit terminates, take out negative electrode 3, namely obtain the first sample;
304th step: the first sample is placed in the ultrasonic cleaning pond that dehydrated alcohol is housed, the ultrasonic frequency regulating ultrasonic cleaning instrument is 40kHz, and ultrasonic cleaning time 2min, obtains the second sample after cleaning;
305th step: the second sample is placed in the ultrasonic cleaning pond that deionized water is housed, the ultrasonic frequency regulating ultrasonic cleaning instrument is 28kHz, and ultrasonic cleaning time 10min, obtains the 3rd sample after cleaning;
In the present invention, the negative electrode 3 after completing galvanic deposit uses dehydrated alcohol, deionized water ultrasonic cleaning successively, is the muriate in order to remove in galvanic deposit Ir layer.
306th step: the 3rd sample after standing and drying, is obtained the 4th sample at temperature is 35 DEG C; Described 4th sample is the sample that deposited iridium layer at cathode surface, also referred to as deposition iridium layer sample.
In described deposition iridium layer sample, the thickness of iridium deposition iridium layer is 0.03mm.
In the present invention, the model that galvanic deposit power supply selects Beijing Dahua Radio Instruments Factory to produce is the DC current regulator power supply of DH1719A-2.
In the present invention, the ultrasonic model selecting Kunshan Ultrasonic Instruments Co., Ltd. to produce is the ultrasonic cleaning instrument of KQ5200B.
The deposition iridium layer sample obtained to embodiment 2 utilizes HIT S-530 scanning electron microscope (SEM) to observe, and its pattern, has densification, even, flawless settled layer at Pt matrix surface.
The deposition iridium layer sample obtained to embodiment 2 utilizes Japanese Shimadzu business administration (China) company limited XRD-7000S/L type X-ray diffractometer to carry out thing and characterizes mutually, and result shows that in the deposition iridium layer sample obtained, settled layer is Ir simple substance.
embodiment 3
Step one: preparation electrodeposit liquid
101st step: by being that the sodium chloride nacl (analytical pure) that takes of 1 ︰ 1 and potassium chloride (KCl) (analytical pure) carry out being mixed to get mixture in molar ratio, then described mixture is joined in electrolyzer 7, subsequently good seal electrolyzer 7;
102nd step: vacuumized by vacuum orifice 21 pairs of electrolyzers 7, makes vacuum tightness in electrolyzer 7 reach 4 × 10
-5pa;
103rd step: regulate well formula resistance furnace 5, and be 10 DEG C/min with temperature rise rate, be warming up to 300 DEG C, after keeping 300 DEG C to dewater 3.5 hours, vacuumize while be filled with argon gas (mass percent concentration of high-purity argon gas is 99.99%) by argon filling gas port 22 in electrolyzer 7;
104th step: add tribromide iridium IrBr by charging opening 23 in electrolyzer 7 after continuing to be warmed up to working temperature 890 DEG C
3, leave standstill 5min at keeping working temperature 890 DEG C, obtain molten chloride 6(and galvanic deposit tank liquor);
Consumption: be first that 1 ︰ 1 carries out being mixed to get mixture by NaCl and KCl with mol ratio; The tribromide iridium IrBr of 5g is added in the described mixture of 100g
3;
Step 2: select electrode
Anode 1: graphite (Φ 3mm, spectroscopically pure);
Negative electrode 3: negative electrode selects Pt(size 2mm × 8mm);
Step 3: galvanostatic conditions galvanic deposit
301st step: the negative electrode 3 chosen and anode 1 are assembled with electrolyzer 7 and DC current regulator power supply respectively; Space D between anode 1 and negative electrode 3 is 30mm;
302nd step: the cathode current density arranging DC current regulator power supply output is 45mA/cm
2;
303rd step: arranging well formula resistance furnace 5 working temperature is at 880 DEG C, and the working hour (electrodeposition time) is 2h; After galvanic deposit terminates, take out negative electrode 3, namely obtain the first sample;
304th step: the first sample is placed in the ultrasonic cleaning pond that dehydrated alcohol is housed, the ultrasonic frequency regulating ultrasonic cleaning instrument is 28kHz, and ultrasonic cleaning time 6min, obtains the second sample after cleaning;
305th step: the second sample is placed in the ultrasonic cleaning pond that deionized water is housed, the ultrasonic frequency regulating ultrasonic cleaning instrument is 28kHz, and ultrasonic cleaning time 6min, obtains the 3rd sample after cleaning;
In the present invention, the negative electrode 3 after completing galvanic deposit uses dehydrated alcohol, deionized water ultrasonic cleaning successively, is the muriate in order to remove in galvanic deposit Ir layer.
306th step: the 3rd sample after standing and drying, is obtained the 4th sample at temperature is 15 DEG C; Described 4th sample is the sample that deposited iridium layer at cathode surface, also referred to as deposition iridium layer sample.
In described deposition iridium layer sample, the thickness of iridium deposition iridium layer is 0.06mm.
In the present invention, the model that galvanic deposit power supply selects Beijing Dahua Radio Instruments Factory to produce is the DC current regulator power supply of DH1719A-2.
In the present invention, the ultrasonic model selecting Kunshan Ultrasonic Instruments Co., Ltd. to produce is the ultrasonic cleaning instrument of KQ5200B.
The deposition iridium layer sample obtained to embodiment 3 utilizes HIT S-530 scanning electron microscope (SEM) to observe, and its pattern, has densification, even, flawless settled layer at Pt matrix surface.
The deposition iridium layer sample obtained to embodiment 3 utilizes Japanese Shimadzu business administration (China) company limited XRD-7000S/L type X-ray diffractometer to carry out thing and characterizes mutually, and result shows that in the deposition iridium layer sample obtained, settled layer is Ir simple substance.
Claims (1)
1. in Chlorides molten salts, Pt matrix substrates prepares a method for Ir layer, and the method application Chlorides molten salts carries out the step that galvanic deposit prepares Ir layer on negative electrode to be had:
Step one: preparation electrodeposit liquid
101st step: by being that the sodium chloride nacl that takes of 1 ︰ 1 and potassium chloride (KCl) carry out being mixed to get mixture in molar ratio, then described mixture is joined in electrolyzer (7), good seal electrolyzer (7) subsequently;
102nd step: vacuumized electrolyzer (7) by vacuum orifice (21), makes electrolyzer (7) interior vacuum tightness reach 2 × 10
-5pa ~ 4 × 10
-5pa;
103rd step: regulate well formula resistance furnace (5), and be 3 ~ 10 DEG C/min with temperature rise rate, be warming up to 300 DEG C, after keeping 300 DEG C to dewater 2 ~ 5 hours, vacuumize while be filled with argon gas by argon filling gas port (22) in electrolyzer (7);
104th step: add iridium salt by charging opening (23) in electrolyzer (7) after continuing to be warmed up to working temperature 790 DEG C ~ 890 DEG C, leaves standstill 5min ~ 10min at keeping working temperature 790 DEG C ~ 890 DEG C, obtains galvanic deposit tank liquor;
Consumption: be first that 1 ︰ 1 carries out being mixed to get mixture by NaCl and KCl with mol ratio; The iridium salt of 2g ~ 15g is added in the described mixture of 100g;
Described iridium salt can be iridous chloride IrCl
3, borontrifluoride iridium IrF
3, tribromide iridium IrBr
3in one;
Step 2: select electrode
Anode (1): the one in graphite, platinum or iridium;
Negative electrode (3): negative electrode selects Pt;
It is characterized in that: the method adopts continuous current mode in high temperature environments to carry out galvanic deposit;
Step 3: galvanostatic conditions galvanic deposit
301st step: the negative electrode chosen (3) and anode (1) are assembled with electrolyzer (7) and DC current regulator power supply respectively; Spacing between the 301st step Anodic (1) and negative electrode (3) is 30mm;
302nd step: the cathode current density arranging DC current regulator power supply output is 5mA/cm
2~ 50mA/cm
2;
303rd step: arranging well formula resistance furnace (5) working temperature is that at 790 DEG C ~ 890 DEG C, electrodeposition time is 0.5h ~ 5h; After galvanic deposit terminates, take out negative electrode (3), namely obtain the first sample;
304th step: the first sample is placed in the ultrasonic cleaning pond that dehydrated alcohol is housed, the ultrasonic frequency regulating ultrasonic cleaning instrument is 20kHz ~ 50kHz, and ultrasonic cleaning time 2min ~ 10min, obtains the second sample after cleaning;
305th step: the second sample is placed in the ultrasonic cleaning pond that deionized water is housed, the ultrasonic frequency regulating ultrasonic cleaning instrument is 20kHz ~ 50kHz, and ultrasonic cleaning time 2min ~ 10min, obtains the 3rd sample after cleaning;
306th step: the 3rd sample after standing and drying, is obtained deposition iridium layer sample at temperature is 15 DEG C ~ 35 DEG C;
In described deposition iridium layer sample, settled layer is Ir simple substance;
In described deposition iridium layer sample, the thickness of iridium deposition iridium layer is 0.01mm ~ 0.2mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210247725.1A CN102776537B (en) | 2012-07-17 | 2012-07-17 | Method for preparing Ir layer on Pt matrix in chloride fused salt system through electrolytic deposition |
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|---|---|---|---|
| CN201210247725.1A CN102776537B (en) | 2012-07-17 | 2012-07-17 | Method for preparing Ir layer on Pt matrix in chloride fused salt system through electrolytic deposition |
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| CN103806043B (en) * | 2014-01-24 | 2016-06-01 | 中国人民解放军国防科学技术大学 | Non-columnar crystalline substance organizes the fused salt electroplating preparation method of iridium coating layer |
| CN103806044B (en) * | 2014-01-24 | 2016-08-17 | 中国人民解放军国防科学技术大学 | The method of electrolytic preparation iridium coating layer in chloro-iridic acid caesium-Chlorides molten salts |
| CN106119945B (en) * | 2016-08-01 | 2017-12-15 | 陕西三毅有岩材料科技有限公司 | Termination processing method when a kind of drawing iridium and its B alloy wire |
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