CN117219319A - Voltage equalizing electrode and preparation method thereof - Google Patents
Voltage equalizing electrode and preparation method thereof Download PDFInfo
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- CN117219319A CN117219319A CN202311158535.7A CN202311158535A CN117219319A CN 117219319 A CN117219319 A CN 117219319A CN 202311158535 A CN202311158535 A CN 202311158535A CN 117219319 A CN117219319 A CN 117219319A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 224
- 239000000523 sample Substances 0.000 claims abstract description 152
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 113
- 239000011159 matrix material Substances 0.000 claims abstract description 33
- 238000009713 electroplating Methods 0.000 claims description 54
- 238000007747 plating Methods 0.000 claims description 50
- 239000002585 base Substances 0.000 claims description 39
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 36
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- 238000000034 method Methods 0.000 claims description 22
- 229910001220 stainless steel Inorganic materials 0.000 claims description 19
- 239000010935 stainless steel Substances 0.000 claims description 19
- 239000000758 substrate Substances 0.000 claims description 19
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 18
- 235000019270 ammonium chloride Nutrition 0.000 claims description 18
- 239000000908 ammonium hydroxide Substances 0.000 claims description 18
- 229910052759 nickel Inorganic materials 0.000 claims description 14
- 239000002253 acid Substances 0.000 claims description 13
- 230000004913 activation Effects 0.000 claims description 6
- 238000007598 dipping method Methods 0.000 claims description 6
- 238000005238 degreasing Methods 0.000 claims description 5
- 125000003963 dichloro group Chemical group Cl* 0.000 claims description 5
- 239000003513 alkali Substances 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 230000005540 biological transmission Effects 0.000 abstract description 14
- 238000001816 cooling Methods 0.000 abstract description 9
- CLSUSRZJUQMOHH-UHFFFAOYSA-L platinum dichloride Chemical compound Cl[Pt]Cl CLSUSRZJUQMOHH-UHFFFAOYSA-L 0.000 description 13
- 239000011248 coating agent Substances 0.000 description 10
- 238000000576 coating method Methods 0.000 description 10
- 239000003792 electrolyte Substances 0.000 description 10
- 239000007788 liquid Substances 0.000 description 10
- 230000008569 process Effects 0.000 description 10
- 230000001105 regulatory effect Effects 0.000 description 10
- 239000000498 cooling water Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000008021 deposition Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- -1 platinum ions Chemical class 0.000 description 3
- 239000010963 304 stainless steel Substances 0.000 description 2
- 229910000589 SAE 304 stainless steel Inorganic materials 0.000 description 2
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 2
- 239000002738 chelating agent Substances 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000006911 nucleation Effects 0.000 description 2
- 238000010899 nucleation Methods 0.000 description 2
- 230000036632 reaction speed Effects 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- CYEJMVLDXAUOPN-UHFFFAOYSA-N 2-dodecylphenol Chemical compound CCCCCCCCCCCCC1=CC=CC=C1O CYEJMVLDXAUOPN-UHFFFAOYSA-N 0.000 description 1
- 241001391944 Commicarpus scandens Species 0.000 description 1
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 description 1
- 241000080590 Niso Species 0.000 description 1
- 239000002033 PVDF binder Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910001453 nickel ion Inorganic materials 0.000 description 1
- 229940051841 polyoxyethylene ether Drugs 0.000 description 1
- 229920000056 polyoxyethylene ether Polymers 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- Electroplating And Plating Baths Therefor (AREA)
Abstract
The invention relates to a voltage equalizing electrode and a preparation method thereof. The voltage equalizing electrode comprises a base and a probe arranged on the base, wherein the probe comprises a probe matrix and a platinum layer arranged on the surface of the probe matrix, and the probe matrix and the base are integrally formed. Among the above-mentioned voltage-sharing electrode, the probe includes the probe base member and sets up the platinum layer on probe base member surface, and probe base member and base integrated into one piece have mechanical properties good, and anti tangential impact force's characteristics can reduce the risk that the probe receives rivers effort to take place to break with the base junction, simultaneously, probe base member surface is provided with the platinum layer, makes voltage-sharing electrode and pure platinum probe voltage-sharing electrode have the same chemistry, electrochemical stability, can be applied to in the high-voltage direct current transmission converter valve cooling system.
Description
Technical Field
The invention relates to the technical field of high-voltage direct-current transmission, in particular to a voltage equalizing electrode and a preparation method thereof.
Background
Long-distance power transmission is an efficient and low-cost way of energy deployment. In the power transmission technology, high-voltage direct current (HVDC) transmission has the advantages of long transmission distance, large capacity, flexible control, convenient scheduling and the like.
The working environment of the equalizing electrode of the high-voltage direct-current transmission converter valve cooling system is harsh, and the equalizing electrode plays a role in balancing the potential of cooling water in internal circulating cooling water with high voltage (higher than 10 kV), high impact force (water flow speed of 0.1-10 m/s), high temperature field (45-60 ℃) and low ion conductivity (lower than 0.5 mu s/cm), and has the characteristics of low resistance, high electronic conductivity, high chemical stability, high electrochemical stability and the like.
The current production voltage equalizing electrode consists of a base and a probe. Wherein, the base is 304 stainless steel material, and the material cost is low. Because of the harsh conditions of high voltage, strong magnetic field and the like, the circulating cooling water path of the converter valve cooling system has the difficult problems of chemical stability, electrochemical stability and the like, and therefore, the pressure equalizing electrode probe contacted with cooling water adopts a metal platinum material with high chemical stability and high electrochemical stability.
In the high-voltage direct-current transmission converter valve cooling system, a platinum probe is arranged on a stainless steel base, a polyvinylidene fluoride pipe is vertically inserted, and the platinum probe is soaked in cooling water and is in low-impedance contact with water so as to reduce the potential difference of a waterway. The water impacts the probe at a certain flow velocity, the probe is stressed tangentially, and the joint of the probe and the base is easy to break. In particular, in the long-term operation process of the high-voltage direct-current transmission system, scaling substances are easy to form on the surface of the pressure equalizing electrode probe, so that the stress in the water flow direction is further increased, and the risk of breakage of the joint of the probe and the base is increased.
Disclosure of Invention
Based on the above, it is necessary to provide a voltage equalizing electrode and a preparation method thereof, so as to solve the problem that the joint of the probe and the base is broken under the action of water flow.
One of the purposes of the invention is to provide a voltage equalizing electrode, which comprises the following scheme:
the voltage equalizing electrode comprises a base and a probe arranged on the base, wherein the probe comprises a probe matrix and a platinum layer arranged on the surface of the probe matrix, and the probe matrix and the base are integrally formed.
In one embodiment, the probe substrate and the base are made of stainless steel.
In one embodiment, a nickel layer is disposed between the probe substrate and the platinum layer.
In one embodiment, the platinum layer has a thickness of 0.5 μm to 5 μm.
In one embodiment, the platinum layer is formed by a platinating process.
Another object of the present invention is to provide a method for preparing a voltage equalizing electrode according to any one of the above embodiments, which comprises the following steps:
the preparation method of the voltage equalizing electrode comprises the following steps:
preparing an integrally formed base and a probe matrix;
immersing the probe substrate in an electroplating solution, and carrying out electroplating platinum treatment on the probe substrate to form a platinum layer on the surface of the probe substrate.
In one embodiment, the plating solution includes: water, dichloro diammine platinum and/or dichloro dihydroxy diammine platinum with the concentration of 5-30 g/L, ammonium chloride with the concentration of 10-27 g/L and ammonium hydroxide with the concentration of 7-68 g/L.
In one embodiment, the pH of the plating solution is 8.9 to 9.3.
In one embodiment, the temperature of the plating solution is controlled to be 5-20 ℃ during the platinum plating process.
In which it is arrangedIn one embodiment, the cathode current density of the electroplated platinum treatment is 0.1A/dm 2 ～0.5A/dm 2 。
In one embodiment, the method of preparing the probe substrate prior to the platinating treatment further comprises the steps of:
and carrying out nickel pre-plating treatment on the probe matrix.
In one embodiment, the method of preparing further comprises the steps of:
and sequentially carrying out alkali degreasing treatment, acid dipping treatment and acid activation treatment on the probe matrix.
Compared with the traditional scheme, the voltage equalizing electrode and the preparation method thereof have the following beneficial effects:
among the above-mentioned voltage-sharing electrode, the probe includes the probe base member and sets up the platinum layer on probe base member surface, and probe base member and base integrated into one piece have mechanical properties good, and anti tangential impact force's characteristics can reduce the risk that the probe receives rivers effort to take place to break with the base junction, simultaneously, probe base member surface is provided with the platinum layer, makes voltage-sharing electrode and pure platinum probe voltage-sharing electrode have the same chemistry, electrochemical stability, can be applied to in the high-voltage direct current transmission converter valve cooling system.
Detailed Description
In order that the invention may be readily understood, a more particular description of the invention will be rendered by reference to specific embodiments that are now described. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.
The invention provides a voltage equalizing electrode. The voltage equalizing electrode can be applied to a high-voltage direct-current transmission converter valve cooling system.
The voltage equalizing electrode comprises a base and a probe arranged on the base, wherein the probe comprises a probe matrix and a platinum layer arranged on the surface of the probe matrix. And, the probe base body and the base are integrally formed.
Among the above-mentioned voltage-sharing electrode, the probe includes the probe base member and sets up the platinum layer on probe base member surface, and probe base member and base integrated into one piece have mechanical properties good, and anti tangential impact force's characteristics can reduce the risk that the probe receives rivers effort to take place to break with the base junction, simultaneously, probe base member surface is provided with the platinum layer, makes voltage-sharing electrode and pure platinum probe voltage-sharing electrode have the same chemistry, electrochemical stability, can be applied to in the high-voltage direct current transmission converter valve cooling system.
In one embodiment, the probe base and the base are made of stainless steel. Further, in one embodiment, the probe base and the base are made of 304 stainless steel. The electroplating technology of platinum on the surface of the stainless steel probe matrix is simple and easy to control.
In one embodiment, the probe substrate is a columnar structure. Further, in one embodiment, the probe substrate is a cylindrical structure.
In one embodiment, the platinum layer has a thickness of 0.5 μm to 5 μm. Further, in one embodiment, the platinum layer has a thickness of 1 μm to 4 μm. In some specific embodiments, the platinum layer has a thickness of 0.5 μm, 1 μm, 1.5 μm, 2 μm, 2.5 μm, 3 μm, 3.5 μm, 4 μm, 4.5 μm, 5 μm, etc.
In one embodiment, the platinum layer is formed by a platinating process. The platinum layer is formed through electroplating platinum treatment, so that the surface smoothness of the platinum probe can be improved, and the nucleation and growth of aluminum hydroxide on the surface of the platinum probe can be slowed down, so that the effect of slowing down the scaling on the surface of the platinum probe can be achieved.
The invention also provides a preparation method of the voltage equalizing electrode in any embodiment.
The preparation method of the voltage equalizing electrode in one embodiment comprises the following steps:
preparing an integrally formed base and a probe matrix;
the probe substrate is immersed in the plating solution, and a platinum plating treatment is performed on the probe substrate to form a platinum layer on the surface of the probe substrate.
In one embodiment, the plating solution includes: water, dichloro-diammine platinum and/or dichloro-dihydroxy-diammine platinum, ammonium chloride and ammonium hydroxide.
The electroplating solution is adopted, ammonium chloride and ammonium hydroxide in the electroplating solution are used as chelating agents, the activity of platinum ions and the diffusion coefficient of the platinum ions in the electroplating solution are limited, the reduction reaction speed of platinum is controlled, and the compactness of a platinum deposition layer is ensured.
In one embodiment, the concentration of platinum dichloride and/or platinum dichloride dihydroxy is in the range of 5g/L to 30g/L. Further, in one embodiment, the concentration of dichlorodiammineplatinum and/or dichlorodihydroxy diammineplatinum is in the range of 10g/L to 20g/L. In some specific embodiments, the concentration of platinum dichloride and/or platinum dichloride dihydroxy is 5g/L, 10g/L, 15g/L, 20g/L, 25g/L, 30g/L, etc.
In one embodiment, the concentration of ammonium chloride is 10g/L to 27g/L. Further, in one embodiment, the concentration of ammonium chloride is 15g/L to 22g/L. In some specific embodiments, the concentration of ammonium chloride is 10g/L, 12g/L, 15g/L, 20g/L, 25g/L, etc.
In one embodiment, the concentration of ammonium hydroxide is 7g/L to 68g/L. Further, in one embodiment, the concentration of ammonium hydroxide is 20g/L to 50g/L. In some specific embodiments, the concentration of ammonium hydroxide is 10g/L, 20g/L, 30g/L, 40g/L, 50g/L, 60g/L, etc.
In this embodiment, the electroplating solution containing the components with specific amounts is used, and ammonium chloride and ammonium hydroxide in the electroplating solution are used as chelating agents to limit the activity of platinum ions and the diffusion coefficient thereof in the electroplating solution, control the reduction reaction speed of platinum, and ensure the compactness of the platinum deposition layer.
In one embodiment, the pH of the plating solution is 8.9 to 9.3. Further, in one embodiment, the pH of the plating solution is 9 to 9.2. In some specific embodiments, the plating solution has a pH of 8.9, 9, 9.1, 9.2, 9.3, etc.
In one embodiment, the temperature of the plating solution is controlled to be 5-20 ℃ during the platinum plating process. Further, in one embodiment, the temperature of the plating solution is 10℃to 15 ℃. In some specific embodiments, the temperature of the plating solution is 5 ℃, 8 ℃, 10 ℃, 12 ℃, 14 ℃, 16 ℃, 18 ℃, 20 ℃, etc.
In one embodiment, the cathodic current density of the electroplated platinum treatment is 0.1A/dm 2 ～0.5A/dm 2 . Further, in one embodiment, the cathode current density of the platinized treatment is 0.2A/dm 2 ～0.4A/dm 2 . In some specific embodiments, the cathodic current density of the platinized treatment is 0.1A/dm 2 、0.15A/dm 2 、0.2A/dm 2 、0.25A/dm 2 、0.3A/dm 2 、0.35A/dm 2 、0.4A/dm 2 、0.45A/dm 2 、0.5A/dm 2 Etc.
In one embodiment, the method of preparing the probe substrate prior to the platinating treatment further comprises the steps of:
and carrying out nickel pre-plating treatment on the probe matrix.
If the platinum is directly plated on the surface of the stainless steel, the platinum is not easy to deposit into a compact layer, and the platinum layer is easy to fall off. In the above example, a nickel layer is plated first, nickel ions are easily deposited on the surface of stainless steel, and the nickel layer is formed to be better combined with stainless steel, and platinum is plated again on the surface of the nickel layer, so that platinum deposition is easy to realize and the bonding force is high.
In one embodiment, the nickel preplating process includes:
the plating solution for nickel preplating comprises: 1M-5M NiSO 4 ；1M～5M NiCl 2 The method comprises the steps of carrying out a first treatment on the surface of the 0.001M-0.005M dodecylphenol polyoxyethylene ether. The pH is adjusted to 3.0 with an acid such as hydrochloric acid.
In one of the embodiments of the present invention,technological conditions of nickel preplating: the temperature is 45-55 ℃; the current density was 0.01A/dm 2 ～0.05A/dm 2 The method comprises the steps of carrying out a first treatment on the surface of the The electroplating time is 1 to 5 minutes.
After the nickel pre-plating treatment, the plating solution is washed clean by deionized water and then enters a plating tank for plating platinum.
In one embodiment, the probe substrate is pre-treated. The pretreatment includes alkali degreasing treatment, acid dipping treatment and acid activation treatment.
In one embodiment, the alkaline degreasing treatment comprises: and 1M-5M NaOH solution is adopted to wash the probe matrix at 70-85 ℃. And after the probe matrix is degreased, washing the probe matrix with deionized water.
In one embodiment, the acid dip treatment comprises: 1M-2M H 2 SO 4 And 1M to 3MKNO 3 Dipping the probe matrix at 60-75 ℃ for 10-15 minutes. After acid dipping, the probe matrix is washed clean with deionized water.
In one embodiment, the acid activation treatment comprises: using 0.1M-1M H 2 SO 4 And 0.2M-2M HCl, and soaking the probe matrix for 1-3 minutes at room temperature. After acid activation of the probe matrix, the probe matrix is rinsed clean with deionized water.
For a better understanding of the present invention, the following examples are further illustrated by the following examples, but the scope of the present invention is not limited to the following examples.
Example 1
The embodiment provides an integrated voltage-equalizing electrode, and the preparation method thereof comprises the following steps:
and step 1, processing a stainless steel workpiece to obtain an integrated voltage-equalizing electrode to be plated, wherein the voltage-equalizing electrode to be plated comprises a base and a probe connected to the base.
And 2, performing alkali degreasing, acid dipping, acid activation and nickel preplating on the probe of the voltage-equalizing electrode to be plated.
And step 3, placing the probe of the voltage equalizing electrode to be plated in electroplating solution, electroplating, and forming a platinum coating on the surface of the stainless steel probe.
Specifically, the voltage of the regulated power supply is controlled to be 0.3V, and the voltage-equalizing electrode to be plated is used as a working electrode and connected with a cathode. An annular platinum sheet with a diameter of 8mm and a height of 150mm was used as a counter electrode to connect the anode. The probe of the voltage equalizing electrode to be plated is placed in the middle of the annular platinum sheet and is immersed in the electroplating liquid in an electrified manner.
Wherein the plating solution comprises water, 5g/L of diammine platinum dichloride, 17g/L of ammonium chloride and 56g/L of ammonium hydroxide, and the pH value is 9.3.
In the electroplating treatment process, the temperature of the electrolyte is 15 ℃, and the cathode current density is 0.1A/dm 2 。
The platinum plating layer formed on the probe in this example had a thickness of 0.5. Mu.m.
Example 2
The embodiment provides an integrated voltage-equalizing electrode, and the preparation method thereof comprises the following steps:
step 1 and step 2 are the same as in example 1.
And step 3, placing the probe of the voltage equalizing electrode to be plated in electroplating solution, electroplating, and forming a platinum coating on the surface of the stainless steel probe.
Specifically, the voltage of the regulated power supply is controlled to be 0.3V, and the voltage-equalizing electrode to be plated is used as a working electrode and connected with a cathode. An annular platinum sheet with a diameter of 8mm and a height of 150mm was used as a counter electrode to connect the anode. The probe of the voltage equalizing electrode to be plated is placed in the middle of the annular platinum sheet and is immersed in the electroplating liquid in an electrified manner.
Wherein the plating solution comprises water, 12g/L of dichloro dihydroxy diammine platinum, 10g/L of ammonium chloride and 68g/L of ammonium hydroxide, and the pH is 8.9.
In the electroplating treatment process, the temperature of the electrolyte is 5 ℃, and the cathode current density is 0.5A/dm 2 。
The platinum plating layer formed on the probe in this example had a thickness of 1.5. Mu.m.
Example 3
The embodiment provides an integrated voltage-equalizing electrode, and the preparation method thereof comprises the following steps:
step 1 and step 2 are the same as in example 1.
And step 3, placing the probe of the voltage equalizing electrode to be plated in electroplating solution, electroplating, and forming a platinum coating on the surface of the stainless steel probe.
Specifically, the voltage of the regulated power supply is controlled to be 0.3V, and the voltage-equalizing electrode to be plated is used as a working electrode and connected with a cathode. An annular platinum sheet with a diameter of 8mm and a height of 150mm was used as a counter electrode to connect the anode. The probe of the voltage equalizing electrode to be plated is placed in the middle of the annular platinum sheet and is immersed in the electroplating liquid in an electrified manner.
Wherein the plating solution comprises water, 18g/L of diammine platinum dichloride, 12g/L of ammonium chloride and 55g/L of ammonium hydroxide, and the pH value is 9.1.
In the electroplating treatment, the temperature of the electrolyte is 17 ℃, and the cathode current density is 0.3A/dm 2 。
The platinum plating layer formed on the probe in this example had a thickness of 2. Mu.m.
Example 4
The embodiment provides an integrated voltage-equalizing electrode, and the preparation method thereof comprises the following steps:
step 1 and step 2 are the same as in example 1.
And step 3, placing the probe of the voltage equalizing electrode to be plated in electroplating solution, electroplating, and forming a platinum coating on the surface of the stainless steel probe.
Specifically, the voltage of the regulated power supply is controlled to be 0.3V, and the voltage-equalizing electrode to be plated is used as a working electrode and connected with a cathode. An annular platinum sheet with a diameter of 8mm and a height of 150mm was used as a counter electrode to connect the anode. The probe of the voltage equalizing electrode to be plated is placed in the middle of the annular platinum sheet and is immersed in the electroplating liquid in an electrified manner.
Wherein the plating solution comprises water, 20g/L of diammine platinum dichloride, 15g/L of ammonium chloride and 45g/L of ammonium hydroxide, and the pH value is 9.2.
In the electroplating treatment process, the temperature of the electrolyte is 20 ℃, and the cathode current density is 0.5A/dm 2 。
The platinum plating layer formed on the probe in this example had a thickness of 3. Mu.m.
Example 5
The embodiment provides an integrated voltage-equalizing electrode, and the preparation method thereof comprises the following steps:
step 1 and step 2 are the same as in example 1.
And step 3, placing the probe of the voltage equalizing electrode to be plated in electroplating solution, electroplating, and forming a platinum coating on the surface of the stainless steel probe.
Specifically, the voltage of the regulated power supply is controlled to be 0.3V, and the voltage-equalizing electrode to be plated is used as a working electrode and connected with a cathode. An annular platinum sheet with a diameter of 8mm and a height of 150mm was used as a counter electrode to connect the anode. The probe of the voltage equalizing electrode to be plated is placed in the middle of the annular platinum sheet and is immersed in the electroplating liquid in an electrified manner.
Wherein the plating solution comprises water, 25g/L of diammine platinum dichloride, 27g/L of ammonium chloride and 68g/L of ammonium hydroxide, and the pH value is 9.3.
In the electroplating treatment, the temperature of the electrolyte is 19 ℃ and the cathode current density is 0.4A/dm 2 。
The platinum plating layer formed on the probe in this example had a thickness of 4. Mu.m.
Example 6
The embodiment provides an integrated voltage-equalizing electrode, and the preparation method thereof comprises the following steps:
step 1 and step 2 are the same as in example 1.
And step 3, placing the probe of the voltage equalizing electrode to be plated in electroplating solution, electroplating, and forming a platinum coating on the surface of the stainless steel probe.
Specifically, the voltage of the regulated power supply is controlled to be 0.3V, and the voltage-equalizing electrode to be plated is used as a working electrode and connected with a cathode. An annular platinum sheet with a diameter of 8mm and a height of 150mm was used as a counter electrode to connect the anode. The probe of the voltage equalizing electrode to be plated is placed in the middle of the annular platinum sheet and is immersed in the electroplating liquid in an electrified manner.
Wherein the plating solution comprises water, 30g/L of diammine platinum dichloride, 24g/L of ammonium chloride and 62g/L of ammonium hydroxide, and the pH value is 9.0.
In the electroplating treatment process, the temperature of the electrolyte is 8 ℃, and the cathode current density is 0.5A/dm 2 。
The platinum plating layer formed on the probe in this example had a thickness of 45. Mu.m.
Example 7
The embodiment provides an integrated voltage-equalizing electrode, and the preparation method thereof comprises the following steps:
step 1 and step 2 are the same as in example 1.
And step 3, placing the probe of the voltage equalizing electrode to be plated in electroplating solution, electroplating, and forming a platinum coating on the surface of the stainless steel probe.
Specifically, the voltage of the regulated power supply is controlled to be 0.3V, and the voltage-equalizing electrode to be plated is used as a working electrode and connected with a cathode. An annular platinum sheet with a diameter of 8mm and a height of 150mm was used as a counter electrode to connect the anode. The probe of the voltage equalizing electrode to be plated is placed in the middle of the annular platinum sheet and is immersed in the electroplating liquid in an electrified manner.
Wherein the plating solution comprises water, 29g/L of diammine platinum dichloride, 22g/L of ammonium chloride and 45g/L of ammonium hydroxide, and the pH value is 9.2.
In the electroplating treatment, the temperature of the electrolyte is 16 ℃, and the cathode current density is 0.2A/dm 2 。
The platinum plating layer formed on the probe in this example had a thickness of 4.5. Mu.m.
Example 8
The embodiment provides an integrated voltage-equalizing electrode, and the preparation method thereof comprises the following steps:
step 1 and step 2 are the same as in example 1.
And step 3, placing the probe of the voltage equalizing electrode to be plated in electroplating solution, electroplating, and forming a platinum coating on the surface of the stainless steel probe.
Specifically, the voltage of the regulated power supply is controlled to be 0.3V, and the voltage-equalizing electrode to be plated is used as a working electrode and connected with a cathode. An annular platinum sheet with a diameter of 8mm and a height of 150mm was used as a counter electrode to connect the anode. The probe of the voltage equalizing electrode to be plated is placed in the middle of the annular platinum sheet and is immersed in the electroplating liquid in an electrified manner.
Wherein the plating solution comprises water, 23g/L of diammine platinum dichloride, 23g/L of ammonium chloride and 36g/L of ammonium hydroxide, and the pH value is 9.2.
In the electroplating treatment, the temperature of the electrolyte is 17 ℃, and the cathode current density is 0.3A/dm 2 。
The platinum plating layer formed on the probe in this example had a thickness of 3.5. Mu.m.
Example 9
The embodiment provides an integrated voltage-equalizing electrode, and the preparation method thereof comprises the following steps:
step 1 and step 2 are the same as in example 1.
And step 3, placing the probe of the voltage equalizing electrode to be plated in electroplating solution, electroplating, and forming a platinum coating on the surface of the stainless steel probe.
Specifically, the voltage of the regulated power supply is controlled to be 0.3V, and the voltage-equalizing electrode to be plated is used as a working electrode and connected with a cathode. An annular platinum sheet with a diameter of 8mm and a height of 150mm was used as a counter electrode to connect the anode. The probe of the voltage equalizing electrode to be plated is placed in the middle of the annular platinum sheet and is immersed in the electroplating liquid in an electrified manner.
Wherein the plating solution comprises water, 13g/L of diammine platinum dichloride, 23g/L of ammonium chloride and 33g/L of ammonium hydroxide, and the pH value is 9.3.
In the electroplating treatment, the temperature of the electrolyte is 7 ℃ and the cathode current density is 0.3A/dm 2 。
The platinum plating layer formed on the probe in this example had a thickness of 3. Mu.m.
Example 10
The embodiment provides an integrated voltage-equalizing electrode, and the preparation method thereof comprises the following steps:
step 1 and step 2 are the same as in example 1.
And step 3, placing the probe of the voltage equalizing electrode to be plated in electroplating solution, electroplating, and forming a platinum coating on the surface of the stainless steel probe.
Specifically, the voltage of the regulated power supply is controlled to be 0.3V, and the voltage-equalizing electrode to be plated is used as a working electrode and connected with a cathode. An annular platinum sheet with a diameter of 8mm and a height of 150mm was used as a counter electrode to connect the anode. The probe of the voltage equalizing electrode to be plated is placed in the middle of the annular platinum sheet and is immersed in the electroplating liquid in an electrified manner.
Wherein the plating solution comprises water, 6g/L of diammine platinum dichloride, 16g/L of ammonium chloride and 66g/L of ammonium hydroxide, and the pH value is 8.9.
In the electroplating treatment, the temperature of the electrolyte is 16 ℃, and the cathode current density is 0.4A/dm 2 。
The platinum plating layer formed on the probe in this example had a thickness of 2.5. Mu.m.
Comparative example 1
In the voltage equalizing electrode of the comparative example, the probe was made of platinum metal, and the probe was not subjected to plating treatment.
The overall shape and dimensions of the probes were uniform in the voltage-equalizing electrodes prepared in examples 1 to 10 and the voltage-equalizing electrode in comparative example 1, and were cylindrical with a diameter of 2mm and a length of 30 mm.
And installing the voltage equalizing electrode in an experimental device of a simulated high-voltage direct-current transmission converter valve cooling system, and simultaneously working. After 180 days of operation, the probe was taken out, and the scaling amount on the surface of the probe and the maximum thickness of the scaling layer were measured. The measurement results are shown in table 1.
TABLE 1
| Amount of fouling of probe surface (mg) | Maximum thickness (mm) of scale layer | |
| Example 1 | 56.2 | 0.05 |
| Example 2 | 41.3 | 0.04 |
| Example 3 | 57.4 | 0.07 |
| Example 4 | 45.9 | 0.09 |
| Example 5 | 84.2 | 0.06 |
| Example 6 | 92.1 | 0.03 |
| Example 7 | 79.5 | 0.07 |
| Example 8 | 64.3 | 0.04 |
| Example 9 | 89.5 | 0.06 |
| Example 10 | 43.7 | 0.03 |
| Comparative example 1 | 376.1 | 0.38 |
In the voltage-sharing electrode, the probe comprises the probe matrix and the platinum layer arranged on the surface of the probe matrix, the integrated formation of the probe matrix and the base has the characteristics of good mechanical property and high tangential impact resistance, the risk of breakage caused by water flow acting force at the joint of the probe and the base can be reduced, and meanwhile, the platinum layer is arranged on the surface of the probe matrix, so that the voltage-sharing electrode and the pure platinum probe voltage-sharing electrode have the same chemical and electrochemical stability, and the voltage-sharing electrode can be applied to a cooling system of a high-voltage direct-current transmission converter valve.
Further, the platinum layer is preferably formed by electroplating platinum on the probe substrate, so that the surface smoothness of the platinum probe can be improved, and the nucleation and growth of aluminum hydroxide on the surface of the platinum probe can be slowed down, so that the effect of slowing down the scaling on the surface of the platinum probe can be achieved.
The technical features of the above-described embodiments may be arbitrarily combined, and all possible combinations of the technical features in the above-described embodiments are not described for brevity of description, however, as long as there is no contradiction between the combinations of the technical features, they should be considered as the scope of the description.
The above examples illustrate only a few embodiments of the invention, which are described in detail and are not to be construed as limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.
Claims (10)
1. The voltage equalizing electrode is characterized by comprising a base and a probe arranged on the base, wherein the probe comprises a probe matrix and a platinum layer arranged on the surface of the probe matrix, and the probe matrix and the base are integrally formed.
2. The voltage-sharing electrode according to claim 1, wherein the probe base and the base are made of stainless steel; and/or
A nickel layer is arranged between the probe matrix and the platinum layer.
3. The voltage-equalizing electrode according to claim 1, wherein the thickness of the platinum layer is 0.5 μm to 5 μm.
4. The voltage-grading electrode according to claim 1, wherein the platinum layer is formed by a platinating treatment.
5. A method of producing a voltage-equalizing electrode according to any one of claims 1 to 4, comprising the steps of:
preparing an integrally formed base and a probe matrix;
immersing the probe substrate in an electroplating solution, and carrying out electroplating platinum treatment on the probe substrate to form a platinum layer on the surface of the probe substrate.
6. The method of manufacturing according to claim 5, wherein the plating solution comprises: water, dichloro diammine platinum and/or dichloro dihydroxy diammine platinum with the concentration of 5-30 g/L, ammonium chloride with the concentration of 10-27 g/L and ammonium hydroxide with the concentration of 7-68 g/L.
7. The method according to claim 5, wherein the pH of the plating solution is 8.9 to 9.3.
8. The method according to claim 5, wherein the temperature of the plating solution is controlled to be 5 ℃ to 20 ℃ during the platinum plating treatment.
9. The method according to claim 5, wherein the cathode current density of the platinum plating treatment is 0.1A/dm 2 ～0.5A/dm 2 。
10. The method according to any one of claims 5 to 9, wherein before the platinum plating treatment is performed on the probe substrate, the method further comprises the steps of:
performing nickel pre-plating treatment on the probe matrix;
optionally, before the probe substrate is subjected to the nickel pre-plating treatment, the preparation method further comprises the following steps:
and sequentially carrying out alkali degreasing treatment, acid dipping treatment and acid activation treatment on the probe matrix.
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