CN102071441A - Method for preparing material containing sulfur and nickel - Google Patents
Method for preparing material containing sulfur and nickel Download PDFInfo
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- CN102071441A CN102071441A CN 201010595789 CN201010595789A CN102071441A CN 102071441 A CN102071441 A CN 102071441A CN 201010595789 CN201010595789 CN 201010595789 CN 201010595789 A CN201010595789 A CN 201010595789A CN 102071441 A CN102071441 A CN 102071441A
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- nickel
- sulfur
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- electroplating
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 171
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 80
- 239000011593 sulfur Substances 0.000 title claims abstract description 57
- 229910052717 sulfur Inorganic materials 0.000 title claims abstract description 57
- 239000000463 material Substances 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 17
- 238000009713 electroplating Methods 0.000 claims abstract description 20
- 238000002360 preparation method Methods 0.000 claims abstract description 14
- 150000001875 compounds Chemical class 0.000 claims abstract description 8
- 229910001453 nickel ion Inorganic materials 0.000 claims abstract description 3
- 238000005234 chemical deposition Methods 0.000 claims abstract 4
- 238000004070 electrodeposition Methods 0.000 claims abstract 4
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 claims abstract 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 4
- DPLVEEXVKBWGHE-UHFFFAOYSA-N potassium sulfide Chemical compound [S-2].[K+].[K+] DPLVEEXVKBWGHE-UHFFFAOYSA-N 0.000 claims description 4
- 239000010936 titanium Substances 0.000 claims description 4
- UYJXRRSPUVSSMN-UHFFFAOYSA-P ammonium sulfide Chemical compound [NH4+].[NH4+].[S-2] UYJXRRSPUVSSMN-UHFFFAOYSA-P 0.000 claims description 3
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 3
- 229910052979 sodium sulfide Inorganic materials 0.000 claims description 3
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims description 3
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims description 2
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 2
- 239000007770 graphite material Substances 0.000 claims description 2
- 229910000037 hydrogen sulfide Inorganic materials 0.000 claims description 2
- 229910001220 stainless steel Inorganic materials 0.000 claims description 2
- 239000010935 stainless steel Substances 0.000 claims description 2
- 229910001200 Ferrotitanium Inorganic materials 0.000 claims 1
- -1 nickel fluoroborate Chemical compound 0.000 claims 1
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims 1
- KERTUBUCQCSNJU-UHFFFAOYSA-L nickel(2+);disulfamate Chemical compound [Ni+2].NS([O-])(=O)=O.NS([O-])(=O)=O KERTUBUCQCSNJU-UHFFFAOYSA-L 0.000 claims 1
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims 1
- 238000000151 deposition Methods 0.000 abstract description 7
- 230000005684 electric field Effects 0.000 abstract description 3
- 239000000047 product Substances 0.000 abstract description 3
- 239000007795 chemical reaction product Substances 0.000 abstract description 2
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- 238000005580 one pot reaction Methods 0.000 abstract 1
- 239000005864 Sulphur Substances 0.000 description 22
- 239000000243 solution Substances 0.000 description 18
- 238000007747 plating Methods 0.000 description 12
- 239000007788 liquid Substances 0.000 description 8
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 8
- 230000008021 deposition Effects 0.000 description 6
- 239000010405 anode material Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000007772 electroless plating Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 2
- 150000002815 nickel Chemical class 0.000 description 2
- DITXJPASYXFQAS-UHFFFAOYSA-N nickel;sulfamic acid Chemical compound [Ni].NS(O)(=O)=O DITXJPASYXFQAS-UHFFFAOYSA-N 0.000 description 2
- 238000003672 processing method Methods 0.000 description 2
- 235000010265 sodium sulphite Nutrition 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 206010017472 Fumbling Diseases 0.000 description 1
- ZGSDJMADBJCNPN-UHFFFAOYSA-N [S-][NH3+] Chemical compound [S-][NH3+] ZGSDJMADBJCNPN-UHFFFAOYSA-N 0.000 description 1
- XAQHXGSHRMHVMU-UHFFFAOYSA-N [S].[S] Chemical compound [S].[S] XAQHXGSHRMHVMU-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 239000007792 gaseous phase Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- NPURPEXKKDAKIH-UHFFFAOYSA-N iodoimino(oxo)methane Chemical compound IN=C=O NPURPEXKKDAKIH-UHFFFAOYSA-N 0.000 description 1
- DYJOUBLHPAIUEU-UHFFFAOYSA-N nickel(2+) sulfane Chemical compound S.[Ni+2] DYJOUBLHPAIUEU-UHFFFAOYSA-N 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Electroplating Methods And Accessories (AREA)
Abstract
一种含硫镍材料的制备方法，是在含镍电镀液的电镀体系中，将含硫化合物溶液滴入电镀液中阴极板附近；含硫化合物与电镀液中的镍离子按式S2-+Ni2+→NiS↓直接一步反应：在阴极板上，NiS化学沉积与镍的电沉积同时进行，制备出含硫镍材料。反应产物NiS沉积在阴极上；同时，在电镀过程中镍在电场作用下在阴极上不断的电沉积，即NiS的化学沉积与镍的电沉积同时进行，从而制备出含硫镍材料。本发明工艺简单、操作方便，通过选择新的含S化合物硫源，采用硫的化学沉积和镍的电沉积的共沉积方式制备含硫镍材料，有利于控制含硫镍材料的硫含量，解决了当前含硫镍材料的难制备以及含硫量难以控制的问题，产品质量稳定，工艺流程短，可实现规模化生产。A kind of preparation method of sulfur-containing nickel material is that in the electroplating system of nickel-containing electroplating solution, the sulfur-containing compound solution is dropped into the vicinity of the cathode plate in the electroplating solution; the sulfur-containing compound and nickel ions in the electroplating solution are expressed according to the formula S 2- +Ni 2+ →NiS↓ direct one-step reaction: On the cathode plate, the chemical deposition of NiS and the electrodeposition of nickel are carried out simultaneously to prepare sulfur-containing nickel materials. The reaction product NiS is deposited on the cathode; at the same time, nickel is continuously electrodeposited on the cathode under the action of an electric field during the electroplating process, that is, the chemical deposition of NiS is carried out simultaneously with the electrodeposition of nickel, thereby preparing a sulfur-containing nickel material. The invention has simple process and convenient operation. By selecting a new sulfur source of S-containing compound and adopting the co-deposition method of chemical deposition of sulfur and electrodeposition of nickel to prepare sulfur-containing nickel material, it is beneficial to control the sulfur content of the sulfur-containing nickel material and solve the problem of The problem of difficult preparation of sulfur-containing nickel materials and difficult control of sulfur content is solved, the product quality is stable, the process flow is short, and large-scale production can be realized.
Description
Technical field
The invention discloses a kind of preparation method of sulfur-bearing nickel material, specifically be meant a kind of method that adopts sedimentary mode behind the nickel sulfonium ion direct reaction to prepare active sulfur-bearing nickel anode material.Belong to technical field of electrochemistry.
Background technology
The sulfur-bearing nickel material mainly is the active anode material as electronickelling industry.Owing to adopt the sulfur-bearing nickel anode can effectively reduce bath voltage, improve sedimentation velocity and electroplating efficiency, the equipment corrosion of avoiding chloride electrolyte system to cause, and obtain advantage such as low-stress coating, become most popular in the world active nickel anode material.
Canada INCO company has monopolized the world market of this product since having developed sulfur-bearing nickel active anode material.To its production technology, particularly to taking strict secrecy provision for sulphur sulphur source.China still is in the stage of fumbling to the production technology of sulfur-bearing nickel at present.The method that current trial in the world prepares sulfur-bearing nickel mainly contains two kinds: the one, adopt to contain=C-SO
2The organism of-group is the electrolytic mode in sulphur source, promptly adds to contain=C-SO in electrolytic solution
2The organics additive of-group progressively is reduced element sulphur and is deposited on the Ni substrate; The 2nd, adopt the mode of vapour deposition, thereby promptly under gaseous phase, make the nickel element sulphur form the sulfur-bearing nickel material by decomposing deposition.Have the quality instability of sulfur-bearing nickel in the production process, sulphur content is difficult to problems such as control.
Summary of the invention
The object of the present invention is to provide that a kind of processing method is simple, easy to operate, technical process is short, be the sulphur source to contain the S compound, by the method for nickel element sulphur direct chemical prepared in reaction sulfur-bearing nickel material in electroplating solution.
The preparation method of a kind of sulfur-bearing nickel material of the present invention is to adopt following proposal to realize:
A kind of preparation method of sulfur-bearing nickel material is in containing the plating system of nickel plating solution, and sulfocompound solution is splashed in the electroplate liquid near the negative plate; On negative plate, the galvanic deposit of NiS electroless plating and nickel is carried out simultaneously, prepares the sulfur-bearing nickel material.
Among the preparation method of a kind of sulfur-bearing nickel material of the present invention, the anode of described plating system adopts metallic nickel or graphite material; Described negative electrode adopts metal titanium or stainless material; Described cathode current density is controlled at 5～10A/dm
2Describedly contain that nickel concentration is 30～100g/L in the nickel plating solution.
Among the preparation method of a kind of sulfur-bearing nickel material of the present invention, the described nickel plating solution that contains is selected from least a in single nickel salt, nickelous chloride, nickel sulfamic acid, the nickel fluoborate solution.
Among the preparation method of a kind of sulfur-bearing nickel material of the present invention, described sulfocompound is selected from least a in hydrogen sulfide, sodium sulphite, potassium sulphide, the ammonium sulfide.
Among the preparation method of a kind of sulfur-bearing nickel material of the present invention, the concentration of described sulfocompound solution is controlled at 0.001～0.01mol/L, and near its rate of addition negative plate is controlled at 0.04～0.2L/dm
2H; The massfraction of the sulphur of the sulfur-bearing nickel material of preparation is 0.02%～0.2%.
The present invention is owing to adopt above-mentioned processing method, and sulfocompound is fed in the electroplate liquid near the negative plate, and under electric field action, the nickel ion in sulfocompound and the electroplate liquid is pressed the direct single step reaction of following formula:
S
2-+Ni
2+→NiS↓
Reaction product NiS is deposited on the negative electrode; Simultaneously, nickel constantly galvanic deposit on negative electrode under electric field action in electroplating process, i.e. the galvanic deposit of the electroless plating of NiS and nickel is carried out simultaneously, thereby prepares the sulfur-bearing nickel material.
By nickel concentration and current density in the control plating bath, with negative electrode and anode water placing flat, the plating of negative electrode is faced up, can on the plating face of negative electrode, obtain the sulfur-bearing nickel material.
The process of the galvanic deposit by the control electroless plating of NiS and nickel is promptly controlled current density, the bath concentration of electroplating process, the addition and the interpolation speed of sulfocompound, can realize effective control of the sulphur content in the sulfur-bearing nickel material.Wherein: current density, bath concentration are according to the nickel content M in the sulfur-bearing nickel material of design
NiCalculate; Because, M
Ni=KQ, K is the electrochemical equivalent of electric deposition nickel, is a constant, promptly 1.095, Q is the ampere-hour number of electroplating process; Therefore, as nickel content M
NiAfter determining, the ampere-hour number of electroplating process can determine, thereby, can determine corresponding current density and electroplating time.After the volume of plating tank is determined, promptly can be according to the nickel content M in the sulfur-bearing nickel material of design
Ni, calculate the initial concentration of electroplate liquid, require the initial concentration of electroplate liquid to separate out M in galvanic deposit
NiAfter, still can keep the works better of the system of electroplating.Conversion obtains the addition of sulfocompound according to the sulphur content in the sulfur-bearing nickel material of design equally; After the addition and electroplating time of determining sulfocompound, then can determine the concentration of sulfocompound solution according to the interpolation speed of being convenient to control.Thereby realize controlling more accurately within the specific limits the sulphur content in the prepared sulfur-bearing nickel material.
In sum; technology of the present invention is simple, easy to operate; by selecting the new S compound sulphur source that contains, adopt the codeposition mode of the galvanic deposit of the electroless plating of sulphur and nickel to prepare the sulfur-bearing nickel material, help controlling the sulphur content of sulfur-bearing nickel material; the difficulty preparation and the unmanageable problem of sulphur content of current sulfur-bearing nickel material have been solved; the sulfur-bearing nickel material of preparing, its sulphur content can be controlled in 0.02%～0.2% scope, constant product quality; technical process is short, can accomplish scale production.
Embodiment
Embodiment 1
Adopt the galvanized mode of solution, adopt the metal nickel plate plate at anode, electroplate liquid adopts single nickel salt and nickel fluoborate to press 1: 2 blended solution of mass ratio, nickel concentration is controlled at 90～100g/L, negative electrode adopts stainless steel plate, the equal horizontal positioned of negative electrode and anode, the plating of negative electrode faces up, and current density is controlled at 9～10A/dm
2Sodium sulphite is selected in the sulphur source, and sodium sulfide solution feeds near the negative electrode with pipeline, and the concentration of sodium sulfide solution is controlled at 0.001～0.002mol/L, and near its rate of addition negative plate is controlled at 0.04～0.06L/dm
2H after the deposition of 100Ah, obtains gross weight and is about 105 grams, and sulphur content is 0.02%～0.04% sulfur-bearing nickel material.
Embodiment 2
Adopt the galvanized mode of solution, anode adopts metal nickel plate, and electroplate liquid adopts nickel sulfamic acid solution, nickel concentration is controlled at 50～60g/L, and negative electrode adopts metallic titanium plate, the equal horizontal positioned of negative electrode and anode, the plating of negative electrode faces up, and current density is controlled at 5～8A/dm
2Sodium sulphite and potassium sulphide are selected in the sulphur source, sodium sulphite and potassium sulphide are pressed 1: 1 blended aqueous solution of mass ratio with near the pipeline feeding negative electrode, the total concn of element sulphur is controlled at 0.004～0.006mol/L in the solution, and near its rate of addition negative plate is controlled at 0.05～0.15L/dm
2H after the deposition of 500Ah, obtains gross weight and is about 540 grams, and sulphur content is 0.08%～0.12% sulfur-bearing nickel material.
Embodiment 3
Adopt the galvanized mode of solution, anode adopts graphite cake, and electroplate liquid adopts nickel chloride solution, nickel concentration is controlled at 30～40g/L, and negative electrode adopts metallic titanium plate, the equal horizontal positioned of negative electrode and anode, the plating of negative electrode faces up, and current density is controlled at 7～10A/dm
2Ammonium sulfide is selected in the sulphur source, and the aqueous solution of ammonium sulfide is fed near the negative electrode with pipeline, and the total concn of element sulphur is controlled at 0.009～0.01mol/L in the solution, and near its rate of addition negative plate is controlled at 0.06～0.1L/dm
2H after the deposition of 800Ah, obtains gross weight and is about 870 grams, and sulphur content is 0.18%～0.2% sulfur-bearing nickel material.
Claims (5)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010595789 CN102071441A (en) | 2010-12-20 | 2010-12-20 | Method for preparing material containing sulfur and nickel |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010595789 CN102071441A (en) | 2010-12-20 | 2010-12-20 | Method for preparing material containing sulfur and nickel |
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| Publication Number | Publication Date |
|---|---|
| CN102071441A true CN102071441A (en) | 2011-05-25 |
Family
ID=44030191
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201010595789 Pending CN102071441A (en) | 2010-12-20 | 2010-12-20 | Method for preparing material containing sulfur and nickel |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106623969A (en) * | 2016-11-23 | 2017-05-10 | 昆明理工大学 | Method of preparing nanometer nickel-sulfur alloy through replacement deposition of low eutectic ionic liquid |
| CN107723769A (en) * | 2017-10-24 | 2018-02-23 | 宝鸡市铭坤有色金属有限公司 | A kind of preparation method of nano-crystal nickel material |
| CN109023440A (en) * | 2018-09-04 | 2018-12-18 | 中国科学院兰州化学物理研究所 | Utilize the carbon-free method taken sulphur agent and prepare sulfur-bearing nickel material |
| CN112323096A (en) * | 2020-09-23 | 2021-02-05 | 河北东恩企业管理咨询有限公司 | Preparation method of sulfur-nickel-containing round cake |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0285385A (en) * | 1988-09-22 | 1990-03-26 | Tosoh Corp | Electrode manufacturing method |
| JPH02163392A (en) * | 1988-12-15 | 1990-06-22 | Tosoh Corp | Electrode manufacturing method |
| CN1844462A (en) * | 2006-03-16 | 2006-10-11 | 郑州大学 | Nickel-sulfur active hydrogen evolution cathode with gradient structure and preparation method thereof |
-
2010
- 2010-12-20 CN CN 201010595789 patent/CN102071441A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0285385A (en) * | 1988-09-22 | 1990-03-26 | Tosoh Corp | Electrode manufacturing method |
| JPH02163392A (en) * | 1988-12-15 | 1990-06-22 | Tosoh Corp | Electrode manufacturing method |
| CN1844462A (en) * | 2006-03-16 | 2006-10-11 | 郑州大学 | Nickel-sulfur active hydrogen evolution cathode with gradient structure and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 《天津大学学报》 19911231 覃齐贤等 镍-硫化镍复合物析氢活性阴极的研究 80-84 1-5 , 2 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106623969A (en) * | 2016-11-23 | 2017-05-10 | 昆明理工大学 | Method of preparing nanometer nickel-sulfur alloy through replacement deposition of low eutectic ionic liquid |
| CN107723769A (en) * | 2017-10-24 | 2018-02-23 | 宝鸡市铭坤有色金属有限公司 | A kind of preparation method of nano-crystal nickel material |
| CN109023440A (en) * | 2018-09-04 | 2018-12-18 | 中国科学院兰州化学物理研究所 | Utilize the carbon-free method taken sulphur agent and prepare sulfur-bearing nickel material |
| CN112323096A (en) * | 2020-09-23 | 2021-02-05 | 河北东恩企业管理咨询有限公司 | Preparation method of sulfur-nickel-containing round cake |
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Application publication date: 20110525 |