CN109321964A - A kind of plating production technology of high purity sulphur nickel anode - Google Patents
A kind of plating production technology of high purity sulphur nickel anode Download PDFInfo
- Publication number
- CN109321964A CN109321964A CN201811194524.3A CN201811194524A CN109321964A CN 109321964 A CN109321964 A CN 109321964A CN 201811194524 A CN201811194524 A CN 201811194524A CN 109321964 A CN109321964 A CN 109321964A
- Authority
- CN
- China
- Prior art keywords
- nickel
- sulfur
- production technology
- anode
- metal sulfide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0089—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with other, not previously mentioned inorganic compounds as the main non-metallic constituent, e.g. sulfides, glass
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D17/00—Constructional parts, or assemblies thereof, of cells for electrolytic coating
- C25D17/10—Electrodes, e.g. composition, counter electrode
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Mechanical Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Inorganic Chemistry (AREA)
- Electroplating And Plating Baths Therefor (AREA)
- Sliding-Contact Bearings (AREA)
Abstract
The invention belongs to sulfur-bearing nickel material manufacturing field, in particular to a kind of plating production technology of high purity sulphur nickel anode, step includes selecting metal sulfide according to target sulphur content demand；Metal sulfide is made an addition in nickel, is then the crude product of the sulfur-bearing nickel material with certain sulfur content with vacuum induction melting；The scaling loss amount for recording sulphur is added metal sulfide in crude product and compensates to blow-on additive amount, is then heat-treated, obtains sulfur-bearing nickel material；According to anode construction by sulfur-bearing nickel material machine-shaping.The present invention can manufacture the nickel anode of nickel content purity 99.9wt%, and anode material obtained is highly suitable for the electronickelling occasion of coating film thickness 1nm~100um.
Description
Technical field
The invention belongs to sulfur-bearing nickel material manufacturing field, in particular to a kind of plating production works of high purity sulphur nickel anode
Skill.
Background technique
In Bright Nickel Electroplating field, if dissolubility is poor with pure nickel as anode, be easy passivation, it is not easy to allow plating in nickel
Ion concentration is maintained at preferable states in 100~400ppm.Sulfur-bearing nickel material is primarily used to the active anode of electronickelling industry
Material.Since tank voltage can be effectively reduced using sulfur-bearing nickel anode, deposition velocity and electroplating efficiency are improved, avoids being electrolysed containing chlorine
The corrosion of equipment caused by liquid system, and obtain the advantages such as low stress coating becomes active nickel anode most popular in the world
Material.
Current trial in the world is prepared there are mainly two types of the methods of sulfur-bearing nickel: first is that using containing=C-SO2Group has
Machine object is the mode of the electrolysis of sulphur source, i.e., addition contains=C-SO in the electrolytic solution2The organics additive of group, makes element sulphur
It is gradually reduced and is deposited on Ni substrate；Second is that making nickel element sulphur logical under gaseous state by the way of vapor deposition
Decomposition deposition is crossed to form sulfur-bearing nickel material.There are the unstable quality of sulfur-bearing nickel in production process, sulfur content is difficult to control
The problems such as.
Chinese patent application CN102071441A, which is disclosed, a kind of manufactures sulfur-bearing nickel material, sulfur-bearing using electrochemical method
Amount is can be controlled in 0.02~0.2% range.But for the nickel thin-film technique of 1nm~100um very narrow thickness to be manufactured,
This sulfur content is still higher.
Summary of the invention
The main object of the present invention is to provide for a kind of production technology of plating high purity sulphur nickel anode, can prepare one
Kind is suitble to the sulphur nickel anode material of the nickel film of plating 1nm~100um thickness.
The present invention is achieved through the following technical solutions above-mentioned purpose: a kind of plating production technology of high purity sulphur nickel anode,
Include the following steps:
1. selecting metal sulfide according to target sulphur content demand；
It is then with certain sulfur content with vacuum induction melting 2. the metal sulfide of step 1. is made an addition in nickel
The crude product of sulfur-bearing nickel material；
3. recording the scaling loss amount of sulphur, the metal sulfide of step 1. is added in step 2. resulting crude product and compensates to blow-on
Then additive amount is heat-treated, sulfur-bearing nickel material is obtained；
4. according to anode construction by sulfur-bearing nickel material machine-shaping.
Specifically, the metal sulfide uses one of nickel sulfide, copper sulfide, ferrous sulfide, iron sulfide.
Further, the sulfur content in the metal sulfide accounts for 1~50ppm of gross weight.
Specifically, the vacuum induction melting is using non-oxidizing gas as protective gas.
Further, the protective gas is nitrogen.
Specifically, 600~1000 DEG C of the heat treatment temperature, the processing time is 0.5~2.5hr.
Compared with prior art, the beneficial effects of the present invention are:
The present invention can manufacture the nickel anode of nickel content purity 99.9wt%, and anode material obtained is highly suitable for plating film thickness
Spend the electronickelling occasion of 1nm~100um.
Specific embodiment
The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention..
Examples 1 to 4
Nickel anode is manufactured using following steps:
1. selecting metal sulfide according to the sulfur content demand of 1~50ppm, metal sulfide uses nickel sulfide, copper sulfide, sulphur
Change one of ferrous, iron sulfide or a variety of.
2. metal sulfide is made an addition in nickel, then it is the crude product of sulfur-bearing nickel material with vacuum induction melting, that is, passes through
Using electromagnetic inductive heating principle come melting nickel, is melted with current vortex by nickel, disperse sulfur-bearing ingredient in nickel.
3. recording the scaling loss amount of sulphur, metal sulfide is added in crude product and compensates to blow-on additive amount, then 600~
In 1000 DEG C of temperature, 0.5~2.5hr of heat treatment is carried out, the distribution of sulphur is allowed to homogenize, obtains sulfur-bearing nickel material.
4. according to anode construction by sulfur-bearing nickel material machine-shaping.
Because vacuum induction melting cannot allow nickel to aoxidize, non-oxidizing gas can be used as protective gas, preferably
For low-cost nitrogen.
The additional amount of the raw material of each embodiment is as shown in table 1:
Table 1:
Use the nickel anode of CN102071441A contained technology manufacture as reference examples, by nickel anode obtained by Examples 1 to 4 and
Reference examples are compared experiment, the results are shown in Table 2.
Table 2:
As shown in Table 2, using the nickel anode sulfur content error of this technique manufacture between ± 5ppm, more than the prior art
Accurately.And it can more easily manufacture the electronickelling film of 1nm~100um very narrow thickness.Since sulfur-bearing can promote anode
Stability keeps film forming uniform more preferably, and film film thickness can be measured by AFM (atomic force analysis microscope).
Above-described is only some embodiments of the present invention.For those of ordinary skill in the art, not
Under the premise of being detached from the invention design, various modifications and improvements can be made, these belong to protection model of the invention
It encloses.
Claims (6)
1. the production technology that high purity sulphur nickel anode is used in a kind of plating, characterized by the following steps:
1. selecting metal sulfide according to target sulphur content demand；
It is then the sulfur-bearing with certain sulfur content with vacuum induction melting 2. the metal sulfide of step 1. is made an addition in nickel
The crude product of nickel material；
3. recording the scaling loss amount of sulphur, the metal sulfide of step 1. is added in step 2. resulting crude product and compensates to blow-on addition
Amount, is then heat-treated, obtains sulfur-bearing nickel material；
4. according to anode construction by sulfur-bearing nickel material machine-shaping.
2. production technology according to claim 1, it is characterised in that: the metal sulfide using nickel sulfide, copper sulfide,
One of ferrous sulfide, iron sulfide are a variety of.
3. production technology according to claim 1 or 2, it is characterised in that: the sulfur content in the metal sulfide accounts for always
1~50ppm of weight.
4. production technology according to claim 1, it is characterised in that: the vacuum induction melting is with non-oxidizing gas
Protective gas.
5. production technology according to claim 4, it is characterised in that: the protective gas is nitrogen.
6. production technology according to claim 1, it is characterised in that: 600~1000 DEG C of the heat treatment temperature, when processing
Between be 0.5~2.5hr.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811194524.3A CN109321964A (en) | 2018-10-15 | 2018-10-15 | A kind of plating production technology of high purity sulphur nickel anode |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811194524.3A CN109321964A (en) | 2018-10-15 | 2018-10-15 | A kind of plating production technology of high purity sulphur nickel anode |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109321964A true CN109321964A (en) | 2019-02-12 |
Family
ID=65261995
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811194524.3A Pending CN109321964A (en) | 2018-10-15 | 2018-10-15 | A kind of plating production technology of high purity sulphur nickel anode |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109321964A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112410830A (en) * | 2020-11-19 | 2021-02-26 | 金川集团股份有限公司 | Auxiliary agent bag for promoting uniform dissolution of nickel anode in electroplating and use method thereof |
-
2018
- 2018-10-15 CN CN201811194524.3A patent/CN109321964A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112410830A (en) * | 2020-11-19 | 2021-02-26 | 金川集团股份有限公司 | Auxiliary agent bag for promoting uniform dissolution of nickel anode in electroplating and use method thereof |
| CN112410830B (en) * | 2020-11-19 | 2023-06-13 | 金川集团股份有限公司 | Auxiliary agent bag for promoting nickel anode to be uniformly dissolved in electroplating and use method thereof |
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| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190212 |
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| RJ01 | Rejection of invention patent application after publication |