CN108917579B - Reagent for detecting thickness of chemical nickel plating on copper by coulombic method - Google Patents
Reagent for detecting thickness of chemical nickel plating on copper by coulombic method Download PDFInfo
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- CN108917579B CN108917579B CN201810812448.1A CN201810812448A CN108917579B CN 108917579 B CN108917579 B CN 108917579B CN 201810812448 A CN201810812448 A CN 201810812448A CN 108917579 B CN108917579 B CN 108917579B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- G01B7/00—Measuring arrangements characterised by the use of electric or magnetic techniques
- G01B7/02—Measuring arrangements characterised by the use of electric or magnetic techniques for measuring length, width or thickness
- G01B7/06—Measuring arrangements characterised by the use of electric or magnetic techniques for measuring length, width or thickness for measuring thickness
Abstract
The invention discloses a reagent for detecting the thickness of chemical nickel plating on copper by a coulometry method, which comprises ammonium thiocyanate, potassium iodide, potassium thiocyanate and potassium carbonate. At normal temperature, dissolving 30-50 g of ammonium thiocyanate, 30-40 g of potassium iodide, 90-360 g of potassium thiocyanate and 30-50 g of potassium carbonate in 1ml of water, mixing, and fully dissolving; and preparing the reagent for detecting the thickness of the chemical nickel plating on the copper by the coulomb method. The reagent provided by the invention has high stability, and can accurately detect the thickness of the chemical nickel plating on copper.
Description
Technical Field
The invention relates to the field of chemical detection, in particular to a reagent for detecting the thickness of chemical nickel plating on copper by a coulomb method.
Background
Chemical nickel plating has many advantages as a novel environment-friendly surface treatment technology, has very good electroplating uniformity, is particularly suitable for workpieces with high precision, and can achieve very high hardness through heat treatment after plating. In the prior art, the following three common plating layer thickness detection methods are available: a. detecting by a metallographic method; b. detecting by ray method; c. the coulometric method is to measure the thickness by electrolysis.
a. The method of the metallographic microscope has the advantages that all conditions have high measurement precision, the defects are obvious, and much time is spent on cutting, polishing, microscopic measurement and pretreatment. b. The ray detection has the advantages of high measurement speed and high detection precision below 10 microns. The disadvantage is high cost. c. The electrolytic thickness gauge is a coulometric thickness gauge, and other formula reagents have no obvious potential change until the base material is electrolyzed in the application of the electrolytic thickness gauge, so that the test end cannot be judged, and an accurate detection result cannot be obtained.
In view of the above-mentioned drawbacks, the inventors of the present invention have finally obtained the present invention through a long period of research and practice.
Disclosure of Invention
In order to solve the technical defects, the invention adopts the technical scheme that a reagent for detecting the thickness of chemical nickel plating on copper by a coulometry method is provided, and is characterized by comprising ammonium thiocyanate, potassium iodide, potassium thiocyanate and potassium carbonate.
Preferably, at normal temperature, dissolving 30-50 g of ammonium thiocyanate, 30-40 g of potassium iodide, 90-360 g of potassium thiocyanate and 30-50 g of potassium carbonate in 1L of water, mixing, and fully dissolving; and preparing the reagent for detecting the thickness of the chemical nickel plating on the copper by the coulomb method.
Preferably, the current of the coulometric electrolytic thickness gauge is set as follows: 20mA, current density set to: 407mA/cm2。
Preferably, the reagent contains 30 grams of the ammonium thiocyanate, 40 grams of the potassium iodide, 180 grams of the potassium thiocyanate and 30 grams of the potassium carbonate per liter of reagent.
Preferably, each liter of the reagent contains 50 g of ammonium thiocyanate, 40 g of potassium iodide, 200 g of potassium thiocyanate and 50 g of potassium carbonate.
Preferably, each liter of the reagent contains 50 g of ammonium thiocyanate, 40 g of potassium iodide, 200 g of potassium thiocyanate and 50 g of potassium carbonate.
Preferably, each liter of the reagent contains 30 g of ammonium thiocyanate, 40 g of potassium iodide, 200 g of potassium thiocyanate and 30 g of potassium carbonate.
Preferably, each liter of the reagent contains 30 g of ammonium thiocyanate, 30 g of potassium iodide, 160 g of potassium thiocyanate and 40 g of potassium carbonate.
Preferably, each liter of the reagent contains 30 g of ammonium thiocyanate, 40 g of potassium iodide, 360 g of potassium thiocyanate and 30 g of potassium carbonate.
Preferably, each liter of the reagent contains 30 g of ammonium thiocyanate, 40 g of potassium iodide, 90 g of potassium thiocyanate and 30 g of potassium carbonate.
Compared with the prior art, the invention has the beneficial effects that:
1, the reagent meets the requirements of GB/T4955-2005 electrolyte: does not react with the metal covering layer under the condition of no external current; when the cover layer is anodically dissolved to penetrate and the exposed substrate area is continuously increased, the electrode potential should undergo a detectable sharp change;
2, the reagent has high stability, and can accurately detect the thickness of the chemical nickel plating on the copper;
3, the reagent has low cost, simple preparation method and simple and convenient operation method during detection; the utilization rate of the reagent is effectively improved.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below.
FIG. 1 is a graph of the potential profile of a conventional universal reagent according to the present invention;
FIG. 2 shows the results of detection of the reagents described in examples 1 to 5 of the present invention;
FIG. 3 shows the results of detection of the reagent described in example 6 of the present invention;
FIG. 4 is a graph comparing the results of detection of 90 g of potassium thiocyanate, 180 g of potassium thiocyanate, and 360 g of potassium thiocyanate in the reagent according to the present invention;
FIG. 5 shows the results of two measurements of the conventional reagent A11 under the same conditions as those described in the present invention.
Detailed Description
The above and further features and advantages of the present invention are described in more detail below with reference to the accompanying drawings.
The national standard GB/T4955-2005\ ISO2177-2003 only has a general reagent for detecting a plating layer, and has no reagent for detecting chemical nickel plating by a coulomb method. The invention relates to a reagent for detecting the thickness of chemical nickel plating on copper by a coulomb method, which solves the problem that an electrolytic thickness gauge cannot accurately detect the chemical nickel plating on copper.
Certain domestic manufacturer utilizes the existing detection reagent to detect the thickness of the copper plating chemical nickel by a coulomb method, a machine gives a constant current of 20mA electrolytic plating layer, the metal nickel is dissolved in the reagent by electrolysis, but when the nickel is electrolyzed, the copper layer is electrolyzed, and no obvious potential change exists. The test potential trend graph is shown in fig. 1, and it can be seen from fig. 1 that the potential curve after electrolysis is messy and has poor stability, and the detection result cannot be accurately obtained by the existing method.
In the prior art, only two methods AB can be selected for detection under the condition that no test reagent can be matched, and the thickness of the electroless nickel plating on the copper can be quickly and accurately analyzed by matching the third detection method, namely the electrolytic thickness gauge.
Example 1
A reagent for detecting the thickness of chemical nickel plating on copper by a coulometry method comprises the following components in each liter of solution: 30 g of ammonium thiocyanate, 40 g of potassium iodide, 180 g of potassium thiocyanate and 30 g of potassium carbonate.
At normal temperature, 30 g of ammonium thiocyanate, 40 g of potassium iodide, 180 g of potassium thiocyanate and 30 g of potassium carbonate are dissolved in 1L of water, and the materials are fully dissolved and mixed; and preparing the reagent for detecting the thickness of the chemical nickel plating on the copper by the coulomb method.
The potassium thiocyanate has unstable chemical property at normal temperature, is easy to deliquesce in the air and absorbs a large amount of heat to reduce the temperature; and the ammonium thiocyanate and the potassium thiocyanate have certain dangers, so the ammonium thiocyanate and the potassium thiocyanate are stored in a shady, dry and well ventilated position to keep the container sealed; when in use, the operation is strictly carried out according to the operation rules.
The reagent used in the method is the same as the existing reagent.
The standard chemical nickel sheet with 6-8% of the content of KOCOUR phosphorus in the United states is tested, the thickness is 5.5 mu m +/-5%, and the constant current is given by an electrolytic thickness gauge: 20mA, current density: 407mA/cm2(ii) a The detection result is as follows: 5.297 μm.
The electrolytic nickel ion reacts with the reagent to generate nickel thiocyanate which is dissolved in the reagent. Equipotential with the medium when continuously electrolyzing the chemical nickel coating. When the copper substrate is electrolyzed, because the ion replacement potential of different media can be quickly pulled up, the machine can acquire the potential change and stop to obtain a reliable thickness result.
Example 2
A reagent for detecting the thickness of chemical nickel plating on copper by a coulometry method comprises the following components in each liter of solution: 40 g of ammonium thiocyanate, 30 g of potassium iodide, 180 g of potassium thiocyanate and 50 g of potassium carbonate.
Dissolving 40 g of ammonium cyanate, 30 g of potassium iodide, 180 g of potassium thiocyanate and 50 g of potassium carbonate in 1L of water at normal temperature, and fully dissolving and mixing; and preparing the reagent for detecting the thickness of the chemical nickel plating on the copper by the coulomb method.
The reagent used in the method is the same as the existing reagent.
The standard chemical nickel sheet with 6-8% of the content of KOCOUR phosphorus in the United states is tested, the thickness is 5.5 mu m +/-5%, and the constant current is given by an electrolytic thickness gauge: 20mA, current density: 407mA/cm2(ii) a The detection result is as follows: 5.310 μm.
Example 3
A reagent for detecting the thickness of chemical nickel plating on copper by a coulometry method comprises the following components in each liter of solution: 50 g of ammonium thiocyanate, 40 g of potassium iodide, 200 g of potassium thiocyanate and 50 g of potassium carbonate.
At normal temperature, 50 g of ammonium thiocyanate, 40 g of potassium iodide, 200 g of potassium thiocyanate and 50 g of potassium carbonate are dissolved in 1L of water, and then the materials are fully dissolved and mixed; and preparing the reagent for detecting the thickness of the chemical nickel plating on the copper by the coulomb method.
The reagent used in the method is the same as the existing reagent.
The standard chemical nickel sheet with 6-8% of the content of KOCOUR phosphorus in the United states is tested, the thickness is 5.5 mu m +/-5%, and the constant current is given by an electrolytic thickness gauge: 20mA, current density: 407mA/cm2(ii) a The detection result is as follows: 5.385 μm.
Example 4
A reagent for detecting the thickness of chemical nickel plating on copper by a coulometry method comprises the following components in each liter of solution: 50 g of ammonium thiocyanate, 40 g of potassium iodide, 200 g of potassium thiocyanate and 50 g of potassium carbonate.
At normal temperature, 50 g of ammonium thiocyanate, 40 g of potassium iodide, 200 g of potassium thiocyanate and 50 g of potassium carbonate are dissolved in 1L of water, and then the materials are fully dissolved and mixed; and preparing the reagent for detecting the thickness of the chemical nickel plating on the copper by the coulomb method.
The reagent used in the method is the same as the existing reagent.
The standard chemical nickel sheet with 6-8% of the content of KOCOUR phosphorus in the United states is tested, the thickness is 5.5 mu m +/-5%, and the constant current is given by an electrolytic thickness gauge: 20mA, current density: 407mA/cm2(ii) a The detection result is as follows: 5.497 μm.
Example 5
A reagent for detecting the thickness of chemical nickel plating on copper by a coulometry method comprises the following components in each liter of solution: 30 g of ammonium thiocyanate, 40 g of potassium iodide, 200 g of potassium thiocyanate and 30 g of potassium carbonate.
At normal temperature, 30 g of ammonium thiocyanate, 40 g of potassium iodide, 200 g of potassium thiocyanate and 30 g of potassium carbonate are dissolved in 1L of water, and the materials are fully dissolved and mixed; and preparing the reagent for detecting the thickness of the chemical nickel plating on the copper by the coulomb method.
The reagent used in the method is the same as the existing reagent.
Testing standard nickel sheet with 6-8% of phosphorus content in KOCOAR in USA, and measuring thickness5.5 μm. + -. 5%, the electrolytic thickness gauge gives a constant current of: 20mA, current density: 407mA/cm2(ii) a The detection result is as follows: 5.461 μm.
Example 6
A reagent for detecting the thickness of chemical nickel plating on copper by a coulometry method comprises the following components in each liter of solution: 30 g of ammonium thiocyanate, 30 g of potassium iodide, 160 g of potassium thiocyanate and 40 g of potassium carbonate.
At normal temperature, 30 g of ammonium thiocyanate, 30 g of potassium iodide, 160 g of potassium thiocyanate and 40 g of potassium carbonate are dissolved in 1L of water, and the materials are fully dissolved and mixed; and preparing the reagent for detecting the thickness of the chemical nickel plating on the copper by the coulomb method.
The reagent used in the method is the same as the existing reagent.
The standard chemical nickel sheet with 6-8% of the content of KOCOUR phosphorus in the United states is tested, the thickness is 5.5 mu m +/-5%, and the constant current is given by an electrolytic thickness gauge: 20mA, current density: 407mA/cm2(ii) a The detection result is as follows: 5.461 μm.
The potential diagram is shown in FIG. 2, and FIG. 2 shows the test results of examples 1-5. In the figure, the first point is the detection result of example 5, the second point is the detection result of example 2, the third point is the detection result of example 4, the fourth point is the detection result of example 3, and the fifth point is the detection result of example 1.
The test reagent meets the requirements of GB/T4955-2005 electrolyte: 1. does not react with the metal covering layer under the condition of no external current; 2. as the cover layer is anodically dissolved to penetrate and the exposed substrate area continues to increase, a detectable sharp change in the electrode potential should occur.
Example 7
A reagent for detecting the thickness of chemical nickel plating on copper by a coulometry method comprises the following components in each liter of solution: 30 g of ammonium thiocyanate, 40 g of potassium iodide, 360 g of potassium thiocyanate and 30 g of potassium carbonate.
At normal temperature, 30 g of ammonium thiocyanate, 40 g of potassium iodide, 360 g of potassium thiocyanate and 30 g of potassium carbonate are dissolved in 1L of water, and the materials are fully dissolved and mixed; and preparing the reagent for detecting the thickness of the chemical nickel plating on the copper by the coulomb method.
The reagent used in the method is the same as the existing reagent.
The standard chemical nickel sheet with 6-8% of the content of KOCOUR phosphorus in the United states is tested, the thickness is 5.5 mu m +/-5%, and the constant current is given by an electrolytic thickness gauge: 20mA, current density: 407mA/cm2(ii) a The detection result is as follows: 5.334 mu m; the test results are plotted in fig. 3.
The reagent has low cost, simple preparation method and simple and convenient operation method during detection; the utilization rate of the reagent is effectively improved.
Example 8
A reagent for detecting the thickness of chemical nickel plating on copper by a coulometry method comprises the following components in each liter of solution: 30 g of ammonium thiocyanate, 40 g of potassium iodide, 90 g of potassium thiocyanate and 30 g of potassium carbonate.
At normal temperature, 30 g of ammonium thiocyanate, 40 g of potassium iodide, 90 g of potassium thiocyanate and 30 g of potassium carbonate are dissolved in 1L of water, and the materials are fully dissolved and mixed; and preparing the reagent for detecting the thickness of the chemical nickel plating on the copper by the coulomb method.
The reagent used in the method is the same as the existing reagent.
The standard chemical nickel sheet with 6-8% of the content of KOCOUR phosphorus in the United states is tested, the thickness is 5.5 mu m +/-5%, and the constant current is given by an electrolytic thickness gauge: 20mA, current density: 407mA/cm2(ii) a The detection result is as follows: 5.703 μm. The test result curve is shown in fig. 4;
in the figure, the first point is the detection result of example 6, the second point is the detection result of example 1, and the third point is the detection result of example 7.
The reagent provided by the invention has high stability, and can accurately detect the thickness of the chemical nickel plated on the copper
As shown in figure 5, the reagent of nickel plating A11 on the national standard GB/T4955-2005 copper is adopted, and the current density is 407mA/cm2Testing a chemical nickel standard sheet with 6-8% of the content of KOCOUR phosphorus in the United states to be 5.5m +/-5%, and testing twice by using a constant current time method coulometric thickness tester without changing machine parameters like the previous tests, wherein the first point and the second point are respectively shown in the figure; as can be seen from the graph of FIG. 5, the potential curve is messy and stableThe sex is very poor, the difference of the results of two tests is doubled, and the test result has serious fovea.
The foregoing is merely a preferred embodiment of the invention, which is intended to be illustrative and not limiting. It will be understood by those skilled in the art that various changes, modifications and equivalents may be made therein without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (8)
1. A reagent for detecting the thickness of chemical nickel plating on copper by a coulometry method is characterized by comprising ammonium thiocyanate, potassium iodide, potassium thiocyanate and potassium carbonate;
at normal temperature, dissolving 30-50 g of ammonium thiocyanate, 30-40 g of potassium iodide, 90-360 g of potassium thiocyanate and 30-50 g of potassium carbonate in 1L of water, mixing, and fully dissolving; and preparing the reagent for detecting the thickness of the chemical nickel plating on the copper by the coulomb method.
2. The reagent for detecting the thickness of electroless nickel plating on copper by the coulometry method as claimed in claim 1, wherein the current of the electrolytic thickness meter of the coulometry method is set as follows: 20mA, current density set to: 407mA/cm2。
3. The reagent for coulometric detection of the thickness of electroless nickel plating onto copper according to claim 2, wherein said reagent contains 30 grams of said ammonium thiocyanate, 40 grams of said potassium iodide, 180 grams of said potassium thiocyanate and 30 grams of said potassium carbonate per liter.
4. The reagent for coulometric detection of the thickness of electroless nickel plating onto copper according to claim 2, wherein said reagent contains 50 g of said ammonium thiocyanate, 40 g of potassium iodide, 200 g of potassium thiocyanate and 50 g of potassium carbonate per liter.
5. The reagent for coulometric detection of the thickness of electroless nickel plating onto copper according to claim 2, wherein said reagent contains 30 g of said ammonium thiocyanate, 40 g of potassium iodide, 200 g of potassium thiocyanate and 30 g of potassium carbonate per liter.
6. The reagent for coulometric detection of the thickness of electroless nickel plating onto copper according to claim 2, wherein said reagent contains 30 g of said ammonium thiocyanate, 30 g of potassium iodide, 160 g of potassium thiocyanate and 40 g of potassium carbonate per liter.
7. The reagent for coulometric detection of the thickness of electroless nickel plating onto copper according to claim 2, wherein said reagent contains 30 g of said ammonium thiocyanate, 40 g of potassium iodide, 360 g of potassium thiocyanate and 30 g of potassium carbonate per liter.
8. The reagent for coulometric detection of the thickness of electroless nickel plated onto copper according to claim 2 wherein said reagent contains 30 grams of ammonium thiocyanate, 40 grams of potassium iodide, 90 grams of potassium thiocyanate and 30 grams of potassium carbonate per liter of reagent.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1650796A1 (en) * | 1988-08-24 | 1991-05-23 | Предприятие П/Я А-3771 | Coulometric method for determination of coat thickness |
| CN201093996Y (en) * | 2007-09-19 | 2008-07-30 | 喻晖 | Coulomb thickness measuring equipment |
| CN106705826A (en) * | 2017-03-15 | 2017-05-24 | 四维尔丸井(广州)汽车零部件有限公司 | Test method for plating thickness of electroplated part |
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- 2018-07-23 CN CN201810812448.1A patent/CN108917579B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1650796A1 (en) * | 1988-08-24 | 1991-05-23 | Предприятие П/Я А-3771 | Coulometric method for determination of coat thickness |
| CN201093996Y (en) * | 2007-09-19 | 2008-07-30 | 喻晖 | Coulomb thickness measuring equipment |
| CN106705826A (en) * | 2017-03-15 | 2017-05-24 | 四维尔丸井(广州)汽车零部件有限公司 | Test method for plating thickness of electroplated part |
Non-Patent Citations (1)
| Title |
|---|
| 库仑-称重法测量金属镀层厚度的研究;董秀文 等;《分析科学学报》;20041031;第20卷(第5期);第555-556页 * |
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Address after: Room 210-3, building 041, block B, No. 188 Jinghua Road, high tech Zone, Ningbo, Zhejiang 315000 Patentee after: SANSI EVERLASTING TECHNOLOGY (ZHEJIANG) Co.,Ltd. Address before: 315821 Building 1, 111 Weisan Road, Xiaogang street, Beilun District, Ningbo City, Zhejiang Province Patentee before: SANSI EVERLASTING TECHNOLOGY (ZHEJIANG) Co.,Ltd. |