CN106705826A - Test method for plating thickness of electroplated part - Google Patents

Test method for plating thickness of electroplated part Download PDF

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Publication number
CN106705826A
CN106705826A CN201710154050.9A CN201710154050A CN106705826A CN 106705826 A CN106705826 A CN 106705826A CN 201710154050 A CN201710154050 A CN 201710154050A CN 106705826 A CN106705826 A CN 106705826A
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China
Prior art keywords
electrolyte
concentration
layers
testing
coating
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Pending
Application number
CN201710154050.9A
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Chinese (zh)
Inventor
郑静涛
吴姝婷
肖义洪
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Siweier Wanjing (guangzhou) Automotive Components Co ltd
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Siweier Wanjing (guangzhou) Automotive Components Co ltd
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Priority to CN201710154050.9A priority Critical patent/CN106705826A/en
Publication of CN106705826A publication Critical patent/CN106705826A/en
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01BMEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
    • G01B7/00Measuring arrangements characterised by the use of electric or magnetic techniques
    • G01B7/02Measuring arrangements characterised by the use of electric or magnetic techniques for measuring length, width or thickness
    • G01B7/06Measuring arrangements characterised by the use of electric or magnetic techniques for measuring length, width or thickness for measuring thickness

Abstract

The invention relates to a test method for plating thickness of an electroplated part. Two or more of a copper layer, multiple nickel layers and a chromium layer which are overlapped are arranged as plating layers. The test method comprises the following steps: taking the electroplated part and then detecting the plating layers in turn according to the overlapped sequence. A detection method comprises the following steps: detecting the copper layer: adopting a coulometric method for detecting by taking ammonium nitrate and ammonium hydroxide aqueous solution as electrolyte; detecting the multiple nickel layers: adopting the coulometric method for detecting by taking nickel chloride, sodium chloride and boric acid aqueous solution as electrolyte, or adopting the coulometric method for detecting by taking sodium thiocyanate and ammonium sulfate aqueous solution as electrolyte; and detecting the chromium layer: adopting the coulometric method for detecting by taking sodium sulfate and phosphoric acid aqueous solution as electrolyte. The test method provided by the invention can be used for independently performing electrolysis test on each plating layer and the test result is accurate.

Description

The thickness of coating method of testing of plated item
Technical field
The present invention relates to coating detection, the thickness of coating method of testing of more particularly to a kind of plated item.
Background technology
Plating is exactly the process for plating other metal or alloy of a thin layer on substrate material surface using electrolysis principle, is Make one layer of technique of coating of surface attachment of metal or other materials product using electrolysis.Electroplated on the surface of product The superior in quality coating of formation can be played prevents metal from aoxidizing (such as corrosion), improves wearability, electric conductivity, reflective, anti-corruption Corrosion (sour sulphur copper etc.) and having improved aesthetic appearance etc. are acted on.
The thickness of coating is one of factor of influence quality of coating, therefore it is detection coating matter that detection is carried out to thickness of coating Amount whether qualified important means.Current detection method mainly includes microsection method and coulomb method, wherein, microsection method Although testing result is directly perceived, accurate, because testing cost is too high, the cycle is more long, therefore cannot be widely applied.Storehouse Logical sequence method is to carry out local anode dissolving to the coating for being tested part, and electric current is invariable, and dissolved area is certain, by time length To carry out the measurement of thickness of coating, can greatly save testing cost compared with microsection method and shorten the testing time.Additionally, to make system Part can better meet consumer demand, and various different materials coating would generally be laminated on the surface of product in production, and The plated item of many coating is more due to the number of plies, and each layer can interact in detection, be carried out therefore, it is difficult to the thickness to each coating Independent, accurate detection.
Based on this, it is technical problem urgently to be resolved hurrily that accurately detection how is carried out to the thickness of coating of many coating plated items One of.
The content of the invention
Based on this, it is necessary to provide a kind of thickness of coating method of testing of the accurate many coating plated items of testing result.
A kind of method of testing of plated item thickness of coating, the coating is layers of copper, the multilayer nickel dam, Yi Jige being stacked Layer;The method of testing includes:Power taking plating piece, then examines to the coating successively according to the order being stacked Survey, the method for detection includes:
Layers of copper is detected:It is that 0.5~2g/mL, ammoniacal liquor volumetric concentration are 0.5~5% with ammonium nitrate concn using coulomb method The aqueous solution is detected as electrolyte, obtained final product;
Multilayer nickel dam is detected:Using coulomb method, with chlorination nickel concentration as 0.1~5g/mL, sodium chloride concentration be 0.01~ 0.1g/mL, boric acid concentration are that the aqueous solution of 0.01~0.1g/mL is detected as electrolyte, are obtained final product;Using the electrolyte, The each layer of thickness of nickel in the acquisition multilayer nickel dam can respectively be detected;Or,
It is that 0.01~0.1g/mL, ammonium sulfate concentrations are 0.01~0.1g/mL's with sodium sulfocynanate concentration using coulomb method The aqueous solution is detected as electrolyte, obtained final product;Using the electrolyte, the gross thickness for obtaining the multilayer nickel dam is can detect;
Layers of chrome is detected:It is 0.01~0.1g/mL, phosphoric acid volumetric concentration for 1~10% with sodium sulfate concentration using coulomb method The aqueous solution detected as electrolyte, obtain final product.
During coulomb method thickness measuring, be by between electrolyte and coated metal since cell reaction to stop Time period carries out thickness metering.Therefore, when many thickness of coating are detected, to ensure the accuracy of each thickness of coating test, Need as far as possible control coating just electrolysis complete when cell reaction can stop at once, without further with next coating Generation cell reaction, or cell reaction has stopped when coating is not electrolysed also and finishes.And in this process, to corresponding coating It is the key point for controlling cell reaction process that the composition and concentration of electrolyte carry out rationally control.
The method of testing of plated item thickness of coating of the invention, by substantial amounts of experimental study, by preparing specific composition With the electrolyte of each coating of concentration, when can effectively ensure that electrolyte occurs cell reaction with corresponding coating, plating just Layer stops cell reaction when being electrolysed completely, and reaction does not occur completely and with adjacent coating further reaction, thus can independently, standard True carries out electrolysis test to each coating to obtain corresponding thickness of coating, it is to avoid interacting between each layer, reduces detection and misses Difference.
It is 0.01~0.05g/mL, phosphoric acid body with sodium sulfate concentration in the layers of chrome inspection wherein in one embodiment Product concentration be 2~6% the aqueous solution as electrolyte.
It is 0.1~0.5g/mL, chlorination with chlorination nickel concentration in the multilayer nickel dam detection wherein in one embodiment The aqueous solution that na concn is 0.02~0.08g/mL, boric acid concentration is 0.01~0.05g/mL is used as electrolyte.
Wherein in one embodiment, in multilayer nickel dam detection, with sodium sulfocynanate concentration as 0.02~0.06g/mL, Ammonium sulfate concentrations are the aqueous solution of 0.02~0.06g/mL as electrolyte.
It is 0.6~1.2g/mL, ammoniacal liquor volume with ammonium nitrate concn in the layers of copper detection wherein in one embodiment Concentration be 0.8~1.5% the aqueous solution as electrolyte.
Wherein in one embodiment, in the layers of chrome detection, the Faradaic current for using is 0.3~0.4mA, and voltage is 2 ~3V.
Wherein in one embodiment, in the multilayer nickel dam detection, the Faradaic current for using is 10~15mA, and voltage is 2~3V.
Wherein in one embodiment, in layers of copper detection, the Faradaic current for using be 10~15mA, voltage for 1~ 2V。
In addition, the present invention also has found under study for action, for different coating, the electric current and voltage during electrolysis are rationally controlled, Electric current and voltage can be avoided to the error that causes of test, in addition constant current and voltage ensure that electrolyte only with it is corresponding Coating reacts, and improves the quasi- accuracy of detection.
Wherein in one embodiment, the coating is to stack gradually layers of copper in substrate surface, multilayer nickel dam and layers of chrome.
Wherein in one embodiment, the MULTI-LAYER NICKEL includes the semi-bright nickel, bright nickel and the microporous nickel that stack gradually.
Brief description of the drawings
Fig. 1 is the structural representation of plated item in the embodiment of the present invention.
Specific embodiment
Further details of theory is made to the thickness of coating method of testing of plated item of the invention below in conjunction with specific embodiment It is bright.
Embodiment
A kind of method of testing of plated item thickness of coating of the present embodiment, plated item to be measured is respectively 2CG luggage compartment panels Panel (2) under (1#) and 2WS, structure is as shown in figure 1, its coating includes stacking gradually layers of copper in resin substrate surface, many Layer nickel dam and layers of chrome, wherein the MULTI-LAYER NICKEL includes the semi-bright nickel, bright nickel and the microporous nickel that stack gradually.The method of testing Comprise the following steps:
(1) using coulomb method ZD-B intelligence calibrators, extract layers of chrome electrolyte and inject in its electrolysis cup, cup bottom there can not be gas Bubble, then extracts out if any bubble and refills;The layers of chrome electrolyte is sodium sulfate concentration for 0.03g/mL, phosphoric acid volumetric concentration are 4% aqueous solution;
(2) clamp plated item to be measured with test anode clamp to be put into electrolysis cup, setting Faradaic current is 0.37mA, voltage is 2~3V, is electrolysed;After the completion of layers of chrome dissolving, coulomb method calibrator is automatically stopped, and potential curve is analyzed, and is obtained Go out the thickness of layers of chrome;
(3) plated item after being electrolysed through step (2) is taken out, is cleaned and is dried;Extract the injection electrolysis of multilayer nickel dam electrolyte In cup, the multilayer nickel dam electrolyte is that chlorination nickel concentration is that 0.26g/mL, sodium chloride concentration are that 0.05g/mL, boric acid concentration are The aqueous solution of 0.023g/mL;
(4) plated item is clamped with test anode clamp to be put into electrolysis cup, setting Faradaic current be 12.5mA, voltage be 2~ 3V, is electrolysed;After the completion of the dissolving of multilayer nickel dam, coulomb method calibrator is automatically stopped, and potential curve is analyzed, point The thickness of semi-bright nickel, bright nickel and microporous nickel in multilayer nickel dam is not drawn;
(5) plated item after being electrolysed through step (4) is taken out, is cleaned and is dried;Layers of copper electrolyte is extracted to inject in electrolysis cup, The layers of copper electrolyte is that ammonium nitrate concn is 0.82g/mL, the aqueous solution that ammoniacal liquor volumetric concentration is 1.2%;
(6) plated item is clamped with test anode clamp to be put into electrolysis cup, setting Faradaic current be 12.0mA, voltage be 1~ 2V, is electrolysed;After the completion of layers of copper dissolving, coulomb method calibrator is automatically stopped, and potential curve is analyzed, and obtains copper The thickness of layer.
In above-mentioned steps, in order to reduce the error that other factors are caused, electric current and voltage need to change and stabilization, this External pelivimetry area needs monitor in real time, it is ensured that the area tested is constant.
As needed, above-mentioned steps (3) and (4) also can be replaced following method and directly the gross thickness of MULTI-LAYER NICKEL surveyed Examination:
(3 ') plated item after being electrolysed through step (2) is taken out, is cleaned and is dried;Extract in electrolyte injection electrolysis cup, be somebody's turn to do Electrolyte is the aqueous solution that sodium sulfocynanate concentration is 0.04g/mL, ammonium sulfate concentrations are 0.04g/mL;
(4 ') are clamped plated item and are put into electrolysis cup with test anode clamp, setting Faradaic current be 12.5mA, voltage be 2~ 3V, is electrolysed;After the completion of the dissolving of multilayer nickel dam, coulomb method calibrator is automatically stopped, and potential curve is analyzed, and is obtained Go out the gross thickness of multilayer nickel dam.
Comparative example 1
A kind of method of testing of plated item thickness of coating of this comparative example, plated item to be measured and method of testing similar embodiment, Difference is:Step (1) use layers of chrome electrolyte in, with sodium sulfate concentration as 0.08g/mL, phosphoric acid volumetric concentration be 4% The aqueous solution is used as electrolyte.
Comparative example 2
A kind of method of testing of plated item thickness of coating of this comparative example, plated item to be measured and method of testing similar embodiment, Difference is:In the multilayer nickel dam electrolyte that step (3) is used, chlorination nickel concentration is 0.8g/mL, sodium chloride concentration is 0.05g/ ML, boric acid concentration are the aqueous solution of 0.06g/mL as electrolyte.
Comparative example 3
A kind of method of testing of plated item thickness of coating of this comparative example, plated item to be measured and method of testing similar embodiment, Difference is:Step (3 ') use multilayer nickel dam electrolyte in, by with sodium sulfocynanate concentration as 0.08g/mL, ammonium sulfate concentrations It is the aqueous solution of 0.08g/mL as electrolyte.
Comparative example 4
A kind of method of testing of plated item thickness of coating of this comparative example, plated item to be measured and method of testing similar embodiment, Difference is:Step (5) use layers of copper electrolyte in, by with ammonium nitrate concn as 0.4g/mL, ammoniacal liquor volumetric concentration be 1.9% aqueous solution is used as electrolyte.
The test result of each thickness of coating collects as shown in table 1 in embodiment and comparative example, and is obtained with microsection method Each thickness of coating be compared:
Table 1
As shown in Table 1, in each layer electrolyte the concentration of chemical substance have to the accuracy of test product thickness it is more bright Aobvious influence.Electrolyte according to certain concentration of the present invention carries out the test of each coating, and coating can be controlled to be electrolysed just Cell reaction can stop at once during completion, without further there is cell reaction with next coating or also not electric in coating Cell reaction has stopped when solution is finished, and then ensures the accuracy of thickness measuring.
Each technical characteristic of embodiment described above can be combined arbitrarily, to make description succinct, not to above-mentioned reality Apply all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited In contradiction, the scope of this specification record is all considered to be.
Embodiment described above only expresses several embodiments of the invention, and its description is more specific and detailed, but simultaneously Can not therefore be construed as limiting the scope of the patent.It should be pointed out that coming for one of ordinary skill in the art Say, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention Scope.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.

Claims (10)

1. a kind of method of testing of plated item thickness of coating, it is characterised in that the coating is layers of copper, the MULTI-LAYER NICKEL being stacked Layer, and layers of chrome;The method of testing includes:Power taking plating piece, then according to the order being stacked successively to the plating Layer is detected that the method for detection includes:
Layers of copper is detected:Using coulomb method, with ammonium nitrate concn be 0.5~2g/mL, ammoniacal liquor volumetric concentration be 0.5~5% it is water-soluble Liquid is detected as electrolyte, obtained final product;
Multilayer nickel dam is detected:It is 0.1~5g/mL, sodium chloride concentration for 0.01~0.1g/ with chlorination nickel concentration using coulomb method ML, boric acid concentration are that the aqueous solution of 0.01~0.1g/mL is detected as electrolyte, are obtained final product;Or,
It is that 0.01~0.1g/mL, ammonium sulfate concentrations are the water-soluble of 0.01~0.1g/mL with sodium sulfocynanate concentration using coulomb method Liquid is detected as electrolyte, obtained final product;
Layers of chrome is detected:Using coulomb method, it is 0.01~0.1g/mL with sodium sulfate concentration, the water that phosphoric acid volumetric concentration is 1~10% Solution is detected as electrolyte, obtained final product.
2. the method for testing of plated item thickness of coating according to claim 1, it is characterised in that in the layers of chrome inspection, It is 0.01~0.05g/mL using sodium sulfate concentration, the aqueous solution that phosphoric acid volumetric concentration is 2~6% is used as electrolyte.
3. the method for testing of plated item thickness of coating according to claim 1, it is characterised in that the multilayer nickel dam detection In, with chlorination nickel concentration as 0.1~0.5g/mL, sodium chloride concentration be 0.02~0.08g/mL, boric acid concentration be 0.01~ The aqueous solution of 0.05g/mL is used as electrolyte.
4. the method for testing of plated item thickness of coating according to claim 1, it is characterised in that the multilayer nickel dam detection In, it is 0.02~0.06g/mL using sodium sulfocynanate concentration, the aqueous solution that ammonium sulfate concentrations are 0.02~0.06g/mL is used as electrolysis Liquid.
5. the method for testing of plated item thickness of coating according to claim 1, it is characterised in that in the layers of copper detection, It is 0.6~1.2g/mL using ammonium nitrate concn, the aqueous solution that ammoniacal liquor volumetric concentration is 0.8~1.5% is used as electrolyte.
6. the method for testing of the plated item thickness of coating according to claim any one of 1-5, it is characterised in that the layers of chrome In detection, the Faradaic current for using is 0.3~0.4mA, and voltage is 2~3V.
7. the method for testing of the plated item thickness of coating according to claim any one of 1-5, it is characterised in that the multilayer In nickel dam detection, the Faradaic current for using is 10~15mA, and voltage is 2~3V.
8. the method for testing of the plated item thickness of coating according to claim any one of 1-5, it is characterised in that the layers of copper In detection, the Faradaic current for using is 10~15mA, and voltage is 1~2V.
9. the method for testing of the plated item thickness of coating according to claim any one of 1-5, it is characterised in that the coating To stack gradually layers of copper, the multilayer nickel dam in substrate surface, and layers of chrome.
10. the method for testing of the plated item thickness of coating according to claim any one of 1-5, it is characterised in that described many Layer nickel includes the semi-bright nickel, bright nickel and the microporous nickel that stack gradually.
CN201710154050.9A 2017-03-15 2017-03-15 Test method for plating thickness of electroplated part Pending CN106705826A (en)

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CN108917579A (en) * 2018-07-23 2018-11-30 三思永恒科技(浙江)有限公司 A kind of reagent of the electroless nickel thickness on coulomb method detection copper
CN109186441A (en) * 2018-09-26 2019-01-11 三思永恒科技(浙江)有限公司 The reagent of electroless nickel thickness, preparation method and application on coulomb method detection iron aluminium

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108917579A (en) * 2018-07-23 2018-11-30 三思永恒科技(浙江)有限公司 A kind of reagent of the electroless nickel thickness on coulomb method detection copper
CN108917579B (en) * 2018-07-23 2021-01-01 三思永恒科技(浙江)有限公司 Reagent for detecting thickness of chemical nickel plating on copper by coulombic method
CN109186441A (en) * 2018-09-26 2019-01-11 三思永恒科技(浙江)有限公司 The reagent of electroless nickel thickness, preparation method and application on coulomb method detection iron aluminium

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