CN107525700A - The pre-treating method of the silver layer chemical composition detection of silver-bearing copper composite contact - Google Patents

The pre-treating method of the silver layer chemical composition detection of silver-bearing copper composite contact Download PDF

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Publication number
CN107525700A
CN107525700A CN201710607034.0A CN201710607034A CN107525700A CN 107525700 A CN107525700 A CN 107525700A CN 201710607034 A CN201710607034 A CN 201710607034A CN 107525700 A CN107525700 A CN 107525700A
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China
Prior art keywords
silver
silver layer
composite contact
bearing copper
copper
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CN201710607034.0A
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Chinese (zh)
Inventor
陈晓统
沈涛
祁更新
陈晓
张玲洁
樊先平
杨辉
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Zhejiang University ZJU
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Zhejiang University ZJU
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Priority to CN201710607034.0A priority Critical patent/CN107525700A/en
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/286Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/34Purifying; Cleaning
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/286Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
    • G01N2001/2866Grinding or homogeneising

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Biomedical Technology (AREA)
  • Molecular Biology (AREA)
  • Engineering & Computer Science (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)

Abstract

The present invention relates to metallic element detection technique, it is desirable to provide a kind of pre-treating method of the silver layer chemical composition detection of silver-bearing copper composite contact.Comprise the following steps:Grinding removes most of layers of copper on silver-bearing copper composite contact surface, silver-bearing copper composite contact after grinding is placed in 20~100 DEG C of hydrogen peroxide hydrochloric acid composite solution and soaked, is completely dissolved layers of copper and retain silver layer;The silver chlorate for removing silver layer surface is soaked with ammoniacal liquor;After being cleaned with water, drying.The present invention can carry out quantitative detection to silver-bearing copper composite contact silver layer chemical composition, have the advantages of retaining silver layer to greatest extent, applicability is wide, easy to operate.The present invention can be studied for electrical contact material industry technology and quality control provides support.

Description

The pre-treating method of the silver layer chemical composition detection of silver-bearing copper composite contact
Technical field
The present invention relates to metallic element detection technique, more particularly to a kind of silver-bearing copper composite contact that is used for is (such as silver and silver alloy The contacts such as the multiple iron of the multiple copper of multiple copper, silver and silver alloy) the detection of silver layer chemical composition pre-treating method.
Background technology
Silver-bearing copper composite contact is used widely in low voltage electrical apparatus industry, and the chemical composition of wherein silver layer is to be related to One of key factor of contact performance.Detection method general at present is to grind off layers of copper with sand paper, then the silver layer that will be left behind passes through Chemical composition is detected with instrument after processing, this method is only applicable to the thicker contact of silver layer, not applied to for the thin contact of silver layer, Noble metal can be lost simultaneously.Or lossless inspection directly is carried out to silver layer with x ray fluorescence spectrometry or ESEM spectroscopy Survey, the method for such Non-Destructive Testing is the detection of sxemiquantitative, and measured data can only be used as reference, and add for micro Added elements can not be detected accurately.
It is at present to soak copper with sodium chloride solution and concentrated nitric acid by the public technology of chemical method selective retention silver layer Silver-colored composite contact, silver layer is protected after silver layer surface forms the silver chloride layer of densification, then layers of copper is redissolved and retains silver Layer.But defect is still suffered from this method:It can make part silver layer dissolving in initial reaction stage, cause silver layer to lose, be not suitable for thin Silver layer contact.
The content of the invention
The technical problem to be solved in the present invention is to overcome deficiency of the prior art, there is provided a kind of silver-bearing copper composite contact The pre-treating method of silver layer chemical composition detection.
To solve technical problem, solution of the invention is:
A kind of pre-treating method of the silver layer chemical composition detection of silver-bearing copper composite contact is provided, comprised the steps:
(1) grinding removes most of layers of copper on silver-bearing copper composite contact surface, it is ensured that will not manifest silver layer;
(2) silver-bearing copper composite contact after grinding is placed in 20~100 DEG C of hydrogen peroxide-hydrochloric acid composite solution, soak time 0.5h~5h, it is completely dissolved layers of copper and retains silver layer;
(3) 0.1~1h is soaked with the ammoniacal liquor that mass concentration is 5%~30% again, removes the silver chlorate of silver layer surface;Use water After cleaning, drying;
The collocation method of the hydrogen peroxide-hydrochloric acid composite solution is:Take 10~100ml hydrogen peroxide, 10~100ml salt The water of acid and 10~1000ml, sequentially adds in container and mixes.
In the present invention, the silver thickness of the silver-bearing copper composite contact is in 0.05~5mm, and copper layer thickness is in 0.05~5mm.
In the present invention, the grinding is ground by 50~3000 sand paper of granularity.
In the present invention, the temperature of the drying is 50~200 DEG C, and the time is 5~30min.
The realization principle description of the present invention:
The present invention, with being chemically treated the technology being combined, silver-bearing copper composite contact is ground with sand paper and removed using physical treatment Most of layers of copper, then soaked with hydrogen peroxide hydrochloric acid composite solution, carrying out heating makes the quick and complete dissolving of layers of copper and retains silver layer, then The silver chlorate of silver layer surface is removed with ammoniacal liquor soaking and washing, with water cleaning, drying, obtain silver layer be used for it is follow-up quantitatively into go-on-go Survey.By the use to hydrogen peroxide hydrochloric acid composite solution, make silver layer from contact separation and completely retain.Its reaction mechanism is dioxygen Water in acid condition can with copper react and can not be with silver reaction.
Hydrogen peroxide under the conditions of hydrochloric acid with copper reaction equation be:H2O2+ 2HCl+Cu=CuCl2+2H2O。
Compared with prior art, the technical effects of the invention are that:
1st, the present invention can carry out quantitative detection to silver-bearing copper composite contact silver layer chemical composition, have and retain silver to greatest extent Layer, the advantages of applicability is wide, easy to operate.
2nd, the present invention can study for electrical contact material industry technology and quality control provides support.
Embodiment
The present invention is specifically described below by example, is served only for further describing the present invention, it is impossible to manage Solving can make for limiting the scope of the present invention, the technician in the field according to the content of foregoing invention to the present invention Some nonessential modifications and adaptations.
Embodiment 1
Silver-bearing copper composite rivet type contact, silver thickness 0.1mm, copper layer thickness 0.9mm.
After selecting multiple sand paper (granularity is 50~3000) from coarse to fine gradually to grind off most of layers of copper, with hydrogen peroxide- Hydrochloric acid composite solution soaks (hydrogen peroxide-hydrochloric acid composite solution is mixed by hydrochloric acid 50ml, hydrogen peroxide 50ml, water 20ml), and 60 DEG C 2h being dissolved by heating, then soak 0.5h with the ammoniacal liquor that mass concentration is 20% and clean the silver chlorate on surface, deionized water is cleaned, 15min is dried after 120 DEG C, obtains silver layer, for subsequent detection chemical composition.
Embodiment 2
The multiple compound button type contact of three layers of iron of the multiple copper of silver, silver thickness 0.05mm, copper layer thickness 5mm, iron layer thickness 0.2mm。
After selecting multiple sand paper (granularity is 50~3000) from coarse to fine gradually to grind off most of layers of copper, with hydrogen peroxide- Hydrochloric acid composite solution soaks (hydrogen peroxide-hydrochloric acid composite solution is mixed by hydrochloric acid 10ml, hydrogen peroxide 100ml, water 1000ml), 100 DEG C dissolve by heating 0.5h, then the silver chlorate on surface is cleaned with the ammoniacal liquor immersion 1h that mass concentration is 5%, deionized water cleaning, 50 DEG C of drying 30min, obtain silver layer, for subsequent detection chemical composition.
Embodiment 3
Silver-bearing copper composite contact, silver thickness 5mm, copper layer thickness 0.05mm.
After selecting multiple sand paper (granularity is 50~3000) from coarse to fine gradually to grind off most of layers of copper, with hydrogen peroxide- Hydrochloric acid composite solution soaks (hydrogen peroxide-hydrochloric acid composite solution is mixed by hydrochloric acid 100ml, hydrogen peroxide 10ml, water 10ml), and 20 DEG C dissolving 5h, then soak 0.1h with the ammoniacal liquor that mass concentration is 30% and clean the silver chlorate on surface, deionized water is cleaned, 200 DEG C 5min is dried, silver layer is obtained, for subsequent detection chemical composition.

Claims (4)

1. the pre-treating method of the silver layer chemical composition detection of a kind of silver-bearing copper composite contact, it is characterised in that comprise the steps:
(1) grinding removes most of layers of copper on silver-bearing copper composite contact surface, it is ensured that will not manifest silver layer;
(2) silver-bearing copper composite contact after grinding is placed in 20~100 DEG C of hydrogen peroxide-hydrochloric acid composite solution, soak time 0.5h ~5h, it is completely dissolved layers of copper and retains silver layer;
(3) 0.1~1h is soaked with the ammoniacal liquor that mass concentration is 5%~30% again, removes the silver chlorate of silver layer surface;Cleaned with water Afterwards, dry;
The collocation method of the hydrogen peroxide-hydrochloric acid composite solution is:Take 10~100ml hydrogen peroxide, 10~100ml hydrochloric acid and 10~1000ml water, sequentially adds in container and mixes.
2. according to the method for claim 1, it is characterised in that the silver thickness of the silver-bearing copper composite contact 0.05~ 5mm, copper layer thickness is in 0.05~5mm.
3. according to the method for claim 1, it is characterised in that the grinding is carried out by 50~3000 sand paper of granularity Grinding.
4. according to the method for claim 1, it is characterised in that the temperature of the drying be 50~200 DEG C, the time be 5~ 30min。
CN201710607034.0A 2017-07-24 2017-07-24 The pre-treating method of the silver layer chemical composition detection of silver-bearing copper composite contact Pending CN107525700A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1475788A (en) * 2003-07-15 2004-02-18 水口山矿务局柏坊铜矿 Method of analyzing gold, silver content in gold, silver containing material
CN102393387A (en) * 2011-11-10 2012-03-28 西安航空动力股份有限公司 Method for analyzing surface silver coating components of high-temperature alloy GH4169 part

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1475788A (en) * 2003-07-15 2004-02-18 水口山矿务局柏坊铜矿 Method of analyzing gold, silver content in gold, silver containing material
CN102393387A (en) * 2011-11-10 2012-03-28 西安航空动力股份有限公司 Method for analyzing surface silver coating components of high-temperature alloy GH4169 part

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
中国标准出版社第二编辑室: "《铜及铜合金标准汇编》", 31 December 2005, 中国标准出版社 *
任颂赞,叶俭等: "《金相分析原理及技术》", 31 August 2013, 上海科学技术文献出版社 *
周玉敏: "《分析化学》", 31 July 2002, 化学工业出版社 *
梅恒星,李耀群: "《铜加工产品性能检测技术》", 31 March 2008, 冶金工业出版社 *

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Application publication date: 20171229