CN108048914A - A kind of method of electrorefining diamond large single crystal Synthetic block - Google Patents

A kind of method of electrorefining diamond large single crystal Synthetic block Download PDF

Info

Publication number
CN108048914A
CN108048914A CN201711298292.1A CN201711298292A CN108048914A CN 108048914 A CN108048914 A CN 108048914A CN 201711298292 A CN201711298292 A CN 201711298292A CN 108048914 A CN108048914 A CN 108048914A
Authority
CN
China
Prior art keywords
single crystal
large single
clamp
synthetic block
diamond large
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.)
Granted
Application number
CN201711298292.1A
Other languages
Chinese (zh)
Other versions
CN108048914B (en
Inventor
邵静茹
李方宜
刘永奇
刘永涛
赵鸣
陈芳
张坤
王英华
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Zhengzhou Synthetic Diamond and Products Engineering Technology Research Center Co Ltd
Original Assignee
Zhengzhou Synthetic Diamond and Products Engineering Technology Research Center Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Zhengzhou Synthetic Diamond and Products Engineering Technology Research Center Co Ltd filed Critical Zhengzhou Synthetic Diamond and Products Engineering Technology Research Center Co Ltd
Priority to CN201711298292.1A priority Critical patent/CN108048914B/en
Publication of CN108048914A publication Critical patent/CN108048914A/en
Application granted granted Critical
Publication of CN108048914B publication Critical patent/CN108048914B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B33/00After-treatment of single crystals or homogeneous polycrystalline material with defined structure
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/02Elements
    • C30B29/04Diamond

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

A kind of method of electrorefining diamond large single crystal Synthetic block, comprises the following steps:1)Diamond large single crystal Synthetic block is placed in anode clamp, is then linked into electrolytic cell;2)Electrolyte is added in into electrolytic cell, is made per 1L electrolyte of following components:30 150 g of hydrochloric acid, 15 30g of activator, 5 35 g of stabilizer, surplus is deionized water;3)Cathode plate is linked into electrolytic cell, anode clamp and cathode plate are connected into conducting wire respectively;4)In current density be 3 5A/dm2Under, it is powered after electrolysis, diamond large single crystal falls into electrolytic cell in diamond large single crystal Synthetic block;5)Take out diamond large single crystal, cleaning.The present invention purifies diamond large single crystal Synthetic block using electrochemical method, contains only a small amount of acid in electrolyte, electrolysis time is short, metal plating is on cathode plate in Synthetic block, metal can be recycled, and reduce environmental pollution, economize on resources and the energy, improve electrolytic efficiency.

Description

A kind of method of electrorefining diamond large single crystal Synthetic block
Technical field
The invention belongs to purification of diamond technical fields, and in particular to a kind of electrorefining diamond large single crystal Synthetic block Method.
Background technology
With the progress of large single crystal synthetic technology, diamond large single crystal product yield rapid growth, but diamond large single crystal It generally requires to purify, at present, diamond large single crystal Synthetic block method of purification is mainly that traditional strong acid is boiled and washed.Usual specific method For:Metal first is removed with chloroazotic acid, then boils washout with the concentrated sulfuric acid, concentrated nitric acid and removes graphite, method is simple, but needs to consume substantial amounts of strong Acid, working environment is poor, strong acid, heavy metals emission in waste liquid, it is impossible to recycle, pollute environment, also waste of resource.
The content of the invention
Present invention aims at provide a kind of method of electrorefining diamond large single crystal Synthetic block.
Based on above-mentioned purpose, the present invention takes following technical scheme:
A kind of method of electrorefining diamond large single crystal Synthetic block, comprises the following steps:
1)Diamond large single crystal Synthetic block is placed in anode clamp, is then linked into electrolytic cell;
2)Electrolyte is added in into electrolytic cell, is made per 1L electrolyte of following components:Hydrochloric acid 30-150 g, activator 15- 30g, stabilizer 5-35 g, surplus is deionized water;
3)Cathode plate is linked into electrolytic cell, anode clamp and cathode plate are connected into conducting wire respectively;
4)In current density be 3-5A/dm2Under, it is powered after electrolysis, diamond large single crystal is fallen into diamond large single crystal Synthetic block Electrolytic cell;
5)Take out diamond large single crystal, cleaning.
Step 1)Anode clamp includes the first clamp, the second clamp and is arranged at the first axle ear of the first clamp both sides, sets The second axis ear of the second clamp both sides is placed in, is connected between first axle ear and the second axis ear by shaft, bullet is arranged in shaft Spring, the both ends of spring are fastened on the first clamp and the second clamp.
First clamp includes first clamping plate and the first clamp holder being connected with first clamping plate, and the second clamp includes and first The second clamping plate and the second clamp holder being connected with second clamping plate that clamping plate is oppositely arranged, first axle ear are arranged on the both sides of the first clamp holder, Second axis ear is arranged on the both sides of the second clamp holder, that one side of first clamping plate towards second clamping plate is equipped with contact brush.
First clamp, the second clamp and contact brush are made of titanium material.
The step 2)Stabilizer is by amount ratio by ascorbic acid, sodium gluconate and sodium citrate(1-10)︰(2- 5)︰(5-25)It is formulated.
Step 2)Activator is that frerrous chloride, sodium chloride according to amount ratio are 10:The mixture that (1-4) is formulated.
The step 3)Cathode plate is made of iron or titanium material.
The step 4)Electrolysis time is 3-4h.
Compared with prior art, the invention has the advantages that:
1)The present invention purifies diamond large single crystal Synthetic block using electrochemical method, and a small amount of acid, electrolysis time are contained only in electrolyte Short, metal plating can recycle metal on cathode plate in Synthetic block, and reduce environmental pollution, economize on resources and the energy, Improve electrolytic efficiency;
2)Contact brush and spring are set on anode clamp, as the metal covering of diamond large single crystal Synthetic block constantly dissolves, contact brush Sustainable follow-up clamps Synthetic block, keeps well conducting.
Description of the drawings
Fig. 1 is the structure diagram of anode clamp;
Fig. 2 is shaft, the partial schematic diagram of spring;
Wherein:1-1, first clamping plate;1-2, second clamping plate;2-1, the first clamp holder;2-2, the second clamp holder;3-1, first axle ear;3- 2nd, the second axis ear;4th, contact brush;5th, shaft;6th, spring.
Specific embodiment
Embodiment 1
As illustrated in fig. 1 and 2, including the first clamp, the second clamp, the first clamp includes first clamping plate 1-1 and with the anode clamp First clamp holder 2-1 of one clamping plate 1-1 connections, the second clamp include the second clamping plate 1-2 that is oppositely arranged with first clamping plate 1-1 and with That one side of second clamp holder 2-2 of second clamping plate 1-2 connections, first clamping plate 1-1 towards second clamping plate 1-2 are equipped with contact brush Both sides of the both sides of 4, the first clamp holder 2-1 equipped with first axle ear 3-1, the second clamp holder 2-2 are equipped with the second axis ear 3-2, first axle ear It is connected between 3-1 and the second axis ear 3-2 by shaft 5, spring 6 is arranged in shaft 5, the both ends of spring 6 are fastened on the first folder On handle 2-1 and the second clamp holder 2-2.First clamp, the second clamp and contact brush 4 are made of titanium material.
A kind of method of electrorefining diamond large single crystal Synthetic block, comprises the following steps:
1)100g diamond large single crystal Synthetic blocks are placed in anode clamp, to the first clamp holder 2-1 and the second clamp holder 2-2 outer surfaces Apply external force, the first clamp holder 2-1 and the second clamp holder 2-2 is made to be drawn close among the two, makes first clamping plate 1-1 and second clamping plate 1-2 Between space open bigger, be then placed in diamond large single crystal Synthetic block, clamp first clamping plate 1-1 and second clamping plate 1-2 Diamond large single crystal Synthetic block(Diamond large single crystal Synthetic block is in roundlet column, including metallic conduction portion and non-conductive portion, Buddha's warrior attendant Stone large single crystal is wrapped in metallic conduction portion, and metallic conduction portion is contacted directly with contact brush 4, similarly hereinafter), then it is linked into electrolysis Slot;
2)2L electrolyte (electrolyte floods diamond large single crystal Synthetic block) is added in into electrolytic cell, per 1L electrolyte by with the following group Divide and be made:30 g of hydrochloric acid, activator 30g, 15 g of stabilizer, surplus is deionized water;Stabilizer is by ascorbic acid, gluconic acid Sodium and sodium citrate are formulated by amount ratio for 2 ︰, 2 ︰ 7;Activator is that frerrous chloride, sodium chloride according to amount ratio are 10:1 matches somebody with somebody Make the mixture formed;
3)Cathode plate is linked into electrolytic cell, cathode plate is made of iron material;Respectively by the first clamping plate 1-1 and the moon of anode clamp Pole plate connects conducting wire;
4)In current density be 4A/dm2, voltage be the electrolysis 4h that under 10V, is powered, metal portion is electroplated onto on cathode plate in Synthetic block, Diamond large single crystal exposes, and falls into electrolytic cell;
5)Diamond large single crystal is taken out, is washed with water.After cleaning, micro- Microscopic observation, diamond large single crystal surface is complete All clear wash clean.
Embodiment 2
Anode clamp is the same as embodiment 1.
A kind of method of electrorefining diamond large single crystal Synthetic block, comprises the following steps:
1)200g diamond large single crystal Synthetic blocks are placed in anode clamp to the first clamp holder 2-1 and the second clamp holder 2-2 outer surfaces Apply external force, the first clamp holder 2-1 and the second clamp holder 2-2 is made to be drawn close among the two, makes first clamping plate 1-1 and second clamping plate 1-2 Between space open bigger, be then placed in diamond large single crystal Synthetic block, clamp first clamping plate 1-1 and second clamping plate 1-2 Diamond large single crystal Synthetic block(Diamond large single crystal Synthetic block is in roundlet column, including metallic conduction portion and non-conductive portion, Buddha's warrior attendant Stone large single crystal is wrapped in metallic conduction portion, and metallic conduction portion is contacted directly with contact brush 4, similarly hereinafter), then it is linked into electrolysis Slot;
2)2L electrolyte (electrolyte floods diamond large single crystal Synthetic block) is added in into electrolytic cell, per 1L electrolyte by with the following group Divide and be made:150 g of hydrochloric acid, activator)15g, 35 g of stabilizer, surplus is deionized water;Stabilizer is by ascorbic acid, glucose Sour sodium and sodium citrate are formulated by amount ratio for 10 ︰, 2 ︰ 25;Activator is frerrous chloride, sodium chloride is according to amount ratio 10:4 mixtures being formulated;
3)Cathode plate is linked into electrolytic cell, cathode plate is made of iron material, respectively by the first clamping plate 1-1 and the moon of anode clamp Pole plate connects conducting wire;
4)In current density be 5A/dm2, voltage be the electrolysis 3.5h that under 10V, is powered, metal portion is electroplated onto cathode plate in Synthetic block On, diamond large single crystal exposes, and falls into electrolytic cell;
5)Diamond large single crystal is taken out, is washed with water.After cleaning, micro- Microscopic observation, diamond large single crystal surface is complete All clear wash clean.
Embodiment 3
Anode clamp is the same as embodiment 1.
A kind of method of electrorefining diamond large single crystal Synthetic block, comprises the following steps:
1)200g diamond large single crystal Synthetic blocks are placed in anode clamp to the first clamp holder 2-1 and the second clamp holder 2-2 outer surfaces Apply external force, the first clamp holder 2-1 and the second clamp holder 2-2 is made to be drawn close among the two, makes first clamping plate 1-1 and second clamping plate 1-2 Between space open bigger, be then placed in diamond large single crystal Synthetic block, clamp first clamping plate 1-1 and second clamping plate 1-2 Diamond large single crystal Synthetic block(Diamond large single crystal Synthetic block is in roundlet column, including metallic conduction portion and non-conductive portion, Buddha's warrior attendant Stone large single crystal is wrapped in metallic conduction portion, and metallic conduction portion is contacted directly with contact brush 4, similarly hereinafter), then it is linked into electrolysis Slot;
2)2L electrolyte is added in into electrolytic cell, is made per 1L electrolyte of following components:It is 100 g of hydrochloric acid, activator 20g, steady Determine 5 g of agent, surplus is deionized water;Stabilizer is 10 ︰, 5 ︰ 15 by amount ratio by ascorbic acid, sodium gluconate and sodium citrate It is formulated;Activator is that frerrous chloride, sodium chloride according to amount ratio are 10:3 mixtures being formulated;
3)Cathode plate is linked into electrolytic cell, cathode plate is made of iron material, respectively by the first clamping plate 1-1 and the moon of anode clamp Pole plate connects conducting wire;
4)In current density be 6A/dm2, voltage be the electrolysis 4h that under 8V, is powered, metal portion is electroplated onto on cathode plate in Synthetic block, Diamond large single crystal exposes, and falls into electrolytic cell;
5)Diamond large single crystal is taken out, is washed with water.After cleaning, micro- Microscopic observation, diamond large single crystal surface is complete All clear wash clean.

Claims (8)

  1. A kind of 1. method of electrorefining diamond large single crystal Synthetic block, which is characterized in that comprise the following steps:
    1)Diamond large single crystal Synthetic block is placed in anode clamp, is then linked into electrolytic cell;
    2)Electrolyte is added in into electrolytic cell, is made per 1L electrolyte of following components:Hydrochloric acid 30-150 g, activator 15- 30g, stabilizer 5-35 g, surplus is deionized water;
    3)Cathode plate is linked into electrolytic cell, anode clamp and cathode plate are connected into conducting wire respectively;
    4)In current density be 3-5A/dm2Under, it is powered after electrolysis, diamond large single crystal falls into electricity in diamond large single crystal Synthetic block Solve slot;
    5)Take out diamond large single crystal, cleaning.
  2. 2. the method for electrorefining diamond large single crystal Synthetic block as described in claim 1, which is characterized in that step 1)Anode Fixture includes the first clamp, the second clamp and is arranged at the first axle ear of the first clamp both sides, is arranged at the second clamp both sides Second axis ear is connected between first axle ear and the second axis ear by shaft, and spring is arranged in shaft, and the both ends of spring are fastened on On first clamp and the second clamp.
  3. 3. the method for electrorefining diamond large single crystal Synthetic block as claimed in claim 2, which is characterized in that first folder Body includes first clamping plate and the first clamp holder being connected with first clamping plate, and the second clamp includes be oppositely arranged with first clamping plate second Clamping plate and the second clamp holder being connected with second clamping plate, first axle ear are arranged on the both sides of the first clamp holder, and the second axis ear is arranged on the second folder The both sides of handle, that one side of first clamping plate towards second clamping plate are equipped with contact brush.
  4. 4. the method for electrorefining diamond large single crystal Synthetic block as claimed in claim 3, which is characterized in that first folder Body, the second clamp and contact brush are made of titanium material.
  5. 5. the method for electrorefining diamond large single crystal Synthetic block as described in claim 1, which is characterized in that the step 2) Stabilizer is by amount ratio by ascorbic acid, sodium gluconate and sodium citrate(1-10)︰(2-5)︰(5-25)It is formulated.
  6. 6. the method for electrorefining diamond large single crystal Synthetic block as claimed in claim 5, which is characterized in that step 2)Activation Agent is that frerrous chloride, sodium chloride according to amount ratio are 10:The mixture that (1-4) is formulated.
  7. 7. the method for electrorefining diamond large single crystal Synthetic block as described in claim 1, which is characterized in that the step 3) Cathode plate is made of iron or titanium material.
  8. 8. the method for electrorefining diamond large single crystal Synthetic block as described in claim 1, which is characterized in that the step 4) Electrolysis time is 3-4h.
CN201711298292.1A 2017-12-08 2017-12-08 Method for electrolytic purification of large diamond monocrystal synthetic block Active CN108048914B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201711298292.1A CN108048914B (en) 2017-12-08 2017-12-08 Method for electrolytic purification of large diamond monocrystal synthetic block

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201711298292.1A CN108048914B (en) 2017-12-08 2017-12-08 Method for electrolytic purification of large diamond monocrystal synthetic block

Publications (2)

Publication Number Publication Date
CN108048914A true CN108048914A (en) 2018-05-18
CN108048914B CN108048914B (en) 2023-11-07

Family

ID=62123652

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201711298292.1A Active CN108048914B (en) 2017-12-08 2017-12-08 Method for electrolytic purification of large diamond monocrystal synthetic block

Country Status (1)

Country Link
CN (1) CN108048914B (en)

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1068153A (en) * 1991-06-22 1993-01-20 中国有色金属工业总公司矿产地质研究院 Artificial diamond purifying apparatus using electrical power to remove catalyst metal
CN1454853A (en) * 2002-04-29 2003-11-12 三国株式会社 Anolyte and its making method
CN101049929A (en) * 2007-05-18 2007-10-10 河南中南工业有限责任公司 Technical method for electrorefining diamond
CN101556225A (en) * 2009-05-22 2009-10-14 北京科技大学 Method adopting neutral salt electrolyte to electrolytically extract tiny impurities from steel
CN103898552A (en) * 2014-04-01 2014-07-02 安庆市凯立金刚石科技有限公司 Formula of diamond synthesis and purification rapid electrolyte
CN104328476A (en) * 2014-09-16 2015-02-04 邯郸学院 Electrolyte and method for removing color spots on surface of silverware by use of electrolyte
CN104562080A (en) * 2013-10-18 2015-04-29 浙江蓝龙科技有限公司 Electrolyte solution for electrolyzing diamond synthesis column and using method of electrolyte solution
CN104986761A (en) * 2015-06-25 2015-10-21 河南黄河旋风股份有限公司 Efficient electrolyte purified through artificial diamond
CN106365161A (en) * 2016-08-19 2017-02-01 富耐克超硬材料股份有限公司 Diamond purification method and use thereof

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1068153A (en) * 1991-06-22 1993-01-20 中国有色金属工业总公司矿产地质研究院 Artificial diamond purifying apparatus using electrical power to remove catalyst metal
CN1454853A (en) * 2002-04-29 2003-11-12 三国株式会社 Anolyte and its making method
CN101049929A (en) * 2007-05-18 2007-10-10 河南中南工业有限责任公司 Technical method for electrorefining diamond
CN101556225A (en) * 2009-05-22 2009-10-14 北京科技大学 Method adopting neutral salt electrolyte to electrolytically extract tiny impurities from steel
CN104562080A (en) * 2013-10-18 2015-04-29 浙江蓝龙科技有限公司 Electrolyte solution for electrolyzing diamond synthesis column and using method of electrolyte solution
CN103898552A (en) * 2014-04-01 2014-07-02 安庆市凯立金刚石科技有限公司 Formula of diamond synthesis and purification rapid electrolyte
CN104328476A (en) * 2014-09-16 2015-02-04 邯郸学院 Electrolyte and method for removing color spots on surface of silverware by use of electrolyte
CN104986761A (en) * 2015-06-25 2015-10-21 河南黄河旋风股份有限公司 Efficient electrolyte purified through artificial diamond
CN106365161A (en) * 2016-08-19 2017-02-01 富耐克超硬材料股份有限公司 Diamond purification method and use thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
赵月秋,胡跃华,李华,胡国程: "人造金钢石快速电解提纯工艺研究", 湖南冶金, no. 03, pages 5 - 7 *

Also Published As

Publication number Publication date
CN108048914B (en) 2023-11-07

Similar Documents

Publication Publication Date Title
CN105914375B (en) A kind of preparation method of the disulphide and graphene composite material of molybdenum or tungsten
CN102618903B (en) Anode special for oxidation of deep hole aluminum piece hard anode and oxidation method of deep hole aluminum piece hard anode
CN109264835A (en) Continuous electrochemical element extraction system
CN103266343B (en) The surface roughening approach of metallic substance
CN102230208B (en) Special anode of plating chromium on cavity of slender pipe and chromium plating method thereof
CN103898552B (en) The synthetic purification quick electrolysis liquid of a kind of diamond
CN103160868A (en) Electrolyte for producing active nickel with sulfur and use method thereof
CN108048914A (en) A kind of method of electrorefining diamond large single crystal Synthetic block
CN210711782U (en) Oxidation tool of inside lining
CN207552497U (en) A kind of anode clamp suitable for diamond large single crystal Synthetic block electrorefining
CN105624721B (en) One kind prepares copper amine(Ammonia)The method of complex compound
CN101012571B (en) Anode poling processing technique before electric plating
CN113293411B (en) Gradient composite lead dioxide anode plate and preparation method and application thereof
CN110342618B (en) Device and method for cooperatively treating pickling waste liquid and electroplating sludge by utilizing electrodialysis technology
CN210458373U (en) Bipolar electrolysis device
CN106350835A (en) Manufacture method of rare earth anode plate in electrolytic manganese electrolysis process
CN209397292U (en) A kind of strip electrolytic cleaned electrode plate
CN102206849B (en) Device for removing harmful impurities from chromeplating solution
JPS5475497A (en) Electrolyzing method for aqueous solution of sodium chloride
CN108620961A (en) The surface roughening approach of metal material
CN109881217A (en) Manganese electrodeposition carbon fiber-based amorphous state Pb-Mn-RuOx gradient anode material and preparation method
CN207567376U (en) A kind of correction silk electrochemical polish tooling
CN104562172A (en) Electrolytic polishing method for aluminum alloy workpieces
CN201933185U (en) Electroplating structure for wire tinning
CN202530185U (en) Platelike titanium alloy anodic oxidation fixture

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant