CN110144618A - Method for removing metallic cobalt in polycrystalline diamond compact - Google Patents
Method for removing metallic cobalt in polycrystalline diamond compact Download PDFInfo
- Publication number
- CN110144618A CN110144618A CN201910478653.3A CN201910478653A CN110144618A CN 110144618 A CN110144618 A CN 110144618A CN 201910478653 A CN201910478653 A CN 201910478653A CN 110144618 A CN110144618 A CN 110144618A
- Authority
- CN
- China
- Prior art keywords
- diamond
- composite polycrystal
- electrolysis
- electrolyte
- metallic cobalt
- 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.)
- Pending
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- 239000010432 diamond Substances 0.000 title claims abstract description 59
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 58
- 229910017052 cobalt Inorganic materials 0.000 title claims abstract description 42
- 239000010941 cobalt Substances 0.000 title claims abstract description 42
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 32
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 34
- 239000003792 electrolyte Substances 0.000 claims abstract description 32
- 239000010935 stainless steel Substances 0.000 claims abstract description 18
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 18
- 238000002360 preparation method Methods 0.000 claims abstract description 5
- 239000002131 composite material Substances 0.000 claims description 41
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 26
- 229910045601 alloy Inorganic materials 0.000 claims description 17
- 239000000956 alloy Substances 0.000 claims description 17
- 239000011780 sodium chloride Substances 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 238000000354 decomposition reaction Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims 4
- 150000001336 alkenes Chemical class 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 6
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 235000013495 cobalt Nutrition 0.000 description 31
- 239000001103 potassium chloride Substances 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 5
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 229910009043 WC-Co Inorganic materials 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000005087 graphitization Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 230000009972 noncorrosive effect Effects 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F3/00—Electrolytic etching or polishing
- C25F3/02—Etching
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
Abstract
The invention belongs to the field of superhard material preparation, and particularly relates to a method for removing metallic cobalt in a polycrystalline diamond compact, which comprises the steps of taking a PCD part of the polycrystalline diamond compact as an anode and a stainless steel plate as a cathode, electrically connecting an electrolysis power supply, immersing the PCD part and the stainless steel plate into electrolyte for electrolysis, wherein the pH value of the electrolyte is 7, and the electrolysis voltage is 1.5-3V. The invention utilizes the principle of electrolysis, has simple process, low cost and no corrosiveness, and can effectively solve the series problems of corrosiveness, high requirement on equipment and easy environmental pollution of the conventional electrolyte for electrolytic cobalt removal.
Description
Technical field
The invention belongs to metallic cobalts in superhard material preparation field more particularly to a kind of removal composite polycrystal-diamond
Method.
Background technique
Superhard material is primarily referred to as diamond and cubic boron nitride, and superhard material is suitable for being used to manufacturing processing other materials
Tool has unrivaled superiority, occupies irreplaceable critical role especially in terms of processing hard material.It is poly-
Diamond (PCD) composite sheet is in high temperature and pressure by many fine-particle diamonds and cemented carbide substrate joint sintering
Made of bulk agglomerate.It has high intensity, high rigidity, high-wearing feature and high toughness.As machining tool,
PCD is mainly used for petroleum, metallurgy, geological drill bit, reamer etc., and rate of penetration and timeliness are many of natural diamond
Times, while aperture can also be effectively kept in drilling process.
In the production process of composite polycrystal-diamond, a certain amount of Co powder can be added, to promote diadust shape
At polycrystalline diamond.However due to friction in the use process of composite polycrystal-diamond, impact can generate high temperature, a side
The thermal expansion coefficient of face, Co phase and diamond has larger difference, can generate biggish internal stress under high temperature, will cause diamond
Crystal grain falls off and the case where disintegrating tablet；On the other hand, in the case of a high temperature, Co, which meets, promotes diamond graphitization, to reduce
The wearability and service life of product.Therefore in composite sheet before use, needing to remove the cobalt of a part.
Commonly de- cobalt method has chemical method and two kinds of electrolysis method both at home and abroad at present, and the selection of the solution of both methods is logical
Acid or alkalinity condition is often needed, either acid or alkali is all harmful for environment, due to the corrosivity of soda acid, is held
The safety of staff easily is threatened, and hard alloy can be corroded, and the de- cobalt rate of existing de- cobalt method is lower, cost
Height can no longer meet current production needs.
Summary of the invention
The object of the present invention is to provide it is a kind of removal composite polycrystal-diamond in metallic cobalt method, present invention utilizes
The principle of electrolysis, simple process and low cost and non-corrosive can effectively solve the problem that and current be electrolysed de- cobalt electrolyte and have corruption
Corrosion, the high requirements on the equipment and environment series problem easy to pollute.
In order to solve the above technical problems, The technical solution adopted by the invention is as follows:
A kind of method of metallic cobalt in removal composite polycrystal-diamond, including using the portion PCD of composite polycrystal-diamond as
Anode, stainless steel plate as cathode and are electrically connected electrolysis power, and the portion PCD and stainless steel plate are immersed in electrolyte and are electrolysed, described
The pH of electrolyte is 7, and decomposition voltage is 1.5-3V.
Specifically, the electrolyte is made of the electrolyte that quality proportioning is 1-8:90-110 and water.
Preferably, the electrolyte is one of NaCl, KCl or mixing.
Preferably, the electrolyte has quality proportioning to be mixed for NaCl, KCl and water of 1-3:3-5:90-110.
Preferably, the electrolyte has quality proportioning to be mixed for NaCl, KCl and water of 2:4:100.
Preferably, the electrolyte has quality proportioning to be mixed for NaCl, KCl and water of 3:5:100.
Preferably, it also needs to carry out package processing to the hard alloy portion of composite polycrystal-diamond before the electrolysis.
Preferably, the package processing is as follows, is passing through magnet for the hard alloy of conducting wire and composite polycrystal-diamond
After portion's electrical connection, it is set to be isolated from the outside hard alloy portion surface package using polytetrafluoroethylene (PTFE).
Specifically, the method for removing metallic cobalt in composite polycrystal-diamond, steps are as follows:
1) prepare electrolysis power, electrolytic cell, and will connect the positive and negative conducting wire of electrolysis power respectively with composite polycrystal-diamond
Hard alloy portion and stainless steel plate electrical connection；
2) preparation electrolyte is taken by the mass ratio, the portion PCD of composite polycrystal-diamond and stainless steel plate is placed in electrolyte
In, electrolysis power is powered and voltage is that 1.5 ~ 3V carries out electrolysis 20-30 hours.
Electrolysis method of the invention takes off cobalt principle: using the portion PCD of composite polycrystal-diamond as anode, stainless steel plate is made
For cathode, preferably the mixed solution of NaCl, KCl or NaCl and KCl are as electrolyte, by the PCD of composite polycrystal-diamond
Portion is soaked in the electrolytic solution, and hard alloy portion and air and electrolyte completely cut off, and under the action of decomposition voltage, the Co atom of anode is lost
De-electromation is oxidized to Co2+(the later period Co of cell reaction2+It is oxidized to Co again3+), the H of cathode2O obtains electronics and is reduced
At H2And OH-, under the action of electric field, Co ion and OH-It is detached from anode and cathode respectively, enters and forms Co(OH in solution)2
Precipitating, so that the cobalt in the portion PCD be removed.
Since composite polycrystal-diamond is by polycrystalline diamond portion, that is, portion PCD and hard alloy portion (WC-Co) two parts group
At polycrystalline diamond portion is for being ground and being crushed, and hard alloy one end is used to fix polycrystalline diamond portion, and the other end is then used to weld
Connect bit matrix.Due to also containing cobalt in hard alloy portion, reaction also will do it in electrolysis, therefore the present invention is to hard alloy
Portion has carried out the processing of surface package, for completely cutting off air and electrolyte.
Compared with the prior art, the invention has the following advantages: present invention employs neutral electrolyte, with polycrystalline diamond
Portion is anode, and stainless steel plate is cathode, by the effect of decomposition voltage, has carried out de- cobalt to polycrystalline diamond portion and has handled, thus
The service life and wear-resisting property of composite polycrystal-diamond are increased, preparation process of the present invention is simple, without any corrosive goods
Matter, it is low in cost, and the cobalt in polycrystalline diamond portion can be effectively removed, can effectively solve the problem that existing de- cobalt method it is existing at
The serial problem such as this higher, complex process, environmental pollution.Using the method for the present invention for being electrolysed de- cobalt, it is bright to take off cobalt effect
It is aobvious, 500 ~ 800 microns of de- cobalt depth can be reached.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
Embodiment 1
A kind of method of metallic cobalt in removal composite polycrystal-diamond, steps are as follows:
1) prepare electrolysis power, electrolytic cell, and will connect the positive and negative conducting wire of electrolysis power respectively with composite polycrystal-diamond
Hard alloy portion and stainless steel plate electrical connection；
2) it takes NaCl, KCl and water to prepare electrolyte by the mass ratio of 2:4:100, then electrolyte is poured into electrolytic cell, then will
In the portion PCD of composite polycrystal-diamond and stainless steel plate merging electrolyte, electrolysis power is powered, initial voltage 0.73V, so
After be slowly increased to 1.5V, the cobalt at this time it can be observed that cathode has bubble generation, with the progress of reaction, in polycrystalline diamond
It is gradually removed, taking off the cobalt time is that for 24 hours, taking off cobalt depth is 500 microns.
Embodiment 2
A kind of method of metallic cobalt in removal composite polycrystal-diamond, steps are as follows:
1) prepare electrolysis power, electrolytic cell, and will connect the positive and negative conducting wire of electrolysis power respectively with composite polycrystal-diamond
Hard alloy portion and stainless steel plate electrical connection；
2) it takes NaCl, KCl and water to prepare electrolyte by the mass ratio of 3:5:100, then electrolyte is poured into electrolytic cell, then will
In the portion PCD of composite polycrystal-diamond and stainless steel plate merging electrolyte, electrolysis power is powered, initial voltage 0.73V, so
After be slowly increased to 1.5V, the cobalt at this time it can be observed that cathode has bubble generation, with the progress of reaction, in polycrystalline diamond
It is gradually removed, taking off the cobalt time is that for 24 hours, taking off cobalt depth is 550 microns.
Embodiment 3
A kind of method of metallic cobalt in removal composite polycrystal-diamond, steps are as follows:
1) prepare electrolysis power, electrolytic cell, and will connect the positive and negative conducting wire of electrolysis power respectively with composite polycrystal-diamond
Hard alloy portion and stainless steel plate electrical connection；
2) it takes NaCl, KCl and water to prepare electrolyte by the mass ratio of 3:5:100, then electrolyte is poured into electrolytic cell, then will
In the portion PCD of composite polycrystal-diamond and stainless steel plate merging electrolyte, electrolysis power is powered, initial voltage 0.73V, so
After be slowly increased to 2.0V, the cobalt at this time it can be observed that cathode has bubble generation, with the progress of reaction, in polycrystalline diamond
It is gradually removed, taking off the cobalt time is that for 24 hours, taking off cobalt depth is 800 microns.
Claims (9)
1. a kind of method of metallic cobalt in removal composite polycrystal-diamond, including the portion the PCD work with composite polycrystal-diamond
As cathode and it is electrically connected electrolysis power for anode, stainless steel plate, the portion PCD and stainless steel plate are immersed in electrolyte and are electrolysed,
It is characterized in that, the pH of the electrolyte is 7, and decomposition voltage is 1.5-3V.
2. removing the method for metallic cobalt in composite polycrystal-diamond as described in claim 1, which is characterized in that the electrolysis
Liquid is made of the electrolyte that quality proportioning is 1-8:90-110 and water.
3. removing the method for metallic cobalt in composite polycrystal-diamond as claimed in claim 2, which is characterized in that the electrolysis
Matter is one of NaCl, KCl or mixing.
4. removing the method for metallic cobalt in composite polycrystal-diamond as claimed in claim 3, which is characterized in that the electrolysis
Liquid is mixed by NaCl, KCl that quality proportioning is 1-3:3-5:90-110 and water.
5. removing the method for metallic cobalt in composite polycrystal-diamond as claimed in claim 4, which is characterized in that the electrolysis
Liquid is mixed by NaCl, KCl that quality proportioning is 2:4:100 and water.
6. removing the method for metallic cobalt in composite polycrystal-diamond as claimed in claim 4, which is characterized in that the electrolysis
Liquid is mixed by NaCl, KCl that quality proportioning is 3:5:100 and water.
7. removing the method for metallic cobalt in composite polycrystal-diamond as described in claim 1, which is characterized in that the electrolysis
It is preceding also to need to carry out package processing to the hard alloy portion of composite polycrystal-diamond.
8. removing the method for metallic cobalt in composite polycrystal-diamond as claimed in claim 7, which is characterized in that the package
Processing is as follows, after being electrically connected the hard alloy portion of conducting wire and composite polycrystal-diamond by magnet, using polytetrafluoroethyl-ne
Hard alloy portion surface package is made it be isolated from the outside by alkene.
9. the method for metallic cobalt in removal composite polycrystal-diamond a method as claimed in any one of claims 1-8, which is characterized in that step
It is rapid as follows:
1) prepare electrolysis power, electrolytic cell, and will connect the positive and negative conducting wire of electrolysis power respectively with composite polycrystal-diamond
Hard alloy portion and stainless steel plate electrical connection；
2) preparation electrolyte is taken by the mass ratio, the portion PCD of composite polycrystal-diamond and stainless steel plate is placed in electrolyte
In, electrolysis power is powered and voltage is that 1.5 ~ 3V carries out electrolysis 20-30 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910478653.3A CN110144618A (en) | 2019-06-03 | 2019-06-03 | Method for removing metallic cobalt in polycrystalline diamond compact |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910478653.3A CN110144618A (en) | 2019-06-03 | 2019-06-03 | Method for removing metallic cobalt in polycrystalline diamond compact |
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| Publication Number | Publication Date |
|---|---|
| CN110144618A true CN110144618A (en) | 2019-08-20 |
Family
ID=67590348
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910478653.3A Pending CN110144618A (en) | 2019-06-03 | 2019-06-03 | Method for removing metallic cobalt in polycrystalline diamond compact |
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| Country | Link |
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| CN (1) | CN110144618A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113445117A (en) * | 2021-06-29 | 2021-09-28 | 中国地质大学（武汉） | Electrolytic method and device for removing metallic cobalt in polycrystalline diamond compact |
| CN115125537A (en) * | 2022-08-05 | 2022-09-30 | 四川轻化工大学 | Method for removing cobalt in polycrystalline diamond compact |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0461756A1 (en) * | 1990-05-09 | 1991-12-18 | Ykk Corporation | Electrolytic machining using pulsed electric current |
| US6866769B2 (en) * | 2001-11-14 | 2005-03-15 | General Electric Company | Drive head and ECM method and tool for making same |
| CN104389012A (en) * | 2014-10-21 | 2015-03-04 | 西南石油大学 | Preparation method of cobalt-removed PDC (polycrystalline diamond) composite sheet |
| CN104862771A (en) * | 2015-05-28 | 2015-08-26 | 吉林大学 | Method for removing partial metal cobalt in polycrystalline diamond compact by electrolytic method |
| JP2015231642A (en) * | 2014-06-09 | 2015-12-24 | 三菱電機株式会社 | Electrolytic processing method and electrolytic processing device for hard metal |
| CN105705283A (en) * | 2013-11-05 | 2016-06-22 | 三菱电机株式会社 | Electrochemical machining method, electrochemical machining device, and electrochemical machining solution |
-
2019
- 2019-06-03 CN CN201910478653.3A patent/CN110144618A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0461756A1 (en) * | 1990-05-09 | 1991-12-18 | Ykk Corporation | Electrolytic machining using pulsed electric current |
| US6866769B2 (en) * | 2001-11-14 | 2005-03-15 | General Electric Company | Drive head and ECM method and tool for making same |
| CN105705283A (en) * | 2013-11-05 | 2016-06-22 | 三菱电机株式会社 | Electrochemical machining method, electrochemical machining device, and electrochemical machining solution |
| JP2015231642A (en) * | 2014-06-09 | 2015-12-24 | 三菱電機株式会社 | Electrolytic processing method and electrolytic processing device for hard metal |
| CN104389012A (en) * | 2014-10-21 | 2015-03-04 | 西南石油大学 | Preparation method of cobalt-removed PDC (polycrystalline diamond) composite sheet |
| CN104862771A (en) * | 2015-05-28 | 2015-08-26 | 吉林大学 | Method for removing partial metal cobalt in polycrystalline diamond compact by electrolytic method |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113445117A (en) * | 2021-06-29 | 2021-09-28 | 中国地质大学（武汉） | Electrolytic method and device for removing metallic cobalt in polycrystalline diamond compact |
| CN115125537A (en) * | 2022-08-05 | 2022-09-30 | 四川轻化工大学 | Method for removing cobalt in polycrystalline diamond compact |
| CN115125537B (en) * | 2022-08-05 | 2023-04-11 | 四川轻化工大学 | Method for removing cobalt in polycrystalline diamond compact |
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Application publication date: 20190820 |