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 PDFInfo
- 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
Links
- 239000013078 crystal Substances 0.000 title claims abstract description 62
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 59
- 239000010432 diamond Substances 0.000 title claims abstract description 59
- 238000000034 method Methods 0.000 title claims abstract description 20
- 239000003792 electrolyte Substances 0.000 claims abstract description 16
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000012190 activator Substances 0.000 claims abstract description 10
- 239000003381 stabilizer Substances 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000004140 cleaning Methods 0.000 claims abstract description 6
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 6
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 10
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 5
- 239000011668 ascorbic acid Substances 0.000 claims description 5
- 229960005070 ascorbic acid Drugs 0.000 claims description 5
- 235000010323 ascorbic acid Nutrition 0.000 claims description 5
- 229910052742 iron Inorganic materials 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 239000011780 sodium chloride Substances 0.000 claims description 5
- 239000001509 sodium citrate Substances 0.000 claims description 5
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 5
- 239000010936 titanium Substances 0.000 claims description 5
- 229910052719 titanium Inorganic materials 0.000 claims description 5
- AEQDJSLRWYMAQI-UHFFFAOYSA-N 2,3,9,10-tetramethoxy-6,8,13,13a-tetrahydro-5H-isoquinolino[2,1-b]isoquinoline Chemical compound C1CN2CC(C(=C(OC)C=C3)OC)=C3CC2C2=C1C=C(OC)C(OC)=C2 AEQDJSLRWYMAQI-UHFFFAOYSA-N 0.000 claims description 3
- 229960001790 sodium citrate Drugs 0.000 claims description 3
- 235000011083 sodium citrates Nutrition 0.000 claims description 3
- 239000000176 sodium gluconate Substances 0.000 claims description 3
- 229940005574 sodium gluconate Drugs 0.000 claims description 3
- 235000012207 sodium gluconate Nutrition 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 230000004913 activation Effects 0.000 claims 1
- 230000005611 electricity Effects 0.000 claims 1
- 229910052751 metal Inorganic materials 0.000 abstract description 9
- 239000002184 metal Substances 0.000 abstract description 9
- 239000002253 acid Substances 0.000 abstract description 5
- 238000002848 electrochemical method Methods 0.000 abstract description 2
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 238000007747 plating Methods 0.000 abstract description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- 239000004575 stone Substances 0.000 description 3
- 238000006424 Flood reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- NICDRCVJGXLKSF-UHFFFAOYSA-N nitric acid;trihydrochloride Chemical compound Cl.Cl.Cl.O[N+]([O-])=O NICDRCVJGXLKSF-UHFFFAOYSA-N 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- UPMFZISCCZSDND-JJKGCWMISA-M sodium gluconate Chemical compound [Na+].OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C([O-])=O UPMFZISCCZSDND-JJKGCWMISA-M 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-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
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-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
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/04—Diamond
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
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)
- 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. 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. 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. 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. 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. 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. 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. 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.
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