CN107620119A - A kind of activation method for the electrochemical polish liquid that fails - Google Patents
A kind of activation method for the electrochemical polish liquid that fails Download PDFInfo
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- CN107620119A CN107620119A CN201710833692.1A CN201710833692A CN107620119A CN 107620119 A CN107620119 A CN 107620119A CN 201710833692 A CN201710833692 A CN 201710833692A CN 107620119 A CN107620119 A CN 107620119A
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Abstract
The invention provides a kind of activation method for the electrochemical polish liquid that fails, including：The failure electrochemical polish liquid is electrolysed；The temperature of the electrolysis is 30~90 DEG C；The electric current of the electrolysis is 30~120A.Method provided by the invention, by institute's limiting temperature and the electrolytic process of amperage conditions, effective removal of moisture in failure electrochemical polish liquid is realized, solves the polishing fluid Problem of Failure caused by the water imbibition of polishing fluid itself.The present invention is on the basis of electrolysis removes water, handled by the way that acid is heavy with ingredient balance, the metal ion in failure electrochemical polish liquid can effectively be removed, and composition is able to equilibrium in polishing fluid, meet the requirement that polishing fluid reuses, solve due to the Problem of Failure of polishing fluid caused by the metal ion that polishing process gradually increases.
Description
Technical field
The present invention relates to electrochemical polish liquid technical field, more particularly to a kind of activation side for the electrochemical polish liquid that fails
Method.
Background technology
Being the crucial manufacturing procedure before intermetallic composite coating is processed by shot blasting to metal parts surface, electrochemical polish is thrown with it
The advantages such as flatness is high after light, polishing speed is fast receive significant attention.The operation principle of electrochemical polish is by polished workpiece
Anode is placed in, as negative electrode under the conditions of certain temperature, Current Voltage, redox occurs in polishing fluid for inert electrode anti-
The polishing for treating polishing workpiece surface should be realized.
But electrochemical polish liquid during using and depositing often because the concentrated sulfuric acid or concentrated phosphoric acid are to moisture in air
Absorption so that in polishing fluid bulk composition content decline；Meanwhile as glossing is constantly carried out, in polishing process,
Produce concentration of the metal ion in polishing solution to increase severely, through after a period of time, electrochemical polish liquid further makes
Influenceed with meeting by certain, can cause the failure of electrochemical polish liquid, it is difficult to be recycled for a long time.
In order to improve the use value of failure electrochemical polish liquid, at present, people are more by the way of blending, i.e., from failure
The polishing fluid that do not fail for adding respective amount after a part of polishing fluid again is taken out in electrochemical polish liquid, with enable polishing fluid after
It is continuous to use.However, the method blent, simply the problem of temporary alleviation electrochemical failure, does not efficiently solve reality really
Border problem, with the continuous progress of glossing, the failure polishing fluid of accumulation can be more and more, necessarily lead to can not handle it is useless
Liquid can increase severely.
The content of the invention
In view of this, it is provided by the invention it is an object of the invention to provide a kind of activation method of electrochemical polish liquid
Method, can fundamentally solve electrochemical polish liquid Problem of Failure, improve the service life of electrochemical polish liquid.
The invention provides a kind of activation method for the electrochemical polish liquid that fails, including：To the failure electrochemical polish
Liquid is electrolysed；The temperature of the electrolysis is 30~90 DEG C；The electric current of the electrolysis is 30~120A.
Preferably, the time of the electrolysis is 72~96h.
Preferably, the water content of the failure electrochemical polish liquid is >=10wt%.
Preferably, when metal ion total concentration is not less than 20g/L in the failure electrochemical polish liquid, after the electrolysis
Also include：By the sour heavy and ingredient balance processing of electrolyte progress for being electrolysed and obtaining.
Preferably, the acid, which sinks, is：Concentrated sulfuric acid solution is mixed with the electrochemical polish liquid after electrolysis.
Preferably, the mass concentration of the concentrated sulfuric acid solution is 98%；
The dosage of the concentrated sulfuric acid solution in the electrochemical polish liquid that fails on the basis of metal ion content to count, sulfuric acid and gold
The mol ratio for belonging to ion is (8~15)：1.
Preferably, the ingredient balance, which is handled, is：Filtrate of the acid after heavy is mixed with phosphoric acid solution and additive；
The additive includes thiocarbamide, ammonium citrate, monohydrate potassium, diethylene triamine pentacetic acid (DTPA), ammonium sulfate and sweet
One or more in oil.
Preferably, the mass concentration of the phosphoric acid solution is 85%.
Preferably, the mass ratio of the phosphoric acid solution and concentrated sulfuric acid solution is (2~3)：1.
Preferably, the mass ratio of the additive and phosphoric acid solution is (3~4)：(150~200).
The invention provides a kind of activation method for the electrochemical polish liquid that fails, including：To the failure electrochemical polish
Liquid is electrolysed；The temperature of the electrolysis is 30~90 DEG C；The electric current of the electrolysis is 30~120A.Side provided by the invention
Method, by institute's limiting temperature and the electrolytic process of amperage conditions, realize that the effective of moisture goes in failure electrochemical polish liquid
Remove, solve the polishing fluid Problem of Failure caused by the water imbibition of polishing fluid itself.
Further, the present invention is sunk by acid on the basis of electrolysis removes water and ingredient balance is handled, can effectively removed
Metal ion in failure electrochemical polish liquid, and composition is able to equilibrium in polishing fluid, meets the requirement that polishing fluid reuses,
The Problem of Failure of polishing fluid caused by the metal ion that solution gradually increases due to polishing process.
Brief description of the drawings
Fig. 1 is water content of the electrochemical polish liquid in polishing process and is polished the relation song of Hastelloy base band length
Line；
Fig. 2 is phosphorus acid content and sulfuric acid content of the electrochemical polish liquid in polishing process with being polished Hastelloy base band
The relation curve of length；
Fig. 3 is metal ion content of the electrochemical polish liquid in polishing process and is polished Hastelloy base band length
Relation curve.
Embodiment
The invention provides a kind of activation method for the electrochemical polish liquid that fails, including：To the failure electrochemical polish
Liquid is electrolysed；The temperature of the electrolysis is 30~90 DEG C；The electric current of the electrolysis is 30~120A.
Method provided by the invention realizes failure electrochemistry by institute's limiting temperature and the electrolytic process of amperage conditions
Effective removal of moisture in polishing fluid, solves the polishing fluid Problem of Failure caused by the water imbibition of polishing fluid itself.
The present invention is electrolysed to the failure electrochemical polish liquid.In the present invention, the failure electricity of required activation process
Chemical polishing solution is preferably due to absorption of the electrolyte to moisture in air so that solutes content reduces in electrolyte, it is difficult to full
The failure electrochemical electrolysis liquid that foot electrolysis is required and formed.The present invention is not special to the composition of the failure electrochemical polish liquid
It is required that using failure electrochemical polish liquid well-known to those skilled in the art；In an embodiment of the present invention, the mistake
Effect electrochemical polish liquid is specially Hastelloy failure electrochemical polish liquid.
In the present invention, it is described failure electrochemical polish liquid water content preferably >=10wt%, further preferably >=
15wt%, more preferably >=20wt%, most preferably 25~50wt%.
In the present invention, the temperature of the electrolysis is 30~90 DEG C, preferably 35~85 DEG C, more preferably 40~70
DEG C, more preferably 50~60 DEG C.In the present invention, the current strength of the electrolysis is 30~120A, preferably 35~110A, is entered
One step is preferably 40~100A, more preferably 50~80A；In the present invention, the voltage of electrolysis can with current strength difference and
Change.In the present invention, the time of the electrolysis is preferably 72~96h, more preferably 75~90h, more preferably
80~85h.The present invention does not have particular/special requirement to the implementation of electrolysis, using electrolysis unit well-known to those skilled in the art
；In an embodiment of the present invention, electrolysis unit is specially the electrolytic cell of semi-enclosed anti-strong acid.
In the present invention, the electrolysis is preferably carried out under ventilation condition；The ventilation condition preferably uses extractor fan
Realize, the present invention does not have particular/special requirement to the type of the extractor fan, is filled using exhausting well-known to those skilled in the art
Put.
After the electrolysis, the electrolyte after electrolysis described in preferred pair of the present invention is cooled down.In the present invention, the cooling
Temperature afterwards is preferably room temperature, more preferably 25~30 DEG C；In the present invention, the cooling is preferably natural cooling.This
Invention does not have particular/special requirement to the embodiment of the cooling, is using the type of cooling well-known to those skilled in the art
Can.
In the present invention, when metal ion total concentration is not less than 20g/L in the failure electrochemical polish liquid, the electricity
Preferably also include after solution:By the sour heavy and ingredient balance processing of electrolyte progress for being electrolysed and obtaining.In the present invention, required work
Change metal ion total concentration in the failure electrochemical polish liquid of processing and be preferably not lower than 20g/L, be more preferably not less than
25g/L, more preferably not less than 28g/L, most preferably 30~100g/L.The present invention is to the species of the metal ion without spy
It is different to require, any metal ion caused during electrolyte electrobrightening.
In the present invention, the acid is heavy is preferably：Concentrated sulfuric acid solution is mixed with the electrochemical polish liquid after electrolysis.At this
In invention, the dosage of the concentrated sulfuric acid solution in the electrochemical polish liquid that fails on the basis of metal ion content to count, the sulfuric acid
Mol ratio with metal ion is preferably (8~15)：1, more preferably (10~14)：1, more preferably 12：1.In this hair
In bright, the mass concentration of the sulfuric acid solution is preferably 98%.In the present invention, the concentrated sulfuric acid contributes to quick realize to polish
The deposition of metal ion separates out in liquid, and avoids the introducing of impurity.
The present invention does not have particular/special requirement to the source of the concentrated sulfuric acid solution, using sulphur well-known to those skilled in the art
The commercial goods of acid solution.
The present invention does not have particular/special requirement to the hybrid mode of the electrochemical polish liquid after the sulfuric acid and electrolysis, using ability
The hybrid mode of sulfuric acid and solution known to field technique personnel.In the present invention, the sulfuric acid and the electrification after electrolysis
During the mixing of optical polishing liquid, in the presence of the concentrated sulfuric acid, various metals salt is formed, is separated out with precipitation form；The precipitation is preferred
Including metal sulfate and metal phosphate.
The present invention is stood after preferably the mixed liquor of the sulfuric acid and electrochemical polish liquid is cooled down.In the present invention, it is described
The temperature of mixed liquor after cooling is preferably room temperature, more preferably 25~30 DEG C；The present invention does not have to the mode of the cooling
There is particular/special requirement, using the type of cooling well-known to those skilled in the art.In the present invention, the time of the standing is excellent
Elect 6~12h, more preferably 8~10h as.The present invention further realizes sulfuric acid and gold during the cooling and standing
Belong to the precipitation reaction of ion, fully remove metal ion.
Complete the acid it is heavy after, the filtrate after acid is heavy described in preferred pair of the present invention carries out ingredient balance processing.In the present invention
In, the filtrate after the acid is heavy to mixed liquor of the acid after heavy preferably by being filtrated to get.The present invention is to the filtering
Mode there is no particular/special requirement, using filter type well-known to those skilled in the art.It is described in the embodiment of the present invention
It is filtered through high pressure filter completion.
In the present invention, the ingredient balance processing preferably includes to mix filtrate of the acid after heavy with phosphoric acid solution and additive
Close.In the present invention, the mass ratio of the phosphoric acid solution and the concentrated sulfuric acid is preferably (2~3)：1, more preferably (2.5~
2.8)：1.In the present invention, the mass concentration of the phosphoric acid solution is preferably 85%.Source of the present invention to the phosphoric acid solution
There is no particular/special requirement, using the commercial goods of phosphoric acid solution well-known to those skilled in the art.Acid is sunk it by the present invention
Filtrate afterwards mixes with phosphoric acid, has both avoided the influence of the addition of phosphoric acid to the solubility in the heavy shallow lake of acid, it is ensured that the analysis of metal ion
Go out, and avoid dissolving the sediment that slow additive is precipitated and take away.
In the present invention, the additive preferably includes thiocarbamide, ammonium citrate, monohydrate potassium, diethylenetriamine five
One or more in acetic acid, ammonium sulfate and glycerine.The present invention is to the thiocarbamide, ammonium citrate, monohydrate potassium, divinyl
The source of pentaacetic acid (DPTA), ammonium sulfate and glycerine does not have particular/special requirement, is using well-known to those skilled in the art
Can.In the present invention, the glycerine that act as of the additive plays wetting action；Ammonium sulfate plays conductive salt action；Ammonium citrate, one
Citric acid monohydrate plays complexing agent effect in the solution；Thiocarbamide, diethylene triamine pentacetic acid (DTPA) play bright, leveling agent in the solution
Effect.
In the present invention, the mass ratio of the additive and phosphoric acid solution is preferably (3~4)：(150~200), further
Preferably (3.2~3.8)：(160~180).
The present invention is sunk by acid on the basis of electrolysis removes water and ingredient balance is handled, can effectively remove failure electrification
Metal ion in optical polishing liquid, and composition is able to equilibrium in polishing fluid, meets the requirement that polishing fluid reuses, solve due to
The Problem of Failure of polishing fluid caused by the metal ion that polishing process gradually increases
The invention provides a kind of activation method for the electrochemical polish liquid that fails, including：To the failure electrochemical polish
Liquid is electrolysed；The temperature of the electrolysis is 30~90 DEG C；The electric current of the electrolysis is 30~120A.Side provided by the invention
Method, by institute's limiting temperature and the electrolytic process of amperage conditions, realize that the effective of moisture goes in failure electrochemical polish liquid
Remove, solve the polishing fluid Problem of Failure caused by the water imbibition of polishing fluid itself.
The present invention is sunk by acid on the basis of electrolysis removes water and ingredient balance is handled, can effectively remove failure electrification
Metal ion in optical polishing liquid, and composition is able to equilibrium in polishing fluid, meets the requirement that polishing fluid reuses, solve due to
The Problem of Failure of polishing fluid caused by the metal ion that polishing process gradually increases.
Activation method provided by the invention, it is possible to increase the polishing effect of the electrochemical polish liquid of failure significantly improves, from
And reach and can be continuing with, extend the service life of polishing fluid indirectly, realize recycling for failure polishing fluid, effectively reduce danger
Dangerous, susceptibility-to-corrosion, harmful substance discharge caused by environmental pollution sex chromosome mosaicism.Method provided by the invention, simple to operate, peace
Complete and whole processing technology process ring, it is easy to operation, operation is repeated, is recycled.
In order to further illustrate the present invention, with reference to work of the embodiment to failure electrochemical polish liquid provided by the invention
Change method is described in detail, but they can not be interpreted as into limiting the scope of the present invention.
Embodiment 1
The failure procedure of electrochemical polish liquid：By density about 1.723g/cm3, water content about 3.64wt% Suzhou new material
The polishing fluid of the spontaneous development of Co., Ltd of research institute, shift in the electrolytic cell as semiclosed anti-strong acid corrosion, be heated to 40 DEG C,
Faradaic current is arranged to 80 amperes, decomposition voltage 20V, extractor fan is opened, on this condition, Hastelloy base band can be polished
7326 meters, it is pumped and is down to 0.10 by 0.30, the density of polishing fluid is by 1.723g/cm3It is down to 1.580g/cm3。
When being further continued for carrying out the electrochemical polish of Hastelloy base band using the polishing fluid, base band rough surface is not up to standard,
Base band after the polishing measured, it is base band its rough surface after measure polishing in 5 μ ms in the length of side under AFM
Degree is far above 1nm, reaches 2nm.Electrochemical polish liquid fails, it is impossible to is continuing with.
The water content of polishing fluid in polishing process is tested, with the continuous progress of polishing process, polishing fluid reclaimed water
Content is with being polished the relation curve of Hastelloy base band length as shown in figure 1, abscissa is length in Fig. 1；To polishing process
The phosphoric acid and sulfuric acid content of middle polishing fluid are tested, with the continuous progress of polishing process, phosphorus acid content and sulphur in polishing fluid
Acid content and the relation curve for being polished Hastelloy base band length are as shown in Figure 2；To the metal of polishing fluid in polishing process from
Sub- content is tested, and with the continuous progress of polishing process, metal ion content is with being polished Hastelloy base in polishing fluid
The relation curve of strip length is as shown in figure 3, abscissa is length in Fig. 3.
Analyzed from Fig. 1, Fig. 2, Fig. 3, with the continuous progress of electrochemical polish, in polishing process and polishing later stage people
It is improper to be safeguarded for factor, caused by water content is higher in polishing fluid and polishing process in caused metal ion in polishing fluid
Concentration is continuously increased, and sulfuric acid, phosphorus acid content can be caused significantly to decline, and finally, causes polishing fluid to fail, it is impossible to meets polishing
Technological requirement.
The activation of failure electrochemical polish liquid：By water content it is too high, it is caused failure polishing fluid go in semi-enclosed spy
In the electrolytic cell for making anti-highly acid corrosion, 30 DEG C are heated to, Faradaic current is arranged to 120 amperes, decomposition voltage is changed into therewith
5V, extractor fan is opened, after this condition heating electrolysis 72 hours, allow it to naturally cool to room temperature, polishing fluid density can be from original
First 1.580g/cm3It is increased to the density of electrochemical polish liquid needs, about 1.710g/cm3。
Polishing fluid after activated processing is reused for polishing to the polishing of Hastelloy base band：With vavuum pump by activation
In polishing fluid injection polishing pond after reason, it is slowly preheating to 80 DEG C or so, electrolysis power is opened, by polishing fluid Faradaic current
It is adjusted under 50 amperes, sets base band to carry out electrochemical polish with about 2m/min polishing velocity, thrown by this burnishing device
Kazakhstan metallurgy base band after light.
The Harbin metallurgy base band after polishing is observed using light microscope, finds base band surfacing, light；Adopt
Band is detected with laser, finds to significantly reduce compared with base band existing defects before polishing after polishing；AFM
Under, base band after the polishing measured, it is in 5 μ ms in the length of side, base band its surface roughness display numerical value after measure polishing is
0.5nm.It can be seen that after activated processing, the electrochemical polish liquid after failure can be reused for the polishing of metal surface.
It can be seen that the polishing fluid that will be obtained after activation process, when carrying out electrochemical polish, can efficiently remove sheet metal strip surface
Spot, significantly improve its surface smoothness, brightness, hence it is evident that to reduce its surface roughness.
Embodiment 2
The failure of electrochemical polish liquid：By the density about 1.710g/cm after the activation process of embodiment 13, water content about
4.74wt% electrochemical polish liquid, shift in the electrolytic cell as semiclosed anti-strong acid corrosion, 80 DEG C are heated to, by electrolysis electricity
Stream is arranged to 90 amperes, decomposition voltage 7V, opens extractor fan, on this condition, 24630 meters of polishing Hastelloy base band, pump
Pressure rises to 0.84 by 0.22, and density is by 1.710g/cm3Rise to 1.758g/cm3, it is further continued for carrying out Hastelloy using the polishing fluid
During the electrochemical polish of base band, base band rough surface is not up to standard, under AFM, base band after the polishing measured, in the length of side
For in 5 μ ms, base band its surface roughness after measure polishing be far above 1nm, reaches 5nm, electrochemical polish liquid fails, no
It can be continuing with.From pump pressure, variable density, now the concentration of metal ions in polishing fluid is higher, reach 21g/L, it is necessary to
Carry out activation process.
The activation of failure electrochemical polish liquid：Polishing fluid after above-mentioned failure is shifted as semi-enclosed special anti-strong acid
Property corrosion electrolytic cell in, be heated to 90 DEG C, Faradaic current be arranged to 30 amperes, decomposition voltage is changed into 40V therewith, and opening is taken out
Wind apparatus, it is 12 according to the mol ratio of sulfuric acid and metal ion after heating electrolysis 96h on this condition：1, it is dense to add 98wt%
Sulfuric acid, allow it to naturally cool to room temperature and placed for 12 hours, separate out a large amount of white depositions, this polishing fluid passes through high-pressure filteration
After device filtering, according to phosphoric acid solution and the mass ratio 3 of concentrated sulfuric acid solution:1, the mass ratio of additive and phosphoric acid solution is 4:200,
Add 200kg 85wt% concentrated phosphoric acids and 4kg additives, the composition of additive：Thiocarbamide, ammonium citrate, monohydrate potassium, two
Ethene pentaacetic acid (DPTA), ammonium sulfate and glycerine, the polishing fluid of electrochemical polishing process requirement can be met, polished
Concentration of metal ions in liquid is about 11g/L.
Polishing fluid after activated processing is reused for polishing Hastelloy using contactless electrochemical polishing process
The polishing of base band：At ambient temperature, Kazakhstan metallurgy base band is arranged on the guide wheel of burnishing device, by the electricity after activation process
Chemical polishing solution vavuum pump is injected in polishing pond, and it is slowly preheating to 40 DEG C or so, opens electrolysis power, by polishing fluid electricity
Solution electric current is adjusted to 130 amperes, sets base band to carry out electrochemical polish with about 2m/min polishing velocity, is obtained by this burnishing device
Kazakhstan metallurgy base band after must polishing.
The Harbin metallurgy base band after polishing is observed using light microscope, finds base band surfacing, light；Adopt
Band is detected with laser, finds to significantly reduce compared with base band existing defects before polishing after polishing；AFM
Under, base band after the polishing measured, it is that its surface roughness can reach below 1nm, reach 0.3nm in 5 μ ms in the length of side.Can
See, after activated processing, the electrochemical polish liquid after failure can be reused for the polishing of metal surface.
Embodiment 3
The failure of electrochemical polish liquid：By the density about 1.710g/cm after the activation process of embodiment 13, water content about
4.74wt% electrochemical polish liquid, shift in the electrolytic cell as semiclosed anti-strong acid corrosion, 80 DEG C are heated to, by electrolysis electricity
Stream is arranged to 90 amperes, decomposition voltage 7V, opens extractor fan, on this condition, 24630 meters of polishing Hastelloy base band, pump
Pressure rises to 0.84 by 0.22, and density is by 1.710g/cm3Rise to 1.758g/cm3, it is further continued for carrying out Hastelloy using the polishing fluid
During the electrochemical polish of base band, base band rough surface is not up to standard, under AFM, base band after the polishing measured, in the length of side
For in 5 μ ms, base band its surface roughness after measure polishing be far above 1nm, reaches 5nm, electrochemical polish liquid fails, no
It can be continuing with.From pump pressure, variable density, now the concentration of metal ions in polishing fluid is higher, reach 21g/L, it is necessary to
Carry out activation process.
The activation of failure electrochemical polish liquid：Polishing fluid after above-mentioned failure is shifted as semi-enclosed special anti-strong acid
Property corrosion electrolytic cell in, be heated to 90 DEG C, Faradaic current be arranged to 100 amperes, decomposition voltage is changed into 6V therewith, and opening is taken out
Wind apparatus, it is 15 according to the mol ratio of sulfuric acid and metal ion after heating electrolysis 72h on this condition：1, it is dense to add 98wt%
Sulfuric acid, allow it to naturally cool to room temperature and placed for 12 hours, separate out a large amount of white depositions, this polishing fluid passes through high-pressure filteration
After device filtering, according to phosphoric acid solution and the mass ratio 2 of concentrated sulfuric acid solution:1, the mass ratio of additive and phosphoric acid solution is 3:150,
Add 150kg 85wt% concentrated phosphoric acids and 3kg additives, the composition of additive：Thiocarbamide, ammonium citrate, monohydrate potassium, two
Ethene pentaacetic acid (DPTA), ammonium sulfate and glycerine, the polishing fluid of electrochemical polishing process requirement can be met, polished
Concentration of metal ions in liquid is about 9g/L.
Polishing fluid after activated processing is reused for polishing Hastelloy using contactless electrochemical polishing process
The polishing of base band：At ambient temperature, Kazakhstan metallurgy base band is arranged on the guide wheel of burnishing device, by the electricity after activation process
Chemical polishing solution vavuum pump is injected in polishing pond, and it is slowly preheating to 40 DEG C or so, opens electrolysis power, by polishing fluid electricity
Solution electric current is adjusted to 130 amperes, sets base band to carry out electrochemical polish with about 2m/min polishing velocity, is obtained by this burnishing device
Kazakhstan metallurgy base band after must polishing.
The Harbin metallurgy base band after polishing is observed using light microscope, finds base band surfacing, light；Adopt
Band is detected with laser, finds to significantly reduce compared with base band existing defects before polishing after polishing；AFM
Under, base band after the polishing measured, it is that its surface roughness can reach below 1nm, reach 0.2nm in 5 μ ms in the length of side.Can
See, after activated processing, the electrochemical polish liquid after failure can be reused for the polishing of metal surface.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of activation method for the electrochemical polish liquid that fails, including：The failure electrochemical polish liquid is electrolysed；It is described
The temperature of electrolysis is 30~90 DEG C；The electric current of the electrolysis is 30~120A.
2. activation method according to claim 1, it is characterised in that the time of the electrolysis is 72~96h.
3. activation method according to claim 1 or 2, it is characterised in that the water content of the failure electrochemical polish liquid
>=10wt%.
4. activation method according to claim 1, it is characterised in that when metal ion in the failure electrochemical polish liquid
When total concentration is not less than 20g/L, also include after the electrolysis：By the sour heavy and ingredient balance of electrolyte progress for being electrolysed and obtaining
Processing.
5. activation method according to claim 4, it is characterised in that the acid, which sinks, is：After concentrated sulfuric acid solution and electrolysis
Electrochemical polish liquid mixing.
6. activation method according to claim 5, it is characterised in that the mass concentration of the concentrated sulfuric acid solution is 98%；
The dosage of the concentrated sulfuric acid solution to be counted in the electrochemical polish liquid that fails on the basis of metal ion content, sulfuric acid and metal from
The mol ratio of son is (8~15)：1.
7. according to the activation method described in claim 4,5 or 6, it is characterised in that the ingredient balance, which is handled, is：By the acid
Filtrate after heavy mixes with phosphoric acid solution and additive；
The additive is included in thiocarbamide, ammonium citrate, monohydrate potassium, diethylene triamine pentacetic acid (DTPA), ammonium sulfate and glycerine
One or more.
8. activation method according to claim 7, it is characterised in that the mass concentration of the phosphoric acid solution is 85%.
9. activation method according to claim 8, it is characterised in that the mass ratio of the phosphoric acid solution and concentrated sulfuric acid solution
For (2~3)：1.
10. the activation method according to claim 7 or 9, it is characterised in that the mass ratio of the additive and phosphoric acid solution
For (3~4)：(150~200).
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103923571A (en) * | 2014-04-25 | 2014-07-16 | 苏州新材料研究所有限公司 | Polishing solution as well as preparation method and application of polishing solution |
| CN104141165A (en) * | 2013-05-10 | 2014-11-12 | 盛美半导体设备（上海）有限公司 | Polishing solution recycling apparatus |
| CN105568358A (en) * | 2016-03-21 | 2016-05-11 | 苏州新材料研究所有限公司 | Electrochemical polishing solution for Hastelloy substrate, and preparation method and polishing method of electrochemical polishing solution |
-
2017
- 2017-09-15 CN CN201710833692.1A patent/CN107620119B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104141165A (en) * | 2013-05-10 | 2014-11-12 | 盛美半导体设备（上海）有限公司 | Polishing solution recycling apparatus |
| CN103923571A (en) * | 2014-04-25 | 2014-07-16 | 苏州新材料研究所有限公司 | Polishing solution as well as preparation method and application of polishing solution |
| CN105568358A (en) * | 2016-03-21 | 2016-05-11 | 苏州新材料研究所有限公司 | Electrochemical polishing solution for Hastelloy substrate, and preparation method and polishing method of electrochemical polishing solution |
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