CN105331959A - Pole lug nickel strap surface treatment passivation solution - Google Patents
Pole lug nickel strap surface treatment passivation solution Download PDFInfo
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- CN105331959A CN105331959A CN201510730679.4A CN201510730679A CN105331959A CN 105331959 A CN105331959 A CN 105331959A CN 201510730679 A CN201510730679 A CN 201510730679A CN 105331959 A CN105331959 A CN 105331959A
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- nickel strap
- graphene
- passivation solution
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- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/24—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing hexavalent chromium compounds
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- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/24—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing hexavalent chromium compounds
- C23C22/26—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing hexavalent chromium compounds containing also organic compounds
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- C23C22/24—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing hexavalent chromium compounds
- C23C22/26—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing hexavalent chromium compounds containing also organic compounds
- C23C22/27—Acids
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- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
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- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/24—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing hexavalent chromium compounds
- C23C22/33—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing hexavalent chromium compounds containing also phosphates
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- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/34—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing fluorides or complex fluorides
- C23C22/37—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing fluorides or complex fluorides containing also hexavalent chromium compounds
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- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/34—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing fluorides or complex fluorides
- C23C22/37—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing fluorides or complex fluorides containing also hexavalent chromium compounds
- C23C22/38—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing fluorides or complex fluorides containing also hexavalent chromium compounds containing also phosphates
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- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/40—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing molybdates, tungstates or vanadates
- C23C22/43—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing molybdates, tungstates or vanadates containing also hexavalent chromium compounds
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- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/40—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing molybdates, tungstates or vanadates
- C23C22/44—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing molybdates, tungstates or vanadates containing also fluorides or complex fluorides
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- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
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Abstract
The invention discloses a pole lug nickel strap surface treatment passivation solution and a preparing method thereof. A composition comprises water, chromium trioxide, mineral acid and a film formation accelerant. By means of the pole lug nickel strap surface treatment passivation solution, the problems that the passivation film compactness is low, and the bonding performance between a film and pole lug glue is poor are solved.
Description
Technical field
The present invention relates to new energy resource power battery lug sheet field of surface treatment, especially, the present invention relates to nickel strap lug sheet Surface treatment passivation solution.
Background technology
Because having good intensity, excellent electroconductibility, thermal conductivity and plasticity-, new energy resource power battery lug sheet field has a wide range of applications Ni-based ultrafine powder.But, Ni-based ultrafine powder moist, containing the alkaline medium such as industrial gasses, fuel gas and salt solution in use time very easily there is the destruction of the forms such as spot corrosion, crevice corrosion, stress corrosion and corrosion fatigue, therefore, carrying out rotproofing to its surface is required technique.
Passivation Treatment is the effective means preventing nickel lug sheet to be corroded, and at present, conventional inactivating treatment liquid because of easily generation toxic substance and carcinogenic substance, and causes the pollution of harm to the mankind and the mankind.European Union formally implements " about prohibitting the use some Hazardous Substances Directive in electric/electronic device " on July 1st, 2006.Meanwhile, nickel lug sheet is carried out processing the binding property of the passive film of Passivation Treatment and tab poor.
Present stage is badly in need of by the improvement to formula, obtains a kind of nontoxic, good passivation effect, comparatively strong with the binding property of tab, and to the passivating solution that air is safe from harm.
Summary of the invention
In order to solve the problem, the invention provides a kind of environment-friendly type, binding property is strong, compactness is high and salt spray resistance is good passive film.
One aspect of the present invention provides a kind of lug nickel strap Surface treatment passivation solution, comprising:
Water 100;
Chromium trioxide 0.01-0.3;
Mineral acid 0.01-0.5;
Film forming accelerating 0.01-0.1.
As a kind of embodiment, described mineral acid is one or more in sulfuric acid, hydrochloric acid, phosphoric acid, perchloric acid, lactic acid, hydrofluoric acid, acetic acid.
As a kind of embodiment, described film forming accelerating is one or more in ammonium vanadate, strontium chloride, hydrofluoric acid, propanedioic acid, oxalic acid, pentanedioic acid, oxysuccinic acid, toxilic acid.
As a kind of embodiment, described lug nickel strap Surface treatment passivation solution also comprises the ring-type polyether compounds of 0.01-1 weight part and the mixture of modified graphene, and the structural formula of described ring-type polyether compounds is:
Wherein, R is amino, carboxyl, methylol, phenyl, acyl group or alkoxyl group;
X is one or more in O, S and N;
n=1-10。
As a kind of embodiment, described modified graphene is hydroxylation Graphene, carboxylated Graphene, sulfonic group functionalized graphene or amination Graphene.
As a kind of optimal way, described modified graphene is sulfonic group functionalized graphene or hydroxylation Graphene.
As a kind of optimal way, in described sulfonic group functionalized graphene, the ratio of S element is 5-10at%; In described hydroxylation Graphene and carboxylated Graphene, the ratio of O element is 5-15at%; In described amination Graphene, the ratio of N element is 10-20at%.
As a kind of embodiment, the mol ratio of described ring-type polyether compounds and modified graphene is 35-15:1.
The present invention provides a kind of metal surface treatment process using described a kind of lug nickel strap Surface treatment passivation solution on the other hand, and its step comprises:
(1) weakly alkaline liquid is adopted, the grease on removing lug nickel strap;
(2) weakly alkaline liquid distilled water in step (1) is cleaned up;
(3) use the product in distilled water cleaning step (2) again, and dry, be immersed in described lug nickel strap Surface treatment passivation solution;
(4) with product in distilled water cleaning step (3), dry, cropping of products (3).
In the present invention, described passivating solution also comprises further:
Organic phospho acid 0.01-0.05;
Phytic acid 0.01-0.05;
Cetyl trimethylammonium bromide 0.01-0.05;
Benzotriazole 0.01-0.05.
Embodiment
Unless otherwise defined, all technology used herein and scientific terminology have the identical implication usually understood with one skilled in the art of the present invention.When there is contradiction, be as the criterion with the definition in this specification sheets.
Term as used herein " by ... preparation " and " comprising " synonym.Term used herein " comprises ", " comprising ", " having ", " containing " or its other distortion any, be intended to cover the comprising of non-exclusionism.Such as, comprise the composition of listed elements, step, method, goods or device and need not be only limitted to those key elements, but other key element of clearly not listing or the intrinsic key element of this kind of composition, step, method, goods or device can be comprised.
Conjunction " by ... composition " get rid of any key element, step or the component do not pointed out.If in claim, this phrase will make claim be closed, make it not comprise material except those materials described, but except relative customary impurities.When phrase " by ... composition " to appear in the clause of claim main body instead of immediately preceding after theme time, it is only limited to the key element described in this clause; Other key element is not excluded outside described claim as a whole.
During the Range Representation that equivalent, concentration or other value or parameter limit with scope, preferable range or a series of upper limit preferred value and lower preferable values, this is appreciated that all scopes specifically disclosing and formed by arbitrary pairing of any range limit or preferred value and any range lower limit or preferred value, no matter and whether this scope separately discloses.Such as, when disclosing scope " 1 to 5 ", described scope should be interpreted as comprising scope " 1 to 4 ", " 1 to 3 ", " 1-2 ", " 1-2 and 4-5 ", " 1-3 and 5 " etc.When numerical range is described in this article, unless otherwise indicated, otherwise this scope intention comprises its end value and all integers within the scope of this and mark.
In addition, the indefinite article " one " before key element of the present invention or component and " one " are to quantitative requirement (i.e. occurrence number) unrestriction of key element or component.Therefore " one " or " one " should be read as and comprise one or at least one, and the key element of singulative or component also comprise plural form, unless the obvious purport of described quantity refers to singulative.
The detailed description of the following preferred implementation method of the present invention of participation in the election and the embodiment comprised more easily can understand present disclosure.Can mention a large amount of term in following specification sheets and claims, these terms are defined as following implication.
Singulative comprises plural number and object is discussed, unless clearly indicated in addition in context.
" optional " or " optionally " refers to that the item that describes thereafter or event can occur or not occur, and this description comprises situation that event occurs and the situation that event does not occur.
Approximate term in specification sheets and claims is used for modifying quantity, represents that the present invention is not limited to this concrete quantity, also comprises close to this quantity acceptable and can not cause the part of the correction of the change of relevant basic function.In some example, approximate term may correspond to the precision of the instrument measuring numerical value.In present specification and claims, scope limits and can combine and/or exchange, if do not illustrate that these scopes comprise contained all subranges therebetween in addition.
One aspect of the present invention provides a kind of lug nickel strap Surface treatment passivation solution, comprising:
Water 100;
Chromium trioxide 0.01-0.3;
Mineral acid 0.01-0.5;
Film forming accelerating 0.01-0.1.
As a kind of embodiment, described mineral acid is one or more in sulfuric acid, hydrochloric acid, phosphoric acid, perchloric acid, lactic acid, hydrofluoric acid, acetic acid.
As a kind of embodiment, described film forming accelerating is one or more in ammonium vanadate, strontium chloride, hydrofluoric acid, propanedioic acid, oxalic acid, pentanedioic acid, oxysuccinic acid, toxilic acid.
As a kind of embodiment, described lug nickel strap Surface treatment passivation solution also comprises the ring-type polyether compounds of 0.01-1 weight part and the mixture of modified graphene, and the structural formula of described ring-type polyether compounds is:
Wherein, R is amino, carboxyl, methylol, phenyl, acyl group or alkoxyl group;
X is one or more in O, S and N;
n=1-10。
As a kind of embodiment, described modified graphene is hydroxylation Graphene, carboxylated Graphene, sulfonic group functionalized graphene or amination Graphene.
As a kind of optimal way, described modified graphene is sulfonic group functionalized graphene or hydroxylation Graphene.
As a kind of optimal way, in described sulfonic group functionalized graphene, the ratio of S element is 5-10at%; In described hydroxylation Graphene and carboxylated Graphene, the ratio of O element is 5-15at%; In described amination Graphene, the ratio of N element is 10-20at%.
As a kind of embodiment, the mol ratio of described ring-type polyether compounds and modified graphene is 35-15:1.
The present invention provides a kind of metal surface treatment process using described a kind of lug nickel strap Surface treatment passivation solution on the other hand, and its step comprises:
(1) weakly alkaline liquid is adopted, the grease on removing lug nickel strap;
(2) weakly alkaline liquid distilled water in step (1) is cleaned up;
(3) use the product in distilled water cleaning step (2) again, and dry, be immersed in described lug nickel strap Surface treatment passivation solution;
(4) with product in distilled water cleaning step (3), dry, cropping of products (3).
ring-type polyether compounds
The structural formula of the polyether of ring-type described in the present invention compounds is:
Wherein, R is amino, carboxyl, methylol, phenyl, acyl group or alkoxyl group
X is one or more in O, N and S;
n=1-10。
The term " ring-type polyether compounds " that the present invention uses refers to and includes (CH
2cH
2x)
nthe ring compound of repeated structural unit, wherein X is represented as heteroatoms.In the present invention, X is one or more in O, N and S.
When X is O entirely, described ring-type polyether compounds is cyclic polyether.
When n is 2, described cyclic polyether is 12-crown ether-4; When n is 4, described cyclic polyether is hexaoxacyclooctadecane-6-6; When n is 1-10, the like.
Described cyclic polyether can use any method well known by persons skilled in the art to be prepared, and comprises highly dilution method, template synthesis method and stepwise condensation etc.
Such as, template can be used to prepare ring-type polyether compounds as follows: dihydroxy compound and multiethylene-glycol dichloride or two p-toluenesulfonic esters to be reacted in the basic conditions, so form two C-O keys and be cyclized into ring-type polyether compounds.
When in ring-type polyether compounds, X is O and N, described ring-type polyether compounds is Azacrown ether containing.When n is 2, O is 3, and when N is 1, described ring-type polyether compounds is azepine-12-crown ether-4; When n is 4, O is 4, and when N is 2, described ring-type polyether compounds is diaza-hexaoxacyclooctadecane-6-6.
When n be 1-10, O is m (m<n), when N is n-m, the like.
When X is N entirely, described ring-type polyether compounds is cyclic polyamines.
When n is 4, described cyclic polyamines is macrocyclic tetraamines.
Described Azacrown ether containing can use any method well known by persons skilled in the art to be prepared, and comprises highly dilution method, template synthesis method and stepwise condensation etc.
Such as, highly dilution method can be used to prepare compund of aza crown ether as follows: the chain polyamines replace p-toluenesulfonyl and the ester condensation of multiethylene-glycol two tosic acid obtain Azacrown ether containing, then slough p-toluenesulfonyl and obtain Azacrown ether containing.
When in ring-type polyether compounds, X is O and S, described ring-type polyether compounds is thia crown ether.
When n is 2, O is 3, and when S is 1, described ring-type polyether compounds is thia-12-crown ether-4; When n is 4, O is 4, and when S is 2, described ring-type polyether compounds is dithia-hexaoxacyclooctadecane-6-6.
When n be 1-10, O is m (m<n), when N is n-m, the like.
When X is S entirely, described ring-type polyether compounds is ring-type polythioether.
Described thia crown ether can use any method well known by persons skilled in the art to be prepared.
Such as, thia crown ether compound can be prepared as follows:
under ethanol condition, thia crown ether compound is synthesized with sodium sulphite.
When in ring-type polyether compounds, X is N and S, described ring-type polyether compounds is ring-type nitrogen thia ether.
When n is 2, N is 2, and when S is 2, described ring-type polyether compounds is 1,7-bis-sulphur-4,10 diazacyclo dodecane.
When n be 1-10, S is m (m<n), when N is n-m, the like.
Described ring-type nitrogen thia ether can use any method well known by persons skilled in the art to be prepared: aminoethyl thioether and 2-[(2-chloro-2-oxo ethyl) sulfenyl] excess acetyl chloride are generated 1,7-bis-sulphur-4,10 diazacyclo dodecanes-3,11-diketone, and then through being reduced into 1,7-bis-sulphur-4,10 diazacyclo dodecane.
When in ring-type polyether compounds, X is N, O and S, described ring-type polyether compounds is Azacrown ether containing sulfur.
Such as, as n=1, when O is 1, when N is 1, when S is 1, described Azacrown ether containing sulfur is 1-azepine-4-thia-crown ether-3
Described ring-type nitrogen thia ether can use any method well known by persons skilled in the art to be prepared: by para toluene sulfonamide and 2,2'-oxygen two (ethyltoluene sulfonic acid) reacts generation 1,7-bis-sulphur-4,10 diazacyclo dodecanes-3,11-diketone, and then through being reduced into 1,7-bis-sulphur-4,10 diazacyclo dodecane.
It is also commercially available for may be used for ring-type polyether compounds of the present invention.
When R is methylol, described ring-type polyether compounds is methylol-crown ether; When n be 4, X is O, described methylol-crown ether is methylol-hexaoxacyclooctadecane-6-6.
When n be 1-10, X is one or more in O, N and S, the like.
When R is phenyl, the structural formula of described phenyl is as follows:
Wherein, R
1for amino, sulfonic group, carboxyl, acyl group, ester group or phosphate; Y is 1-3.
In one embodiment, described R
1for formyl radical, X is O, n when being 3, and described ring-type polyether compounds is formylphenyl-15-crown ether-5.
Work as R
1for amino, sulfonic group, carboxyl, acyl group, ester group or phosphate, n is 1-10, X when being one or more in O, N or S, by that analogy.
X heteroatoms in ring-type polyether compounds in the present invention can carry out coordination with nickel ion, forms stable polynary ring, and the complex compound of ring-type polyether compounds and nickel ion easily precipitates under certain pH value, forms certain conversion film.Further, through the lot of experiment validation of the present inventor, unforeseeable discovery, as n=2, the salt spray resistance of the conversion film that ring-type polyether compounds/modified graphene and nickel ion are formed and the stability of conversion film best.Contriver think possible reason be due to, as n=2, described ring-type polyether compounds is 12-crown ether-4, and ring-type polyether compounds can form stable planar shape structure with nickel ion.Simultaneously after ring-type polyether compounds and modified graphene carry out compound, described modified graphene can present certain hydrophobicity again, now formed one deck composite membrane before this on the surface at lug nickel strap, on the surface of composite membrane, form one deck hydrophobic structure simultaneously, improve salt spray resistance and the corrosion resisting property of lug nickel strap.Further, can there is intermolecular reactive force with tab in the amino on described crown ether and carboxyl, and improve the binding property of passive film and tab.
modified graphene
Modified graphene for the application can be hydroxylation Graphene, carboxylated Graphene, sulfonic group functionalized graphene, amination Graphene.
Modified graphene for the application is not particularly limited, and can be commercially available, also can be obtained by synthesis.
Such as, described hydroxylation Graphene can be prepared by the method for low temperature (with reference to Chinese patent 201110093909.2).
Such as, described carboxylated Graphene can be prepared by solution method (with reference to Chinese patent CN104445163A).
Such as, described sulfonic group functionalized graphene can be prepared by reduction method (with reference to Chinese patent CN102706934A).
Such as, described amination Graphene can be prepared by reduction method (with reference to Chinese patent CN104140094A).
In the present invention, in described sulfonic group functionalized graphene, the ratio of element sulphur is 5-10at%, and preferably, described element sulphur ratio is 6-9at%; In described hydroxylation Graphene and carboxylated Graphene, the ratio of oxygen element is 5-35at%, and preferably, described oxygen element is 10-20at%; In described amination Graphene, the ratio of N element is 10-20at%, preferred, the ratio of described nitrogen element is 15-20at%.
In the present invention, the mol ratio of described ring-type polyether compounds and modified graphene is 35-15:1, and preferably, the mol ratio of described ring-type polyether compounds and modified graphene is 30-20:1.
organic phospho acid
Organic phospho acid is the compound without replacement phosphoric acid atom combining 2 hydroxyls.Organic phospho acid can be strong with metal chelating, be formed with machine phosphonic acid film in metallic surface self-assembly, and at the organic phosphonate film on Ni substrate surface, there is very strong hydrophobicity.Organic phospho acid described in the present invention is: Amino Trimethylene Phosphonic Acid, 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid, ethylene diamine tetra methylene phosphonic acid, two methene phosphonate group glycine, hydroxyl own fork base di 2 ethylhexyl phosphonic acid, 2-phosphate-1, one in 2,4-butane tricarboxylate and hydroxy ethylene diphosphonic acid
The 3d unoccupied orbital lone-pair electron of described organic phospho acid can form stable coordination compound with metal ion.
Amino Trimethylene Phosphonic Acid, is also called nitrilo trimethylene tri methylene phosphonic acid, i.e. ATMP, namely has the effect of Scale inhibitors, simultaneously stable in properties, not facile hydrolysis in water.
Ethylene diamine tetra methylene phosphonic acid, is also called ethylenediaminetetramethylene phosphonic acids, i.e. EDTMPA, and molecular formula is C
6h
20o
12n
2p
4.EDTMPA has the ability of very strong chelated metal ions, and sequestering power is far more than EDTA and DTPA.
Two methene phosphonate group glycine, are also called glycine two methylenephosphonic acid, i.e. GDMP, had both had the effect of Scale inhibitors, also have good corrosion mitigating effect simultaneously.
Hydroxyl own fork base di 2 ethylhexyl phosphonic acid, its poly-hydroxy sequestering action, changes the corrosion potential of passivation film, is conducive to the corrosion resistance nature improving passivation film.
2-phosphate-1,2,4-butane tricarboxylate, is called for short: PBTCA, another name: 1,2,4-tricarboxylic acid-2-phosphonic acid butane, PBTCA; Outward appearance: colourless to light yellow transparent liquid, molecular formula C
7h
11o
9p.Because it has the structural performance of phosphonic acids and carboxylic acid, make it have good scale inhibition and corrosion inhibition, be better than the organic phospho acid commonly used, special at high temperature scale-inhibiting properties is much better than conventional organic phospho acid, can improve the solubleness of zinc, the oxidation susceptibility of chlorine-resistant is good, and composite synergetic property is good.
Hydroxy ethylene diphosphonic acid, is also called 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid, is called for short HEDP, molecular formula C
2h
8o
7p
2, HEDP is a kind of organic phosphine acids anti-incrustation corrosion inhibitor, can form stable complex compound by many kinds of metal ions, the oxide compound on energy dissolution of metals surface.
phytic acid
Phytic acid is a kind of strong acid; another name is phytinic acid or nucite phosphoric acid ester; there is very strong sequestering power; it is with 24 Sauerstoffatoms; 12 phosphorus hydroxyls and 6 phosphate-based, within the scope of wider pH, can form multiple chelate ring with metal ion, simultaneously phytic acid C-structure sterie configuration is chair form type; 6 phosphates have 4 to be in same plane, thus easily form the unit molecule protective membrane of one deck densification in metallic surface when metal generation coordination reaction.Further, owing to containing hydroxyl and phosphate isoreactivity group in rete, can have an effect with organic coating, so through planting acid-treated metal alloy, having with the binding ability of coating and significantly improving.
cetyl trimethylammonium bromide
In the present invention, cetyl trimethylammonium bromide adds as wetting agent, can soak alloy surface, makes titanium-zirconium passive film uniform and delicate, improves compactness and the solidity to corrosion of passive film.
Cetyl trimethylammonium bromide for the application is not particularly limited, and can be commercially available, also can be obtained by synthesis.
Any method well known by persons skilled in the art can be used in the application to be prepared.
Such as, dropped into by trimethylamine aqueous solution in vaporization still, be heated to boil, the Trimethylamine 99 gas of generation uses acetone after drying, generates Trimethylamine 99 acetone soln in absorption tower, makes it enter quaternized still.Then under agitation drip bromohexadecane, the two mol ratio is 1.10 ︰ 1.Be incubated 30-40 DEG C in dropping process, drip after finishing insulated and stirred 1 hour again.Crystallisation by cooling, obtains crude product, with washing with acetone, dries, is drying to obtain.
In one embodiment, with parts by weight, the add-on of described cetyl trimethylammonium bromide is 0.01-0.05 weight part.
In the present invention, cetyl trimethylammonium bromide is the citing as a kind of wetting agent, and the wetting agent in the present invention can also comprise other some tensio-active agents, and is not limited only to cetyl trimethylammonium bromide.Such as, can also comprise in carboxy betaine type amphoterics, alkyl polyoxyethylene ether, alkyl alcohol ethoxylates sodium sulfate, alkylsurfuric acid ammonium, alkyl phosphide ester trolamine and sodium alkyl sulfate one or more.
benzotriazole
Benzotriazole for the application is not particularly limited, and can be commercially available, also can be obtained by synthesis.
Any method well known by persons skilled in the art can be used in the application to be prepared.
Such as, benzotriazole can be prepared as follows: dissolved in organic solvent by ortho-nitrophenyl hydrazine, have thanomin and catalyzer in solvent, prepare benzotriazole by high-pressure hydrogenation.
Benzotriazole also can German YOUNGING ocean cherry production and sales.
In one embodiment, with parts by weight, the add-on of described benzotriazole is 0.01-0.05 weight part.
What be necessary to herein means out is; above-mentioned citing is only for the invention will be further described; limiting the scope of the invention can not be interpreted as; some nonessential improvement and adjustment that the professional and technical personnel in this field makes according to the content of the invention described above, still belong to protection scope of the present invention.
film forming accelerating
Film forming accelerating to shorten the Passivation Treatment time, improve a class material of quality of forming film, film forming accelerating described in the application is material and the metal chelator with oxidisability, specifically can list ammonium vanadate, strontium chloride, hydrofluoric acid, propanedioic acid, oxalic acid, pentanedioic acid, oxysuccinic acid, toxilic acid, hydrogen peroxide, potassium permanganate, trisodium citrate, plumbic oxide, clorox, molybdenum dioxide, Potassium Iodate, potassium periodate, permanganic acid, chloric acid, chlorous acid, perchloric acid, nitrous acid, ammonium nitrate, DL-Lactic acid ammonium salt, ammonium formiate, ammonium acetate, ammonium oxalate, tetrabutylammonium perchlorate, tetrabutyl ammonium nitrate, ammonium iodide, brometo de amonio, ammonium thiosulfate, Potassium Persulphate, Sodium Persulfate, ammonium persulphate, ammonium dithionate, ammonium tartrate, ammonium citrate, fluorine nickel acid ammonium, ammonium meta-vanadate, ammonium hypophosphite, Ammonium Heptamolybdate, ammonium fluozirconate, ammonium bifluoride, ground acid disodium calcium, diethylene triamine pentacetic acid (DTPA), chelating carboxylic acids, Hedta, two [two (carboxymethyl) amine] diethyl ether of 2,2-, 1,2-diamino cyclohexane tetraacethyl, hydroxyethyl diamine nitrilotriacetic trisodium salt, hydroxyethyl diamine tetraacethyl trisodium salt, disodium ethylene diamine tetraacetate, tetrasodium ethylenediamine tetraacetate, oxalic acid, citric acid, 1, 3, 6-hexane tricarboxylic acid, tartrate, Sorbitol Powder, 1,3-propanedioic acid, 1, 4-succinic acid, nitrilotriacetic acid, diethylene triaminepentaacetic acid(DTPA), hydroxyethylethylene diamine tri-acetic acid, butene dioic acid, hydroxyl ethylene dinitrilotetra-acetic acid, dihydroxyl glycine, amino two methene phosphonates, Amino Trimethylene Phosphonic Acid salt, ethylene diamine tetra methylene phosphonic acid salt, diethylene triamine pentamethylene phosphonic salt, one or more in hydroxyethyl diamine three methene phosphoric acid, preferably, described film forming accelerating is ammonium vanadate, strontium chloride, hydrofluoric acid, propanedioic acid, oxalic acid, pentanedioic acid, oxysuccinic acid, one or more in toxilic acid.The add-on of described film forming accelerating is 0.1-2 weight part.
mineral acid
Mineral acid described in the application can list sulfuric acid, hydrochloric acid, phosphoric acid, perchloric acid, lactic acid, hydrofluoric acid, acetic acid, acid iodide, telluric acid, osmic acid, rehenic acid, chromic acid, silicic acid, cobalt acid, vanadic acid, chloric acid, mangaic acid, molybdic acid, nickel acid, boric acid, plumbic acid, arsenic acid, metatitanic acid, carbonic acid, ferrous acid, wolframic acid, selenic acid, stannic acid, zincic acid, bromic acid, xenic acid, orthosilicic acid, former phosphoric acid, ortho-sulfuric acid, orthocarbonic acid, metasilicic acid, metaboric acid, metatitanic acid, inclined ferrous acid, metaphosphoric acid, metaphosphorous acid, meta-arsenous acid, meta-aluminic acid, metavanadic acid, metaperiodic acid, tellurous acid, sulfurous acid, phosphorous acid, chlorous acid, chromous acid, plumbous acid, arsenus acid, nitrous acid, sub-stannic acid, Hydroxyl fluoride, hypoiodous acid, hypochlorous acid, hypobromous acid, Hypophosporous Acid, 50, sulfoxylic acid, perrhenic acid, permanganic acid, ferric acid, Periodic acid, hyperbromic acid, tetra-sodium, triphosphoric acid, pyrophosphorous acid, phospho-molybdic acid, phospho-wolframic acid, thiosulfuric acid, chlorsulfonic acid, fluosulfonic acid, hydroiodic acid HI, hydrosulphuric acid, Hydrogen bromide, fluoroboric acid, silicofluoric acid, hydrofluotitanic acid, hexafluorophosphoric acid, fluoplatinic acid, hydrochloro-auric acid, Platinic chloride, one or more in chloro-platinous acid, preferably, described mineral acid is sulfuric acid, hydrochloric acid, phosphoric acid, perchloric acid, lactic acid, hydrofluoric acid, one or more in acetic acid.Described nickel strap lug sheet surface treatment mineral acid also comprises hydrofluoric acid further.The effect of the fluorion in passivating solution has two: the first usually, under film forming treatment condition, makes the element of complex fluorides in treatment solution keep stable.The second, etching nickel alloy surfaces, and make solution keep stable to the nickel ion in treatment solution.The add-on of described mineral acid is 0.003-0.007 weight part.
other
Various additive can be contained within the scope without prejudice to the object of the present invention.As the object lesson of additive, Ce, La, Y or Nd rare-earth salts can be enumerated; Permanganate, oxymuriate, molybdate or (NH
4)
2s
2o
8oxygenant; Halogenide, vitriol, oxalate membrane-forming agent; Acetate, glycol acid, citric acid, tartrate, propanedioic acid, formic acid, pentanedioic acid, propionic acid, succsinic acid, oxysuccinic acid complexing agent, silicon-dioxide etc.
Embodiment
Below by embodiment, the present invention is specifically described.What be necessary to herein means out is; following examples are only for the invention will be further described; limiting the scope of the invention can not be interpreted as; some nonessential improvement and adjustment that the professional and technical personnel in this field makes according to the content of the invention described above, still belong to protection scope of the present invention.
In addition, if do not have other to illustrate, raw materials used is all commercially available, and following material number used is weight part.
Table 1
B: chromium trioxide
C: mineral acid
D: film forming accelerating
E: phytic acid
H: water
I: other: cetyl trimethylammonium bromide, benzotriazole, organic phospho acid
Table 2 is for preparing composition of raw materials and the consumption (parts by weight) of lug nickel strap passivation liquid composition
testing method
Hundred lattice tests: test according to " scratch experiment of GBT9286-1998 paint and varnish paint film ".Utilize cross-cut tester to mark the square of 100 lattice of 10 × 10, draw compartment apart from being 1mm, with the adhesive tape sticking of 3M600 or 610 in hundred lattice, quick pull-up 3M adhesive tape, tests the quantity sticked by adhesive tape.
Result evaluation: evaluate with ISO grade standard
0 grade: the edge of otch is completely smooth, and grid edge is without any peeling off;
1 grade: have small pieces to peel off in the intersection of otch, actual spoilage≤5% in Hua Ge district;
2 grades: the edge of otch and/or intersection have is peeled off, and its area is greater than 5% ~ 15%;
3 grades: have part to peel off or whole sheet peels off along notching edge, or partial grid is peeled off by full wafer.The area peeled off is more than 15% ~ 35%;
4 grades: notching edge sheet peels off/or some grid Part or all peel off, its area is greater than 35% ~ 65% of Hua Ge district;
5 grades: have peeling paint in blocks at the edge of line and point of crossing place, and the total area that comes off is greater than 65%.
Salt spray resistance is tested: test according to national standard " GB/T10125-1997 metal cladding salt air corrosion experimental technique ".Be mixed with salt-fog test solution with sodium-chlor and distilled water, strength of solution is 5at%, and pH value is between 6.5-7.5.Select the temperature in the salt-spray cabinet of DCTC1200P model, adjusting tank to be 35 ± 2 DEG C, salt fog sinkability is 1.0-2.0ml/80cm
2h, be that 30-45 ° of direction is placed in salt fog cabinet by the base material after described passivation and level, every 24h checks a base material.After 72h, experiment terminates, and by the seasoning at ambient temperature of described base material, then with room temperature water cleaning, and dries up immediately, measures sample corrosion rate with 3mm × 3mm grid.
Spot test: according to industrial standard HB5056-77 tests.By 3gK
2cr
2o
7be dissolved in 75ml distilled water with 25mlHCl and be mixed with testing liquid.Dripped by testing liquid in nickelalloy specimen surface, solution penetrates into substrate surface and its interaction, and solution colour becomes green from orange-yellow, and required time is the anti-corrosion time.
Boiling water test: test according to GB2530-2000, boils 5 hours being more than or equal in the deionized water of 95 degree.Criterion of acceptability: coating surface do not have wrinkle, crackle, bubble, come off and variable color.
Penetration testing:
Nickel strap is made nickel strap lug sheet, the cohesiveness between test nickel strap lug sheet and tab
Test procedure: lug sheet is put into the packing film sack good seal filling electrolytic solution (adding moisture 1000ppm); Put into 85 DEG C of high temperature roasters, carry out 24 hours aging; After aging, in sack, take out lug sheet must rinse well with clear water and dry up; The lug sheet rinsed well to be immersed in corrosion-free red penetrating fluid 1 hour; Rinse well with water, between nickel strap lug sheet and tab, redfree penetrating fluid enters as qualified again
Heat seal strength is tested:
Nickel strap is made nickel strap lug sheet, the cohesiveness between test nickel strap lug sheet and tab
Test procedure: nickel strap lug sheet is put into the packing film sack good seal filling electrolytic solution (adding moisture 1000ppm water); Put into 85 DEG C of high temperature roasters, carry out 24 hours aging; After aging, in sack, take out nickel strap lug sheet must rinse well with water and dry up; Nickel strap lug sheet glue shoulder is eliminated; Clamp metal place, nickel strap lug sheet two ends and do tensile test, nickel strap lug sheet can be obtained and tab seals combined strength bination.
Table 3
Above data can be found out, compared with the product of ring-type polyether compounds/modified graphene, lug nickel strap passivation liquid composition prepared by the present invention has higher salt spray resistance, stronger corrosion resisting property, because herein is provided Advantageous Effects of the present invention.
Aforesaid example is only illustrative, for explaining some features of feature of the present disclosure.Appended claim is intended to the scope wide as far as possible that requirement it is contemplated that, and the embodiment presented herein is only the explanation of the embodiment of the selection of combination according to all possible embodiment.Therefore, the purpose of applicant is the selectional restriction that appended claim is not illustrated the example of feature of the present invention.And progress in science and technology is not replaced to be formed due to the inaccurate reason of language performance by the possible equivalent considered at present or son, and these changes also should be interpreted as being covered by appended claim in the conceived case.
Claims (10)
1. a lug nickel strap Surface treatment passivation solution, is characterized in that, by weight, comprising:
Water 100;
Chromium trioxide 0.01-0.3;
Mineral acid 0.01-0.5;
Film forming accelerating 0.01-0.1.
2. a kind of lug nickel strap Surface treatment passivation solution as claimed in claim 1, it is characterized in that, described mineral acid is one or more in sulfuric acid, hydrochloric acid, phosphoric acid, perchloric acid, lactic acid, hydrofluoric acid, acetic acid.
3. a kind of lug nickel strap Surface treatment passivation solution as claimed in claim 1, it is characterized in that, described film forming accelerating is one or more in ammonium vanadate, strontium chloride, hydrofluoric acid, propanedioic acid, oxalic acid, pentanedioic acid, oxysuccinic acid, toxilic acid.
4. a kind of lug nickel strap Surface treatment passivation solution as claimed in claim 1, is characterized in that, also comprises the ring-type polyether compounds of 0.01-1 weight part and the mixture of modified graphene, and the structural formula of described ring-type polyether compounds is:
Wherein, R is amino, carboxyl, methylol, phenyl, acyl group or alkoxyl group;
X is one or more in O, S and N;
n=1-10。
5. a kind of lug nickel strap Surface treatment passivation solution according to claim 4, it is characterized in that, described R is methylol, alkoxyl group, amino, carboxyl or ester group;
X be in O and N one or more;
n=1-4。
6. a kind of lug nickel strap Surface treatment passivation solution according to claim 4, is characterized in that, described modified graphene is hydroxylation Graphene, carboxylated Graphene, sulfonic group functionalized graphene or amination Graphene.
7. a kind of lug nickel strap Surface treatment passivation solution according to claim 6, is characterized in that, described modified graphene is sulfonic group functionalized graphene or hydroxylation Graphene.
8. a kind of lug nickel strap Surface treatment passivation solution according to claim 7, it is characterized in that, in described sulfonic group functionalized graphene, the ratio of S element is 5-10at%; In described hydroxylation Graphene and carboxylated Graphene, the ratio of O element is 5-15at%; In described amination Graphene, the ratio of N element is 10-20at%.
9. a kind of lug nickel strap Surface treatment passivation solution according to claim 8, is characterized in that, the mol ratio of described ring-type polyether compounds and modified graphene is 35-15:1.
10. use a metal surface treatment process for a kind of lug nickel strap Surface treatment passivation solution as described in claim 1-9 any one, its step comprises:
(1) weakly alkaline liquid is adopted, the grease on removing lug nickel strap;
(2) weakly alkaline liquid distilled water in step (1) is cleaned up;
(3) use the product in distilled water cleaning step (2) again, and dry, be immersed in described lug nickel strap Surface treatment passivation solution;
(4) with product in distilled water cleaning step (3), dry, cropping of products (3).
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