BE441793A - PREPARATION OF PHOSPHATE-BASED LAYERS ON METALS AND PRODUCTS FOR THE IMPLEMENTATION OF THIS PROCESS - Google Patents

PREPARATION OF PHOSPHATE-BASED LAYERS ON METALS AND PRODUCTS FOR THE IMPLEMENTATION OF THIS PROCESS

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Publication number
BE441793A
BE441793A BE441793DA BE441793A BE 441793 A BE441793 A BE 441793A BE 441793D A BE441793D A BE 441793DA BE 441793 A BE441793 A BE 441793A
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Belgium
Prior art keywords
bath
phosphate
metals
grams
implementation
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French (fr)
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I.G. Farbenindustrie Ag
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Application filed by I.G. Farbenindustrie Ag filed Critical I.G. Farbenindustrie Ag
Publication of BE441793A publication Critical patent/BE441793A/en

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    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C22/00Chemical 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
    • C23C22/05Chemical 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
    • C23C22/06Chemical 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
    • C23C22/07Chemical 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 phosphates
    • C23C22/08Orthophosphates
    • C23C22/12Orthophosphates containing zinc cations
    • C23C22/14Orthophosphates containing zinc cations containing also chlorate anions
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C22/00Chemical 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
    • C23C22/05Chemical 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
    • C23C22/06Chemical 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
    • C23C22/07Chemical 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 phosphates
    • C23C22/08Orthophosphates
    • C23C22/18Orthophosphates containing manganese cations
    • C23C22/182Orthophosphates containing manganese cations containing also zinc cations

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  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Treatment Of Metals (AREA)

Description

       

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  Préparation de couches à base de phosphates sur des métaux et produits pour la mise en oeuvre de ce procédé. 
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  On connaît d4a praat3a qui Qnt pour but la ;prOd.uct1.on de jscuches à base de pha sphatas sur dea aurfaoas en iex, $Il. acier, an zino et en autres- nidtaux par traitamant avec des bains de I?hoaphatea di.u8a qui ont ttd ad.ditiMU5 df,g8i\11.ts d'oxydati on pour &oo4ldrer le prmesans, Ospendait, om a oqnotatd que loaplic t.0 des divatru agents d*asyâatism ne do.mie&t pas des résultats umf(u:'#s et qutil fallait scocrder la préfrn9e aux nitrataR . 



  On a également prsyp oe aux :$m9S fins lapplioatijon des ohloratea comme agents dfoxydatiQ:iI1l. Cette aIditicm o8!Jsn... n 

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 EMI2.1 
 dant entraîne certains à±savantBgee parce qu'elle provoque une hydrolyse très forte accompagnée d'un trcuble laiteux immédiat 
 EMI2.2 
 de la solution du bain qui se sépare 1)liz tard en flocons et donne lieu à un fort dépôt de boue.

   De oette façon. il se ferme aussi sur les objets   à   traiter une couche blanche que, 
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 ;parfois, en ne peut pas l:1mirJar des obj9ta phosphatés par m lavage, un brossage 4tant alors   nécessaire,   
Or, il s'est révélé qu'en Observant des conditions CI$ pH 
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 déterm3.nas, on peut réduire cette hydrolyse nuisible qui se produit dans des bains de traitement comportant de l'acide phosphorique, du phosphate de zino et des   ohlorates   de métaux 
 EMI2.5 
 moins précieux que le far, Toutefois le xég,laga de la concen. trU.Grta.mae8siire en ions à'hy3rcgéna n'est pas &-Ë-4-,'cutable par l'addition d'acide phosphorique en excès,, La Demanderesse a fait oette observation surprenante que la nature de l'anion :introduit dansle bain par addition de l'acide n'est pas 
 EMI2.6 
 indifférente.

   Il est de prendra lliapcrtsnce que cat anion ne d6:puoe pas Îléquilihre des phosphates dans la solution. Comme acides à ajouter entrent en ligne de oompte,/tou7.ea acides qui ne forment pas des sels insolubles avec les cations pré- sent$ dans la solution. Par exemple l'acide sulfurique ou l'acide borique conviennent particulièrement bien. gaz' addition de petites   quantités   de ces acides on amèns la précipite qui s  e présente   en une   massa   gélatineuse donc gênante à 
 EMI2.7 
 l'état pulvérulent et il se dépose alors a faciler#nt.

   Des car4- oentratia.ns avantageuses sont par e mple, celles qui cor-. reapondent aux quantités al1iva.ntas. calai-Liées sur 1 litre de bain; 4 à 8>5 grammes de Zn, 1;à,5 à 27 grammes de pSQ5 et 1 à 5 grammes. de Olo6, de préférence 5,7 grammes de Z., 18 gr arn- mgà de P 2 0, fi et 2,2 granynEs de t1I03 et moins de 0,1 gramme   diacide   sulfurique. 
 EMI2.8 
 En outre on 8,' constat que l'on Put accélérer le passage du premier état au second par   introduction   de criet aux tout 

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 EMI3.1 
 formas da phosphates de zinc et/au de fer pour dol&noher la troosfQr#tiQ\Q;

   ce soat surtout les orolâtea de phosphate Bolides précipitées des baims finis qui se prêtent à 1'uili a,t.a dans ce sens Il est Sov;rt8gs'OX de combiner les deux mesurée etest-à-dire ltditi(}a:l de l'acide et l'introduction de cris/taux. En ajou-4 tant de petites quantités d'aside, par exl0 dicLe STiL-< uriq'u.a, et des cristaux aqusirpt"t des :phQs;phates solides préoip.ts dans des bains antérieurs, on pariet à rdz3.r l'hydrolyse mnslhle à un mmim1.1!Il (parfois elle n'a presque pas lie m8.r  lors CI'=@ ora-tion 8= me échelle ÙD.d#tr :na),... le) et à r4çluire la masse boueuse qui se forme pendant teo-te la d-#6e dtutuivatiqu du bam à. une treat4ge de la q ua.nt 1t4 éliminée au 0 w.rs du tra1t$J#nt nr,a7,.

   De ce .a3t on réussit à utiliser le b miz bea-uccup ;plï#J longtemps. ' Quand on cpere ai.&sjLuae. introdatien'de oristae dams les bainp de traitement, l'addition d'acides autres que 1;11Ieide phoephox.que t l' a;sida oh,7.oriqua peut $tra Bpylne, L'hydrolyse des phosphates de J#t8.'\.lX lourde dpd de 1,u 0QU'oentr,%tio,u de ces 1 et de l'excès diacide phoepheriqua libre. Bile s tabais Sa de pair avec l '4i1CoroÍiUiI$J1I!)nt de la cols oentràtiGrl d# phosphates et s'élève avas Italemmtatlgn CIO la 9ono .tr,t ip. de l'aaid" , Lta'UgD1enta.tioiI::J. de la eo&oent tion des phosphates de méta-us lourds est lîmitde par le ;rait qut 6,i,U d lè, d'un certain degr la Stsache aux le far ne se forme que lentement et offre une structure or.ata7.la plus grossiers. 



  Si l'on ajaute des ohlQratas ces désa-atos se fomt sentir ' beaucoup moins. lu quantité de ghlo-tate à utiU s  est l3ita supe rieur eoent par l' ìOorottseroant de 3.hydr..ya et inférieuramiat par le fait que,la teceur 9. hloxata augmex:#. tant, des .3rrgularita apparaissent dans le oomporteNaat du bain, ;par û)G9m,ple, par s1Uite d'une formation Et!Itoess.1va de boue et de la l1éQee slt de rég6niratJl.Qns fréq#ntea de 00 baâm, on 

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 EMI4.1 
 obtient un9 OiCI'l1O ha superficielle qui est plus fine et ]plus mince que les couchas Obtenues par df mztres procédés da p1:106'" pbatationi elle est méoan3quament beaucoup :plut! résistant par exemple an pliige et est :pertitl1J1.Hre.n1:mt bien apirdpriea à la. rëaeption dtm enduit de vernis. 



  L'épaiJl 1Jl' aga cm2,ehos obtenùae par la procédt. da la pr4 Bmte in-vention na sidil-ve gutà Ità à 5 mior, t:and:ia que, par tous les proo4dés connus jusqu'à -08 jr&u:r, 0:111. ±-(1 Pzmt obtenir que des couches de 30 miarons et plus. La strict'lyre cl8 la osnehe ocmpaxée à celles des ocuehas produitea par les m6thcdsB connues, offre donc un int6*rt industriel 0 on a id rab 1 a, On peut appliquer les chlorates avantgeuaement saeur la forme de ohlorates da nà tavx lourde, par exemple, d1tl chlorate de zina. 



  :Pour maints besoins, .11 convient de se servir d me teneur en solde phosphorique libre plue élevée p.our enlever par ace ple dés traces de rouille plus fortes nu pour former des oouches sur des tlas , plus hauts ré si5tanc/h Des ilol11tiQns contenant 25 d'acide phosphorique libre ea sont montrer bien iiUj\6r1eurea ,aux aolutiona contenait environ 20 da cet acide.

   Toutefois, l'!1.ddit.iQ!i1. de l'aide libre est limitée supérieurement c ar la ooashe sfacorctii avec il bugmentat-lon d.9 
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 lucidité et prend -,une structure plue grossière, 
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 par des aààitiono compensent la consommation on peut maintenir au bain son efficacité maxiinoni en ce qui conogrna non seulement la vitesse de la fornmtion de la couche mais ausaï la qualité de la oC1JQhe produite. gour compléter la bain il il iest rêve le favorable de ne réduire qua de 4 le anambr des :pointl1 pour 10 am3 de solution da bain par aKeJ11'4 ple de le mainten:1r entre 42 et 38 et, p uzr supler" bzz consomm tion cle oblerate çllajauter, par exempl e, lor de lfuti.lieation du chlorate de zinc 3niron 30% da la aciuticn pho aphat .qae amenée (densité 1 p6 j .

   Tandis, que la prméu 

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 EMI5.1 
 normal dà phoaphatation don!!a, suivait l'âge du b& de ocuohee de rev"eàxlt çygat des couleurs' et des struotaea cristallines différent as par exataple dei 0 oeebea à gros criratwx, on obtient par la nouveau Vrw4&it une oeuche dont la couleur et la. qualité superficielle sont imifçirmoiit La. raison en. est que le far, paiaeut an fiQlut10n au ooiria de ce pr'QOd ss précipite à l'état de phoejphate ferrig#. 



  On prépare un bain an utilisant par litre,., 48 grammes d'u# solution de phosphate de zinc (densité 1t6; environ 10 de zine et une quantlté tota.le d':Jib ide pbo :p#r 1q:us clten- vircm 521; aveo environ 205% da 19 éotcle :p1:1Q :pb#-igue libre) 3 gre-maee de chlorate de zino et O,Q9 gramme diacide alllfu" rique oono entré, On introduit dans la îwlttirin des moceaax de croûtes provanait de baims prëoedsits On forme 1 souohe de rev"tte.arat oux du fer à Bmrfaue purement mttalljqn  à une ta.pratura de 9.,1,,13a en 8 à 10 minutes selon l'aapeea du fr, la treltenant prala.ble et le but 'de 1al.atian, 
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 On prépare un bain en utilisait par litres 48 grammes 
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 solution de I?hoaphata de zi1l9 (clo-naite 16),3 grammes da chlorate de z1n(,>" Of09 gr<aame dtsoiçio iuJ.furiq1:lS ei3oen" trë, 8,5 granm# décide phosphoriqua (d$nilit 1;

  7), La ter neur en acide phoarhorique libre olélbve ex env3r<m on introduit des "ratites provenant de bainil pr4cgdentij Le tre tar#nt des Qbjeta de fer est le mtme q &ma 3.eele 1. 



  ESEtMpLE 3i on prépare un bain en U.tilii t par xra: 48 gravez d'âme solution de phosphate de zino (d$;nsit4 1,6),3 grimez de: chlorate de zin.a et 8 gratmea d'aeide boriques Le traitement de oea objets de zinc est la robe que dais 1'azp.e 1. 



  E4: On prépara un bain on utilisant par litre; 48 grammes d'une solution de phosphate de zinc (densité 1g6; environ 10 de zing et mue <i111antité totale rltenviron 62% d's-oid 

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 EMI6.1 
 phQil/hQ'l'].Q1J9 aV,3,3 environ 2l5fa df seilie pho,horiqus libre) et 3 gramme; de a3lor.to de zinc@ 0n a 1 out à au bain. le résidu et, les orqetes prsavensxa,t a.11.1)1. traitant pdent. Il n'y a :pei de trouble lsteux La traitent àoe ç)b di at 9 ÇIO fsr Cl:1t le ïnÂm6 que dans l'axemple 1. 



  %XI<IPLZ Dànc 5 araxple chaufàit ' iraotoeoeant liquiàa EXEMPLE Dans 1 t sxsnple 4, 4n cbauffait ci iraot art le liquida du bsin, dans la gobslat" par la flamme du gaz. J)taprèa la 9 r4 ient eKemplo où plw,1JJ:f"" le bain* pr4cré é d. e' 18 m:1lC' .:naniàra sn es q aonoe\ 119 le solution de phospbate cle zinc et le ohlora,ts de zinc, au baiaa marie pour éviter un brtißage. On ajoute au bain ,5 grammes de croûtos p1JJ.vér iëéa prnvaaait d'un bain Br6O4éent, Taudis qutun hain prdpsré tpna C9-ttSl adàd.tlan 3 se clarifie q-til à la dix-bultibrae o,pttra t lO1 cet ,effet se produit d.é;1à dài.\ la cinquième opération dans un balia 'réal3oé conformément à l'inventif RESU14:E La préiszte inventie-n  Qnoarn: 1 ) Un pr acd.6 de prd.1Jtion da arsuchec à be.a'" d.EI phoa. 



  :phat :. 'minces, à fin. critW1X et très adli--rentau, svr (les ,Métaux, j?artlC1V.lièrerrant d.e 1.'scier, du far et. du zinc, par traitament par des b qui contiennent da Ilsoicie phr,).gpho-4 riq# 1 d.u phosphate de zinc et des ohlor1::t# de métaux njinli préolaug que le fer, procédi6 caractérir.4 en oa qu'on ajoute 
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 aux bains une petite quantité d'un acide qui ne forme pas de 
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 sels i inul1'bla avo3 les cation présents dama la solution, earosptin. fait9 de l r ide phorphnriqufte ) Des mc&# de réalîsaticn du procédé &;péeif 14 mg 1   QSP0rtSnt lez, I>artjaulerit8 iuivs..1Jlt0i t ]Irises isol.nent en selon les diverses comblais one possibles : 
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 a) on ajouta au bain de traitant une petite quantité 
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 d t ac i de sulfurique ou d'acide borique;

   

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 b) la qtla,atit de l'acide sulfurique ajouta à 1 litre de b ain e4 l va à 0, l gramme de H2804 au p 1 9) la teneur du bain c'$ l8vsr p our 1 litre de ligu1d&, a 8,5 grammes de zince l$15 à 87 grammes de p205 et 1 grammes de Ol03 , d ) la teneur de bain poujr 1 litr de liquide est de 517 gratamea de zino, 18 gr8JUme de p20  et 4,941 gr<1Wlilil8i de 61; e) an ajputa aux beiau, a.wnt de les utiliser, clos cristaux servant à Molenoher la rét3 et ocnuiztant ai phosphate da zijis et/ou, du phosphate de fer; g ) lori de lt:u.tiliii8.tiGn da Briataax IJpifih i1in 9)* en iïuopriiue l'addition d'201daa autres que l'taeifue :phos:phtc.. rique t l'acide chloriques :

   ) à titre de pycd!H-its mduetriel nOUV6at, a) las bains qui p4 dn.t les oompoeitoà définies !lUi 1Q et 20 b) -lei métaux rerituil de eouohea. â buse de phrpbatea par le proo4u ip6c:ifU: #a 10 eu .  vu à 1. aide des' b,ginil mtiQnn6 sous a) de 3 .



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 EMI1.1
 



  Preparation of layers based on phosphates on metals and products for the implementation of this process.
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  We know d4a praat3a which Qnt for purpose the; prOd.uct1.on of jscuches based on pha sphatas on aurfaoas in iex, $ Il. steel, an zino and in other- nidtals by treating with baths of I? hoaphatea di.u8a which have been ad.ditiMU5 df, g8i \ 11.ts of oxidation to oo4ldre the prmesans, Ospendait, om a oqnotatd que loaplic t.0 of divatru agents of asyâatism does not give results umf (u: '# s and that it was necessary to scocrder the preference to nitrataR.



  We have also prepared for: $ m9S the application of ohlorates as defoxydatiQ agents: iI1l. This aIditicm o8! Jsn ... n

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 EMI2.1
 dant leads some to ± savantBgee because it causes a very strong hydrolysis accompanied by an immediate milky trcuble
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 of the bath solution which separates 1) later into flakes and gives rise to a heavy deposit of sludge.

   In this way. it also closes on the objects to be treated a white layer that,
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 ; sometimes, by not being able to: 1mirJar the phosphated objects by m washing, a brushing 4 then being necessary,
However, it turned out that by observing conditions CI $ pH
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 determ3.nas, this harmful hydrolysis which occurs in treatment baths comprising phosphoric acid, zino phosphate and metal ohlorates can be reduced.
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 less valuable than the far, However the xég, laga de la concen. TrU.Grta.mae8siire in ions to'hy3rcgéna is not cuttable by the addition of phosphoric acid in excess, The Applicant has made this surprising observation that the nature of the anion: introduced into the bath by adding the acid is not
 EMI2.6
 indifferent.

   It is to take into account that the cat anion does not balance the phosphates in the solution. As acids to be added come in hand, all acids which do not form insoluble salts with the cations present in the solution. For example sulfuric acid or boric acid are particularly suitable. gas' addition of small amounts of these acids we bring the precipitate which is present in a gelatinous mass thus troublesome to
 EMI2.7
 the powdery state and it settles to facilitate # nt.

   Advantageous car4- oentratia.ns are by e mple, those which cor-. respond to al1iva.ntas quantities. calai-bound on 1 liter of bath; 4 to 8> 5 grams of Zn, 1; to, 5 to 27 grams of pSQ5 and 1 to 5 grams. of Olo6, preferably 5.7 grams of Z., 18 grams of arn-mg of P 2 O, fi and 2.2 grams of tlO 3 and less than 0.1 gram of sulfuric acid.
 EMI2.8
 In addition one 8, 'note that one Put accelerate the passage from the first state to the second by introduction of criet to all

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 EMI3.1
 formas da zinc and / or iron phosphates to dol & noher the troosfQr # tiQ \ Q;

   this soat especially the phosphate orolâtea Bolides precipitated from the finished baims which lend themselves to 1'uili a, ta in this sense It is Sov; rt8gs'OX to combine the two measured and is to say ltditi (} a: l of l acid and the introduction of cries / rates. By adding small amounts of aid, eg dicLe STiL- <uriq'u.a, and crystals obtained from the: phQs; preoip.ts solid phates in previous baths, we bet to rdz3.r the hydrolysis mnslhle to a mmim1.1! It (sometimes it hardly binds m8.r during CI '= @ ora-tion 8 = me scale ÙD.d # tr: na), ... le) and to reduce the muddy mass which forms during teo-te the d- # 6e dtutuivatiqu du bam to. a treatment of the q ua.nt 1t4 eliminated at 0 w.rs of the tra1t $ J # nt nr, a7 ,.

   From this .a3t we manage to use the b miz bea-uccup; plï # J for a long time. 'When we cpere ai. & SjLuae. introdatien'de oristae in the treatment baths, the addition of acids other than 1; 11Ieide phoephox. that aids oh, 7.oriqua can $ tra Bpylne, The hydrolysis of J # t8 phosphates. ' \ .lX heavy dpd of 1, u 0QU'oentr,% tio, u of these 1 and the excess phoepheriqua free diacid. Bile s tabais Sa together with the 4i1CoroÍiUiI $ J1I!) Nt of the cols oentràtiGrl d # phosphates and rises avas Italemmtatlgn CIO the 9ono .tr, t ip. of the aaid ", Lta'UgD1enta.tioiI :: J. of the eo & oent tion of heavy meta-us phosphates is limited by the qut 6, i, U d lè, to a certain degree the Stsache aux le far forms only slowly and has a coarser or.ata7.la structure.



  If we add ohlQratas these disa-atos are made to feel much less. the quantity of ghlo-tate to be used is higher by the ìOorottseroant of 3.hydr..ya and lower by the fact that, the teceur 9. hloxata augmex: #. so much, .3rrgularita appear in the oomporteNaat of the bath,; by û) G9m, ple, by the result of a formation And! Itoess.1va of mud and the l1éQee slt of reg6niratJl.Qns freq # ntea of 00 baâm, we

 <Desc / Clms Page number 4>

 
 EMI4.1
 obtains a superficial OiCI'l1O ha which is finer and] thinner than the layers Obtained by several methods in p1: 106 '"pbatationi it is meoan3quament a lot: rather! resistant for example to pliige and is: pertitl1J1.Hre.n1 : mt well apirdpriea to the reception of dtm coated with varnish.



  The epaiJl 1Jl 'aga cm2, ehos obtained by the procedure. da la pr4 Bmte in-vention na sidil-ve gutà Ità at 5 mior, t: and: ia que, by all the known proo4dés up to -08 jr & u: r, 0: 111. ± - (1 Pzmt obtain only layers of 30 miarons and more. The strict'lyria cl8 the osnehe ocmpaxed to those of the ocuehas produced by the known methcdsB, therefore offers an industrial interest 0 we have id rab 1 a, We can apply chlorates beforehand in the form of heavy ohlorates, for example, zina chlorate.



  : For many purposes, the higher free phosphoric balance content should be used to remove heavier traces of rust in order to form streaks on sheets, higher density / h. containing 25 free phosphoric acid are shown well, in the solutions containing about 20 of this acid.

   However, the! 1.ddit.iQ! I1. free help is severely limited due to the ooashe sfacorctii with il bugmentat-lon d.9
 EMI4.2
 lucidity and takes -, a more coarse structure,
 EMI4.3
 by aàitiono compensate for the consumption one can maintain in the bath its maximum efficiency in what conogrna not only the speed of the formation of the layer but also the quality of the produced oC1JQhe. gour complete the bath it is the dream the favorable to reduce only by 4 the anambr of: pointl1 for 10 am3 of solution in the bath by aKeJ11'4 full of the mainten: 1r between 42 and 38 and, p uzr increase "bzz consumed tion key oblerate çllajauter, for example, the gold of the use of zinc chlorate 3niron 30% da aciuticn pho aphat .qae brought (density 1 p6 d.

   While the prméu

 <Desc / Clms Page number 5>

 
 EMI5.1
 normal dà phoaphatation don !! a, followed the age of the b & of ocuohee of rev "eàxlt çygat of the colors' and the crystalline struotaea different as by exataple dei 0 oeebea with big criratwx, one obtains by the new Vrw4 & it an egg whose color The. reason for this is that the far, pays an fiQlut10n at the ooiria of this pr'QOd ss precipitates as phoejphate ferrig #.



  A bath is prepared using per liter,., 48 grams of a solution of zinc phosphate (density 1t6; about 10 of zine and a total amount of: Jib ide pbo: p # r 1q: us clten - vircm 521; aveo about 205% of 19 th eotcle: p1: 1Q: pb # -igue free) 3 gre-maee of zino chlorate and O, Q9 gram of alllfu "ric acid oono entered, We introduce into the îwlttirin moceaax of crusts came from pre-edged baims One forms 1 souohe of rev "tte.arat orx iron in Bmrfaue purely mttalljqn at a ta.pratura of 9., 1,, 13a in 8 to 10 minutes depending on the aapeea of the fr, the treltenant prala .ble and the goal 'of 1al.atian,
 EMI5.2
 We prepare a bath used per liters 48 grams
 EMI5.3
 zi1l9 I? hoaphata solution (clo-naite 16), 3 grams of z1n chlorate (,> "Of09 gr <aame dtsoiçio iuJ.furiq1: lS ei3oen" trë, 8,5 granm # decides phosphoriqua (d $ nilit 1 ;

  7), The ter neur in free phoarhoric acid olélbve ex env3r <m one introduces "ratites coming from bainil pr4cgdentij The tar # nt of Qbjeta of iron is the same as that of my 3.eele 1.



  SEStMpLE 3i a bath is prepared in U. use by xra: 48 burn zino phosphate solution core (d $; nsit4 1.6), 3 grimea: zin.a chlorate and 8 boric acid gratmea The treatment of oea zinc objects is the dress dais 1'azp.e 1.



  E4: We prepared a bath using per liter; 48 grams of a zinc phosphate solution (density 1g6; about 10 zinc and molt <total amount rt about 62% s-oid

 <Desc / Clms Page number 6>

 
 EMI6.1
 phQil / hQ'l ']. Q1J9 aV, 3.3 approximately 2l5fa df seilie pho, horiqus free) and 3 gram; of a3lor.to of zinc @ 0n has 1 out to the bath. the residue and, the prsavensxa orqetes, t a.11.1) 1. treating pdent. There is: little of lstous disorder The treat atoe ç) b di at 9 ÇIO fsr Cl: 1t the ïnÂm6 only in the example 1.



  % XI <IPLZ Dànc 5 araxple chaufàit 'iraotoeoeant liquiàa EXAMPLE In 1 t sxsnple 4, 4n cbauffait ci iraot art le liquida du bsin, in the gobslat "by the gas flame. J) taprèa the 9 r4 ient eKemplo where plw, 1J : f "" the pre-created bath * d. e '18 m: 1lC'.: naniàra sn es q aonoe \ 119 the solution of zinc phospbate and zinc ohlora, ts, with baiaa mixed to avoid burning. add to the bath, 5 grams of croutos p1JJ. ver iëéa prnvaaait of a Br6O4éent bath, Slum that a hain prepared tpna C9-ttSl adàd.tlan 3 is clarified q-til with ten-bultibrae o, pttra t lO1 this, effect is produced d.é; 1à dài. \ the fifth operation in a balia 'carried out in accordance with the inventive RESU14: E The preiszte inventie-n Qnoarn: 1) A pr acd.6 of prd.1Jtion da arsuchec to be.a' "d.EI phoa.



  : phat:. 'thin, at the end. critW1X and very adli - rentau, svr (les, Métaux, j? artlC1V.lièrerrant of 1.'s steel, of far and. of zinc, by treatment by b which contain da Ilsoicie phr,). gpho-4 riq # 1 of zinc phosphate and ohlor1 :: t # of metals njinli preolaug that iron, proceedi6 characterized. 4 in which one adds
 EMI6.2
 in the baths a small amount of an acid which does not form
 EMI6.3
 salts i inul1'bla avo3 the cation present in the solution, earosptin. fact9 of the phorphnriqufte) Steps for carrying out the process &; weight 14 mg 1 QSP0rtSnt lez, I> artjaulerit8 iuivs..1Jlt0i t] Irises are isolated according to the various possible fillings:
 EMI6.4
 a) a small amount was added to the treatment bath
 EMI6.5
 d t aci of sulfuric or boric acid;

   

 <Desc / Clms Page number 7>

 
 EMI7.1
 b) the qtla, atit sulfuric acid added to 1 liter of b ain e4 l goes to 0.1 gram of H2804 at p 1 9) the content of the bath c '$ l8vsr for 1 liter of ligu1d &, a 8 , 5 grams of zince l $ 15 to 87 grams of p205 and 1 gram of Ol03, d) the bath content for 1 liter of liquid is 517 gratamea de zino, 18 gr8JUme of p20 and 4.941 gr <1Wlil8i of 61; e) an adjputa to beiau, a.wnt to use them, closed crystals used to Molenoher the ret3 and ocnuiztant ai phosphate da zijis and / or, iron phosphate; g) lori de lt: u.tiliii8.tiGn da Briataax IJpifih i1in 9) * in iïuopriiue the addition of 201daa other than taeifue: phos: phtc .. ric t chloric acid:

   ) as pycd! H-its new mduetriel, a) the baths which p4 dn.t the oompoeitoà defined! lUi 1Q and 20 b) -lei rerituil metals of eouohea. â phrpbatea nozzle by the proo4u ip6c: ifU: #a 10 eu. seen at 1. using 'b, ginil mtiQnn6 under a) of 3.


    
BE441793D 1940-06-19 1941-06-19 PREPARATION OF PHOSPHATE-BASED LAYERS ON METALS AND PRODUCTS FOR THE IMPLEMENTATION OF THIS PROCESS BE441793A (en)

Applications Claiming Priority (6)

Application Number Priority Date Filing Date Title
DE228450X 1940-06-19
DE879429X 1940-06-19
DEI67216D DE747085C (en) 1940-06-19 1940-06-20 Process for the production of phosphate layers on metals
DE237628X 1942-06-18
DE110243X 1943-02-11
FR53035T 1943-06-17

Publications (1)

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BE441793A true BE441793A (en) 1941-07-31

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BE451583D BE451583A (en) 1940-06-19 1943-07-23 PREPARATION OF PHOSPHATE-BASED LAYERS ON METALS AND PRODUCTS FOR THE IMPLEMENTATION OF THIS PROCESS

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CH (2) CH228450A (en)
DE (1) DE747085C (en)
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE859843C (en) * 1949-02-28 1952-12-15 Metallgesellschaft Ag Process for the phosphating of metals
US2884351A (en) * 1956-01-25 1959-04-28 Parker Rust Proof Co Method of cold rolling ferrous strip stock

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB247071A (en) * 1925-06-26 1926-02-11 Thomas Watts Coslett Improvements in or relating to processes for the treatment of iron or steel for preveting oxidation or rusting
GB473974A (en) * 1935-05-24 1937-10-22 Pyrene Co Ltd Improvements in solutions for use in coating metals

Also Published As

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BE451583A (en) 1943-08-31
CH228450A (en) 1943-08-31
CH237628A (en) 1945-05-15
FR879429A (en) 1943-02-23
DE747085C (en) 1944-09-06
FR53035E (en) 1945-09-06

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