SU1346699A1 - Phosphating electrolyte - Google Patents

Phosphating electrolyte Download PDF

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Publication number
SU1346699A1
SU1346699A1 SU864000303A SU4000303A SU1346699A1 SU 1346699 A1 SU1346699 A1 SU 1346699A1 SU 864000303 A SU864000303 A SU 864000303A SU 4000303 A SU4000303 A SU 4000303A SU 1346699 A1 SU1346699 A1 SU 1346699A1
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SU
USSR - Soviet Union
Prior art keywords
proxanol
sodium chloride
phosphating
electrolyte
coatings
Prior art date
Application number
SU864000303A
Other languages
Russian (ru)
Inventor
Лев Константинович Бобровский
Владимир Владимирович Селевин
Владимир Борисович Доброхотов
Владимир Леонидович Николаев
Виктор Алексеевич Чумаевский
Александр Викторович Капралов
Original Assignee
Буйский Химический Завод
Ярославский политехнический институт
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Publication date
Application filed by Буйский Химический Завод, Ярославский политехнический институт filed Critical Буйский Химический Завод
Priority to SU864000303A priority Critical patent/SU1346699A1/en
Application granted granted Critical
Publication of SU1346699A1 publication Critical patent/SU1346699A1/en

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C23—COATING 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
    • C23C—COATING 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
    • C23C22/00—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
    • C23C22/07—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 phosphates
    • C23C22/08—Orthophosphates
    • C23C22/20—Orthophosphates containing aluminium cations
    • C—CHEMISTRY; METALLURGY
    • C23—COATING 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
    • C23C—COATING 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
    • C23C22/00—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
    • C23C22/07—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 phosphates
    • C23C22/08—Orthophosphates
    • C23C22/12—Orthophosphates containing zinc cations
    • C23C22/13—Orthophosphates containing zinc cations containing also nitrate or nitrite anions
    • C—CHEMISTRY; METALLURGY
    • C23—COATING 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
    • C23C—COATING 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
    • C23C22/00—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
    • C23C22/07—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 phosphates
    • C23C22/08—Orthophosphates
    • C23C22/22—Orthophosphates containing alkaline earth metal cations

Abstract

Изобретение относитс  -к электро осаждению фосфатных покрытий на углеродистые и нержавеющие стали и может быть использовано в металлургии и машиностроении. Цель изобретени  - повышение мелкозернистости и адгезии покрытий при снижении содержани  цинка в покрытии. Фосфатирование ведут при катодной плотности тока 10- 30 А/дм , температуре 18-40 0, рН электролита составл ет 1,8-2,5. Электролит содержит, г/л: фосфорнокислый цинк (однозамещенный) 100-150; азотнокислый кальций или магний или алюминий 10-20; фосфорна  кислота 4-8; хлористый натрий 2-4; органическа  добавка, выбранна  из группы, включающей: смачиватель ОС-20, синтанол ДС-10, проксанол-146, проксанол-186 0,05-0,10; хлористый натрий 2-4. 1 табл. О) 00 4 05 05 СОThe invention relates to electro-deposition of phosphate coatings on carbon and stainless steels and can be used in metallurgy and mechanical engineering. The purpose of the invention is to increase the fine grain size and adhesion of the coatings while reducing the zinc content in the coating. Phosphating is carried out at a cathode current density of 10-30 A / dm, a temperature of 18-40 0, the pH of the electrolyte is 1.8-2.5. The electrolyte contains, g / l: zinc phosphate (monosubstituted) 100-150; calcium nitrate or magnesium or aluminum 10-20; phosphoric acid 4-8; sodium chloride 2-4; organic additive selected from the group including: wetting agent OC-20, sintanol DS-10, proxanol-146, proxanol-186 0.05-0.10; sodium chloride 2-4. 1 tab. O) 00 4 05 05 SB

Description

Изобретение относитс  к нанесению фосфатных покрытий на поверхность углеродистых и нержавеющих сталей и может быть использовано в металлургии и машиностроении.The invention relates to the deposition of phosphate coatings on the surface of carbon and stainless steels and can be used in metallurgy and mechanical engineering.

Цель изобретени  - повышение мелкозернистости и адгезии покрытий при снижении содержани  цинка в покрытииThe purpose of the invention is to increase the fine grain and adhesion of coatings while reducing the zinc content in the coating.

Фосфатирование ведут при плотности катодного тока 10-30 А/дм температуре IS-AO C, рН электролита составл ет 1,8-2,5. Анодом служит графит , свинец, цинк или их комбинаци Phosphating is carried out at a cathode current density of 10-30 A / dm at an IS-AO C temperature, the pH of the electrolyte is 1.8-2.5. The anode is graphite, lead, zinc, or a combination of them.

Введение полиэтиленгликолевых эфи ров высших жирных спиртов (смачиватель ОС-20, синтанол ДС-10) или блок сополим ров окиси этилена и окиси пропилена (проксанол-146,проксанол- 186) позвол ет получить равномерную мелкокристаллическую пленку с высокой адгезией к подложке и сниженным содержанием металлического цинка в покрытии на нержавеющих и углеродистых стал х за счет адсорбции органических добавок на цинке.The introduction of polyethylene glycol esters of higher fatty alcohols (OC-20 wetting agent, DS-10 sintanol) or a block of copolymers of ethylene oxide and propylene oxide (proxanol-146, proxanol-186) allows to obtain a uniform fine-crystalline film with high adhesion to the substrate and reduced content zinc metal in the coating on stainless and carbon steels due to the adsorption of organic additives on zinc.

При концентрации органических добавок меньше 0,05 г/л увеличиваетс  содержание металлического цинка в покрытии , ухудшаетс  адгези  пленки, а при концентрации добавок больше О,1 г/л возможно образование рыхлых покрытий.When the concentration of organic additives is less than 0.05 g / l, the content of metallic zinc in the coating increases, the adhesion of the film deteriorates, and if the concentration of additives is greater than 0, 1 g / l, formation of loose coatings is possible.

Хлористый натрий в количестве 2-4 г/л улучшает адгезию фосфатного покрыти  к подложке. Увеличение его концентрации свьгае А г/л положительного эффекта на катоде не дает, но в то же врем  отрицательно вли ет на работу анода, способству  его более быстрому разрушению.Sodium chloride in the amount of 2-4 g / l improves adhesion of the phosphate coating to the substrate. An increase in its concentration in the coil A g / l does not give a positive effect on the cathode, but at the same time it negatively affects the work of the anode, contributing to its more rapid destruction.

Образцы перед фосфатированием обезжиривают и анодно трав т при и плотности тока 15 А/дм вSamples before phosphating are degreased and anodically etched at a current density of 15 A / dm in

10ten

2020

5 five

466992466992

15%-ной серной кислоте. Среднеуслов- ный размер зерна определ ют по методу сравнени  с контрольной шкалой. Количество металлического цинка в покрытии определ ют по количеству выделившегос  водорода при растворении покрыти  в 5%-ной серной кислоте. Адгезию покрыти  определ ют механической навивкой проволоки на цилиндрическую оправку, а также на приборе НГ-2 по количеству гибов образца на 180° на оправке радиусом 20 мм до отслоени  покрыти .15% sulfuric acid. The average conditional grain size is determined by the method of comparison with a control scale. The amount of zinc metal in the coating is determined by the amount of hydrogen released when the coating is dissolved in 5% sulfuric acid. The adhesion of the coating is determined by mechanical winding of the wire on a cylindrical mandrel, as well as on an NG-2 instrument, by the number of sample bends 180 ° on the mandrel with a radius of 20 mm before peeling of the coating.

Изобретение иллюстрируетс  данными таблицы.The invention is illustrated in the data table.

Как видно из таблицы, предлагае- Nbift электролит позвол ет осаждать мелкозернистые фосфатные покрыти  с пониженным содержанием цинка, обладающие хорошей адгезией к подложке.As can be seen from the table, the proposed Nbift electrolyte precipitates fine-grained phosphate coatings with a reduced zinc content, which have good adhesion to the substrate.

Claims (1)

Формула изобретени Invention Formula Электролит фосфатировани , содержащий фосфорнокислый цинк, азотнокислый кальций или магний или алюминий и фосфорную кислоту, отличающийс  тем, что, с целью повьш1ени  мелкозернистости и адгезии покрытий при снижении содержани  цинка в покрытии, он дополнительно содержит хлористый натрий и органическую добавку, выбранную из группы, включающей смачиватель ОС-20, синтанол ДС-10, проксанол-1 46, проксанол-186, при следующем соотношении компонентов, г/л: Фосфорнокислый цинк (однозамещенный) 100-150 Азотнокислы кальций или магний или алюминий 10-20 Фосфорна  кислота 4-8 Хлористый натрий 2-4 Органическа  добавка 0,05-0,10Phosphating electrolyte containing zinc phosphate, calcium nitrate or magnesium or aluminum and phosphoric acid, characterized in that, in order to increase the fine grain and adhesion of the coatings while reducing the zinc content of the coating, it additionally contains sodium chloride and an organic additive selected from the group including OC-20 wetting agent, DS-10 syntanol, Proxanol-1 46, Proxanol-186, with the following ratio of components, g / l: Zinc phosphate (monosubstituted) 100-150 Calcium or magnesium nitrate or aluminum 10-20 Fo sour acid 4-8 sodium chloride 2-4 organic additive 0.05-0.10
SU864000303A 1986-01-03 1986-01-03 Phosphating electrolyte SU1346699A1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
SU864000303A SU1346699A1 (en) 1986-01-03 1986-01-03 Phosphating electrolyte

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SU864000303A SU1346699A1 (en) 1986-01-03 1986-01-03 Phosphating electrolyte

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7521249B2 (en) * 2003-12-12 2009-04-21 L'oreal Method and composition for the preparation of a sample for analysis
RU2791305C1 (en) * 2022-12-17 2023-03-07 федеральное государственное бюджетное образовательное учреждение высшего образования "Новгородский государственный университет имени Ярослава Мудрого" Method of steel phosphating

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
Бадаль н Г. М. Защита металлов фосфатными и окисиыми пленками. Суд- промгиз, 1952, с. 40-44. Клочковский С. П. и др. Электрохимическое нанесение подсмазочного сло на легированную проволоку. Технический прогресс в метизном производстве. Сборник, 99. М. : Металлурги , 1981, с. 24-26. *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7521249B2 (en) * 2003-12-12 2009-04-21 L'oreal Method and composition for the preparation of a sample for analysis
RU2791305C1 (en) * 2022-12-17 2023-03-07 федеральное государственное бюджетное образовательное учреждение высшего образования "Новгородский государственный университет имени Ярослава Мудрого" Method of steel phosphating

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