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SU908950A1 - Process for producing protective coating on zink surface - Google Patents

Process for producing protective coating on zink surface Download PDF

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Publication number
SU908950A1
SU908950A1 SU802969874A SU2969874A SU908950A1 SU 908950 A1 SU908950 A1 SU 908950A1 SU 802969874 A SU802969874 A SU 802969874A SU 2969874 A SU2969874 A SU 2969874A SU 908950 A1 SU908950 A1 SU 908950A1
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SU
USSR - Soviet Union
Prior art keywords
stage
nitric acid
solution containing
components
protective coating
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Application number
SU802969874A
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Russian (ru)
Inventor
Татьяна Михайловна Бершадская
Ян Натанович Липкин
Людмила Васильевна Пугачева
Виталия Моисеевна Альбрут
Лев Дмитриевич Ронис
Original Assignee
Уральский научно-исследовательский институт трубной промышленности
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Priority to SU802969874A priority Critical patent/SU908950A1/en
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Publication of SU908950A1 publication Critical patent/SU908950A1/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
    • C23C22/23Condensed phosphates
    • 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
    • C23C22/82After-treatment
    • C23C22/83Chemical after-treatment

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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

II

Изобретение относитс  к химической обработке поверхности, в частности к способам обработки цинковой поверхности, и может быть использовано в радиотехнической промышленности .The invention relates to chemical surface treatment, in particular to methods for treating a zinc surface, and can be used in the radio industry.

Наиболее близким к предлагаемому  вл етс  способ получени  защитного покрыти  на металлической поверхности, в частности цинковой, включающий последовательную обработку в растворе, содержащем азотную кислоту, фосфаты, сульфаты, нитраты, фторида металлов: железа, алюмини , цинка, никел  или кобальта при комнатной температуре в течение 5 с и более, затем в растворе силиката натри , кали  или лити  при комнатной температуре в течение 5 с и более и сущку гор чим воздухом с температурой 50-200° С 1 .The closest to the present invention is a method of obtaining a protective coating on a metal surface, in particular zinc, comprising sequential treatment in a solution containing nitric acid, phosphates, sulfates, nitrates, metal fluoride: iron, aluminum, zinc, nickel or cobalt at room temperature for 5 s and more, then in a solution of sodium, potassium or lithium silicate at room temperature for 5 s or more and with hot air with a temperature of 50-200 ° C 1.

Цинковое покрытие, обработанное по этому способу, характеризуетс  недостаточной коррозионной стойкостью и отсутствием декоративного вида.The zinc coating treated by this method is characterized by insufficient corrosion resistance and the absence of a decorative appearance.

Цель изобретени  - повышение коррозионной стойкости получаемого покрыти  и придание ему декоративного вида.The purpose of the invention is to increase the corrosion resistance of the resulting coating and make it look decorative.

..

Указанна  цель достигаетс  тем, что в способе получени  защитного покрыти  на цинковой поверхности, включающем последовательную обработку в растворе, содержащем азотную кислоту и фосфат металла, затем в растворе силиката натри  и сушку при This goal is achieved by the fact that in the method of obtaining a protective coating on a zinc surface, which includes sequential treatment in a solution containing nitric acid and a metal phosphate, then in a solution of sodium silicate and drying

10 60-80° С, на первой стадии обработки используют раствор, содержащий азотную кислоту , гексаметафосфат натри  и оксизтилированный фенол (ОП-10) при следующем соотношении компонентов, г/л:10 60-80 ° C, in the first stage of processing, a solution containing nitric acid, sodium hexametaphosphate and oxystilated phenol (OP-10) is used in the following ratio of components, g / l:

ISIS

Азотна  кислота10-20Nitric acid 10-20

ГексаметафосфатHexametaphosphate

натри 5-6rub 5-6

ОП-102-6OP-102-6

и на второй стадии раствор, содержащий and in the second stage a solution containing

20 силикат натри  и 1,2 диоксиантрахинон при следующем соотношении компонентов, г/л:20 sodium silicate and 1,2 dioxyanthraquinone in the following ratio of components, g / l:

Силикат натри 20-50Sodium silicate 20-50

1,2-Диоксиантрахинон0,05-0,11,2-Dioxyanthraquinone 0.05-0.1

Раствор первой стадии обработки готов т следующим образом.The solution of the first stage of processing is prepared as follows.

К воде добавл ют расчетное количество азотной кислоты, затем оксиэтилированный фенол - ОП-10 и в последнюю очередь гексаметафосфат натри . При изменении последовательности введени  компонентов свойства растворов не мен ютс .A calculated amount of nitric acid is added to water, then ethoxylated phenol is OP-10 and lastly sodium hexametaphosphate. When the sequence of introduction of components is changed, the properties of the solutions do not change.

Раствор второй стадии готов т в следующем пор дке. Сначала к воде приливают силикат натри , а затем добавл ют 1,2-диоксиантрахинон (ализарин). Раствор тщательно перемешивают до полного растворени  ализарина. От пор дка смешивани  компонентов свойства раствора не мен ютс .The solution of the second stage is prepared in the following order. Sodium silicate is first added to the water, and then 1,2-dioxyanthraquinone (alizarin) is added. The solution is thoroughly mixed until the alizarin is completely dissolved. From the order of mixing the components, the properties of the solution do not change.

Обработку цинкового покрыти  по предлагаемому способу осуществл ют в растворах с различными концентраци ми компонентов при различных параметрах режимов на обеих стади х обработки.The treatment of the zinc coating by the proposed method is carried out in solutions with different concentrations of the components with different parameters of the modes at both stages of processing.

Режимы приведены в табл. 1.Modes are given in table. one.

Испытани  провод т на образцах радиодеталей , оцинкованных электролитическим способом из кислых, щелочных и цианистых электролитов. Толщина цинкового покрыти  на образцах составл ет 2-6 мкм. Образцы обрабатывают по 12-ти вариантам предлагаемого способа. Эффективность способа оценивют по коррозионной стойкости получаемой защитной пленки и по ее декоративному виду.The tests are carried out on samples of radio components galvanized by an electrolytic method from acidic, alkaline, and cyanic electrolytes. The thickness of the zinc coating on the samples is 2-6 microns. Samples are processed according to 12 variants of the proposed method. The effectiveness of the method is assessed by the corrosion resistance of the resulting protective film and its decorative appearance.

Коррозионную стойкость определ ют по мтоду: выдержка 4 ч при +35° С, затем 48 ч во влажной камере при 25°±2°С, после чего 2 ч при -40° С и 48 ч в обычных атмосферных услови х. О защитной способности пленки суд т по количеству образцов с очагами коррозиии после испытаний.Corrosion resistance is determined by the method: holding for 4 hours at + 35 ° C, then 48 hours in a humid chamber at 25 ° ± 2 ° C, then 2 hours at -40 ° C and 48 hours under normal atmospheric conditions. The protective ability of the film is judged by the number of samples with corrosion foci after testing.

Декоративный вид оценивают визуально, во внимание принимают блеск поверхности, цвет покрыти , наличие п тен, налипших остатков pacTBOpia.The decorative appearance is evaluated visually, taking into account the gloss of the surface, the color of the coating, the presence of spots, adhered pacTBOpia residues.

Результаты испытаний приведены в табл. 2The test results are shown in Table. 2

Из данных табл. 2 видно, что при обработке образцов по предлагаемому способуFrom the data table. 2 shows that when processing samples by the proposed method

(варианты 2-4) коррозионна  стойкость защитной пленки высока , на 100% испытанных образцов отсутствуют следы коррозии цинка. На всех образцах полученна  защитна  пленка светла , однотонна , блест ща , н тен не имеетс .(options 2-4) The corrosion resistance of the protective film is high, 100% of the tested samples show no signs of zinc corrosion. In all samples, the resulting protective film is light, uniform, glossy, no shadow.

При обработке в растворах с уменьщенными коШ1ентраци ми компонентов (вариант 1) против предлагаемых коррозионна  стойкостьWhen processed in solutions with reduced component concentrations (option 1) against the proposed corrosion resistance

получаемой защитной пленки снижаетс . Декоративный вид также ухудщаетс , блеск пленки снижаетс , цвет темнеет.the resulting protective film is reduced. The decorative appearance also deteriorates, the gloss of the film decreases, the color darkens.

Увеличение концентрации компонентов на первой стадии обработки (вариант 5) вызывает повышенное растворение цинкового покрыти  вплоть до полного растворени  на отдельных участках, на второй стадии обработки (вариант 5), вд снижа  коррозионной стойкости, ухудшает декоративный вид;An increase in the concentration of components at the first stage of treatment (option 5) causes an increased dissolution of the zinc coating up to complete dissolution in some areas, at the second stage of treatment (option 5), reducing the corrosion resistance, deteriorating the decorative appearance;

потемнение пленки, наличие п тен.darkening of the film, the presence of spots.

При уменьшении времени обработки на обеих стади х (вариант 6) против оптимальных антикоррозионна  пленка не успевает образоватьс . Увеличение времени обработкиWhen reducing the processing time in both stages (option 6) against the optimal anti-corrosion film does not have time to form. Increase processing time

на первой стадии приводит к растворению 1данка (вариант 7), а на второй стадии (вариант 12) приводит к ухудшению декоративного вида: потемнению. .Нагрев раствора 1 стад11и обработки (вариант 8) ведет к ускоренному растворению цинка, нагрев раствора на второй стадии (вариант 9) ведет к ухудшению декоративного вида. Снижение и увеличение температуры сушки (варианты 10 и 11) против оптимальных вызывает снижение коррозионнойin the first stage, leads to the dissolution of the one (option 7), and in the second stage (option 12) leads to a deterioration of the decorative appearance: darkening. Heating the solution in stage 1 of treatment (variant 8) leads to accelerated dissolution of zinc, heating the solution in the second stage (variant 9) leads to a deterioration of the decorative appearance. A decrease and increase in drying temperature (options 10 and 11) against the optimum causes a decrease in corrosion

стойкости и ухудшение декоративного вида.resistance and deterioration of the decorative appearance.

Предлагаемый способ позвол ет повысить в 1,5-2 раза коррозио1шую стойкость защитной пленки и получить пленку декоративного вида.The proposed method makes it possible to increase the corrosion resistance of the protective film by a factor of 1.5–2 and to obtain a decorative film.

Ожидаема  экономическа  эффективность составит 15-20 тыс.руб. в год за счет повышени  качества продукции.The expected economic efficiency will be 15-20 thousand rubles. per year by improving product quality.

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Claims (1)

Формула изобретенияClaim Способ получения защитного покрытия на цинковой поверхности, включающий последовательную · обработку в растворе, содержащем азотную кислоту и фосфат металла, а затем в растворе силиката натрия и сушку при 60-80° С, отличающийся тем, что, с целью повышения коррозионной стойкости получаемого покрытия и придания ему декоративного вида, на первой стадии обработки используют раствор, содержащий азотную кислоту, гексаметафосфат натрия и оксиэтилированный фенол (ОП-10) при следующем соотношении компонентов, г/л:A method of obtaining a protective coating on a zinc surface, including sequential processing in a solution containing nitric acid and metal phosphate, and then in a sodium silicate solution and drying at 60-80 ° C, characterized in that, in order to increase the corrosion resistance of the resulting coating and giving it a decorative look, at the first stage of processing using a solution containing nitric acid, sodium hexametaphosphate and ethoxylated phenol (OP-10) in the following ratio of components, g / l: Азотная кислота 10—20Nitric acid 10-20 Гексаметафосфат натрия 5-6Sodium hexametaphosphate 5-6 ВНИИПИ Заказ 766/35VNIIIPI Order 766/35 ОП-10 2-6, 40 и на второй стадии раствор, содержащий силикат натрия и 1,2 диоксиантрахинон при следующем соотношении компонентов, г/л:OP-10 2-6, 40 and in the second stage a solution containing sodium silicate and 1,2 dioxoanthraquinone in the following ratio of components, g / l: Силикат натрия 20—50Sodium silicate 20-50 1,2—Диок сиантра45 хинон 0,05—0,11.2 — Dioc Siantra45 quinone 0.05-0.1
SU802969874A 1980-06-23 1980-06-23 Process for producing protective coating on zink surface SU908950A1 (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2487190C2 (en) * 2006-04-19 2013-07-10 Ропаль Аг Method to manufacture substrate protected against corrosion and having mirror shine
CN114029327A (en) * 2021-11-30 2022-02-11 中国原子能科学研究院 Method for cleaning and decontaminating radioactive contaminated soil
CN114085676A (en) * 2021-11-30 2022-02-25 中国原子能科学研究院 Radioactive contaminated soil cleaning agent composition, cleaning agent and preparation method and application thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2487190C2 (en) * 2006-04-19 2013-07-10 Ропаль Аг Method to manufacture substrate protected against corrosion and having mirror shine
CN114029327A (en) * 2021-11-30 2022-02-11 中国原子能科学研究院 Method for cleaning and decontaminating radioactive contaminated soil
CN114085676A (en) * 2021-11-30 2022-02-25 中国原子能科学研究院 Radioactive contaminated soil cleaning agent composition, cleaning agent and preparation method and application thereof

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