RU2706082C1 - Electrically insulating coating for electrotechnical anisotropic steel, which does not contain chromium compounds - Google Patents

Electrically insulating coating for electrotechnical anisotropic steel, which does not contain chromium compounds Download PDF

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RU2706082C1
RU2706082C1 RU2019101362A RU2019101362A RU2706082C1 RU 2706082 C1 RU2706082 C1 RU 2706082C1 RU 2019101362 A RU2019101362 A RU 2019101362A RU 2019101362 A RU2019101362 A RU 2019101362A RU 2706082 C1 RU2706082 C1 RU 2706082C1
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insulating coating
anisotropic
electrically insulating
steel
electrical
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Лариса Соломоновна Каренина
Михаил Александрович Панкратов
Борис Васильевич Паршаков
Александр Юрьевич Бородин
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Общество с ограниченной ответственностью "ВИЗ-Сталь"
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    • 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
    • C23C22/73—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 characterised by the process
    • C23C22/74—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 characterised by the process for obtaining burned-in conversion coatings

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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)
  • Soft Magnetic Materials (AREA)
  • Chemical Treatment Of Metals (AREA)

Abstract

FIELD: metallurgy.
SUBSTANCE: invention relates to ferrous metallurgy, particularly, to production of electrical anisotropic steel used for production of power and distributing magnetic cores of transformers. Composition of electrically insulating coating for anisotropic electrical steel based on phosphates of aluminum and magnesium and silicic acid sol, containing as a modifying additive zirconium silicate, with the following ratio of components, wt %: 20–40 phosphates Al and Mg, 20–40 of silicic acid sol with concentration of SiO2 10–30 %, 0.05–10 zirconium silicate and water up to 100.
EFFECT: invention enables to produce electrotechnical anisotropic steel with an electrically insulating coating produced without using environmentally harmful modifying additives based on CrIII and CrVI, having high adhesion, coefficient of resistance of the electric insulating coating, corrosion and moisture resistance, as well as having a commercial appearance.
1 cl, 1 tbl, 1 ex

Description

Изобретение относится черной металлургии, конкретно - к электроизоляционному покрытию на анизотропной электротехнической стали, используемой для изготовления магнитопроводов силовых и распределительных трансформаторов.The invention relates to ferrous metallurgy, and in particular, to an electrical insulating coating on anisotropic electrical steel used for the manufacture of magnetic cores for power and distribution transformers.

Основное назначение электроизоляционного покрытия электротехнической анизотропной стали (ЭАС) - создание изоляционного слоя между пластинами магнитопроводов трансформаторов. Для обеспечения хорошего качества электротехнических изделий покрытие должно обладать высокими техническими характеристиками - прочностью сцепления с металлом (адгезией), коррозионной стойкостью, диэлектрическими (электроизоляционными) свойствами.The main purpose of the electrical insulating coating of electrical anisotropic steel (EAS) is to create an insulating layer between the plates of the transformer magnetic circuits. To ensure good quality of electrical products, the coating should have high technical characteristics - adhesion to metal (adhesion), corrosion resistance, dielectric (electrical insulation) properties.

Электроизоляционное покрытие в технологическом цикле производства электротехнической анизотропной стали формируется в два этапа и представляет собой композит. Первоначально в процессе высокотемпературного отжига происходит формирование грунтового слоя, близкого по составу к форстериту. Затем на линии агрегата выпрямляющего отжига на поверхность стальной полосы с грунтовым слоем производится нанесение раствора магнитоактивного покрытия (МАП) на основе ортофосфорной кислоты, золя кремниевой кислоты и модифицирующих добавок на основе оксидов металлов с последующей термообработкой при температуре 800-850°С. В процессе термообработки компоненты раствора МАП и грунтового слоя образуют композит, свойства которого определяются физическими характеристиками грунтового слоя и состава раствора МАП.The electrical insulation coating in the technological cycle of production of electrical anisotropic steel is formed in two stages and is a composite. Initially, in the process of high-temperature annealing, a soil layer is formed that is close in composition to forsterite. Then, on the line of the straightening annealing unit, a solution of a magnetically active coating (MAP) based on orthophosphoric acid, silica sol and modifying additives based on metal oxides is applied to the surface of a steel strip with a soil layer, followed by heat treatment at a temperature of 800-850 ° С. During the heat treatment, the components of the MAP solution and the soil layer form a composite, the properties of which are determined by the physical characteristics of the soil layer and the composition of the MAP solution.

На данный момент большинство мировых производителей электротехнической анизотропной стали применяют рецептуру МАП на основе ортофосфорной кислоты и золя кремниевой кислоты, содержащую в качестве модифицирующих добавок соединения CrVI или в различных соотношениях сочетание CrVI с CrIII (United States Patent 3.985.583 (1), United States Patent 3.562.011 (2), United States Patent 2.753.282 (3)). Технический эффект от применения модифицирующих добавок на основе CrVI и/или CrIII в составе электроизоляционного покрытия состоит в высокой коррозионной и влагостойкости фосфатного покрытия (что особенно важно при транспортировке и дальнейшей обработке электротехнической стали в условиях с высокой влажности)At present, most global manufacturers of electrical anisotropic steel use MAP based on orthophosphoric acid and silicic acid sol containing, as modifying additives, CrVI compounds or in various ratios, a combination of CrVI with CrIII (United States Patent 3.985.583 (1), United States Patent 3.562.011 (2), United States Patent 2.753.282 (3)). The technical effect of the use of modifying additives based on CrVI and / or CrIII in the composition of the electrical insulation coating consists in high corrosion and moisture resistance of the phosphate coating (which is especially important during transportation and further processing of electrical steel in high humidity conditions)

Отрицательный эффект от применения CrVI и CrIII в качестве модифицирующих добавок в составе МАП обусловлен:The negative effect of the use of CrVI and CrIII as modifying additives in the composition of MAP is due to:

- рисками при применении и хранении раствора вследствие токсичности этих компонентов;- risks in the use and storage of the solution due to the toxicity of these components;

- ухудшением адгезии покрытия к металлу и товарного вида готовой стали вследствие высокой химической активности раствора.- deterioration in the adhesion of the coating to the metal and the presentation of the finished steel due to the high chemical activity of the solution.

Целью большинства работ, направленных на улучшение рецептуры электроизоляционного покрытия, является отказ от использования в качестве модифицирующих добавок токсичных CrVI и CrIII, а также получение покрытия с требуемым уровнем адгезии к металлу, влагостойкости, матирующими свойствами, улучшающими товарный вид стали. Немаловажным фактором для оценки результатов работ по улучшению рецептуры электроизоляционного покрытия является требование по уровню себестоимости.The goal of most work aimed at improving the formulation of the electrical insulating coating is to abandon the use of toxic CrVI and CrIII as modifying additives, as well as to obtain a coating with the required level of adhesion to the metal, moisture resistance, matting properties that improve the presentation of steel. An important factor for evaluating the results of work to improve the formulation of the electrical insulation coating is the requirement for the cost level.

Существует ряд аналогов - вариантов рецептуры, близких к (1-3), основанных на применении композиции на основе фосфатов и золя кремниевой кислоты с использованием в качестве модифицирующих добавок соединений ванадия (V) - US 20140272399 А1 (4), US 20140245926 A1, ЕР 2180082 B1 (5, 6), соединений бора (В) - US 6.461.741 B1 (9), соединений титана (Ti) - ЕР 3135793 А1, ЕР 3101157 А1 (10, 11). Однако, применение данных материалов, решая проблему токсичности раствора, не позволяет, получить покрытие с требуемым уровнем адгезии к металлу, влагостойкости и товарного вида. Применение соединений V, кроме того, экономически не выгодно из-за высокой стоимости материалов.There are a number of analogues - formulation options close to (1-3), based on the use of a composition based on phosphates and sols of silicic acid using vanadium (V) compounds as modifying additives - US 20140272399 A1 (4), US 20140245926 A1, EP 2180082 B1 (5, 6), boron compounds (B) - US 6.461.741 B1 (9), titanium compounds (Ti) - EP 3135793 A1, EP 3101157 A1 (10, 11). However, the use of these materials, solving the problem of the toxicity of the solution, does not allow to obtain a coating with the required level of adhesion to the metal, moisture resistance and presentation. The use of compounds V, in addition, is not economically viable due to the high cost of materials.

Авторы данного изобретения в качестве прототипа использовали рецептуру на основе United States Patent 3.562.011 (2), продолжили поиск решений в данном направлении и предложили следующее решение: для получения бесхроматного (экологически безопасного) покрытия с требуемым уровнем адгезии, влагостойкости и товарного вида, в состав раствора МАП в качестве модифицирующей добавки взамен соединений CrIII и CrVI вводится добавка силиката циркония (ZrSiO4) при следующем соотношении компонентов (масс. %):The authors of this invention as a prototype used a formulation based on United States Patent 3.562.011 (2), continued to search for solutions in this direction and proposed the following solution: to obtain a chromate-free (environmentally friendly) coating with the required level of adhesion, moisture resistance and presentation, in the composition of the MAP solution as a modifying additive, instead of compounds CrIII and CrVI, an addition of zirconium silicate (ZrSiO 4 ) is introduced in the following ratio of components (wt.%):

Фосфаты Al и MgPhosphates Al and Mg 20-40%20-40% Золь кремниевой кислоты (с концентрацией SiO2 10% - 30%)Silica sol (with a SiO 2 concentration of 10% - 30%) 20-40%20-40% Модифицирующая добавка силиката циркония (ZrSiO4)Zirconium Silicate Modifying Additive (ZrSiO 4 ) 0,05-10%0.05-10% ВодаWater до 100%up to 100%

Граничные условия содержания модифицирующей добавки на основе силиката циркония установлены на основании проведенных лабораторных и промышленных опытов. Нижний предел содержания модифицирующей добавки на основе силиката циркония обусловлен следующими причинами:The boundary conditions for the content of the modifying additive based on zirconium silicate are established on the basis of laboratory and industrial experiments. The lower limit of the content of the modifying additive based on zirconium silicate is due to the following reasons:

- снижение содержания ниже 0,05 массовых % приводит к отсутствию значимого эффекта от применения модифицирующей добавки для получения требуемых технических товарных характеристик анизотропной электротехнической стали (товарный вид, адгезия коэффициент сопротивления электроизоляционного покрытия, коррозионная стойкость).- a decrease in the content below 0.05 mass% leads to the absence of a significant effect from the use of modifying additives to obtain the required technical commodity characteristics of anisotropic electrical steel (presentation, adhesion, coefficient of resistance of electrical insulation coating, corrosion resistance).

Верхний предел содержания модифицирующей добавки на основе силиката циркония обусловлен следующей причинами:The upper limit of the content of the modifying additive based on zirconium silicate is due to the following reasons:

- увеличение содержания модифицирующей добавки силиката циркония более 10 массовых % приводит к техническим трудностям при приготовлении, транспортировке и хранении раствора МАП из-за седиментации частиц модифицирующей добавки;- an increase in the content of the modifying additive of zirconium silicate of more than 10 mass% leads to technical difficulties in the preparation, transportation and storage of the MAP solution due to sedimentation of particles of the modifying additive;

- увеличение содержания модифицирующей добавки силиката циркония более 10 массовых % экономически не оправдано, т.к. значимого улучшения технических и товарных характеристик при использовании модифицирующей добавки в количестве более 10 массовых % не происходит.- an increase in the content of the modifying additive of zirconium silicate of more than 10 mass% is not economically justified, because significant improvement of technical and commercial characteristics when using a modifying additive in an amount of more than 10 mass% does not occur.

Анализ научно-технической и патентной литературы показывает отсутствие совпадения отличительных признаков заявленного способа с признаками известных технических решений. На основании этого делается вывод о соответствии заявляемого технического решения критерию «изобретательский уровень».Analysis of scientific, technical and patent literature shows the lack of coincidence of the distinctive features of the claimed method with the signs of known technical solutions. Based on this, it is concluded that the claimed technical solution meets the criterion of "inventive step".

Применение изобретения позволяет получить ЭАС с электроизоляционным покрытием, произведенным без использования экологически вредных модифицирующих добавок (на основе CrIII и CrVI), одновременно с этим получить требуемые высокие технические и товарные характеристики покрытия на готовой анизотропной электротехнической стали, превосходящие аналоги по уровню адгезии электроизоляционного покрытия, товарному внешнему виду коэффициенту электроизоляционного покрытия готовой ЭАС, с требуемым уровнем коррозионной и влагостойкости.The application of the invention allows to obtain EAS with an insulating coating produced without the use of environmentally harmful modifying additives (based on CrIII and CrVI), while at the same time obtaining the required high technical and commercial characteristics of the coating on the finished anisotropic electrical steel, superior to analogues in the level of adhesion of the electrical insulation coating, the appearance of the coefficient of electrical insulation coating of the finished EAS, with the required level of corrosion and moisture resistance.

Ниже приведены варианты осуществления изобретения, не исключающие другие варианты в пределах формулы изобретения, подтверждающие эффективность использования электроизоляционного покрытия с предлагаемого состава.The following are embodiments of the invention, not excluding other options within the claims, confirming the effectiveness of the use of electrical insulation coatings of the proposed composition.

Пример. Серию плавок выплавляли в 150-тонных конвертерах (состав, масс. %: 3,10-3,14% Si, 0,032-0,-034% С, 0,003-0,004% S, 0,50-0,51%Cu, 0,015-0,017% Al, 0,010-0,011% N) разливали на УНРС на слябы, которые нагревались в нагревательных печах до температуры 1240-1260°С и затем прокатывались на непрерывном широкополосном стане горячей прокатки на полосы толщиной 2,5 мм. Горячекатаные полосы проходили травление. Травленые полосы подвергали двукратной холодной прокатке (на стане 1300 на толщину 0,70 мм и реверсивном стане на толщину 0,27 мм. На холоднокатаные полосы после 2-ой холодной прокатки наносили термостойкое покрытие. Затем полосы с нанесенным термостойким покрытием проходили высокотемпературный отжиг для проведения вторичной рекристаллизации. После высокотемпературного отжига в линии агрегата электроизоляционного покрытия на полосы наносили электроизоляционное покрытие предлагаемого состава и проводили выпрямляющий отжиг. После завершающей обработки производили измерения адгезии, коэффициента сопротивления электроизоляционного покрытия, а также производили оценку коррозионной и влагостойкости покрытия, качества электроизоляционного покрытия готовой стали - товарного внешнего вида.Example. A series of heats was smelted in 150-ton converters (composition, wt.%: 3.10-3.14% Si, 0.032-0, -034% C, 0.003-0.004% S, 0.50-0.51% Cu, 0.015-0.017% Al, 0.010-0.011% N) were poured onto UNRS into slabs that were heated in heating furnaces to a temperature of 1240-1260 ° C and then rolled on a continuous broadband hot rolling mill into strips 2.5 mm thick. Hot rolled strips were etched. The pickled strips were subjected to double cold rolling (on a 1300 mill to a thickness of 0.70 mm and a reversing mill to a thickness of 0.27 mm. A heat-resistant coating was applied to the cold-rolled strips after the second cold rolling. Then, the strips with a heat-resistant coating were subjected to high-temperature annealing for Secondary recrystallization After high-temperature annealing in the line of the electric insulating coating unit, an electrical insulating coating of the proposed composition was applied to the strips and rectifying annealing was performed. During the processing, adhesion, the coefficient of resistance of the electrical insulation coating were measured, and the corrosion and moisture resistance of the coating and the quality of the electrical insulation of finished steel — commodity appearance — were evaluated.

Результаты оценки адгезии и коэффициента сопротивления электроизоляционного покрытия электротехнической анизотропной стали, коррозионной стойкости, оценки качества покрытия и товарного вида, произведенной по известной рецептуре (прототип (2)) и заявляемой рецептуре приведены в таблице 1.The results of evaluating the adhesion and resistance coefficient of the electrical insulation coating of electrical anisotropic steel, corrosion resistance, evaluating the quality of the coating and presentation made according to the well-known recipe (prototype (2)) and the claimed recipe are shown in table 1.

Figure 00000001
Figure 00000001

Figure 00000002
Figure 00000002

Из данных (таблица 1) следует, что использование электроизоляционного покрытия заявленной рецептуры по сравнению с прототипом, использующим модифицирующие добавки на основе Cr, а так же с составами использующими вместо (CrIII и CrVI) другие модифицирующие добавки (5, 6, 9, 10, 11) позволяет получить готовый металл с более качественным электроизоляционным покрытием, обеспечивающим высокие потребительские характеристики по уровню дефектов и внешнему виду с более высокими показателями адгезии (класс адгезии увеличен с показателя C,D до А,В), с требуемым уровнем коэффициента сопротивления электроизоляционного покрытия, с требуемым уровнем коррозионной стойкости, без использования экологически небезопасных материалов в своем составе.From the data (table 1) it follows that the use of an electrical insulating coating of the claimed formulation compared to the prototype using modifying additives based on Cr, as well as with compositions using other modifying additives instead of (CrIII and CrVI) (5, 6, 9, 10, 11) allows you to get finished metal with a better electrical insulating coating, providing high consumer characteristics in terms of defects and appearance with higher adhesion (adhesion class increased from C, D to A, B), with the required the level of resistance coefficient of the electrical insulation coating, with the required level of corrosion resistance, without the use of environmentally unsafe materials in its composition.

Источники информацииInformation sources

1. United States Patent 3.985.583, Oct. 12, 19761. United States Patent 3.985.583, Oct. 12, 1976

2. United States Patent 3.562.011, Feb.9, 19712. United States Patent 3.562.011, Feb.9, 1971

3. United States Patent 2.753.282, July.3, 19563. United States Patent 2.753.282, July.3, 1956

4. US 20140272399 A1, Sep.18.20144. US 20140272399 A1, Sep. 18.2014

5. US 20140245926 A1, Sep.4.20145. US 20140245926 A1, Sep 4.2014

6. EP2 180082 B1 02.04.20146. EP2 180082 B1 04/02/2014

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Claims (4)

Состав электроизоляционного покрытия для анизотропной электротехнической стали на основе фосфатов алюминия и магния и золя кремниевой кислоты, содержащий в качестве модифицирующей добавки силикат циркония при следующем соотношении компонентов, мас. %:The composition of the electrical insulation coating for anisotropic electrical steel based on aluminum and magnesium phosphates and silica sol, containing zirconium silicate as a modifying additive in the following ratio, wt. %: Фосфаты Al и MgPhosphates Al and Mg 20-4020-40
Золь кремниевой кислоты с концентрацией SiO2 10-30%Silica sol with a SiO 2 concentration of 10-30% 20-4020-40
Силикат циркония (ZrSiO4) Zirconium Silicate (ZrSiO 4 ) 0,05-100.05-10 ВодаWater до 100up to 100
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