EP0842309A1 - Verfahren zur einlagerung von solen in mikroporöse deckschichten - Google Patents
Verfahren zur einlagerung von solen in mikroporöse deckschichtenInfo
- Publication number
- EP0842309A1 EP0842309A1 EP96922737A EP96922737A EP0842309A1 EP 0842309 A1 EP0842309 A1 EP 0842309A1 EP 96922737 A EP96922737 A EP 96922737A EP 96922737 A EP96922737 A EP 96922737A EP 0842309 A1 EP0842309 A1 EP 0842309A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- lyosol
- silica
- microporous
- pores
- capillaries
- Prior art date
- Legal status (The legal status 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 status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/18—After-treatment, e.g. pore-sealing
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/30—Anodisation of magnesium or alloys based thereon
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/024—Anodisation under pulsed or modulated current or potential
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/026—Anodisation with spark discharge
Definitions
- aluminum is relatively corrosion-resistant because the metal surface in the air is immediately covered with a 5 to 20 nm thick, firmly adhering and very dense oxide layer which prevents further oxygen access.
- Magnesium and titanium and their alloys are also protected against further oxidation by a thin oxide layer at normal temperature.
- the anodically produced coating consists, for example, of a coherent sub-layer (barrier layer) about 0.15 ⁇ m thick and a microporous cover layer, which consists of capillaries perpendicular to the metal of 0.01 to 0.05 ⁇ m (10 - 50 nm) is penetrated at a distance of about 0.3 ⁇ m.
- the microporous cover layer has an inner surface of about 100 m / g after its production and is very chemically reactive. This high chemical reactivity is caused by active centers, which are formed by OH groups in the near-surface area of the microporous cover layer (see Peri, J.B .: J.Phsy.Chem. 69 (1965), p. 220). With newer methods of anodic oxidation, microporous cover layers down to about 200 ⁇ m can be created on Al materials.
- Anodic oxidation of magnesium can also be used to produce microporous cover layers which are oxidic in nature and, if appropriate
- Anodic oxidation of titanium also forms microporous cover layers with different oxidic compositions
- the pores are of different sizes. They range in size from 10 nm to 30 ⁇ m.
- Coating film on the corrosion-resistant anodized surface film of aluminum products in which this includes subjected to a sealing treatment of the micropores in the oxide film by immersing them in an aqueous sealing liquid containing dispersed silica and then coating them with a thermosetting acrylic resin.
- the purpose of this process is to be able to use coating agents with a drying or curing temperature of 140 ° C. or above due to the sealing treatment, in which problems of cracking and insufficient adhesion previously occurred.
- Oxide films by immersing the aluminum objects in the aqueous sealing liquid containing silica or silicate should also close the micropores so that, for example, sulfuric acid remaining therein can no longer escape; but it was not possible or intends to fill the vertical capillaries with the silica.
- the aim of the invention is to avoid the corrosion caused by the pores and to produce a stable bond between the microporous oxide cover layer and at least one compound forming an inorganic network.
- the invention relates to a process for the treatment of microporous top layers produced by anodic oxidation or by plasma-chemical anodic oxidation on objects made of aluminum, magnesium, titanium or their alloys, in the form of silica in the pores or capillaries of the microporous top layer a lyosol is introduced in which the colloidally distributed Si0 2 particles are at least one dimension smaller than the diameter of the pores or capillaries and the introduced and applied silica lyosol is then coagulated or reacted with the cover layer.
- a lyosol is a colloidal solution in which a solid substance is dispersed in a finely divided form in a liquid.
- Organosols and hydrosols can also be used for the purposes of the invention, depending on whether it is a suspension of the silica in organic liquids, such as alcohols, preferably C 1 -C 6 -alcohols, or water.
- organic liquids such as alcohols, preferably C 1 -C 6 -alcohols, or water.
- the silica lyosol is a silica sol (see Römpp, chemistry lexicon, key words brine and silica sol).
- the sol In order to achieve an incorporation of the sol into the pores or capillaries, it is introduced according to the invention in a form in which the SiO 2 particles are at least one dimension smaller than that
- the size of the particles of colloidal silica in the sol is accordingly about 1 to 50 nm, preferably 1 to 10 nm.
- the particles of the colloidal silica to be introduced are Appropriately as an aqueous and / or organic dispersion.
- the film formers such as alcohols and / or silanes and / or salts of organic acids, which tend to polymerize or polycondense, are added to the SiO 2 sols.
- Silica sols suitable for the purposes of the invention are known. They are produced by in situ growth of Si0 2 micro-nuclei and are then present as a concentrated aqueous dispersion of colloidally distributed pore-free amorphous Si0 2 particles. These Si0 2 dispersions generally contain minor amounts of alkali, which negatively charge the surface of the Si0 2 particles. As a result, the particles repel each other and bring about the stability of the solution. Silica sols which are suitable for the purposes of the invention are commercially available, for example, under the name KLEBOSOL. These can also be modified by other film-forming oxides of the third to eighth group of the periodic system of the elements, for example aluminum, indium, zirconium, titanium, iron, nickel and rare earths. Modification with mono- or polyhydric alcohols, eg diethylene glycol, is also possible. The silica lyosols can be produced by in situ growth of Si0 2 micro-nuclei and are then present as a concentrated aqueous dispersion
- Substances especially alcohols and silanes, are added which form films with the silica.
- the sols can also contain fillers, corrosion inhibitors, dyes, lubricants, surface-active substances, UV stabilizers in amounts which do not affect the reactivity of the sol with the microporous top layer.
- Solids concentration of the silica sol is advantageously 15 to 60%, preferably 30 to 50%.
- Objects with such oxide cover layers are immersed in the lyosol, in particular silica sol, sprayed or painted with them.
- the introduction can be improved in that the object provided with the oxide layer and immersed in the lyosol changes Exposed to pressure conditions.
- An impregnation system is suitable for this, in which the air is first removed from the pores or capillaries using a vacuum. Under the action of the vacuum, the lyosol penetrates into the pores and, after the vacuum is released, is pressed into the pores by atmospheric pressure and thus also reaches the bottom of the vertical capillaries of the anodically produced coatings of aluminum or the finest branches of the microporous cover layers on magnesium or titanium materials or on the oxide ceramic layers produced by plasma chemical oxidation.
- the change from vacuum and pressure, which can also exceed atmospheric pressure, is repeated one or more times if necessary.
- Devices suitable for introducing the particles into the microporous cover layer of the objects are available, for example, in the form of the Maldaner impregnation system.
- microporous cover layers such as hard anodized layers or oxide ceramic layers, which are less than 24 hours old, accelerate the incorporation of the silica sol to the bottom of the capillaries and pores by anodic oxidation or by plasma-chemical anodic oxidation.
- Coagulation of the silica lyosol according to the sol-gel process known per se for the film formation of such brine (Sol-Gel Technology for thin Films, Fibers, Preforms, Electronics, and Specialty Shapes, edited by Lisa Klein, Noyes Publications, S. 50 ff., Sect. 4, Helmut Dislich, Thin Films from the Sol-Gel Process). Coagulation takes place by withdrawing the liquid from the lyosol, in particular the silica sol.
- This silicate glass layer formed on the surface of the microporous cover layer from the Si0 2 particles is provided with pins protruding vertically into the capillaries of the anodized layer and having a diameter of 10 to 50 nm or in the manner of roots which penetrate the capillaries of other oxide layers, in particular ceramic layers. protrude, firmly anchored in the microporous top layer. That is probably the reason for the high corrosion and scratch resistance.
- the invention also relates to components made of aluminum,
- the surface of the microporous cover layer is preferably also covered with a film of these gels and connected to the gels in the pores or capillaries.
- magnesium casting alloys of the ASTM designation are also suitable for the purposes of the invention.
- EP-B-333 084 were treated according to the ORMOCER process in order to fill the capillaries and pores and to seal the surface of the microporous cover layer.
- a scanning electron micrograph on a cross-section shows that the pores and capillaries are filled with the silicon dioxide formed after the thermal treatment or its reaction products.
- the outer sealing layer has a thickness of approximately 5 ⁇ m.
- plates After immersion in soda water glass and subsequent silicification in a CO 2 atmosphere, plates likewise had an approximately 5 ⁇ m thick sealing layer and in the neutral salt spray test mentioned only a service life of approx. 200 hours.
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Other Surface Treatments For Metallic Materials (AREA)
- Laminated Bodies (AREA)
- Manufacturing Of Micro-Capsules (AREA)
- Saccharide Compounds (AREA)
- Paints Or Removers (AREA)
- Polyurethanes Or Polyureas (AREA)
- Materials For Medical Uses (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Physical Vapour Deposition (AREA)
- Chemical Vapour Deposition (AREA)
- Preventing Corrosion Or Incrustation Of Metals (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Description
Claims
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE19527688 | 1995-07-28 | ||
DE19527688 | 1995-07-28 | ||
PCT/DE1996/001188 WO1997005302A1 (de) | 1995-07-28 | 1996-07-02 | Verfahren zur einlagerung von solen in mikroporöse deckschichten |
Publications (3)
Publication Number | Publication Date |
---|---|
EP0842309A4 EP0842309A4 (de) | 1996-09-30 |
EP0842309A1 true EP0842309A1 (de) | 1998-05-20 |
EP0842309B1 EP0842309B1 (de) | 2002-01-16 |
Family
ID=7768067
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP96922737A Expired - Lifetime EP0842309B1 (de) | 1995-07-28 | 1996-07-02 | Verfahren zur einlagerung von solen in mikroporöse deckschichten |
Country Status (7)
Country | Link |
---|---|
EP (1) | EP0842309B1 (de) |
AT (1) | ATE212075T1 (de) |
AU (1) | AU6352796A (de) |
DE (3) | DE59608600D1 (de) |
ES (1) | ES2168491T3 (de) |
PT (1) | PT842309E (de) |
WO (1) | WO1997005302A1 (de) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US8747641B2 (en) | 2007-03-16 | 2014-06-10 | Suddeutsche Aluminium Manufaktur Gmbh | Partial pigmentation of a coating layer to prevent interference on aluminum components or components comprising aluminum |
Families Citing this family (12)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE19741580A1 (de) * | 1997-09-20 | 1999-04-01 | Bosch Gmbh Robert | Verbundwerkstoff |
CA2382164A1 (en) * | 1999-08-17 | 2001-02-22 | Alexandr Sergeevich Shatrov | Light alloy-based composite protective multifunction coating |
DE102006045617B4 (de) * | 2006-09-22 | 2010-06-10 | Innovent E.V. Technologieentwicklung | Verfahren zur Herstellung einer anorganisch-anorganischen Gradientenverbundschicht |
DE102007027628B3 (de) * | 2007-06-12 | 2008-10-30 | Siemens Ag | Verfahren zum Einbringen von Nanopartikeln in eine anodisch oxidierte Aluminiumoberfläche |
EP2166200A1 (de) | 2008-09-23 | 2010-03-24 | Franz Rübig & Söhne GmbH & Co. KG | Ventilfederteller und Verfahren zu dessen Herstellung |
GB2469115B (en) | 2009-04-03 | 2013-08-21 | Keronite Internat Ltd | Process for the enhanced corrosion protection of valve metals |
CN102199785B (zh) * | 2011-06-29 | 2012-12-12 | 上海理工大学 | 一种钛合金耐磨涂层的微弧氧化溶液及其应用 |
GB2513575B (en) * | 2013-04-29 | 2017-05-31 | Keronite Int Ltd | Corrosion and erosion-resistant mixed oxide coatings for the protection of chemical and plasma process chamber components |
CN106435685B (zh) * | 2016-09-18 | 2018-09-07 | 佛山科学技术学院 | 铝表面电沉积制备低吸收率与高半球发射率氧化膜的方法 |
DE102017207589A1 (de) * | 2017-05-05 | 2018-11-08 | Federal-Mogul Nürnberg GmbH | Thermisch isolierende Beschichtung für einen Aluminiumkolben |
US11312107B2 (en) * | 2018-09-27 | 2022-04-26 | Apple Inc. | Plugging anodic oxides for increased corrosion resistance |
FR3101361B1 (fr) * | 2019-09-27 | 2022-01-14 | Liebherr Aerospace Toulouse Sas | Procede de fabrication d’une pièce resistante au feu d’un systeme de conditionnement d’air et pièce obtenue par un tel procede |
Family Cites Families (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR802421A (fr) * | 1936-02-26 | 1936-09-04 | Protection du magnésium contre la corrosion par vitrification | |
JPS582596A (ja) * | 1981-06-30 | 1983-01-08 | Nippon Parkerizing Co Ltd | アルミニウム製熱交換器の表面処理法 |
JPS5959896A (ja) * | 1982-09-28 | 1984-04-05 | Nippon Light Metal Co Ltd | アルミニウム陽極酸化皮膜を封孔処理する方法 |
JPS59179798A (ja) * | 1983-03-30 | 1984-10-12 | Mitsubishi Heavy Ind Ltd | アルミニウム又はその合金部材 |
JPS61250193A (ja) * | 1985-04-26 | 1986-11-07 | Pentel Kk | 滑り止め性を有するアルミニウム又はアルミニウム合金成形体の表面処理法 |
DE3808610A1 (de) * | 1988-03-15 | 1989-09-28 | Electro Chem Eng Gmbh | Verfahren zur oberflaechenveredelung von magnesium und magnesiumlegierungen |
EP0410003B1 (de) * | 1989-02-14 | 1994-11-02 | Sumitomo Electric Industries, Ltd. | Isolierte drahtlitze |
JPH0327043A (ja) * | 1989-06-23 | 1991-02-05 | Fuji Photo Film Co Ltd | 湿し水不要感光性平版印刷版 |
JPH04311595A (ja) * | 1991-04-08 | 1992-11-04 | Nippon Parkerizing Co Ltd | アルミニウムのセラミックコーティング方法 |
JPH06316787A (ja) * | 1993-04-28 | 1994-11-15 | Kojundo Chem Lab Co Ltd | アルマイトの表面処理法 |
-
1996
- 1996-07-02 DE DE59608600T patent/DE59608600D1/de not_active Expired - Fee Related
- 1996-07-02 ES ES96922737T patent/ES2168491T3/es not_active Expired - Lifetime
- 1996-07-02 DE DE29680628U patent/DE29680628U1/de not_active Expired - Lifetime
- 1996-07-02 AT AT96922737T patent/ATE212075T1/de not_active IP Right Cessation
- 1996-07-02 EP EP96922737A patent/EP0842309B1/de not_active Expired - Lifetime
- 1996-07-02 AU AU63527/96A patent/AU6352796A/en not_active Abandoned
- 1996-07-02 DE DE19680596A patent/DE19680596C1/de not_active Expired - Fee Related
- 1996-07-02 PT PT96922737T patent/PT842309E/pt unknown
- 1996-07-02 WO PCT/DE1996/001188 patent/WO1997005302A1/de active IP Right Grant
Non-Patent Citations (1)
Title |
---|
See references of WO9705302A1 * |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US8747641B2 (en) | 2007-03-16 | 2014-06-10 | Suddeutsche Aluminium Manufaktur Gmbh | Partial pigmentation of a coating layer to prevent interference on aluminum components or components comprising aluminum |
Also Published As
Publication number | Publication date |
---|---|
EP0842309B1 (de) | 2002-01-16 |
DE19680596D2 (de) | 1997-09-18 |
ES2168491T3 (es) | 2002-06-16 |
PT842309E (pt) | 2002-07-31 |
AU6352796A (en) | 1997-02-26 |
EP0842309A4 (de) | 1996-09-30 |
WO1997005302A1 (de) | 1997-02-13 |
ATE212075T1 (de) | 2002-02-15 |
DE19680596C1 (de) | 2001-08-23 |
DE29680628U1 (de) | 1998-11-05 |
DE59608600D1 (de) | 2002-02-21 |
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