GB2162865A - Surface preparation for aluminum parts - Google Patents
Surface preparation for aluminum parts Download PDFInfo
- Publication number
- GB2162865A GB2162865A GB08519539A GB8519539A GB2162865A GB 2162865 A GB2162865 A GB 2162865A GB 08519539 A GB08519539 A GB 08519539A GB 8519539 A GB8519539 A GB 8519539A GB 2162865 A GB2162865 A GB 2162865A
- Authority
- GB
- United Kingdom
- Prior art keywords
- chromate
- coated
- coating
- aluminum
- applying
- 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
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J5/00—Adhesive processes in general; Adhesive processes not provided for elsewhere, e.g. relating to primers
- C09J5/02—Adhesive processes in general; Adhesive processes not provided for elsewhere, e.g. relating to primers involving pretreatment of the surfaces to be joined
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2400/00—Presence of inorganic and organic materials
- C09J2400/10—Presence of inorganic materials
- C09J2400/16—Metal
- C09J2400/166—Metal in the pretreated surface to be joined
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Chemical Treatment Of Metals (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
Abstract
For preparing a surface of a part comprising aluminum for subsequent application of a structural bonding adhesive, a coating of chromate of predetermined thickness is first applied to the surface of the part. A primer layer having predetermined thickness is applied over the chromate coating and the chromate- coated and primed part heated at a predetermined temperature for a predetermined time. The part is subsequently cooled to substantially room temperature. The thusly treated part may be adhesively bonded to a similarly prepared part by applying an adhesive to at least one of the treated surfaces of the parts, bonding the parts together, and curing the adhesive. <IMAGE>
Description
SPECIFICATION
Surface preparation for aluminum parts
Background of the Invention
This invention relates generally to the art of structural adhesive bonding of metals and more particularly to preparation of the surfaces of aluminum, or aluminum alloy, parts for structural adhesive bonding of such parts.
As is known, proper preparation of the surfaces of the aluminum parts to be adhesively bonded is necessary if a durable bond between them is to be achieved. One surface preparation technique is Phosphoric Acid Anodizing (PAA), a process described in U.S. Patent No.
4,085,012, issued to Marceau et al in which the aluminum parts are immersed in a phosphoric acid solution while an electric current is passed through the parts. This anodizing produces a film of aluminum oxide on the surface of the parts which facilitates adhesive bonding thereto.
While the PAA process has yielded satisfactory results, the produced aluminum oxide film is quite fragile, making the PAA treated surface very sensitive to handling.
Another method of preparing the surface of aluminum parts for structural adhesive bonding is chromate conversion coating, wherein a layer of chromate material is applied to the surfaces of the aluminum parts to be bonded. The applied chromate coating converts each such surface to a superficial layer containing a complex mixture of chromium compounds to provide the subsequently bonded joint with increased corrosion protection. An article entitled "Effect of
Surface Preparation on Stressed Aluminum Joints in Corrosive Saltwater Exposure", appearing in Adhesives Age in October, 1980, noted that when a coating of chromate is applied to the surfaces of aluminum parts followed by a coating of high temperature curing adhesive, and the adhesive cured by heating the thus coated parts for a predetermined time, a durable adhesive bond between them is obtained.However, high temperature curing adhesives are generally inconvenient in a manufacturing environment. The article's author postulated that the high bond durability was possible due to a thermally induced structural change in the chromate. The author further theorized that the use of a room temperature curing adhesive in place of the high temperature curing adhesive would lead to different results; however, he did not pursue this theory- further.
Summary of the Invention
In accordance with the present invention, a process is described for preparing a surface of a part comprising aluminum for subsequent application of a structural bonding adhesive, comprising the steps of: applying a coating of chromate to the surface of the part; heating the chromate-coated part; and, subsequently cooling the chromate-coated part to substantially room temperature for application of the bonding adhesive. By the use of such process, an extremely durable structural bond to the part may be achieved using a room temperature curing adhesive.
In a preferred embodiment of the present invention, the process for preparing a surface of a part comprising aluminum for subsequent application of a structural bonding adhesive first comprises the step of applying a coating of chromate to the surface of the part. A layer of primer is then applied over the chromate layer. The chromate-coated and primed aluminum part is heated to thermally "age" the chromate and cure the primer. The part is subsequently cooled to substantially room temperature. The thusly treated surface of the part may then have a layer of a room temperature curing adhesive applied thereto for structural bonding to a similarly treated surface of another part. In the interim, and unlike Phosphoric Acid Anodizing (PAA) treated aluminum, the surface of the parts treated by the process of the present invention is quite insensitive to handling.
Additionally, the present invention provides a process for bonding a first part comprising aluminum with a second part comprising aluminum. The first step in such process is applying a coating of chromate having a predetermined thickness to a surface of each of the parts. The chromate-coated parts are then heated at a predetermined temperature for a predetermined time and are subsequently cooled to substantially room temperature. An adhesive is applied to the chromate-coated surface of at least one of the cooled parts, and the parts bonded together.
Brief Description of the Drawings
The foregoing features of the present invention and the advantages thereof may be more fully understood from the following detailed description when read in conjunction with the accompanying drawings wherein:
Figure 1 is a flow diagram of a first embodiment of the aluminum surface preparation process of the present invention; and
Figure 2 is a flow diagram of a second embodiment of the aluminum surface preparation process of the present invention.
Description of the Preferred Embodiments
Referring now to Fig. 1, the aluminum surface preparation process of the present invention is illustrated. The first step in this process consists of applying a coating of chromate having a predetermined thickness to the surface of the aluminum, or aluminum alloy, parts which are to
be adhesively bonded together. As hereinafter used, the term aluminum encompasses the metal
aluminum and alloys thereof. One method of applying the- chromate coating is to immerse the
parts in a chromate solution, although the chromate film may also be applied by spraying,
brushing or swabbing the parts.As is known, chromate is a complex mixture of chromium with
additional compounds, and is commercially available under several trade names, such as Iridite,
manufactured by the Allied-Kelite Division of Witco Chemical Corporation of Des Plaines, lowa, and Alodine, manufactured by Amchem Products Inc. of Ambled, Pennsylvania.
Proper chromate thickness is necessary to provide an optimum bond. Sufficient chromate is
needed to prevent moisture from affecting the bonded joint and thus corroding the bond and
reducing durability. However, if the chromate coating is too thick, the bonded joint may fail in the chromate coating itself. The concentration of the chromate solution, its degree of acidity
(pH) and temperature, the immersion time, and the alloy composition of the part being
chromated all influence the thickness of the chromate coating. An acceptable concentration
range for the chromate solution, using Iridite material as the chromate, is between 1.0and 1.5
ounces of Iridite material per gallon of solvent (here, water). This yields a chromate solution with
a pH of between 1.3 and 1.6.The temperature of the solution should be between 60'F and 100"F. Proper immersion time is between 25 and 45 seconds.
Proper chromate thickness is on the order of a few millionths of an inch; therefore, it is
impractical to measure absolutely the thickness of the chromate coating. However, it is possible
to determine whether the chromate coating thickness of a given chromated part is within an
acceptable range, that is, neither too thin nor too thick. This can be done by comparing the
color of such chromated part with color standards. The color of a chromate-coated part ranges
from clear, for a very thin chromate coating, to brown for a much thicker coating. Thus, color
standards representing a color range corresponding to a thickness range can be obtained.The
first-color standard, representing the thinnest acceptable chromate coating, is obtained by
immersing sample sections (called coupons) of aluminum into the weakest chromate solution to
be used (here 1.0 oz. of Iridite chromate/gal. of water) for the minimum practiced time (here 25
sec.). The second color standard, representing the thickest acceptable chromate coating, is
produced by dipping aluminum coupons into the strongest chromate solution to be used (here
1.5 oz of Iridite chromate/gal.) for the maximum practiced time (here 45 sec.). Thus, a
standard color range is found, to which the color of the parts chromated for bonding are
compared to determine if the chromate coating of such parts is of the proper thickness.
By thermally "aging" the chromate a strong and durable adhesive bond may be made to the
chromated aluminum parts. Thermally "aging" the chromate is the second step of the surface
preparation process of the present invention and is performed by heating the chromåte-coated aluminum parts at a predetermined temperature, for example, 350"F, for a predetermined time,
fOr example, two hours. The chromated aluminum parts- are then cooled to substantially room
temperature.The "aged" chromated aluminum parts were examined using Electron Spectros
copy for Chemical Analysis (ESCA) (also called photoelectron spectroscopy), a generally known - surface analysis technique in which x-rays having known energy are directed at the surface of
the "aged" chromated parts and the energy of electrons emitted therefrom in response to the x
rays analyzed to identify the element from which the electrons came and the molecular
configuration of such element.The use of ESCA on the "aged" chromated parts reveals that the
thermal "aging" converts the normally trivalent chromium atom (cur+3) of the chromate to
hexavalent chromium (cur+6). As is known, hexavalent chromium resists corrosion better than
does trivalent chromium; thus, a more durable bond can be obtained by bonding to the "aged" chromate surfaces of the parts. As the table below shows, the higher the aging temperature, the
more complete the conversion. However, care should be taken not to expose the aluminum parts
to excessive temperatures, as this may mechanically weaken the metal. The table also shows
that the conversion process will take place in an inert atmosphere of nitrogen, as well as in air.
This indicates that the conversion reaction is internal to the chromium and is not part of an
oxidation process.
Chromium Oxidation State Percentages
Chromium 2P
Sample Hexavalent Trivalent
Non-thermally aged 36.6% 63.4%
2 hrs. at 2500F in air 41.8% 54.2%
2 hrs. at 3000F in air 48.5% 45.3%
2 hrs. at 3500F in air 55.9% 30.2% 2 hrs. at 2500F in N2 44.% 52.6%
2 hrs. att300 F in N2 47.3% 41.8% 2 hrs. at 350 F in N2 52.4% 31.6%
The next step in the aluminum surface preparation process is to apply a layer of primer to the chromated aluminum parts. As is known, primer is an epoxy-based material containing hexavalent chromium and assists the chromate layer in resisting corrosion of the subsequently bonded joint. Here, the primer is EA-9228, manufactured by the Hysol Division of the Deter Corp. of Pittsburg, California, although other primers may be used.The thickness of the primer layer must be controlled for the same reason as the chromate thickness: sufficient primer must be applied to provide, along with the chromate coating, corrosion protection to prevent moisture from affecting the bonded joint; however, the primer layer must not be so thick that it becomes weaker than the bonded joint itself. An acceptable range of primer thickness is between 0.2 mil to 0.4 mil (i.e., 0.0002 to 0.0004 inches). The primer can be applied either by spraying or by dipping the chromated aluminum parts in a primer solution and conventional techniques may be used to measure primer thickness.
The primer must be cured. Conventionally, this is done by heating the primed aluminum parts at about 250"F for about one hour, although other temperatures and times may be used. While this extra heating cycle will not adversely affect the "aged" chromate (in fact, it may convert more trivalent chromium to hexavalent chromium), the cycle is redundant given the prior step of thermally aging the chromate. Therefore, the preferred method, depicted in the flow diagram of
Fig. 2,-is to apply the primer layer to the chromated aluminum parts prior to thermally aging the chromate. Thus, heating the chromated and primed aluminum parts for two hours at 350"F, for example, both ages the chromate (converts trivalent chromium to hexavalent chromium) and cures the primer.The chromated and primed aluminum parts are cooled to room temperature and are ready to be bonded together. In fact, this process yields even higher adhesive bond strengths than does the process of chromating, aging, priming and primer curing.
Whichever of the two methods is used, once the primer is cured the parts can be stored for long periods of time (up to at least one year) and handled without special sanitary precautions without contaminating the treated surfaces. The surfaces need only be cleaned with, for example, an ordinary solvent prior to bonding.
The surfaces of the aluminum parts having been prepared by the process of the present invention, a room temperature curing adhesive is applied to at least one of the prepared surfaces of the parts, and the surfaces of the parts placed together and held in place by conventional means, such as clamps, while the adhesive cures. Here, the adhesive is EA-9320NA, manufactured by the Hysol Division of the Dexter Corporation of Pittsburg, California, although other adhesives may be used. Typically, a room temperature curing adhesive obtains its maximum adhesive quality after about seven days at room temperature. Once the adhesive has cured, the clamps are removed and the parts durably held together by the adhesive bond.
The parts need not be bonded with room temperature curing adhesive, however. Higher temperature curing (i.e. oven-cured) adhesives may be used as well, with equivalent or better bond strength and durability being achieved, although high temperature curing adhesives are generally inconvenient in a manufacturing environment.
Having described preferred embodiments of the present invention, minor modifications may become apparent to those skilled in the art without departing from the spirit of the invention. It is therefore understood that the scope of the present invention is to be limited only by the scope of the appended claims.
Claims (14)
1. A process for preparing a surface of a part for subsequent application of a structural bonding adhesive, comprising the steps of:
applying a coating of chromate to the surface of the part;
heating the chromate-coated part; and
subsequently cooling the chromåte-coated part to substantially room temperature
2. The process recited in claim 1 wherein the part comprises aluminum.
3. The process recited in claim 2 wherein the heating of the chromate-coated part is for a predetermined time.
4. The process recited in claim 3 wherein said predetermined time is substantially two hours.
5. The process recited in claim 2 wherein the heating of the chromate-coated part is done at a predetermined temperature.
6. The process recited in claim 5 wherein said predetermined temperature is substantially 350"F.
7. The process recited in claim 1, comprising the additional steps of:
applying a layer of primer over the coating of chromate after the chromate-coated part has been cooled to substantially room temperature; and
curing the primer.
8. The process recited in claim 7 wherein the applied primer layer has a predetermined thickness.
9. The process recited in claim 8 wherein said predetermined thickness is substantially 0.2 to 0.4 mil.
10. A process for preparing a surface of a first part comprising aluminum for adhesive bonding to a second part comprising aluminum, said process comprising the steps of:
applying a coating of chromate to the surface of the first part;
heating the chromate-coated first part;
subsequently cooling the chromate-coated first part; and
applying a layer of adhesive to the cooled, chromate-coated first part.
11. The process recited in claim 10 comprising the additional step of:
applying a layer of primer to the chromate-coated first part before said heating step.
1 2. A process for preparing a surface of a part for subsequent application of a structural bonding adhesive, said part being a metal selected from the group consisting of aluminum and alloys of aluminum, said process comprising the steps of:
applying a coating of chromate to the surface of the part;
applying a layer of primer over the chromate coating;
heating the chromate-coated and primed part; and
subsequently cooling the part to substantially room temperature.
1 3. The process recited in claim 1 2 wherein said chromate coating has a first predetermined thickness and said layer of primer has a second predetermined thickness.
14. The process recited in claim 1 3 wherein the second predetermined thickness of the primer layer is substantially between 0.2 to 0.4 mil.
1 5. A process for bonding a first part comprising aluminum with a second part comprising aluminum, comprising the steps of:
applying a coating of chromate having a predetermined thickness to a surface of each of the parts;
heating the chromate-coated parts at a predetermined temperature for a predetermined time and subsequently cooling said parts to substantially room temperature;
applying an adhesive to the chromate-coated surface of at least one of the cooled parts; and
bonding the parts together.
1 6. The process recited in claim 15 further comprising the step of:
applying a layer of primer over the coating of chromate before said heating step.
1 7. A method for determining a chromate thickness of a chromate-coated part relative to a predetermined chromate thickness of a chromate-coated sample part, said method comprising the step of:
comparing the color of the chromate-coated part with the color of chromate-coate sample part.
1 8. The method recited in claim 1 7 further comprising the step of comparing the color of the chromate-coated part with the color of a second chromate-coated sample part to determine whether the chromate thickness of the chromate-coated part is within a predetermined thickness range, and wherein:
the first-mentioned sample part is immersed in a first chromate solution, having a first concentration, for a first predetermined time to develop a chromate coating having a first predetermined thickness, the chromate-coated first-mentioned sample having a first color corresponding to the first predetermined thickness; and
the second sample part is immersed in a second chromate solution, having a second concentration, for a second predetermined time to develop a chromate coating having a second predetermined thickness, the chromate-coated second sample having a second color corresponding to the second predetermined thickness.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US63799984A | 1984-08-06 | 1984-08-06 |
Publications (3)
| Publication Number | Publication Date |
|---|---|
| GB8519539D0 GB8519539D0 (en) | 1985-09-11 |
| GB2162865A true GB2162865A (en) | 1986-02-12 |
| GB2162865B GB2162865B (en) | 1988-07-13 |
Family
ID=24558236
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| GB08519539A Expired GB2162865B (en) | 1984-08-06 | 1985-08-02 | Process for preparing a surface for application of structural bonding adhesive |
Country Status (3)
| Country | Link |
|---|---|
| JP (1) | JPS6148574A (en) |
| CA (1) | CA1249494A (en) |
| GB (1) | GB2162865B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2189816A (en) * | 1986-03-31 | 1987-11-04 | Toshiba Kk | Chromated non-ferrous metal mechanical part |
| EP0467197A2 (en) * | 1990-07-14 | 1992-01-22 | Westfalia-Werke Knöbel GmbH & Co. | Method for fixed connection of metallic building components to a metallic support |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB925904A (en) * | 1960-11-07 | 1963-05-15 | British Iron Steel Research | Improvements in or relating to the treatment of elongate ferrous material |
| GB930755A (en) * | 1959-07-03 | 1963-07-10 | Diversey U K Ltd | Deoxidizer for an aluminium surface, a concentrate therefor and a process for utilising the deoxidizer |
| GB1214643A (en) * | 1967-09-04 | 1970-12-02 | Steel Co Of Wales Ltd | Improvements in and relating to the treatment of steel strip |
| GB1234181A (en) * | 1967-06-14 | 1971-06-03 | ||
| US3954510A (en) * | 1972-10-18 | 1976-05-04 | Diamond Shamrock Corporation | Metal treating compositions of controlled pH |
| GB1478979A (en) * | 1973-11-09 | 1977-07-06 | British Steel Corp | Chromating of metals |
| US4131489A (en) * | 1978-03-31 | 1978-12-26 | Amchem Products, Inc. | Chromate conversion composition and method for coating aluminum using low concentrations of chromate, phosphate and fluoride ions |
| WO1981002749A1 (en) * | 1980-03-25 | 1981-10-01 | Eltzroth & Ass J M | Composition for inhibiting corrosion of metal surfaces |
-
1985
- 1985-07-11 CA CA000486657A patent/CA1249494A/en not_active Expired
- 1985-08-02 GB GB08519539A patent/GB2162865B/en not_active Expired
- 1985-08-06 JP JP17306285A patent/JPS6148574A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB930755A (en) * | 1959-07-03 | 1963-07-10 | Diversey U K Ltd | Deoxidizer for an aluminium surface, a concentrate therefor and a process for utilising the deoxidizer |
| GB925904A (en) * | 1960-11-07 | 1963-05-15 | British Iron Steel Research | Improvements in or relating to the treatment of elongate ferrous material |
| GB1234181A (en) * | 1967-06-14 | 1971-06-03 | ||
| GB1214643A (en) * | 1967-09-04 | 1970-12-02 | Steel Co Of Wales Ltd | Improvements in and relating to the treatment of steel strip |
| US3954510A (en) * | 1972-10-18 | 1976-05-04 | Diamond Shamrock Corporation | Metal treating compositions of controlled pH |
| GB1478979A (en) * | 1973-11-09 | 1977-07-06 | British Steel Corp | Chromating of metals |
| US4131489A (en) * | 1978-03-31 | 1978-12-26 | Amchem Products, Inc. | Chromate conversion composition and method for coating aluminum using low concentrations of chromate, phosphate and fluoride ions |
| WO1981002749A1 (en) * | 1980-03-25 | 1981-10-01 | Eltzroth & Ass J M | Composition for inhibiting corrosion of metal surfaces |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2189816A (en) * | 1986-03-31 | 1987-11-04 | Toshiba Kk | Chromated non-ferrous metal mechanical part |
| GB2189816B (en) * | 1986-03-31 | 1990-11-28 | Toshiba Kk | Non-ferrous metal mechanical part |
| EP0467197A2 (en) * | 1990-07-14 | 1992-01-22 | Westfalia-Werke Knöbel GmbH & Co. | Method for fixed connection of metallic building components to a metallic support |
| EP0467197A3 (en) * | 1990-07-14 | 1992-04-15 | Westfalia-Werke Franz Knoebel & Soehne Kg | Method for fixed connection of metallic building components to a metallic support |
Also Published As
| Publication number | Publication date |
|---|---|
| GB2162865B (en) | 1988-07-13 |
| CA1249494A (en) | 1989-01-31 |
| JPS6148574A (en) | 1986-03-10 |
| GB8519539D0 (en) | 1985-09-11 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PCNP | Patent ceased through non-payment of renewal fee |
Effective date: 19930802 |