WO2014024877A1 - アルミ樹脂接合体及びその製造方法 - Google Patents
アルミ樹脂接合体及びその製造方法 Download PDFInfo
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- WO2014024877A1 WO2014024877A1 PCT/JP2013/071239 JP2013071239W WO2014024877A1 WO 2014024877 A1 WO2014024877 A1 WO 2014024877A1 JP 2013071239 W JP2013071239 W JP 2013071239W WO 2014024877 A1 WO2014024877 A1 WO 2014024877A1
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- Prior art keywords
- aluminum
- resin
- oxygen
- film
- joined body
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- B29C45/00—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor
- B29C45/14—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor incorporating preformed parts or layers, e.g. injection moulding around inserts or for coating articles
- B29C45/14311—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor incorporating preformed parts or layers, e.g. injection moulding around inserts or for coating articles using means for bonding the coating to the articles
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- B29C45/14778—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor incorporating preformed parts or layers, e.g. injection moulding around inserts or for coating articles the article consisting of a material with particular properties, e.g. porous, brittle
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- B29C66/00—General aspects of processes or apparatus for joining preformed parts
- B29C66/40—General aspects of joining substantially flat articles, e.g. plates, sheets or web-like materials; Making flat seams in tubular or hollow articles; Joining single elements to substantially flat surfaces
- B29C66/47—Joining single elements to sheets, plates or other substantially flat surfaces
- B29C66/474—Joining single elements to sheets, plates or other substantially flat surfaces said single elements being substantially non-flat
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- B29C66/00—General aspects of processes or apparatus for joining preformed parts
- B29C66/70—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material
- B29C66/71—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the composition of the plastics material of the parts to be joined
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- B29K2705/00—Use of metals, their alloys or their compounds, for preformed parts, e.g. for inserts
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- B29L2031/00—Other particular articles
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- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/14—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers
- B32B37/24—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers with at least one layer not being coherent before laminating, e.g. made up from granular material sprinkled onto a substrate
- B32B2037/243—Coating
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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
- C23C2222/00—Aspects relating to chemical surface treatment of metallic material by reaction of the surface with a reactive medium
- C23C2222/20—Use of solutions containing silanes
Definitions
- the present invention relates to an aluminum resin joined body in which an aluminum base material made of aluminum or an aluminum alloy and a resin molded body made of a thermoplastic resin are integrally and firmly joined by injection molding or thermocompression bonding of a thermoplastic resin, and its It relates to a manufacturing method.
- the present inventors have already made an aluminum / resin injection integrated molded product in which an aluminum shaped body and a resin molded body are already locked together by a concave portion of an aluminum material and a fitting portion of a thermoplastic resin.
- Patent Document 1 an aluminum alloy member excellent in resin bondability characterized by having a convex portion made of silicon crystal
- Patent Document 2 an aluminum alloy member excellent in resin bondability characterized by having a convex portion made of silicon crystal
- a technique for integrating an aluminum alloy material and a thermoplastic resin composition obtained through a pretreatment immersed in one or more aqueous solutions selected from ammonia, hydrazine, and a water-soluble amine compound by injection molding (Patent Documents 3 and 4), an aqueous solution of triazine dithiols, or a solution using various organic solvents as a solvent is used as an electrodeposition solution, and after the electrochemical surface treatment of the metal, the metal after the surface treatment (Patent Document 5) that joins rubber and plastic has been proposed. Further, an adhesive is applied on a metal plate, or an organic film is formed by surface treatment, and then injection molding is performed.
- Technology for integrating metal and resin (Patent Document 6), or treating the surface of the metal with an acid or alkali and then treating with a silane coupling agent, followed by injection molding Techniques for joining the (Patent Document 7) have been proposed respectively.
- Patent Document 1 and Patent Document 2 the present inventors have so far proposed a physical bonding mainly based on the fitting of the anchor effect, and a special treatment in which halogen ions are contained in the treatment bath as the technique.
- a method by a simple etching process has been proposed. Although these methods have no problem in performance such as bonding strength and airtightness of the bonded portion, gas derived from halogen is generated during this etching process, and the surrounding metal parts and equipment are not corroded. There was another issue of having to take measures to prevent polluting the environment.
- the present inventors have no problem with surrounding equipment and environment when joining the aluminum base and the resin molded body made of thermoplastic resin, are easy operation, low cost, and long-term.
- an oxygen-containing film containing oxygen is formed on the surface of the aluminum base material, and a thermoplastic resin and an additive are formed on the oxygen-containing film.
- thermoplastic resin composition having an element having an unshared electron pair in a repeating unit and / or at the end, and a resin molded body formed of a thermoplastic resin composition containing Bonding by injection molding or thermocompression bonding between an aluminum base and a resin molded body by using one or both of an additive containing an element having an unshared electron pair (aluminum-resin bonding) )of
- an additive containing an element having an unshared electron pair (aluminum-resin bonding)
- an object of the present invention is to provide an aluminum resin joint that exhibits excellent bonding strength between aluminum and resin, and that does not cause a decrease in strength after a durability test and can maintain excellent bonding strength between aluminum and resin over a long period of time. To provide a body.
- the present invention relates to an aluminum substrate made of aluminum or an aluminum alloy, an oxygen-containing film containing oxygen formed on the surface of the aluminum substrate, and a thermoplastic resin bonded to the oxygen-containing film.
- a resin molded body formed of a thermoplastic resin composition containing an additive The thermoplastic resin composition contains either or both of a thermoplastic resin having an element having an unshared electron pair in a repeating unit and / or a terminal, and an additive containing an element having an unshared electron pair. This is an aluminum resin bonded body.
- the present invention also provides a film forming step for forming an oxygen-containing film on the surface of an aluminum substrate made of aluminum or an aluminum alloy, and an oxygen-containing film on the surface-treated aluminum substrate obtained in the film forming step.
- a resin molding step of forming a resin molded body by injection molding of a thermoplastic resin composition containing a thermoplastic resin and an additive, and the aluminum substrate and the resin molded body are joined via the oxygen-containing film Is a method of manufacturing an aluminum resin joined body for producing an aluminum resin joined body,
- the thermoplastic resin composition contains either or both of a thermoplastic resin having an element having an unshared electron pair in a repeating unit and / or a terminal, and an additive containing an element having an unshared electron pair. This is a method for producing an aluminum resin joined body.
- the present invention provides a resin molded body by a film forming step of forming an oxygen-containing film on the surface of an aluminum substrate made of aluminum or an aluminum alloy, and injection molding of a thermoplastic resin composition containing a thermoplastic resin and an additive.
- An aluminum resin joint that joins the resin molded body obtained in the resin molding step on the oxygen-containing film of the surface-treated aluminum base material obtained in the film formation step by thermocompression bonding
- the thermoplastic resin composition contains either or both of a thermoplastic resin having an element having an unshared electron pair in a repeating unit and / or a terminal, and an additive containing an element having an unshared electron pair. This is a method for producing an aluminum resin joined body.
- the material, shape, etc. of the aluminum base material used as the substrate is not particularly limited as long as it is made of aluminum or an aluminum alloy, and the use of the aluminum resin joined body formed using this or the use thereof Can be determined on the basis of various physical properties such as strength, corrosion resistance, and workability required.
- the oxygen-containing film formed on the surface of such an aluminum base material in the film forming step is not particularly limited as long as the adhesion to the aluminum base material is good, but preferably zinc ions Al (OH) 3 , AlO (OH), Al 2 O 3 , which is a film containing zinc element obtained by the zinc-containing film formation treatment using the aqueous alkali solution containing, or derived from the aluminum film formation treatment,
- Al (PO 4 ), Al 2 (HPO 4 ) 3 , and Al (H 2 PO 4 ) 3 an aluminum film forming treatment It is any film selected from a film containing hydrogen bonds between the derived aluminum hydroxyl group and silanol group, and a film containing Al-O-Si bonds derived from the aluminum film formation treatment, or a laser. Formed on the surface of aluminum substrate by processing Good in the range of film.
- zinc oxide (ZnO) and zinc oxide together with zinc element are formed on the surface of the aluminum base material. It suffices if a film containing iron (ZnFeO), zinc oxide aluminum (ZnAlO), or the like can be formed, so that either or both of the thermoplastic resin and the additive constituting the thermoplastic resin composition are non-existent.
- the zinc-containing film-forming process using the zinc ion containing aqueous alkali solution preferably, alkali hydroxide (MOH) and zinc ion (Zn 2+) in a weight ratio (MOH / Zn 2+) 1 or more to 100 or less
- a zinc ion-containing alkaline aqueous solution containing a ratio of 2 to 20, preferably 2 to 20 and more preferably 3 to 10 and contacting the zinc ion-containing alkaline aqueous solution with the surface of the aluminum substrate at room temperature.
- a zinc-containing film containing oxygen is preferably formed on the surface of the aluminum substrate.
- the alkali source in the zinc ion-containing alkaline aqueous solution preferably one or more selected from sodium hydroxide, potassium hydroxide, and lithium hydroxide is used, and this zinc ion-containing alkaline aqueous solution is used.
- the zinc ion source is preferably at least one selected from zinc oxide, zinc hydroxide, zinc peroxide, zinc chloride, zinc sulfate, and zinc nitrate.
- the alkali hydroxide concentration is 10 g / L or more and 1000 g / L or less, preferably 50 g / L or more and 300 g / L or less. It may be 1 g / L or more and 200 g / L or less, preferably 10 g / L or more and 100 g / L or less.
- the aluminum base material which consists of aluminum or an aluminum alloy is immersed in warm water at 50 degreeC or more for 60 seconds or more. Selected from the group consisting of a warm water immersion treatment, a water vapor treatment exposed to a water vapor atmosphere under pressure conditions of 0.1 MPa or more and 1 minute or more, phosphate ions, monohydrogen phosphate ions, and dihydrogen phosphate ions After immersing in a phosphoric acid aqueous solution containing any one or two or more phosphate ion species in the range of 0.1 to 100 g / L for 30 seconds to 30 minutes, hot air at 80 to 400 ° C.
- Al (OH) 3 , AlO (OH), Al 2 O is applied to the surface of this aluminum substrate.
- an aluminum film forming process performed in this film forming step an aluminum base material made of aluminum or an aluminum alloy is added to a solution containing 0.1 to 100 g / L of a silane coupling agent and / or colloidal silica.
- the aluminum substrate is treated with any one aluminum film forming treatment selected from silane coupling treatment and / or silica treatment, which is immersed in hot air of 80 to 400 ° C. for 30 seconds to 30 minutes and then dried for 30 seconds to 30 minutes.
- An oxygen-containing film containing hydrogen bonds between aluminum hydroxyl groups and silanol groups and / or an oxygen-containing film containing Al-O-Si bonds is formed on the surface of the material.
- These hot water immersion treatment, steam treatment, phosphoric acid treatment, anodizing treatment, silane coupling treatment, and silica treatment are carried out by performing only one of these treatments to form an oxygen-containing film on the surface of the aluminum substrate. It may be formed, and if necessary, any two kinds of treatments may be combined to form a necessary oxygen-containing film on the surface of the aluminum substrate.
- the aluminum base is melted in the vicinity of the surface of the aluminum base, preferably only in the vicinity of the surface. It suffices to heat and oxidize to above the temperature and deposit an aluminum oxide (Al 2 O 3 ) near the surface of the aluminum substrate to form an oxygen-containing film containing this aluminum oxide (Al 2 O 3 ). For example, it can be performed using a laser etching apparatus or the like.
- laser treatment requires a large area.
- the surface-treated aluminum base material obtained by forming an oxygen-containing film on the surface of an aluminum base material by the said film formation process it measures by EPMA in the surface layer from the outermost surface to the depth of 3 micrometers.
- the oxygen amount may be 0.1 wt% or more and 20 wt% or less, preferably 0.5 wt% or more and 15 wt% or less, more preferably 1 wt% or more and 10 wt% or less. If the amount of oxygen in the surface layer of this surface-treated aluminum base material is lower than 0.1% by weight, it may be difficult to achieve sufficient aluminum-resin bonding strength between the aluminum and the resin. However, it is difficult to increase the oxygen content exceeding 20% by weight.
- the oxygen content is 1% by weight to 70% by weight, preferably 10% by weight to 60% by weight, more preferably 25% by weight to 55% by weight. It is good. If the oxygen content in the surface layer of this surface-treated aluminum base material is lower than 1% by weight, there is a problem that the film becomes too thin to form a uniform film, and conversely, it exceeds 70% by weight. Increasing the amount of oxygen is accompanied by manufacturing difficulties.
- the surface-treated aluminum substrate thus obtained should have a hydrophilic surface oxygen-containing film, preferably a water droplet contact angle of 70 ° or less, more preferably 10 The angle may be from 50 ° to 50 °, more preferably from 5 ° to 40 °. When the contact angle of water droplets in the oxygen-containing film exceeds 70 °, the bonding with the resin molded body may be reduced due to the hydrophobicity of the surface.
- the oxygen-containing film formed in the film-forming step of the present invention preferably has an OH group on the outermost layer.
- the thermoplastic resin and / or additive in the thermoplastic resin composition has an element or substituent capable of hydrogen bonding or dehydration reaction with the OH group due to the presence of OH group in the outermost layer, this thermoplastic resin This is because the additive and the OH group of the oxygen-containing film form a hydrogen bond or an ester bond by a dehydration reaction.
- the resin molded body is integrated on the oxygen-containing film by injection molding of a thermoplastic resin composition.
- the resin molding process for forming the resin molded body by injection molding of the thermoplastic resin composition, and the obtained resin molded body with the surface-treated aluminum base Aluminum that is integrally bonded by thermocompression using means such as laser welding, vibration welding, ultrasonic welding, hot press welding, hot plate welding, non-contact hot plate welding, or high frequency welding on the oxygen-containing film of the material.
- An aluminum resin bonded body is manufactured by a resin bonding process.
- the thermoplastic resin composition used in the resin molding step is a thermoplastic resin composition containing a thermoplastic resin and an additive, and the thermoplastic resin composition is a repeating unit.
- a thermoplastic resin composition containing either one or both of a thermoplastic resin having an element having an unshared electron pair in the middle and / or terminal and an additive containing an element having an unshared electron pair is used.
- the element having an unshared electron pair contained in the thermoplastic resin and / or additive is preferably one or more selected from sulfur, oxygen, and nitrogen.
- the element which has these unshared electron pairs contained in the repeating unit of a thermoplastic resin it may be contained in the principal chain of a repeating unit, or may be contained in the side chain.
- thermoplastic resin having an element having an unshared electron pair in the repeating unit and / or terminal specifically, a resin containing a sulfur element such as polyphenylene sulfide (PPS) or a sulfone-based resin
- a resin containing a sulfur element such as polyphenylene sulfide (PPS) or a sulfone-based resin
- polyester resins such as polybutylene terephthalate (PBT), resins containing oxygen atoms such as liquid crystal polymers, polycarbonate resins, polyacetal resins, polyether resins, polyphenylene ether resins, such as polyamide (PA), ABS , Thermoplastic resins containing nitrogen atoms such as polyimide and polyetherimide.
- the “additive” constituting the thermoplastic resin composition used for molding the resin molded body in the resin molding step refers to a substance other than the thermoplastic resin constituting the thermoplastic resin composition
- an additive having an element having an unshared electron pair may be one that has an element having an unshared electron pair and is added to the thermoplastic resin composition.
- the production of the thermoplastic resin composition, the moldability and processability of the thermoplastic resin composition, the characteristics of the resin molded body obtained by molding the thermoplastic resin composition, and the like are considered.
- antioxidants for example, antioxidants, mold release agents, plasticizers, UV absorbers, heat stabilizers, antistatic agents, dyes, pigments, lubricants, silane coupling agents, fillers, elastomers, etc.
- UV absorbers for example, antioxidants, mold release agents, plasticizers, UV absorbers, heat stabilizers, antistatic agents, dyes, pigments, lubricants, silane coupling agents, fillers, elastomers, etc.
- antistatic agents for example, antioxidants, mold release agents, plasticizers, UV absorbers, heat stabilizers, antistatic agents, dyes, pigments, lubricants, silane coupling agents, fillers, elastomers, etc.
- silane coupling agents for example, silane coupling agents, fillers, elastomers, etc.
- the additive having an element having an unshared electron pair is preferably one in which the element having an unshared electron pair is oxygen and has a carbon-oxygen bond, and more preferably this carbon
- the additive having an oxygen bond is a carbonyl compound, and more specifically, it may be one or more compounds selected from the group consisting of carboxylic acids, esters, and amides.
- thermoplastic resin composition in which a resin molded body having a peak derived from (around 1730 cm -1 ) is molded.
- C O
- thermoplastic resin composition in which a resin molded product having a peak derived from (around 1730 cm -1 ) is molded.
- trade names RSF10719 and 6150T7 manufactured by Polyplastics Co., Ltd. Examples of such brand names include ADMER and TAFMER.
- an oxygen-containing film is formed on the entire surface of the aluminum base material to be a base, and resin molding is performed by injection molding only at a necessary portion of the obtained surface-treated aluminum base material or by thermocompression bonding.
- the body may be joined, or in consideration of cost, an oxygen-containing film is formed only on a part of the surface of the aluminum base material or at a necessary portion, and the obtained surface-treated aluminum base material is necessary.
- the resin molded body may be joined to the location by injection molding or thermocompression bonding.
- the oxygen-containing film is formed after masking portions other than the part that forms the oxygen-containing film, for example, with a masking tape or the like.
- a process for forming the mask may be performed, and then the masking tape or the like of the masked portion may be removed.
- the method for producing an aluminum resin joined body according to the present invention as necessary, prior to the film formation step for forming the oxygen-containing film, as a pretreatment of the surface of the aluminum substrate, degreasing treatment, etching treatment, desmut treatment, chemical polishing Any one or more treatments selected from a treatment and an electrolytic polishing treatment may be performed.
- the degreasing process performed as said pre-processing it can carry out using the normal degreasing bath which consists of sodium hydroxide, sodium carbonate, sodium phosphate, surfactant, etc.
- immersion temperature is usually 15
- the immersion time is 1 minute or more and 10 minutes or less, preferably 3 minutes or more and 6 minutes or less.
- an alkali aqueous solution such as sodium hydroxide or an acid aqueous solution such as a sulfuric acid-phosphoric acid mixed aqueous solution is usually used.
- concentration of 20 g / L or more and 200 g / L or less is used, Preferably it is 50 g / L or more and 150 g / L or less, Immersion temperature 30 to 70 degreeC, Preferably it is 40 to 60 degreeC.
- the immersion treatment may be performed under a treatment condition of not more than ° C. and a treatment time of 0.5 to 5 minutes, preferably 1 to 3 minutes.
- the sulfuric acid concentration is 10 g / L or more and 500 g / L or less, preferably 30 g / L or more and 300 g / L or less
- the phosphoric acid concentration is 10 g / L or more and 1200 g. / L or less, preferably 30 g / L or more and 500 g / L, immersion temperature 30 ° C. or more and 110 ° C. or less, preferably 55 ° C. or more and 75 ° C. or less, and immersion time 0.5 minutes or more and 15 minutes or less, preferably
- the immersion treatment is preferably performed under a treatment condition of 1 minute or more and 6 minutes or less.
- a desmut bath made of an aqueous nitric acid solution having a concentration of 1 to 30% is used, an immersion temperature of 15 ° C. to 55 ° C., preferably 25 ° C. to 40 ° C., and an immersion time of 1
- the immersion treatment may be performed under a treatment condition of not less than 10 minutes and not more than 10 minutes, preferably not less than 3 minutes and not more than 6 minutes.
- a conventionally well-known method is employable about the chemical polishing process and electropolishing process performed as said pre-processing.
- the surface-treated aluminum base material is exposed for 24 hours to obtain a stearic acid-treated aluminum base material having a monomolecular film of stearic acid on the oxygen-containing film, and carbonyl groups (
- Stearic acid has both a carboxyl group (COOH) which is a hydrophilic group and an alkyl group (C 17 H 35 ) which is a hydrophobic group, and has a property of forming a monomolecular film having a thickness of one molecule.
- COOH carboxyl group
- C 17 H 35 alkyl group
- Stearic acid-treated aluminum PPS joined body the oxygen-containing film of the aluminum base and the carboxyl group side of stearic acid are chemically bonded, and the alkyl group side comes into contact with the PPS molded product. It is thought that the chemical bond between the base material and the PPS compact was hindered, and the joint strength was lower than the joint strength of the aluminum PPS joint.
- the surface-treated aluminum base material before and after the stearic acid treatment was compared and examined by observing the surface, but no difference was found in the surface structure depending on the presence or absence of the stearic acid monomolecular film.
- the contact angle was measured, the contact angle was close to 120 °, and the droplet was almost spherical. This is a result of supporting that the alkyl group side of stearic acid is unevenly distributed on the outermost layer side of the aluminum base material.
- the aluminum resin joined body of the present invention is obtained by coating a surface of an aluminum substrate with an oxygen-containing film, and then a thermoplastic resin composition containing an element having an unshared electron pair in the thermoplastic resin and / or additive. Used by injection molding of this thermoplastic resin composition, or by thermocompression bonding of a resin molded body obtained by injection molding of this thermoplastic resin composition, on the oxygen-containing film on the aluminum substrate surface.
- the aluminum base and the resin molded body are not only firmly bonded via the oxygen-containing film, but also maintain excellent bonding strength between the aluminum and the resin over a long period of time. To get.
- an aluminum resin joined body of the present invention in the film forming process for forming the oxygen-containing film on the surface of the aluminum base material, there is no gas generation and the operation at room temperature is possible. It is possible to manufacture an aluminum resin bonded body that has no problem in facilities and environment, can be easily operated and low in cost, and can exhibit excellent bonding strength between aluminum and resin over a long period of time.
- FIG. 1 is an explanatory view for explaining an aluminum resin joined body produced in Example 1 of the present invention.
- FIG. 2 is an explanatory diagram for explaining a method of an evaluation test of the bonding strength between the aluminum and the resin carried out in Example 1 of the present invention.
- Example 1 (1) Preparation of surface-treated aluminum substrate An aluminum substrate having a size of 40 mm x 40 mm was cut out from a commercially available aluminum plate (A5052; plate thickness 2.0 mm). Further, a zinc ion-containing sodium aqueous solution having a sodium hydroxide concentration of 100 g / L and a zinc oxide concentration of 25 g / L (20 g / L as Zn + ) was prepared as a film-forming treatment agent.
- the above-mentioned aluminum base material is immersed in this zinc ion-containing sodium aqueous solution at room temperature for 3 minutes, then washed with water, and a surface-treated aluminum for testing on which an oxygen-containing film containing zinc element is formed on the surface.
- a substrate was prepared.
- the obtained surface-treated aluminum base material was subjected to mapping analysis using EPMA (manufactured by Shimadzu: EPMA1610) and measuring 512 steps in the vertical and horizontal directions at an irradiation diameter of 40 ⁇ m / step. .
- the measurement area is 20.48 mm ⁇ 20.48 mm
- the sampling time for one step is 20 ms
- the acceleration voltage is 15 kV
- the resolution in the depth direction of oxygen is 3 ⁇ m or less.
- the detected oxygen intensity was calculated as a weight percentage (wt%) from a calibration curve prepared in advance.
- the calibration curve used was calculated and prepared from two points: the oxygen intensity of the Al 2 O 3 standard sample (oxygen amount: 48 wt%) and the oxygen intensity of the high-purity Al foil. The results are shown in Table 1.
- a PPS molded body 3 having a size of 5 mm ⁇ 10 mm ⁇ 30 mm is molded, and the PPS molded body 3 is made of zinc of the surface-treated aluminum base material 2 with an area of 5 mm ⁇ 10 mm. It was made to join on a containing film (not shown), and the aluminum resin joined body 1 for a test was produced.
- the surface-treated aluminum base material 2 of the aluminum resin joined body 1 is fixed to the jig 4, and a load 5 is applied to the upper end of the PPS molded body 3 from above at a speed of 1 mm / min. Conducted a test to evaluate the shear strength of the joint part of the aluminum resin joined body by a method of destroying the joint part between the surface-treated aluminum base material 2 and the PPS molded body 3, and observed the fracture surface at that time.
- Example 2 As the aluminum substrate, the same aluminum plate (A5052; plate thickness 2.0 mm) as in Example 1 is used in Examples 2 to 7, and the aluminum plate (A1050; plate thickness 2.0 mm) is used in Example 8. Further, in Example 9, an aluminum plate material (ADC12; plate thickness 2.0 mm) was used, and the alkali ion concentration and zinc ion concentration shown in Table 1 using the zinc ion-containing alkaline aqueous solution having the liquid composition shown in Table 1. A test aluminum resin joined body was prepared in the same manner as in Example 1 except that the concentration was changed, and an IR analysis of the resin portion and a joint strength evaluation test were performed in the same manner as in Example 1. The results are shown in Table 1.
- Example 10 uses the same aluminum plate (A5052; plate thickness 2.0 mm) as in Example 1, and Example 11 uses the same aluminum plate (ADC12; plate thickness 2.0 mm) as in Example 9.
- ADC12 aluminum plate
- Example 10 uses the same aluminum plate (A5052; plate thickness 2.0 mm) as in Example 1
- Example 11 uses the same aluminum plate (ADC12; plate thickness 2.0 mm) as in Example 9.
- Use soak in a 30wt% nitric acid aqueous solution for 5 minutes at room temperature, then rinse thoroughly with ion-exchanged water, then soak in a 5wt% sodium hydroxide solution at 50 ° C for 1 minute, and then rinse with water. After pre-immersing for 3 minutes at room temperature, a pretreatment of washing with water was performed.
- the aluminum film was formed by hydrating by immersing in 91 ° C.
- Example 1 A test aluminum resin joined body was produced in the same manner as in Example 1, and IR analysis of the resin portion and a joint strength evaluation test were conducted in the same manner as in Example 1. The results are shown in Table 1.
- Example 12 Use the same aluminum plate (A5052; plate thickness 2.0mm) as in Example 1 as the aluminum substrate, degrease for 30 seconds with 2% Surf Cleaner 53S (manufactured by Nippon Paint) at 60 ° C, wash with water, and at 80 ° C. Dried.
- A5052 plate thickness 2.0mm
- Surf Cleaner 53S manufactured by Nippon Paint
- the aluminum substrate is immersed in the surface treatment solution for 10 seconds at room temperature and then dried at 80 ° C., and an aluminum compound Al (PO 4 ) and an aluminum hydroxyl group are formed on the surface of the aluminum substrate.
- a test aluminum resin joined body was prepared in the same manner as in Example 1 except that an oxygen-containing film containing a hydrogen bond between a hydrogen atom and a silanol group was formed.
- a strength evaluation test was conducted. The results are shown in Table 1.
- Example 13 Use the same aluminum plate (A5052; plate thickness 2.0mm) as in Example 1 as the aluminum substrate, degrease for 30 seconds with 2% Surf Cleaner 53S (manufactured by Nippon Paint) at 60 ° C, wash with water, and at 80 ° C. Dried.
- A5052 plate thickness 2.0mm
- Surf Cleaner 53S manufactured by Nippon Paint
- Colloidal silica ST-O (manufactured by Nissan Chemical) is used as SiO 2
- phosphoric acid with a purity of 85% (manufactured by Wako Pure Chemical Industries) is used as H 3 PO 4
- a silane coupling agent KBM manufactured by Shin-Etsu Chemical Co., Ltd.) -803
- a surface treatment liquid blended at the ratio shown in Table 1 was prepared, and an aluminum film was formed by immersing the aluminum base material in this surface treatment liquid at room temperature for 10 seconds and then drying at 120 ° C.
- Example 1 In the same manner as in Example 1 except that an aluminum compound Al (PO 4 ) and an oxygen-containing film containing an aluminum hydroxyl group and a silanol group and an Al—O—Si bond were formed on the surface of the aluminum substrate.
- An aluminum resin joined body for testing was prepared, and an IR analysis of the resin portion and a joint strength evaluation test were performed in the same manner as in Example 1. The results are shown in Table 1.
- Example 14 As an aluminum base material, the same aluminum plate material (A5052; plate thickness 2.0 mm) as in Example 1 is used in Example 14, and the same aluminum plate material (ADC12; plate thickness 2.0 mm) as in Example 9 is used in Example 15. Used, laser etching treatment (device name: Miyachi Technos / ML-7112A, laser light wavelength: 1064nm, spot diameter: 50-60um, oscillation method: Q switch pulse, frequency: 10kHz), pitch width 50 ⁇ m interval in the same direction Except that a thermal oxide film (oxygen-containing film) was formed on the surface layer, a test aluminum resin joined body was prepared in the same manner as in Example 1, and IR analysis of the resin portion was performed in the same manner as in Example 1. In addition, an evaluation test of bonding strength was performed. The results are shown in Table 1.
- Example 16 The same aluminum plate (A5052; plate thickness 2.0 mm) as in Example 1 was used as the aluminum substrate, immersed in a 30 wt% nitric acid aqueous solution at room temperature for 5 minutes, then thoroughly washed with ion-exchanged water, and then 5 wt% sodium hydroxide. The sample was immersed in the solution at 50 ° C. for 1 minute and then washed with water. Further, the sample was immersed in a 30 wt% nitric acid aqueous solution at room temperature for 3 minutes and then washed with water. Next, anodization is performed in a solution having a sulfuric acid concentration of 160 g / L at a melting temperature of 18 ° C.
- a test aluminum resin joined body was prepared in the same manner as in Example 1 except that an oxygen-containing film containing the aluminum compound Al 2 O 3 was formed on the surface of the aluminum base material. Then, the IR analysis of the resin part and the evaluation test of the bonding strength were performed.
- Example 17 Oxygen containing aluminum compound AlO (OH) on the surface of the aluminum substrate in the same manner as in Example 10 except that the conditions of the hydration treatment of Example 10 were changed to conditions for immersing in hot water at 80 ° C. for 5 minutes. A film was formed. Thereafter, a test aluminum resin joined body was prepared in the same manner as in Example 1, and IR analysis of the resin portion and a joint strength evaluation test were conducted in the same manner as in Example 1. The results are shown in Table 1.
- Example 18 Anodization was performed in a solution having a sulfuric acid concentration of 160 g / L at a melting temperature of 18 ° C. and a DC voltage of 20 V to a film thickness of 2 ⁇ m to form an oxygen-containing film containing the aluminum compound Al 2 O 3 on the surface of the aluminum substrate. . Thereafter, a test aluminum resin joined body was prepared in the same manner as in Example 1, and IR analysis of the resin portion and a joint strength evaluation test were conducted in the same manner as in Example 1. The results are shown in Table 1.
- Comparative Examples 1 and 2 A test aluminum resin joined body according to Comparative Examples 1 and 2 was prepared in the same manner as in Example 1 except that the thermoplastic resin having the material shown in Table 2 was used. Analysis and joint strength evaluation tests were conducted. The results are shown in Table 2.
- Example 3 A test aluminum resin joined body was prepared in the same manner as in Example 1 except that the thermoplastic resin having the material shown in Table 2 was used, and in the same manner as in Example 1. Then, the IR analysis of the resin part and the evaluation test of the bonding strength were performed. The results are shown in Table 2.
- Example 4 Use the same aluminum plate (A5052; plate thickness 2.0mm) as in Example 1 as the aluminum base, immerse it in a 30wt% nitric acid aqueous solution at room temperature for 5 minutes, then rinse thoroughly with ion-exchanged water and dry it.
- a test aluminum resin joined body was produced in the same manner as in Example 1 except that an aluminum base material having a natural oxide film was formed on the surface of the resin, and IR analysis and joining strength of the resin part were conducted in the same manner as in Example 1. An evaluation test was conducted. The results are shown in Table 2.
- thermoplastic resin As the thermoplastic resin, the material shown in Table 2 was used, and a test aluminum resin joint was made in the same manner as in Example 1 except that a thermal oxide film was formed on the surface layer by laser treatment in the same manner as in Example 14. A body was prepared, and the IR analysis of the resin part and the evaluation test of the bonding strength were performed in the same manner as in Example 1. The results are shown in Table 2.
- Example 7 The material shown in Table 2 is used as the thermoplastic resin, the hydration treatment of Example 10 is changed to a treatment of immersing in hot water at 70 ° C. for 5 minutes, and an aluminum film forming treatment is performed. Except that an oxygen-containing film containing an aluminum compound AlO (OH) was formed on the surface, a test aluminum resin joined body was prepared in the same manner as in Example 1 above, and IR analysis of the resin portion was performed in the same manner as in Example 1. In addition, an evaluation test of bonding strength was performed. The results are shown in Table 2.
- Example 8 The material shown in Table 2 was used as the thermoplastic resin, the hydration treatment of Example 10 was changed to a treatment of immersing in hot water at 60 ° C. for 10 minutes, and an aluminum film was formed. Except that an oxygen-containing film containing an aluminum compound AlO (OH) was formed on the surface, a test aluminum resin joined body was prepared in the same manner as in Example 1 above, and IR analysis of the resin portion was performed in the same manner as in Example 1. In addition, an evaluation test of bonding strength was performed. The results are shown in Table 2.
- the aluminum resin bonded body of the present invention has excellent bonding strength before and after the durability test, it is suitably used for manufacturing various parts such as parts for various sensors for automobiles, parts for home appliances and parts for industrial equipment. Is possible.
- SYMBOLS 1 Aluminum resin joined body, 2 ... Surface-treated aluminum base material, 3 ... PPS molded object (resin molded object), 4 ... Jig, 5 ... Load.
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Abstract
Description
前記熱可塑性樹脂組成物が、繰返し単位中及び/又は末端に非共有電子対を持つ元素を有する熱可塑性樹脂、及び非共有電子対を持つ元素を含む添加剤のいずれか一方又は双方を含有することを特徴とするアルミ樹脂接合体である。
前記熱可塑性樹脂組成物が、繰返し単位中及び/又は末端に非共有電子対を持つ元素を有する熱可塑性樹脂、及び非共有電子対を持つ元素を含む添加剤のいずれか一方又は双方を含有することを特徴とするアルミ樹脂接合体の製造方法である。
前記熱可塑性樹脂組成物が、繰返し単位中及び/又は末端に非共有電子対を持つ元素を有する熱可塑性樹脂、及び非共有電子対を持つ元素を含む添加剤のいずれか一方又は双方を含有することを特徴とするアルミ樹脂接合体の製造方法である。
なお、上記の温水浸漬処理、水蒸気処理、リン酸処理、陽極酸化処理、シランカップリング処理、及びシリカ処理(いわゆる、湿式処理)とレーザー処理を製造方法として考えた場合、レーザー処理では大面積の処理が難しく、被接合面への部分処理が可能な用途に向いている。一方、レーザー処理を除く湿式処理の場合、小面積の処理は被処理面以外へのマスキングが必要となり、被接合面以外を含めた全面処理が可能な用途に向いている。
また、酸素含有皮膜が陽極酸化皮膜である場合は、酸素量が1重量%以上70重量%以下、好ましくは10重量%以上60重量%以下、より好ましくは25重量%以上55重量%以下であるのがよい。この表面処理済アルミ基材の表層における酸素量が1重量%より低いと、皮膜が薄くなりすぎて均一な皮膜を形成することが出来ないという問題があり、反対に、70重量%よりを超えて酸素量を高くすることには製造上の困難が伴う。
なお、上記前処理として行う化学研磨処理や電解研磨処理については、従来公知の方法を採用することができる。
すなわち、アルミ基材の表面に酸素含有皮膜を有する複数の表面処理済アルミ基材を形成し、一部の表面処理済アルミ基材については、その表面にカルボニル基(C=O)を有するポリフェニレンスルフィド(PPS)の射出成形によりPPS成形体を接合してアルミPPS接合体とし、残りの表面処理済アルミ基材については、先ず、100℃に保持した電気炉中でステアリン酸を揮発させ、その中に表面処理済アルミ基材を24時間暴露し、酸素含有皮膜の上にステアリン酸の単分子膜を有するステアリン酸処理済アルミ基材とし、このステアリン処理済アルミ基材の表面にカルボニル基(C=O)を有するPPSの射出成形によりPPS成形体を接合してステアリン酸処理アルミPPS接合体とし、これらアルミPPS接合体とステアリン酸処理アルミPPS接合体との間における接合強度の違いを測定した。
結果は、ステアリン処理有アルミPPS接合体における接合強度は、アルミPPS接合体の接合強度に比べて明確に低下していた。
〔実施例1〕
(1) 表面処理済アルミ基材の作製
市販のアルミニウム板材(A5052; 板厚2.0mm)から40mm×40mmの大きさのアルミ基材を切り出した。また、皮膜形成処理剤として水酸化ナトリウム濃度100g/L及び酸化亜鉛濃度25g/L(Zn+として20g/L)の亜鉛イオン含有ナトリウム水溶液を調製した。次に、この亜鉛イオン含有ナトリウム水溶液中に上記のアルミ基材を室温下に3分間浸漬し、その後水洗し、表面に亜鉛元素を含有する酸素含有皮膜が形成された試験用の表面処理済アルミ基材を作製した。
得られた表面処理済アルミ基材について、エポキシ樹脂中に埋め込んで固めた後、表面処理済アルミ基材をエポキシ樹脂と共に切断し、断面をエメリー紙で湿式研磨し、酸化マグネシムの研磨剤を用いバフ研磨で鏡面仕上げした。その後、得られた湿式研磨後の断面をSEM(Carl Zeiss社製FE-SEM;50,000倍)で観察し、皮膜部分を厚さを測定した。
結果を表1に示す。
得られた表面処理済アルミ基材について、EPMA(島津製:EPMA1610)を用い、照射径が40μm/stepで縦横方向にそれぞれ512step測定するマッピング分析を実施した。ここで、測定面積は20.48mm×20.48mmであり、1stepのサンプリングタイムは20msであって、加速電圧は15kVであり、酸素の深さ方向の分解能は3μm以下である。次に、検出された酸素強度を事前に作成した検量線から重量百分率(wt%)として算出した。なお、検量線は、Al2O3標準試料(酸素量:48wt%)の酸素強度と高純度Al箔の酸素強度の2点から算出し作成したものを使用した。
結果を表1に示す。
得られた表面処理済アルミ基材の表面(酸素含有皮膜)について、水滴の接触角を測定した。この接触角の測定は、自動接触角計DM-701(協和界面科学株式会社製)を用いた液滴法によって行った。表面処理済アルミ基材の表面に約2μLの純水を滴下し、その際の接触角を測定した結果、水滴の接触角は20°であった。
結果を表1に示す。
得られた表面処理済アルミ基材について、その酸素含有皮膜の最表層に存在する物質(最表層存在物質)をGD-OES分析(グロー放電発光分光分析装置を用いた元素分析;A. Bengtson:J. Anal. At. Spectrom,18(2003),1066参照)により分析した結果、Bi元素が検出された。このGD-OESによる元素分析において、Bi元素はOH基に相当することが知られており、使用したAl合金及び各処理液にはBiが含まれていないため、Biの検出はOH基の存在を意味している。
結果を表1に示す。
熱可塑性樹脂としてPPS(ポリプラスチックス社製商品名:フォートロン、グレード名:RSF10719、C=O基:有り)を用い、上で得られた試験用表面処理済アルミ基材を射出成形機の金型内にセットし、金型温度150℃、樹脂温度320℃、射出速度100mm/s、保圧50MPa、保圧時間3秒の射出成形条件でPPSの射出成形を行い、図1に示すように、5mm×10mm×30mmの大きさのPPS成形体3を成形すると共に、このPPS成形体3を5mm×10mmの面積で表面処理済アルミ基材2の亜鉛含有皮膜(図示せず)上に接合させ、試験用のアルミ樹脂接合体1を作製した。
このようにして作製された試験用アルミ樹脂接合体1について、IR分析装置(Agilent Technologies 660FastImage-IR)を使用し、顕微ATR法により樹脂成形体部分のIR分析を実施し、カルボニル基(C=O)由来のピーク(1730cm-1付近)の有無を確認した。結果は、表1に示す通り、カルボニル基(C=O)由来のピークが検出された。
このようにして作製された試験用アルミ樹脂接合体について、アルミ樹脂接合体を温度85℃及び湿度85%の環境下に1000時間放置してアルミ樹脂接合体の耐食性を評価するアルミ樹脂接合体の耐久試験を行い、この耐久試験の前後のアルミ樹脂接合体について、下記の方法でそのアルミ-樹脂間の接合強度の評価試験を行った。
結果を表1に示す。
作製された試験用アルミ樹脂接合体について、表面硬度としてJIS Z2244のビッカース硬さ試験方法に準じてビッカース硬さ(Hv)を測定すると共に、JIS Z2248の押曲げ法に準じて皮膜欠陥の有無を調べた。
結果を表1に示す。
アルミ基材として、実施例2~7では実施例1と同じアルミニウム板材(A5052;板厚2.0mm)を使用し、また、実施例8ではアルミニウム板材(A1050;板厚2.0mm)を使用し、更に、実施例9ではアルミニウム板材(ADC12;板厚2.0mm)を使用し、亜鉛イオン含有アルカリ水溶液として表1に示す液組成のものを使用して水酸化アルカリ濃度及び亜鉛イオン濃度を表1に示す濃度にした以外は、実施例1と同様にして試験用のアルミ樹脂接合体を作製し、実施例1と同様にして樹脂部分のIR分析及び接合強度の評価試験を行った。
結果を表1に示す。
アルミ基材として、実施例10では実施例1と同じアルミニウム板材(A5052;板厚2.0mm)を使用し、また、実施例11では実施例9と同じアルミニウム板材(ADC12;板厚2.0mm)を使用し、30wt%硝酸水溶液に常温で5分間浸漬した後にイオン交換水で十分に水洗し、次いで5wt%水酸化ナトリウム溶液に50℃で1分間浸漬した後に水洗し、更に、30wt%硝酸水溶液に常温で3分間浸漬した後に水洗する前処理を施した。次に、91℃の熱水で5分間浸漬させる水和処理をすることによりアルミニウム皮膜形成処理を施し、アルミ基材の表面にアルミニウム化合物AlO(OH)を含む酸素含有皮膜を形成した以外は、実施例1と同様にして試験用のアルミ樹脂接合体を作製し、実施例1と同様にして樹脂部分のIR分析及び接合強度の評価試験を行った。
結果を表1に示す。
アルミ基材として実施例1と同じアルミニウム板材(A5052;板厚2.0mm)を使用し、60℃の2%サーフクリーナー53S(日本ペイント製)で30秒脱脂処理した後、水洗し、80℃で乾燥した。SiO2としてコロイダルシリカST-O(日産化学製)を用い、また、H3PO4として純度85%のリン酸(和光純薬製)を用い、表1に示す割合で配合した表面処理液を作製し、この表面処理液中にアルミ基材を室温下で10秒浸漬し、次いで80℃で乾燥するアルミニウム皮膜形成処理を行い、アルミ基材の表面にアルミニウム化合物Al(PO4)及びアルミ水酸基とシラノール基との水素結合を含む酸素含有皮膜を形成した以外は、実施例1と同様にして試験用のアルミ樹脂接合体を作製し、実施例1と同様にして樹脂部分のIR分析及び接合強度の評価試験を行った。
結果を表1に示す。
アルミ基材として実施例1と同じアルミニウム板材(A5052;板厚2.0mm)を使用し、60℃の2%サーフクリーナー53S(日本ペイント製)で30秒脱脂処理した後、水洗し、80℃で乾燥した。SiO2としてコロイダルシリカST-O(日産化学製)を用い、また、H3PO4として純度85%のリン酸(和光純薬製)を用い、更に、シランカップリング剤(信越化学工業製KBM-803)を用い、表1に示す割合で配合した表面処理液を作製し、この表面処理液中にアルミ基材を室温下で10秒浸漬し、次いで120℃で乾燥するアルミニウム皮膜形成処理を行い、アルミ基材の表面にアルミニウム化合物Al(PO4)及びアルミ水酸基とシラノール基との水素結合及びAl-O-Si結合を含む酸素含有皮膜を形成した以外は、実施例1と同様にして試験用のアルミ樹脂接合体を作製し、実施例1と同様にして樹脂部分のIR分析及び接合強度の評価試験を行った。
結果を表1に示す。
アルミ基材として、実施例14では実施例1と同じアルミニウム板材(A5052;板厚2.0mm)を使用し、また、実施例15では実施例9と同じアルミニウム板材(ADC12;板厚2.0mm)を使用し、レーザーエッチング処理(装置名:ミヤチテクノス/ML-7112A、レーザー光波長:1064nm、スポット径:50-60um、発振方式:Qスイッチパルス、周波数:10kHz)により、同一方向にピッチ幅50μm間隔で照射し、表層に熱酸化皮膜(酸素含有皮膜)を形成した以外は、実施例1と同様にして試験用のアルミ樹脂接合体を作製し、実施例1と同様にして樹脂部分のIR分析及び接合強度の評価試験を行った。
結果を表1に示す。
アルミ基材として実施例1と同じアルミニウム板材(A5052;板厚2.0mm)を使用し、30wt%硝酸水溶液に常温で5分間浸漬した後にイオン交換水で十分に水洗し、次いで5wt%水酸化ナトリウム溶液に50℃で1分間浸漬した後に水洗し、更に、30wt%硝酸水溶液に常温で3分間浸漬した後に水洗する前処理を施した。次に、硫酸濃度160g/Lの溶液中で溶温18℃,直流電圧20Vで皮膜厚さが10μmになるよう陽極酸化した後、水洗し、120℃の熱風で5分間乾燥させるアルミニウム皮膜形成処理を行い、アルミ基材の表面にアルミニウム化合物Al2O3を含む酸素含有皮膜を形成した以外は、実施例1と同様にして試験用のアルミ樹脂接合体を作製し、実施例1と同様にして樹脂部分のIR分析及び接合強度の評価試験を行った。
実施例10の水和処理の条件を80℃の熱水で5分間浸漬させる条件に変更した以外は実施例10と同様にして、アルミ基材の表面にアルミニウム化合物AlO(OH)を含む酸素含有皮膜を形成した。その後、実施例1と同様にして試験用のアルミ樹脂接合体を作製し、実施例1と同様にして樹脂部分のIR分析及び接合強度の評価試験を行った。
結果を表1に示す。
硫酸濃度160g/Lの溶液中で溶温18℃,直流電圧20Vで皮膜厚さが2μmになるよう陽極酸化し、アルミ基材の表面にアルミニウム化合物Al2O3を含む酸素含有皮膜を形成した。その後、実施例1と同様にして試験用のアルミ樹脂接合体を作製し、実施例1と同様にして樹脂部分のIR分析及び接合強度の評価試験を行った。
結果を表1に示す。
熱可塑性樹脂として表2に示す材質のものを使用した以外は、上記実施例1と同様にして、比較例1~2に係る試験用のアルミ樹脂接合体を作製し、また、樹脂部分のIR分析及び接合強度の評価試験を行った。
結果を表2に示す。
熱可塑性樹脂として表2に示す材質のものを使用した以外は、上記実施例10と同様にして、実施例1と同様にして試験用のアルミ樹脂接合体を作製し、実施例1と同様にして樹脂部分のIR分析及び接合強度の評価試験を行った。
結果を表2に示す。
アルミ基材として実施例1と同じアルミニウム板材(A5052;板厚2.0mm)を使用し、30wt%硝酸水溶液に常温で5分間浸漬した後にイオン交換水で十分に水洗し、乾燥させ、アルミ基材の表面に自然酸化皮膜を有するアルミ基材を形成した以外は、実施例1と同様にして試験用のアルミ樹脂接合体を作製し、実施例1と同様にして樹脂部分のIR分析及び接合強度の評価試験を行った。
結果を表2に示す。
熱可塑性樹脂として表2に示す材質のものを使用し、上記実施例14と同様にしてレーザー処理により表層に熱酸化皮膜を形成した以外は、実施例1と同様にして試験用のアルミ樹脂接合体を作製し、実施例1と同様にして樹脂部分のIR分析及び接合強度の評価試験を行った。
結果を表2に示す。
熱可塑性樹脂として表2に示す材質のものを使用し、表面に亜鉛元素を含有する酸素含有皮膜を形成した後、150℃で1時間の熱処理をした以外は、上記実施例1と同様にして試験用のアルミ樹脂接合体を作製し、実施例1と同様にして樹脂部分のIR分析及び接合強度の評価試験を行った。
結果を表2に示す。
熱可塑性樹脂として表2に示す材質のものを使用し、上記実施例10の水和処理を70℃の熱水で5分間浸漬させる処理に変更してアルミニウム皮膜形成処理を施し、アルミ基材の表面にアルミニウム化合物AlO(OH)を含む酸素含有皮膜を形成した以外は、上記実施例1と同様にして試験用のアルミ樹脂接合体を作製し、実施例1と同様にして樹脂部分のIR分析及び接合強度の評価試験を行った。
結果を表2に示す。
熱可塑性樹脂として表2に示す材質のものを使用し、上記実施例10の水和処理を60℃の熱水で10分間浸漬させる処理に変更してアルミニウム皮膜形成処理を施し、アルミ基材の表面にアルミニウム化合物AlO(OH)を含む酸素含有皮膜を形成した以外は、上記実施例1と同様にして試験用のアルミ樹脂接合体を作製し、実施例1と同様にして樹脂部分のIR分析及び接合強度の評価試験を行った。
結果を表2に示す。
Claims (29)
- アルミニウム又はアルミニウム合金からなるアルミ基材と、このアルミ基材の表面に形成された酸素を含有する酸素含有皮膜と、この酸素含有皮膜の上に接合され、熱可塑性樹脂及び添加剤を含有する熱可塑性樹脂組成物で形成された樹脂成形体とを有し、
前記熱可塑性樹脂組成物が、繰返し単位中及び/又は末端に非共有電子対を持つ元素を有する熱可塑性樹脂、及び非共有電子対を持つ元素を含む添加剤のいずれか一方又は双方を含有することを特徴とするアルミ樹脂接合体。 - 前記アルミ基材の表面に樹脂成形体が接合される前の表面に形成された酸素含有皮膜は、EPMAで測定された酸素量が0.1重量%以上20重量%以下の範囲内であることを特徴とする請求項1に記載のアルミ樹脂接合体。
- 前記酸素含有皮膜が、亜鉛イオン含有アルカリ水溶液を用いた亜鉛含有皮膜形成処理で得られた亜鉛元素を含有する皮膜であることを特徴とする請求項1又は2に記載のアルミ樹脂接合体。
- 前記酸素含有皮膜が、アルミニウム皮膜形成処理に由来するAl(OH)3、AlO(OH)、Al2O3、Al(PO4)、Al2(HPO4)3、及びAl(H2PO4)3からなる群から選ばれたいずれか1種又は2種以上のアルミニウム化合物を含む皮膜、アルミニウム皮膜形成処理に由来するアルミ水酸基とシラノール基との水素結合を含む皮膜、及び、アルミニウム皮膜形成処理に由来するAl-O-Siの結合を含む皮膜から選ばれたいずれか1種又は2種以上のアルミニウム化合物を含有する皮膜であることを特徴とする請求項1又は2に記載のアルミ樹脂接合体。
- 前記酸素含有皮膜が、レーザー処理によりアルミ基材の表面に形成された皮膜であることを特徴とする請求項1又は2に記載のアルミ樹脂接合体。
- 前記アルミ基材の表面に樹脂成形体が接合される前の表面に形成された酸素含有皮膜が陽極酸化皮膜であり、EPMAで測定された酸素量が1重量%以上70重量%以下の範囲内であることを特徴とする請求項1に記載のアルミ樹脂接合体。
- 前記酸素含有皮膜が、Al2O3のアルミニウム化合物を含む皮膜であることを特徴とする請求項6に記載のアルミ樹脂接合体。
- 前記酸素含有皮膜は、その表面の接触角が70°以下であることを特徴とする請求項1~7のいずれかに記載のアルミ樹脂接合体。
- 前記酸素含有皮膜は、その最表層にOH基を有することを特徴とする請求項1~8に記載のアルミ樹脂接合体。
- 酸素含有皮膜の上に樹脂成形体を接合する接合方法が、射出成形又は熱圧着による方法であることを特徴とする請求項1~9のいずれかに記載のアルミ樹脂接合体。
- 熱可塑性樹脂組成物を構成する熱可塑性樹脂中及び/又は添加剤中に含まれる非共有電子対を持つ元素が、硫黄、酸素、及び窒素からなる群から選ばれたいずれか1種又は2種以上の元素であることを特徴とする請求項1~10のいずれかに記載のアルミ樹脂接合体。
- 熱可塑性樹脂組成物を構成して非共有電子対を持つ元素を有する添加剤が炭素-酸素結合を有することを特徴とする請求項1~10のいずれかに記載のアルミ樹脂接合体。
- 炭素-酸素結合を有する添加剤がカルボニル化合物であることを特徴とする請求項12に記載のアルミ樹脂接合体。
- カルボニル化合物がカルボン酸類、エステル類、及び酸アミド類からなる群から選ばれたいずれか1種又は2種以上の化合物であることを特徴とする請求項13に記載のアルミ樹脂接合体。
- 熱可塑性樹脂組成物を構成して繰返し単位中及び/又は末端に非共有電子対を持つ元素を有する熱可塑性樹脂が、ポリフェニレンスルフィド系樹脂、ポリエステル系樹脂、ポリカーボネート系樹脂、ポリアセタール系樹脂、ポリエーテル系樹脂、ポリフェニレンエーテル系樹脂、ポリイミド系樹脂、ポリエーテルイミド系樹脂、液晶ポリマー、サルフォン系樹脂、ポリフェニレンオキサイド系樹脂、ポリアミド系樹脂、及びポリプロピレン系樹脂からなる群から選ばれたいずれか1種又は2種以上の樹脂であることを特徴とする請求項1~14のいずれかに記載のアルミ樹脂接合体。
- 樹脂成形体がカルボニル基(C=O)を有することを特徴とする請求項1~15のいずれかに記載のアルミ樹脂接合体。
- アルミニウム又はアルミニウム合金からなるアルミ基材の表面に酸素含有皮膜を形成する皮膜形成工程と、
この皮膜形成工程で得られた表面処理済アルミ基材の酸素含有皮膜の上に、熱可塑性樹脂及び添加剤を含有する熱可塑性樹脂組成物の射出成形により樹脂成形体を形成する樹脂成形工程とを有し、
前記酸素含有皮膜を介してアルミ基材と樹脂成形体とが接合されたアルミ樹脂接合体を製造するアルミ樹脂接合体の製造方法であり、
前記熱可塑性樹脂組成物が、繰返し単位中及び/又は末端に非共有電子対を持つ元素を有する熱可塑性樹脂、及び非共有電子対を持つ元素を含む添加剤のいずれか一方又は双方を含有することを特徴とするアルミ樹脂接合体の製造方法。 - アルミニウム又はアルミニウム合金からなるアルミ基材の表面に酸素含有皮膜を形成する皮膜形成工程と、
熱可塑性樹脂及び添加剤を含有する熱可塑性樹脂組成物の射出成形により樹脂成形体を形成する樹脂成形工程と、
前記皮膜形成工程で得られた表面処理済アルミ基材の酸素含有皮膜の上に、前記樹脂成形工程で得られた樹脂成形体を熱圧着により接合するアルミ樹脂接合工程とを有し、
前記酸素含有皮膜を介してアルミ基材と樹脂成形体とが接合されたアルミ樹脂接合体を製造するアルミ樹脂接合体の製造方法であり、
前記熱可塑性樹脂組成物が、繰返し単位中及び/又は末端に非共有電子対を持つ元素を有する熱可塑性樹脂、及び非共有電子対を持つ元素を含む添加剤のいずれか一方又は双方を含有することを特徴とするアルミ樹脂接合体の製造方法。 - 皮膜形成工程では、水酸化アルカリ(MOH)と亜鉛イオン(Zn+2)とを重量比(MOH/Zn+2)1~100の割合で含む亜鉛イオン含有アルカリ水溶液中にアルミ基材を浸漬する亜鉛含有皮膜形成処理により、このアルミ基材の表面に亜鉛元素を含有する酸素含有皮膜を形成することを特徴とする請求項17又は18に記載のアルミ樹脂接合体の製造方法。
- 亜鉛イオン含有アルカリ水溶液中のアルカリ源が、水酸化ナトリウム、水酸化カリウム、及び水酸化リチウムからなる群から選ばれたいずれか1種又は2種以上の水酸化アルカリであることを特徴とする請求項19に記載のアルミ樹脂接合体の製造方法。
- 亜鉛イオン含有アルカリ水溶液中の亜鉛イオン源が、酸化亜鉛、水酸化亜鉛、過酸化亜鉛、塩化亜鉛、硫酸亜鉛、及び硝酸亜鉛からなる群から選ばれたいずれか1種又は2種以上の亜鉛塩であることを特徴とする請求項19又は20に記載のアルミ樹脂接合体の製造方法。
- 皮膜形成工程では、アルミニウム又はアルミニウム合金からなるアルミ基材を、50℃以上の温水に60秒以上浸漬する温水浸漬処理、0.1MPa以上及び1分間以上の加圧条件下の水蒸気雰囲気中に晒す水蒸気処理、リン酸イオン、リン酸一水素イオン、及びリン酸二水素イオンからなる群から選ばれたいずれか1種又は2種以上のリン酸イオン種を0.1~100g/Lの範囲で含有するリン酸系水溶液中に30秒~30分間浸漬した後に80~400℃の熱風で30秒~30分間乾燥させるリン酸処理、又は陽極酸化処理から選ばれたいずれか1種のアルミニウム皮膜形成処理で処理し、このアルミ基材の表面にAl(OH)3、AlO(OH)、Al2O3、Al(PO4)、Al2(HPO4)3、Al(H2PO4)3、及びAlOSiO2から選ばれたいずれか1種又は2種以上のアルミニウム化合物を含有する酸素含有皮膜を形成することを特徴とする請求項17又は18に記載のアルミ樹脂接合体の製造方法。
- 皮膜形成工程では、アルミニウム又はアルミニウム合金からなるアルミ基材を、0.1~100g/Lのシランカップリング剤及び/又はコロイダルシリカを含有する溶液中に30秒~30分間浸漬した後に80~400℃の熱風で30秒~30分間乾燥させるシランカップリング処理及び/又はシリカ処理から選ばれたいずれか1種のアルミニウム皮膜形成処理で処理し、このアルミ基材の表面にアルミ水酸基とシラノール基との水素結合を含む酸素含有皮膜及び/又はAl-O-Siの結合を含む酸素含有皮膜を形成することを特徴とする請求項17又は18に記載のアルミ樹脂接合体の製造方法。
- 皮膜形成工程では、アルミニウム又はアルミニウム合金からなるアルミ基材の表面付近を加熱するレーザー処理により酸素含有皮膜を形成することを特徴とする請求項17又は18に記載のアルミ樹脂接合体。
- 熱可塑性樹脂組成物を構成する熱可塑性樹脂中又は添加剤中に含まれる非共有電子対を持つ元素が、硫黄、酸素、窒素、及び炭素からなる群から選ばれたいずれか1種又は2種以上の元素であることを特徴とする請求項17~24のいずれかに記載のアルミ樹脂接合体の製造方法。
- 熱可塑性樹脂組成物を構成して非共有電子対を持つ元素を有する添加剤が炭素-酸素結合を有することを特徴とする請求項25に記載のアルミ樹脂接合体の製造方法。
- 炭素-酸素結合を有する添加剤がカルボニル化合物であることを特徴とする請求項26に記載のアルミ樹脂接合体。
- カルボニル化合物がカルボン酸類、エステル類、及び酸アミド類からなる群から選ばれたいずれか1種又は2種以上の化合物であることを特徴とする請求項27に記載のアルミ樹脂接合体の製造方法。
- 熱可塑性樹脂組成物を構成して繰返し単位中及び/又は末端に非共有電子対を持つ元素を有する熱可塑性樹脂が、ポリフェニレンスルフィド系樹脂、ポリエステル系樹脂、ポリカーボネート系樹脂、ポリアセタール系樹脂、ポリエーテル系樹脂、ポリフェニレンエーテル系樹脂、ポリイミド系樹脂、ポリエーテルイミド系樹脂、液晶ポリマー、サルフォン系樹脂、ポリフェニレンオキサイド系樹脂、ポリアミド系樹脂、及びポリプロピレン系樹脂からなる群から選ばれたいずれか1種又は2種以上の樹脂であることを特徴とする請求項17~28のいずれかに記載のアルミ樹脂接合体の製造方法。
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