CN106273216B - Metal-resin composite and its heat treatment method - Google Patents

Metal-resin composite and its heat treatment method Download PDF

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Publication number
CN106273216B
CN106273216B CN201610650240.5A CN201610650240A CN106273216B CN 106273216 B CN106273216 B CN 106273216B CN 201610650240 A CN201610650240 A CN 201610650240A CN 106273216 B CN106273216 B CN 106273216B
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Prior art keywords
metal
resin
temperature
resin composite
mold
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CN106273216A (en
Inventor
陈葳
薛奇
刘婧雯
王晓亮
周东山
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Nanjing University
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Nanjing University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C49/00—Blow-moulding, i.e. blowing a preform or parison to a desired shape within a mould; Apparatus therefor
    • B29C49/071—Preforms or parisons characterised by their configuration, e.g. geometry, dimensions or physical properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B11/00—Making preforms
    • B29B11/14—Making preforms characterised by structure or composition
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • 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
    • B29C45/1418—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 inserts being deformed or preformed, e.g. by the injection pressure
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C71/00—After-treatment of articles without altering their shape; Apparatus therefor
    • B29C71/02—Thermal after-treatment
    • 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
    • C25D11/12—Anodising more than once, e.g. in different baths
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • 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
    • B29C45/1418—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 inserts being deformed or preformed, e.g. by the injection pressure
    • B29C2045/14237—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 inserts being deformed or preformed, e.g. by the injection pressure the inserts being deformed or preformed outside the mould or mould cavity
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C71/00—After-treatment of articles without altering their shape; Apparatus therefor
    • B29C71/02—Thermal after-treatment
    • B29C2071/022—Annealing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2949/00—Indexing scheme relating to blow-moulding
    • B29C2949/07—Preforms or parisons characterised by their configuration
    • B29C2949/0715—Preforms or parisons characterised by their configuration the preform having one end closed

Abstract

The invention discloses a kind of metal-resin composite and its heat treatment methods, including being placed in mold to pretreatment of metal surface and mold temperature being arranged more than plexiglas transition temperature, below melting temperature, it will be combined with metal phase in the composition injection mold of resin, obtain metal-resin composite；Complex is stayed in a mold, mold maintains above-mentioned temperature；Make complex into line program cooling to mold to be down near glass transition temperature from original temperature with the rate for being less than 50 DEG C/min.This method make resin preferably keep metal it is nanometer level microporous in, the active force of reinforced resin and oxidation on metal surface layer, improve the binding force between resin and metal, the usual resins such as PPS, PBT, PA and metallic cohesion are not only made to improve 30% or so, it so that the binding force of amorphous resin such as PMMA, PS or PVC and metal is improved 500% or so, widen the application range of NMT products significantly.

Description

Metal-resin composite and its heat treatment method
Technical field
The present invention relates to a kind of metal-resin composite and its heat treatment methods, are widely used in NMT technical fields.
Background technology
Currently, in various e-machines, household article, medical machinery, vehicle structure member, vehicle loading articles for use, building It builds in material, external decoration component or other structures component, often refers to metal and the high intensity tree of mechanical processing method manufacture The integrated complex of fat assembly.
Prior art has disclosed the integrated molding technologies of metal and resin combination, use the thermoplasticity of high intensity mostly Resin such as PPS, PBT are molded, and the annealing steps carried out after injection molding are intended merely to eliminate the internal stress of resin, to itself and metal Adhesive strength influence it is limited.Meanwhile for the not high usual resins of crystallinity, since its tensile resistance difference leads to preparation The metal-resin composite impact of performance is bad, therefore is applied to range and causes apparent limitation.
It would therefore be highly desirable to solve the above problems.
Invention content
Goal of the invention：The first object of the present invention is to provide a kind of Metal tree for being conducive to enhance metal and resin-bonded power The heat treatment method of fat complex；It is compound that the second object of the present invention is to provide the metal-resin obtained by the heat treatment method Body.
Technical solution：The heat treatment method of metal-resin composite of the present invention, includes the following steps：
(1) metal surface is pre-processed, makes metal surface and its internal nanometer level microporous knot formed for injection molding Structure；
(2) metal after surface treatment is placed in mold, glass transition temperature of the setting mold temperature between resin Above, melting temperature is combined hereinafter, then injecting the composition of resin in mold with metal phase, and metal-resin is obtained after molding Complex；
(3) metal-resin composite is stayed in a mold, mold maintains the temperature in step (2)；
(4) cool down into line program to mold so that metal-resin composite is first to be less than the rate of 50 DEG C/min from original There is temperature to be down near glass transition temperature.
Wherein, in step (4), cool down into line program so that the metal-resin composite is first to be less than 20 to mold DEG C/rate of min is down to from original temperature near glass transition temperature.
Preferably, cool down into line program so that the metal-resin composite is first to be less than the speed of 10 DEG C/min to mold Rate is down to from original temperature near glass transition temperature.
More preferably, cool down into line program so that the metal-resin composite is first to be less than the speed of 1 DEG C/min to mold Rate is down to from original temperature near glass transition temperature.
Another scheme of present procedure cooling is to cool down into line program to mold so that metal-resin composite is first It is first down near glass transition temperature from original temperature with the rate for being less than 50 DEG C/min, then to be less than the speed of 60 DEG C/min Rate is down to room temperature near glass transition temperature.Can also be so that metal-resin composite is first to be less than 10 DEG C/min Rate be down near glass transition temperature from original temperature, then to be less than the rate of 20 DEG C/min from glass transition temperature Degree is nearby down to room temperature etc..
In step (3) of the present invention, mold maintains the temperature of step (2), and the duration can be from 0-48h；It can also will deposit There is the mold of metal-resin composite to be placed in baking oven, baking oven maintains the temperature of mold in step (2).
The present invention breaches limitation of the prior art to resin type, can expand range of resin to amorphous resin, example Such as PMMA, PS or PVC.
The resin of the present invention may be PPS, PBT, PA6, PA66 or PPA.
The metal of the present invention can be aluminium, magnesium, copper, stainless steel, titanium, iron, galvanized sheet or brass.
The invention further relates to metal-resin composites, and above-mentioned heat treatment method is used to obtain.
Advantageous effect：Compared with prior art, heat treatment method using the present invention can be such that resin preferably keeps in gold Belong to it is nanometer level microporous in, the active force of reinforced resin and oxidation on metal surface layer, hence it is evident that improve the knot between resin and metal With joint efforts；Studies have shown that the method for the present invention can make the binding force of the usual resins such as PPS, PBT, PA and metal improve 30% or so, more The binding force of amorphous resin such as PMMA, PS or PVC and metal can be made to improve 500% or so, widened NMT products significantly Application range；Meanwhile the method for the present invention simple possible, easily realization large-scale production, green safe environmental protection.
Specific implementation mode
Technical scheme of the present invention is described further below.
Embodiment 1
The present embodiment prepares the aluminum alloy resin complex handled by this heat treatment method based on PPS
The first step：Anodic oxidation
It is polished 1. the aluminium flake Jing Guo conventional surface pre-treatment is put into as anode in electrolytic cell, electrolyte is volume ratio For 1 to 3 perchloric acid and the mixed solution of ethyl alcohol, constant pressure 30V is electrolysed 3min.
2. using metal base as anode among the oxalic acid solution of 0.8M, voltage 40V, temperature 50 C handles 0.8h；
3. becoming 2%H in group2CrO4+ 10%H3PO4Chromium phosphorus mixed acid solution in impregnate 25min, temperature dimension when immersion It holds at 50 DEG C, is then rinsed well with deionized water；
4. continuing using metal base as anode among the oxalic acid solution of 0.8M, voltage 40V, 30 DEG C of temperature, handle 40min
Second step：Injection molding
Aluminum alloy sheet after drying is inserted into injecting molding die, 160 DEG C of mold temperature of setting, 315 DEG C of barrel temperature, Injection pressure 70Mpa, dwell time 1min are molded PPS；
Third walks：Heat treatment method
Metal-resin composite is retained in mold and is immediately placed in 160 DEG C of baking oven, above-mentioned temperature is maintained Then 18h drops to 85 DEG C with the cooling rate of 1 DEG C/min, demoulded after then dropping to room temperature with the cooling rate of 10 DEG C/min To the complex of strong bonded aluminium alloy and PPS together, it is 10 times to repeat experiment.
Comparative example 1
The present embodiment prepares the aluminum alloy resin complex handled without this heat treatment method based on PPS.
The first step, second step are same as Example 1, the difference is that third walks；
Third walks：Metal-resin composite is demoulded to room temperature natural cooling at once, obtains aluminium alloy and the complex of PPS, It is 10 times to repeat experiment, the results are shown in Table 1.
The sample binding force test data of table 1 embodiment 1 and comparative example 1
As it can be seen from table 1 the complex binding force for the PPS and aluminium alloy that through the invention prepared by heat treatment method can be with Reach 1763.82N, the intensity compared to the metal-resin composite without heat treatment method of the present invention improves 30%, pole The earth improves the combination dynamics of metal-resin.
Embodiment 2
The present embodiment prepares the aluminum alloy resin complex handled by this heat treatment method based on PMMA.
The first step：Anodic oxidation
It is polished 1. the aluminium flake Jing Guo conventional surface pre-treatment is put into as anode in electrolytic cell, electrolyte is volume ratio For 1 to 3 perchloric acid and the mixed solution of ethyl alcohol, constant pressure 30V is electrolysed 3min.
2. using metal base as anode among the oxalic acid solution of 0.8M, voltage 40V, temperature 50 C handles 0.8h；
3. becoming 2%H in group2CrO4+ 10%H3PO4Chromium phosphorus mixed acid solution in impregnate 25min, temperature dimension when immersion It holds at 50 DEG C, is then rinsed well with deionized water；
4. continuing using metal base as anode among the oxalic acid solution of 0.8M, voltage 40V, 30 DEG C of temperature, handle 40min
Second step：Injection molding
Aluminum alloy sheet after drying is inserted into injecting molding die, 140 DEG C of mold temperature of setting, 210 DEG C of barrel temperature, Injection pressure 70Mpa, dwell time 1min are molded PMMA；
Third walks：Heat treatment method
Metal-resin composite is retained in mold and is immediately placed in 140 DEG C of baking oven, above-mentioned temperature is maintained Then 18h drops to 90 DEG C with the cooling rate of 1 DEG C/min, demoulded after then dropping to room temperature with the cooling rate of 10 DEG C/min To the complex of strong bonded aluminium alloy and PMMA together, it is 10 times to repeat experiment.
Comparative example 2
The first step, second step are same as Example 1, the difference is that third walks；
Third walks：Metal-resin composite is demoulded to room temperature natural cooling at once, obtains aluminium alloy and the complex of PMMA, It is 10 times to repeat experiment, the results are shown in Table 2.
The sample binding force test data of table 2 embodiment 2 and comparative example 2
From table 2 it can be seen that the complex binding force for the PMMA and aluminium alloy that through the invention prepared by heat treatment method can To reach 520.11N, the intensity compared to the metal-resin composite without heat treatment method of the present invention improves more than 5 times, The significantly larger than prior art, and repeatability is very excellent, and defect rate is very low, has greatly widened the range of resin of NMT.
Embodiment 3
The present embodiment prepares the aluminum alloy resin complex handled by this heat treatment method based on PMMA.
The first step, second step are same as Example 2, the difference is that the heat treatment method of third step；
Third walks：Metal-resin composite is retained in mold and is immediately placed in 140 DEG C of baking oven, is maintained above-mentioned Temperature 18h, then drops to 90 DEG C with the cooling rate of 1 DEG C/min, then naturally rings to demould after room temperature to be firmly bonded to The complex of aluminium alloy and PMMA together repeats the average value for taking binding force after testing 10 times, the results are shown in Table 3.
Embodiment 4
The present embodiment prepares the aluminum alloy resin complex handled by this heat treatment method based on PPS.
The first step, second step are same as Example 1, the difference is that the heat treatment method of third step；
Metal-resin composite is retained in mold and is immediately placed in 160 DEG C of baking oven, above-mentioned temperature is maintained 18h, then drops to 85 DEG C with the cooling rate of 1 DEG C/min, then naturally ring to demoulding after room temperature obtain it is strong bonded together Aluminium alloy and PPS complex, take the average value of binding force after repeating experiment 10 times, the results are shown in Table 3.
3 embodiment 3-4 sample binding force test datas of table
Sample/binding force Embodiment 3 Embodiment 4
1 400.29N 1600.05N
As shown in Table 3, the program cooling step in heat treatment method of the present invention makes resin (either PPS or PMMA) energy Preferably keep metal it is nanometer level microporous in, the active force of reinforced resin and oxidation on metal surface layer, hence it is evident that improve resin Binding force between metal；Illustrate that the first step cooling of the program cooling step of the present invention is particularly critical simultaneously.
Embodiment 5
The present embodiment (8 groups of experiments) prepares the aluminium alloy resin compounded handled by this heat treatment method based on PMMA Body.
The first step, second step are same as Example 3, the difference is that the heat treatment method of third step；
Third walks：Metal-resin composite is retained in mold and is immediately placed in 140 DEG C of baking oven, is maintained above-mentioned Temperature 18h, then respectively with 60 DEG C/min, 50 DEG C/min, 40 DEG C/min, 30 DEG C/min, 20 DEG C/min, 10 DEG C/min, 5 DEG C/ Min, 1 DEG C/min cooling rate drop to 90 DEG C, then naturally ring to demoulding after room temperature and obtain strong bonded aluminium together to close The complex of gold and PMMA repeats the average value that binding force is taken after testing 10 times, in table 4 by data result record respectively.
8 groups of sample binding force test datas in 4 embodiment 5 of table
As shown in Table 4, with the reduction of rate of temperature fall for the first time, the binding force of metal and resin gradually increases, while for the first time Rate of temperature fall control effect within 50 DEG C/min is preferable.

Claims (10)

1. a kind of heat treatment method of metal-resin composite, it is characterised in that include the following steps：
(1) metal surface is pre-processed, makes metal surface and its internal nano micropore structure formed for injection molding；
(2) metal after surface treatment is placed in mold, setting mold temperature more than the glass transition temperature of resin, Melting temperature is combined hereinafter, then injecting the composition of resin in mold with metal phase, and metal-resin composite is obtained；
(3) metal-resin composite is stayed in a mold, mold maintains the temperature in step (2)；
(4) cool down into line program to mold so that metal-resin composite is first to be less than the rate of 50 DEG C/min from original temperature Degree is down near glass transition temperature.
2. the heat treatment method of metal-resin composite according to claim 1, it is characterised in that：In step (4), to mold Cool down into line program so that the metal-resin composite is down to glass with the rate for being less than 20 DEG C/min from original temperature first Change near transition temperature.
3. the heat treatment method of metal-resin composite according to claim 2, it is characterised in that：Mold is dropped into line program Temperature so that the metal-resin composite is down to glass transition temperature with the rate for being less than 10 DEG C/min from original temperature first Near.
4. the heat treatment method of metal-resin composite according to claim 3, it is characterised in that：Mold is dropped into line program Temperature so that the metal-resin composite is down to glass transition temperature with the rate for being less than 1 DEG C/min from original temperature first Near.
5. the heat treatment method of metal-resin composite according to claim 1, it is characterised in that：In step (4), to mold Cool down into line program so that metal-resin composite is down to vitrifying turn with the rate for being less than 50 DEG C/min from original temperature first Near temperature, room temperature is then down near glass transition temperature with the rate for being less than 60 DEG C/min.
6. the heat treatment method of metal-resin composite according to claim 1, it is characterised in that：The resin is amorphous state Resin.
7. the heat treatment method of metal-resin composite according to claim 6, it is characterised in that：The resin be PMMA, PS or PVC.
8. the heat treatment method of metal-resin composite according to claim 1, it is characterised in that：The resin be PPS, PBT, PA6, PA66 or PPA.
9. the heat treatment method of metal-resin composite according to claim 1, it is characterised in that：The metal be aluminium, magnesium, Copper, stainless steel, titanium, iron or galvanized sheet.
10. a kind of metal-resin composite, it is characterised in that it is obtained using any processing methods of claim 1-9.
CN201610650240.5A 2016-08-09 2016-08-09 Metal-resin composite and its heat treatment method Active CN106273216B (en)

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CN106917129B (en) * 2017-01-16 2019-01-04 歌尔股份有限公司 The engaging member and its processing method of stainless steel and plastics

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103290450A (en) * 2012-02-24 2013-09-11 比亚迪股份有限公司 Preparation method of aluminum alloy resin composite and aluminum alloy resin composite

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103290450A (en) * 2012-02-24 2013-09-11 比亚迪股份有限公司 Preparation method of aluminum alloy resin composite and aluminum alloy resin composite

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