CN107353810A - A kind of composite base metal surfaces processing method - Google Patents

A kind of composite base metal surfaces processing method Download PDF

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CN107353810A
CN107353810A CN201710551045.1A CN201710551045A CN107353810A CN 107353810 A CN107353810 A CN 107353810A CN 201710551045 A CN201710551045 A CN 201710551045A CN 107353810 A CN107353810 A CN 107353810A
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weight
parts
base metal
metal surfaces
processing method
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CN107353810B (en
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马可足
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Ningbo Jishi metal new material Co.,Ltd.
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马可足
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
    • C09D175/04—Polyurethanes
    • C09D175/14—Polyurethanes having carbon-to-carbon unsaturated bonds
    • 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
    • C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F1/00—Etching metallic material by chemical means
    • C23F1/10—Etching compositions
    • C23F1/14—Aqueous compositions
    • C23F1/16—Acidic compositions

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  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
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Abstract

The present invention provides a kind of composite base metal surfaces processing method, it passes through polishing, acid treatment, alkali process and polymer treatment, wherein polymer treatment have selected the parts by weight of hydroxy-ethyl acrylate 100, the parts by weight of urethane acrylate 15 25, the parts by weight of epoxy acrylate 10 14, the parts by weight of acrylic acid 38, the parts by weight of dimethacrylate multicondensed ethylene glycol ester 3.5 6.5, the parts by weight of light trigger 0.2 1.2, the base metal surfaces processing method with excellent bonding strength or bonding strength is obtained, and the selection of polymer composition makes it be respectively provided with good bonding strength or bonding strength to a variety of different matrix resin composite materials or adhesive.

Description

A kind of composite base metal surfaces processing method
Technical field
The present invention relates to the field of Treatment of Metal Surface, and in particular to the Treatment of Metal Surface for composite substrate Method.
Background technology
With the fast development of composite, the composite of polymer body has high intensity, low-quality excellent spy Point, it is widely used in many fields, such as：Space flight, aviation, high ferro, plant equipment.The use of composite is not reducing material Space shuttle, aircarrier aircraft, the weight of high ferro can be significantly reduced while intensity, greatly improves its travel speed；Machine The overall weight of tool equipment also decreases, and is readily transported.Above-mentioned composite it is more and more faster with life pattern has been complied with Modern society's life.
While with above-mentioned composite advantage, it may have certain part to be modified.In present technical conditions Under, prepare that aircraft, high ferro etc. are still unrealistic by composite completely, it is essential during the use of metal material, but metal with The connection of composite also has very big improvements.Existing frequently-used uses bonding using metal connecting piece connection or part Agent bonds, but the mode effect used in the prior art has weak point.Using which kind of mode can improve composite with How the bonding strength of metal improves during metal is connected with composite and waits to change as one kind using the adhesion strength of adhesive The aspect entered.Meanwhile how to handle Treatment of Metal Surface can be adapted it to a variety of matrix resins (such as polyurethane, epoxy, Esters of acrylic acid) all there is excellent bonding strength or adhesion strength, it can be widely applied to plant equipment, indoor metal table Face, mechanical electronic equipment internal part etc., in the case of metal and all very thin coating, it can be used for tiny in electronic equipment Part.
The content of the invention
Goal of the invention：In view of the above-mentioned problems, being found by research, the processing of diversification is carried out to metal surface in advance, is made One layer of polymer treatment layer with excellent multicomponent adhesive force of firm attachment on metal surface, the layer assign metal surface with answering Condensation material connective stability and there is good connective stability with multilayer material.
In order to reach the technique effect of above-mentioned introduction, it is achieved through the following technical solutions：
Composite base metal surfaces processing method, comprises the following steps：
Step (1), polishing：It will be polished as composite with base metal surfaces, and remove the rusty stain on surface and organic dirt Thing；
Step (2), acid treatment：Acid solution is sprayed to the surface of the base metal after polishing, stands 30-200min；
Step (3), alkali process：The acid solution of base metal surfaces is wiped, smears sig water, makes metal surface that weak base be presented Property；
Step (4), polymer treatment：Coating composition to be polymerized after treatment, solidification, is produced；
Thickness after composition solidification wherein to be polymerized is about 50-200 μm.
Four steps of above-mentioned steps (1)-(4) are organic wholes, have each served as different effects, and mutual shadow Ring.
Step (1), polishing
In step (1) surface polishing belongs to a kind of conventional means, its to remove the rusty stain of metal surface (such as iron rust, Patina etc.), part organic dirt can also remove simultaneously；Metal is copper, iron, zinc or stainless steel in step (1), can be according to reality The needs of border service condition select specific metal species, substantially, in present inventive concept, can be corroded by customary acid Metal can select to use, and clearly limitation, from the needs of actual use, not have selected the most frequently used above-mentioned metal kind Class.
Step (2), acid treatment
Acid treatment serves two effects in step (2), first, further removing the organic matter dirt of metal surface, is To the supplement of previous step physics polishing, removed by physical-chemical both of which；Second, microcorrosion acts on, it is quiet in metal surface A period of time is put, metal surface is formed small hole, improves the interface contiguity of subsequent polymer.Acid solution in step (2) Occupation mode is needed to spray, and droplet is formed in metal surface, rather than using coating, formed by being coated on metal surface Liquid film, the uniform attachment to metal do not have the effect of increase interface contiguity.
For sour selection, the acid solution used in step (2) is the mixture of sulfuric acid, hydrochloric acid, nitric acid or above-mentioned acid solution, acid Species be difference according to metal species, such as iron, stainless steel, zinc can use sulfuric acid, hydrochloric acid and nitric acid, be aoxidized from being formed Layer angle, zinc should not use nitric acid；Copper preferably uses nitric acid or the mixture sour with other, and the acid of other independent species can not be right Copper is corroded.
The acid strength used in step (2) is 0.001-0.01mol/L.Unsuitable excessive, the excessive corrosivity of the concentration of acid By force, it is excessively serious to metal erosion, influence the using effect of metallic substrates；If concentration is too small, corrosion rate and effect are not It is good, it is impossible to meet the needs of industrialized production is to efficiency.
Step (3), alkali process
In step (3), base extraction is to neutralize the remaining acid in acid treatment, avoid it to the further of metal Corrosion, make final metal surface that alkalescent be presented, avoid the corrosiveness of subsequent polymer a small amount of acidic-group in handling.This hair Bright middle acid solution is equally also required to use dilute highly basic, and sig water selects the excellent sodium hydroxide solution for 0.01mol/L, it is only necessary to neutralization portion Divide diluted acid, if final alkalescence is stronger, there is certain decomposition to polymer treatment layer, also influence finally connects strong Degree；If using weak base, it is too low to neutralize efficiency, it is impossible to meet the needs of industrialized production is to efficiency.Metal watch after treatment The alkalescent in face is preferably pH=7.5-8.5.
Step (4), polymer treatment
Polymer treatment in step (4) makes a core procedure of the invention, and it is carried out by polymer to metal surface Anticipate, during the Treatment of Metal Surface connection of follow-up metal-polymer material become polymeric material-polymeric material The connection of material, bonding strength substantially increase.The composition to be polymerized can be：The parts by weight of hydroxy-ethyl acrylate 100, polyurethane third Olefin(e) acid ester 15-25 parts by weight, epoxy acrylate 10-14 parts by weight, acrylic acid 3-8 parts by weight, dimethacrylate contracting second more Diol ester 3.5-6.5 parts by weight, light trigger 0.2-1.2 parts by weight, the thickness after composition solidification to be polymerized is about 50-200 μ m。
A variety of acrylic polymers are employed in the composition, hydroxy-ethyl acrylate and acrylic acid contain hydroxyl and carboxyl, There is good adhesive attraction to metal base, ensure that the basic demand to metal；Because polyurethane, epoxy resin etc. are extensive For in the preparation process of composite, the selection of urethane acrylate and epoxy acrylate to be to improve the polymer Process layer and composite or the bonding strength of adhesive；Dimethacrylate multicondensed ethylene glycol ester improves as crosslinking agent The crosslink density of system, makes it have some strength.
Inventive polymers use photocuring, coating-solidification is realized the production of serialization, improve industrialized Efficiency.
In order to further improve polymer treatment effect, the polymer treatment in preferred steps (4) of the present invention is divided into two steps, Respectively lower crosslink density polymer treatment and high crosslink density polymer treatment.The polymer treatment is first entered in metal surface Row lower crosslink density polymer treatment, carry out first time solidification；High crosslink density polymer treatment is carried out again, is solidified.
Lower crosslink density polymerization crosslinking density is low, the effective adhesive force improved to metal base；And high density polymer There is good bonding strength or adhesive strength with higher intensity, and with the adhesion of follow-up composite or adhesive.Root Required according to its difference, separately design and used type of polymer similar in two kinds of compositions.
The composition for the polymer A that the lower crosslink density polymer treatment uses includes：The weight of hydroxy-ethyl acrylate 100 Part, urethane acrylate 15-25 parts by weight, acrylic acid 3-8 parts by weight, GDMA 0.5-2.5 weight Part, light trigger 0.2-1.2 parts by weight.
The composition for the polymer B that the high crosslink density polymer treatment uses includes：The weight of hydroxy-ethyl acrylate 100 Part, urethane acrylate 15-25 parts by weight, epoxy acrylate 10-14 parts by weight, acrylic acid 3-8 parts by weight, dimethyl propylene Olefin(e) acid glycol ester 3.5-6.5 parts by weight, light trigger 0.2-1.2 parts by weight.
The dosage of the GDMA as crosslinking agent is significantly improved in polymer B.The low cross-linking It is 1-2 that density, which handles forming layer with thickness ratio after high crosslink density processing forming layer solidification,：3-4.
The application method of metal after being handled in the present invention, its metallic substrates that can be used for after processing and composite Adhesive connects or the direct forming composite in metallic substrates after treatment of composite.
Beneficial technique effect
The present invention is a kind of composite base metal surfaces processing method, its by polishing, acid treatment, alkali process and The selection of polymer treatment, and the condition and two layers of method polymer treatment of acid treatment and alkali process are further selected, obtain Base metal surfaces processing method with excellent bonding strength or bonding strength, and the selection of polymer composition makes it to a variety of Different matrix resin composite materials or adhesive are respectively provided with good bonding strength or bonding strength.
Specific implementation method
In order that technical staff more intuitively knows the technical scheme in the present invention, with preferred embodiment and comparative example Mode carries out exemplary introduction to technical scheme, and the following examples do not form limiting the scope of the present invention, any Modification and adjustment, equivalent substitution and improvement for being made in the spirit and principles in the present invention etc. are all within the scope of the present invention.
The preparation of polymeric compositions：
Polymeric compositions 1：The parts by weight of hydroxy-ethyl acrylate 100, the parts by weight of urethane acrylate 20, epoxy acrylate 14 parts by weight, the parts by weight of acrylic acid 6, the parts by weight of dimethacrylate multicondensed ethylene glycol ester 4, the parts by weight of light trigger 1.
Polymeric compositions 2：The parts by weight of hydroxy-ethyl acrylate 100, the parts by weight of urethane acrylate 34, the weight of acrylic acid 6 Part, the parts by weight of dimethacrylate multicondensed ethylene glycol ester 4, the parts by weight of light trigger 1.
Polymeric compositions 3：The parts by weight of hydroxy-ethyl acrylate 100, the parts by weight of epoxy acrylate 34, the parts by weight of acrylic acid 6, The parts by weight of dimethacrylate multicondensed ethylene glycol ester 4, the parts by weight of light trigger 1.
Polymeric compositions 4：The parts by weight of hydroxy-ethyl acrylate 102, the parts by weight of urethane acrylate 22, epoxy acrylate 16 parts by weight, the parts by weight of dimethacrylate multicondensed ethylene glycol ester 4, the parts by weight of light trigger 1.
Polymer A：
The parts by weight of hydroxy-ethyl acrylate 100, the parts by weight of urethane acrylate 20, the parts by weight of acrylic acid 6, dimethyl allene The sour parts by weight of glycol ester 1.5, the parts by weight of light trigger 0.8.
Polymer B：
The parts by weight of hydroxy-ethyl acrylate 100, the parts by weight of urethane acrylate 20, the parts by weight of epoxy acrylate 12, third The parts by weight of olefin(e) acid 6, the parts by weight of GDMA 6, the parts by weight of light trigger 1.
Embodiment 1
A kind of composite base metal surfaces processing method, comprises the following steps：
Step (1), polishing：Composite base metal stainless steel (25mm*100mm) surface will be used as to polish, removed The rusty stain and organic dirt on surface；
Step (2), acid treatment：It is quiet to the surface sprinkling acid solution (0.005mol/L sulfuric acid) of the base metal after polishing Put 70min；
Step (3), alkali process：The acid solution of base metal surfaces is wiped, smears sig water (0.01mol/L hydroxide Sodium), make metal surface that alkalescent be presented；
Step (4), polymer treatment：Coating composition 1 to be polymerized after treatment, solidification, is produced；Wherein to be polymerized group Thickness after compound solidification is about 100 μm.
Embodiment 2-4
The polymer composition 1 in embodiment 1 is replaced with into polymer composition 2-4 respectively, remaining processing mode is the same as real Apply example 1.
Embodiment 5
Polymer treatment in step (4) in embodiment 1 is replaced with：Polymer treatment first carries out low cross-linking in metal surface Density polymers A processing, thickness is 35 μm after carrying out first time solidification；High crosslink density polymer B processing is carried out again, after solidification Thickness is 65 μm.
Embodiment 6
Polymer A in embodiment 5 and polymer B processing sequence are exchanged, i.e., the poly- of 65 μ m-thicks is first formed in metal surface Compound B layers, re-form the polymer A layer of 35 μ m-thicks.
Embodiment 7-8
The middle polymeric layer of embodiment 5 is replaced with to the polymer that 100 μ m-thicks are formed using polymer A or polymer B respectively Layer.
Embodiment 9
The alkali lye used in embodiment 1 replaces with 0.1M sodium hydroxide, and remaining technique is same as Example 1.
Embodiment 10
It is same as Example 1 without using polymer treatment, remaining technique.
Sample preparation and method of testing：
Epoxide-resin glue and polyurethane adhesive is respectively adopted in the present invention, and carrying out stretching to the metal that different disposal method obtains cuts Cut sample to be handled, refer to《GB7124-86 adhesive tensile shear strength method of testings (metal to metal)》Prepare stretching Sample, sample are tested after solidifying 12 hours at room temperature.
In prepared by sample, the stainless steel base after two panels processing, the bond area 25mm*25mm by way of singly overlapping, 500 μm of bonding agent thickness, tensile strength, draw speed 5mm/min are tested at room temperature using omnipotent mechanics tester.It is each to survey Three samples are tested under the conditions of examination, result is recorded after taking average.
● epoxide-resin glue：Araldite 2011, double-component cold curing pasty state, mixing ratio A:B=100:80；
● polyurethane resin adhesive：Araldite 2018, double-component cold curing polyurethane structural gluing agent, mixing ratio A:B =100:100.
Test result：
By experimental data it can be found that the present invention is entered by the selection and the selection of structure to component to metal base Row surface treatment has, and the surface is respectively provided with good adhesive strength to polyurethane and epoxy resin.Its to a certain degree on characterize Prepare the interlaminar action power after complex layered materials.Find simultaneously, in polymer treatment in polymer monomer selection, ensure that It AA Selection utilization microcorrosion and avoids shadow of the alkaline matter to polymer bonding to epoxy and the bonding strength of polyurethane Ring, improve the intensity of bonding.Meanwhile double-layer structure polymer treatment is a more excellent selection of technical scheme.

Claims (10)

  1. A kind of 1. composite base metal surfaces processing method, it is characterised in that：Comprise the following steps：
    Step（1）, polishing：It will be polished as composite with base metal surfaces, and remove the rusty stain and organic dirt on surface；
    Step（2）, acid treatment：Acid solution is sprayed to the surface of the base metal after polishing, stands 30-200min；
    Step（3）, alkali process：The acid solution of base metal surfaces is wiped, smears sig water, makes metal surface that alkalescent be presented；
    Step（4）, polymer treatment：Coating composition to be polymerized after treatment, solidification, is produced；
    Thickness after composition solidification wherein to be polymerized is about 50-200 μm.
  2. 2. composite according to claim 1 base metal surfaces processing method, it is characterised in that step（1）In Metal is copper, iron, zinc or stainless steel.
  3. 3. composite according to claim 1 base metal surfaces processing method, it is characterised in that step（2）In The acid strength used is 0.001-0.01mol/L.
  4. 4. the composite base metal surfaces processing method according to claim any one of 1-3, it is characterised in that step Suddenly（2）The middle acid solution used is the mixture of sulfuric acid, hydrochloric acid, nitric acid or above-mentioned acid solution.
  5. 5. composite according to claim 1 or 2 base metal surfaces processing method, it is characterised in that step（3） In sig water be 0.01mol/L sodium hydroxide solution.
  6. 6. composite according to claim 1 or 2 base metal surfaces processing method, it is characterised in that step（4） In polymer treatment be divided into two steps, respectively lower crosslink density polymer treatment and high crosslink density polymer treatment.
  7. 7. composite according to claim 6 base metal surfaces processing method, it is characterised in that the polymer Processing first carries out lower crosslink density polymer treatment in metal surface, carries out first time solidification；High crosslink density polymerization is carried out again Thing processing, solidification.
  8. 8. the composite base metal surfaces processing method according to claim 6 or 7, it is characterised in that described low The composition for the polymer A that crosslink density polymer treatment uses includes：The parts by weight of hydroxy-ethyl acrylate 100, polyurethane acroleic acid Ester 15-25 parts by weight, acrylic acid 3-8 parts by weight, GDMA 0.5-2.5 parts by weight, light trigger 0.2- 1.2 parts by weight.
  9. 9. the composite base metal surfaces processing method according to claim 6 or 7, it is characterised in that the height The composition for the polymer B that crosslink density polymer treatment uses includes：The parts by weight of hydroxy-ethyl acrylate 100, polyurethane acroleic acid Ester 15-25 parts by weight, epoxy acrylate 10-14 parts by weight, acrylic acid 3-8 parts by weight, GDMA 3.5-6.5 parts by weight, light trigger 0.2-1.2 parts by weight.
  10. 10. the composite base metal surfaces processing method according to claim 6 or 7, it is characterised in that described low It is 1-2 that crosslink density, which handles forming layer with thickness ratio after high crosslink density processing forming layer solidification,：3-4.
CN201710551045.1A 2017-07-07 2017-07-07 A kind of composite material base metal surfaces processing method Active CN107353810B (en)

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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1527747A (en) * 2000-09-19 2004-09-08 ϣ Process for treating adhesion promoted metal surfaces

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1527747A (en) * 2000-09-19 2004-09-08 ϣ Process for treating adhesion promoted metal surfaces

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