CN106987833B - Aluminum alloy surface silane-lanthanum salt composite membrane preparation method - Google Patents
Aluminum alloy surface silane-lanthanum salt composite membrane preparation method Download PDFInfo
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- CN106987833B CN106987833B CN201710131936.1A CN201710131936A CN106987833B CN 106987833 B CN106987833 B CN 106987833B CN 201710131936 A CN201710131936 A CN 201710131936A CN 106987833 B CN106987833 B CN 106987833B
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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
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/48—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 not containing phosphates, hexavalent chromium compounds, fluorides or complex fluorides, molybdates, tungstates, vanadates or oxalates
- C23C22/56—Treatment of aluminium or alloys based thereon
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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
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/73—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals characterised by the process
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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
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/78—Pretreatment of the material to be coated
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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
Abstract
The present invention relates to aluminum alloy surface silane-lanthanum salt composite membrane preparation methods; belong to technical field of metal material surface treatment; modification is doped to silane film using lanthanum salt; and it is dried in improved air dry oven; silane-lanthanum salt composite membrane is prepared for two-step method; one layer of double-[3-(triethoxy) silicon propyl]-tetrasulfide (BTESPT) film is first deposited in ethanol system; lanthanum salt conversion film is deposited in the aluminium surface through silanization again; the protective performance and self-healing ability for improving protective film, improve the service life of aluminium alloy.
Description
Technical field
The invention belongs to technical field of metal material surface treatment, at the surface before being mainly used for aluminium alloy extrusions coating
Reason, and in particular to aluminum alloy surface silane-lanthanum salt composite membrane preparation method.
Background technique
Aluminium alloy adds various alloying elements in the fabrication process, due to pursuing high mechanical performance and comprehensive performance,
Such as Zn, Mg, Cu, Si.The presence of these elements makes aluminium alloy internal chemical ingredient and nonuniform organization, so that aluminium alloy material
Material is in use environment (especially Cl-Under the conditions of existing) in easily cause micro-cell corrosion, influence the service life of material.Institute
It is increasingly valued by people with the protection of aluminium and its alloy.Chromating processing obtains in the surface treatment of aluminium alloy
It is widely applied, but since Cr VI is toxic, with the development of human society and the raising of scientific and technological level, the ring of people
Border protective awareness is more and more stronger, and it is important that the substitution studies of progress chromating technology have become one, anticorrosive metal field
Direction and urgent problem to be solved.
Metal surface rare earth conversion processing is mainly deposited by rare earth compound in base metal surface, simple process,
It is nontoxic, pollution-free, at low cost, have become the hot spot of Chrome-free alternate process technical research.Such as document " aluminum alloy surface lanthanum conversion
Membrane process optimization " (scientific and technological information, page 2013,15,61) describe one kind with LaCl3·7H2O is closed as main salt in aluminium and aluminium
Gold surface preparation contains the improvement technique of less crackle rare-earth conversion coatings, but the film quality of rare-earth conversion coatings is uneven, and works as film
Reaching certain thickness just becomes fluffy, easy to fall off, its Corrosion Protection is caused to decline.
Advantage of the green silyation technigue in terms of Treatment of Metal Surface is it is clear that caused more and more researchers'
Concern.But due to the thickness very little of silane film (only several hundred nanometers), and only play in corrosion protection the work of physical barrier
With there are holes and crack in film layer, once film layer is destroyed, parent metal starts to corrode rapidly, therefore use single silicon
Alkane film protects the effect of metal ideal not enough.Currently, the rare-earth conversion coatings technology base for aluminum alloy surface of greatest concern
Ce is all based on this3+It carries out.As document " preparation of aluminum tube surfaces BTESPT silane-RE composite membrane and corrosion proof is ground
Study carefully " (plating and environmental protection, 2009,29(5): page 30 ~ 34) use infusion process to prepare silane-RE composite membrane, by elder generation in aluminum pipe
Surface preparation one layer pair-[3-(triethoxy) silicon propyl]-tetrasulfide (abbreviation BTESPT, No. CAS is 40372-72-3)
Silan-based Thin Films, then on film deposition of rare-earth Cerium conversion film silane-RE composite membrane, technique conversion film directly obtained is made
There are more serious problem of Cracking, needs after post treatment or the methods of polymer is compound could inhibit crackle, and cerium salt
The market price is higher, therefore silane-RE composite membrane obtained industrializes higher cost in this way.
Protecting film obtained by above-mentioned document it is different degrees of that there are film layers is thin, protective performance, silane film self-healing ability are undesirable
And the problems such as at high cost.
It is usually to be carried out in air dry oven to the drying process of film in the preparation process of composite membrane in actual conditions,
And the mostly support holder structure in existing air dry oven, cured object will be needed to lie on pallet and solidified, object
Upper surface because with other isoelectric membranes, curing rate is not fast, and its lower surface because and pallet face contact curing rate it is slow, finally
Keep the solidification of object uneven, cause only to object be cured carry out on one side using, cause unnecessary waste, only will
It needs cured object to lie on pallet, by extraneous collision or the vibration from equipment itself, can all object be made to exist
Play inside equipment is unfavorable for the solidification of object, and part clamping device is clamped object using clip and solidified, but can break in this way
The structure on bad object surface layer, influences solidification effect.Therefore need to improve the structure in air dry oven, it can improve
The solidification effect of film avoids the destruction of membrane structure.
Summary of the invention
It is an object of the present invention to provide aluminum alloy surface silane-lanthanum salt composite membrane preparation methods, using lanthanum salt to silane film
It is doped modification, and is dried in improved air dry oven, silane-lanthanum salt composite membrane is prepared for two-step method, i.e.,
One layer of double-[3-(triethoxy) silicon propyl]-tetrasulfide (BTESPT) film is first deposited in ethanol system, then through silane
The aluminium surface of change deposits lanthanum salt conversion film, improves the protective performance and self-healing ability of protective film, improves the use of aluminium alloy
Service life.
To achieve the above object, the present invention the following technical schemes are provided:
Aluminum alloy surface silane-lanthanum salt composite membrane preparation method, including following preparation step:
Step 1: the configuration of solution of silane
Take double-[3-(triethoxy) silicon propyl]-tetrasulfide, dehydrated alcohol and deionization that volume ratio is 10:80:10
Water is configured to solution of silane, is 4.5 with the pH that pH adjusting agent adjusts solution of silane, continuously stirs 2h；
Step 2: the configuration of lanthanum salt solution
According to the La(NO that 5 ~ 20g is added in every liter of solution3)3·6H2The H of O and 8 ~ 15ml2O2Prepare lanthanum salt solution；
Step 3: silane-lanthanum salt composite membrane preparation
At room temperature, 6061 aluminium alloys pre-processed are dipped in the solution of silane of step 1 configuration, room temperature deposition
30min takes out with being dried with nitrogen；6061 aluminium alloys are immersed again in the lanthanum salt solution of step 2 configuration, is 30 ~ 60 DEG C in temperature
Under conditions of handle 20 ~ 50min, take out with being dried with nitrogen, be put into 100 DEG C of air dry oven 60 min of solidification, obtain aluminium close
Gold surface silane-lanthanum salt composite membrane.
Further, the pH adjusting agent is acetic acid or ammonium hydroxide.
Further, described be dried with nitrogen is carried out on nitrogen evaporator.
Further, the air dry oven includes drying box, and dry door, can draw and insert-type company inside the drying box
One group or more of clamp assemblies are connected to, the clamp assemblies include clamping bottom plate and grip part, and the clamping bottom plate is in
Rectangle clamps and offers through slot on the forward and backward side of bottom plate, and the upper plane horizontal array for clamping bottom plate offers rod slot, institute
It states through slot internal activity formula and is connected with the part that grips more than two, the part that grips includes clamping cross bar, clamps and erect
Bar and bottom plate, the top for clamping cross bar are fixed with clamping vertical bar, and clamping vertical bar passes through rod slot, clamps the two sides of vertical bar
Upper end be laid with upper mounted plate respectively, clamp and offer adjusting long hole on the two sides of vertical bar, the adjusting long hole be located at it is upper
The lower part of fixed plate adjusts in long hole and is longitudinally laid with the first pressure spring, and the first pressure spring other end is fixed on bottom plate.
Further, it is described can draw and insert-type be connected as being laid with fixing groove respectively in the inside left and right side walls of drying box, press from both sides
The bottom surface both side for holding bottom plate is respectively fixed with convex block, and being inserted into fixing groove by convex block is fixed on clamp assemblies in drying box
Portion.
Further, fixing groove top semicircular in shape, lower part are in rectangle, the convex block semicircular in shape.
Further, it is described it is movable be connected as offering more than four half slots on the above and below of through slot respectively,
Baffle is connected with by the second pressure spring between the adjacent half slot in above and below, second pressure spring at least there are two, it is described
Preset clearance between the baffle of above and below is less than the diameter of clamping cross bar, and the clamping cross bar is located in half slot.
Further, it is laid with handle on the outer end face of the clamping cross bar, the handle is located in drying box.
Compared with prior art, the beneficial effects of the present invention are:
It is substitution chromium processing technique 1. the present invention is the composite membrane that rare-earth conversion coatings and silyation technigue combine preparation
New method, overcoming chromate has severe toxicity and has the processing cost of carcinogenesis and chromate waste water and residue is sufficiently expensive to lack
Point overcomes and prepares protecting film with single method and have the shortcomings that crackle, protection effect are undesirable, improves aluminum alloy surface
Corrosion resistance has many advantages, such as that treatment process is simple, nontoxic, pollution-free, nontoxic to environment and human body；In preparation method
It is that main salt is lower as the cost of main salt compared to using cerium chloride using lanthanum nitrate, composite membrane corrosion resisting property obtained is more preferable, adopts simultaneously
It is that promotor overcomes using nitrite also more or less to generate pernicious gas in the parkerizing process of promotor with hydrogen peroxide
And sediment, influence the defects of being normally carried out of production；
2. the present invention realizes the solidification to 6061 aluminium alloys by improved air dry oven equipment, pass through air dry oven
In upper and lower fixing plate 6061 aluminium alloy longitudinal bracings are got up, accelerate its curing time, each face enabled aluminum alloy to is cured
It is more uniform；Bottom plate is attached by the first pressure spring, is adjusted between upper and lower fixing plate according to the length of aluminium alloy
Fore-and-aft distance enables aluminum alloy between upper and lower fixing plate, convenient and efficient using more rationalization, hommization；Adjacent folder
It holds two upper and lower fixing plates on vertical bar while carrying out clamping work, keep clamping operation stronger reliable, do not appear in solid
The phenomenon that aluminium alloy is fallen suddenly during change；Adjacent clamp assemblies are limited by baffle, and baffle passes through the second pressure spring
It is fixed, it is convenient that the lateral distance between adjacent clamp assemblies is adjusted as needed, make it to clamp different width
The aluminium alloy of degree；Fixing groove and convex block are all made of semicircular structure, and the cooperation of arc surface structure is compared to the quadrangles knot such as rectangle
Its frictional force of the cooperation of structure is small, more convenient to implement to fetch and deliver operation to clamp assemblies.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of aluminum alloy surface silane of the present invention-lanthanum salt compound membrane preparation method air dry oven.
Fig. 2 is the clamp assemblies of aluminum alloy surface silane of the present invention-lanthanum salt compound membrane preparation method air dry oven
Structural schematic diagram.
Numbering in the drawing are as follows: 1 is drying box, and 2 be dry door, and 3 be fixing groove, and 4 be baffle, and 5 be clamping cross bar, and 6 be folder
Vertical bar is held, 7 be bottom plate, and 8 be upper mounted plate, and 9 be clamping bottom plate, and 10 be half slot, and 11 be handle, and 12 be through slot, and 13 are
Rod slot, 14 is adjust long hole, and 15 be the first pressure spring, and 16 be convex block, and 17 be the second pressure spring.
Specific embodiment
Further statement is made to the present invention combined with specific embodiments below, but is not the limit to the scope of the present invention
Fixed, process involved in embodiment is then conventional method or step unless otherwise instructed, and medicine and reagent used is except special
It is commercially available outside illustrating.
Embodiment 1
Aluminum alloy surface silane-lanthanum salt composite membrane preparation method, comprising the following steps:
Step 1: the configuration of solution of silane
Take double-[3-(triethoxy) silicon propyl]-tetrasulfide, dehydrated alcohol and deionization that volume ratio is 10:80:10
Water is configured to solution of silane, is 4.5 with the pH that the acetic acid of 0.1mol/L adjusts solution of silane, continuously stirs 2 hours.
Step 2: the configuration of lanthanum salt solution
According to the La(NO that 10g is added in every liter of solution3)3·6H2The H of O and 15ml2O2Prepare lanthanum salt solution.
Step 3: silane-lanthanum salt composite membrane preparation
6061 aluminium alloys are cut into 30mm × 30mm × 3mm, 200#Water-proof abrasive paper polishing → 400#Water-proof abrasive paper polishing →
600#Water-proof abrasive paper polishing → alkaline degreasing → hot water wash → cold water washes → alkali cleaning → deionization washing → pickling goes out light → go from
Sub- washing → drying → chemical conversion treatment → washing → naturally dry.
At room temperature, 6061 aluminium alloys pre-processed are dipped in the solution of silane of step 1 configuration, room temperature deposition
30min takes out with being dried with nitrogen；6061 aluminium alloys are immersed again in the lanthanum salt solution of step 2 configuration, is 50 DEG C in temperature
Under the conditions of handle 30min, taking-up, which is put on nitrogen evaporator, to be dried up, and 100 DEG C of solidification 60min of air dry oven are put into, and is obtained aluminium and is closed
Gold surface silane-lanthanum salt composite membrane.
Crackle, even film layer, densification are not present using silane made from the method for the present invention-lanthanum salt composite film surface.
Film layer is still after the salt water that single silane film and silane-lanthanum salt composite membrane mass fraction are 3.5% is impregnated 14 days
Uniformly, it does not fall off, corrosion resistance is high.
Embodiment 2
The present embodiment is substantially the same manner as Example 1, the difference is that: it is adjusted in step 1 with the ammonium hydroxide of 0.1mol/L
The pH of solution of silane is 4.5；According to the La(NO that 5g is added in every liter of solution in step 23)3·6H2The H of O and 8ml2O2Prepare lanthanum
Salting liquid；The treatment temperature that 6061 aluminium alloys immerse in lanthanum salt solution in step 3 is 30 DEG C, and the processing time is 20min.
Embodiment 3
The present embodiment is substantially the same manner as Example 1, the difference is that: according to being added in every liter of solution in step 2
The La(NO of 15g3)3·6H2The H of O and 10ml2O2Prepare lanthanum salt solution；6061 aluminium alloys immerse in lanthanum salt solution in step 3
Treatment temperature is 60 DEG C, and the processing time is 40min.
Embodiment 4
The present embodiment is substantially the same manner as Example 1, the difference is that: according to being added in every liter of solution in step 2
The La(NO of 20g3)3·6H2The H of O and 12ml2O2Prepare lanthanum salt solution；6061 aluminium alloys immerse in lanthanum salt solution in step 3
Treatment temperature is 40 DEG C, and the processing time is 50min.
The aluminum alloy surface silane prepared to 1 ~ embodiment of embodiment 4-lanthanum salt composite membrane carries out corrosion resistance test, as a result
As shown in table 1.As it can be seen from table 1 the aluminum alloy surface silane-lanthanum composite membrane properties prepared using the method for the present invention
It is superior to the performance of single silane film.
Aluminum alloy surface silane-lanthanum salt the composite membrane and single silane film properties ratio of 11 ~ embodiment of embodiment 4 of table preparation
Compared with
| Title | Coating adhesion | Coating resistance k cm2 | CuSO4The drop time (s) | Corrosion current Acm-2 |
| Embodiment 1 | It is excellent | 162.4 | 96 | 7.309E-8 |
| Embodiment 2 | It is good | 82.8 | 86 | 6.543E-7 |
| Embodiment 3 | It is good | 129.4 | 72 | 4.257E-7 |
| Embodiment 4 | It is good | 131.5 | 85 | 4.863E-7 |
| Single silane film | Difference | 71.6 | 50 | 7.542E-5 |
Embodiment 5
As shown in FIG. 1 to FIG. 2, air dry oven used in aluminum alloy surface silane-compound membrane preparation method of lanthanum salt, packet
Include drying box 1, and dry door 2, inside the drying box 1 can draw and insert-type be connected with one group or more of clamp assemblies, it is described can
Draw and insert-type is connected as being laid with fixing groove 3 in the inside left and right side walls of drying box 1 respectively, the bottom surface both side difference of clamping bottom plate 9
It is fixed with convex block 16, being inserted into fixing groove 3 by convex block 16 is fixed on clamp assemblies inside drying box 1, and 3 top of fixing groove is in
Semicircle, lower part is in rectangle, and 16 semicircular in shape of convex block, clamp assemblies include clamping bottom plate 9 and gripping part, the folder
Bottom plate 9 is held in rectangle, clamps and offers through slot 12 on the forward and backward side of bottom plate 9, the upper plane horizontal array of clamping bottom plate 9 is opened
Equipped with rod slot 13, the 12 internal activity formula of through slot is connected with the part that grips more than two, described movable to be connected as
More than four half slots 10 are offered on the above and below of through slot 12 respectively, are passed through between the adjacent half slot 10 in above and below
Second pressure spring 17 is connected with baffle 4, second pressure spring 17 at least there are two, the part that grips includes clamping cross bar 5, folder
Vertical bar 6 and bottom plate 7 are held, the preset clearance between the baffle 4 of the above and below is less than the diameter of clamping cross bar 5, the folder
It holds cross bar 5 to be located in half slot 10, the top of clamping cross bar 5 is fixed with clamping vertical bar 6, and clamping vertical bar 6 passes through rod slot 13, folder
The upper end for holding the two sides of vertical bar 6 is laid with upper mounted plate 8 respectively, clamps and offers adjusting long hole 14 on the two sides of vertical bar 6,
The lower part for adjusting long hole 14 and being located at upper mounted plate 8, adjusts and is longitudinally laid with the first pressure spring 15 in long hole 14, first pressure
15 other end of spring is fixed on bottom plate 7, is clamped and is laid with handle 11 on the outer end face of cross bar 5, and the handle 11 is located at dry
In dry case 1.
In use, exerting a force downwards to the bottom plate 7 on clamping vertical bar 6, compress the first pressure spring 15,7 He of bottom plate
Fore-and-aft distance between upper mounted plate 8 pulls open, and 6061 aluminium alloys are placed between bottom plate 7 and upper mounted plate 8 and are consolidated
It is fixed, be again carried out above-mentioned steps on adjacent clamping vertical bar 6, make two adjacent clamping vertical bars 6 and meanwhile to 6061 aluminium alloys into
Row is fixed, and when the width of 6061 aluminium alloys is larger, handle 11 on the offensive, promotion grips part, 4 stress of baffle, by the
The compression of two pressure springs 17 makes the preset clearance between the baffle 4 of above and below become larger, and grips part across baffle 4 to another
In half slot 10, the no longer stress of baffle 4 is reset to original state, and baffle 4, which blocks, to be gripped part and no longer move, two phases
The adjacent width gripped between part becomes larger, and gripping width biggish 6061 aluminium alloy can be to 6061 aluminium after clamping
Alloy is dried.
The embodiment of the above, only presently preferred embodiments of the present invention, is only used to explain the present invention, not limit
The scope of the present invention processed to those of ordinary skill in the art certainly can be according to skill disclosed in this specification
Art content, makes other embodiments easily by way of replacing or changing, therefore all in the principle of the present invention and technique item
The changes and improvements etc. that part is done, should be included in scope of the present invention patent.
Claims (7)
1. aluminum alloy surface silane-lanthanum salt composite membrane preparation method, which comprises the following steps:
Step 1: the configuration of solution of silane
Double-[3-(triethoxy) silicon propyl]-tetrasulfide, dehydrated alcohol and the deionized water for taking volume ratio to be 10:80:10 is matched
It is set to solution of silane, is 4.5 with the pH that pH adjusting agent adjusts solution of silane, continuously stirs 2h；
Step 2: the configuration of lanthanum salt solution
According to the La(NO that 5 ~ 20g is added in every liter of solution3)3·6H2The H of O and 8 ~ 15ml2O2,Prepare lanthanum salt solution；
Step 3: silane-lanthanum salt composite membrane preparation
At room temperature, 6061 aluminium alloys pre-processed are dipped in the solution of silane of step 1 configuration, room temperature deposition 30min takes
Out with being dried with nitrogen；6061 aluminium alloys are immersed again in the lanthanum salt solution of step 2 configuration, under conditions of temperature is 30 ~ 60 DEG C
20 ~ 50min is handled, is taken out with being dried with nitrogen, is put into 100 DEG C of solidification 60min of air dry oven, obtains aluminum alloy surface silicon
Alkane-lanthanum salt composite membrane；
The air dry oven includes drying box, and dry door, inside the drying box can draw and insert-type be connected with one group or more
Clamp assemblies, the clamp assemblies include clamping bottom plate and grip part, and the clamping bottom plate is in rectangle, clamping bottom plate
Forward and backward side on offer through slot, the upper plane horizontal array for clamping bottom plate offers rod slot, the through slot internal activity
Formula is connected with the part that grips more than two, and the part that grips includes clamping cross bar, clamping vertical bar and bottom plate, folder
The top for holding cross bar is fixed with clamping vertical bar, and clamping vertical bar passes through rod slot, and the upper end for clamping the two sides of vertical bar is laid respectively
There is upper mounted plate, clamp and offer adjusting long hole on the two sides of vertical bar, the lower part for adjusting long hole and being located at upper mounted plate is adjusted
It is longitudinally laid with the first pressure spring in section long hole, the first pressure spring other end is fixed on bottom plate.
2. the preparation method of aluminum alloy surface silane-lanthanum salt composite membrane according to claim 1, which is characterized in that described
PH adjusting agent is acetic acid or ammonium hydroxide.
3. the preparation method of aluminum alloy surface silane-lanthanum salt composite membrane according to claim 1, which is characterized in that described
Be dried with nitrogen is carried out on nitrogen evaporator.
4. the preparation method of aluminum alloy surface silane-lanthanum salt composite membrane according to claim 1, which is characterized in that described
Can draw and insert-type be connected as being laid with fixing groove respectively in the inside left and right side walls of drying box, clamp bottom plate bottom surface both side difference
It is fixed with convex block, being inserted into fixing groove by convex block is fixed on clamp assemblies inside drying box.
5. the preparation method of aluminum alloy surface silane-lanthanum salt composite membrane according to claim 4, which is characterized in that described
Fixing groove top semicircular in shape, lower part are in rectangle, the convex block semicircular in shape.
6. the preparation method of aluminum alloy surface silane-lanthanum salt composite membrane according to claim 1, which is characterized in that described
It is movable to be connected as offering more than four half slots on the above and below of through slot respectively, between the adjacent half slot in above and below
Baffle is connected with by the second pressure spring, second pressure spring at least there are two, between reserved between the baffle of the above and below
Gap is less than the diameter of clamping cross bar, and the clamping cross bar is located in half slot.
7. the preparation method of aluminum alloy surface silane-lanthanum salt composite membrane according to claim 1, which is characterized in that described
It clamps and is laid with handle on the outer end face of cross bar, the handle is located in drying box.
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| CN1670247A (en) * | 2005-01-20 | 2005-09-21 | 上海交通大学 | Method for preparing sulfhydryl silane-rare earth nanometer compound membrane on single crystal silicon sheet surface |
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