CN104451824A - Method and application of peeling titanium surface coating by adopting nanotube treatment method - Google Patents
Method and application of peeling titanium surface coating by adopting nanotube treatment method Download PDFInfo
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Abstract
The invention discloses a method and an application of peeling a coating on the surface of a pure titanium matrix or the surface of a titanium alloy matrix from the matrix. The method comprises the following steps: cleaning; preparing an electrolyte; oxidizing; pressurizing; drying and the like, so as to solve the technical problem that the coating on the surface of the pure titanium matrix or the surface of the titanium alloy matrix is hard to peel. According to the method disclosed by the invention, the inner structure of the coating is not damaged, and the realest information inside the coating can be retained; the maximum use of the method is preparation of a coating profile scanning electron microscope sample for observing the shape of the coating profile, so that the realest profile structure characteristics of the coating are retained. The method can be further used for measuring the thickness of the coating. The method can be further used in other applications for removing, transferring the coating on the surface of the pure titanium matrix or the surface of the titanium alloy matrix and the like.
Description
Technical field
The invention belongs to titanium-based surface coating stripping and coating detection technique field, relate to a kind of electrochemical process for treating that multiple coating is peeled off from pure titanium or titanium alloy substrate, the method can be used for preparation coating profile scanning electron microscopic sample.
Background technology
Titanium or titanium alloy has the plurality of advantages such as specific tenacity is high, good corrosion resistance, good biocompatibility, become one of metallic substance that 21 century attracts most attention, be widely used in aerospace, sports equipment, the fields such as medicine equipment, have the good reputation such as " space metal ", " aerial metal " and " close biological metal ".But, titanium or titanium alloy usually needs to carry out surface modification or coating process makes it that have improvement or new mechanics, biology or chemical property, to meet the requirement of special applications, the document that sees reference [Materials Science and Engineering R 47 (2004) 49-121].The character of titanium or titanium alloy matrix surface coating has important impact to its use properties, and the thickness of coating and coating section microstructure are the conventional sense indexs of coating, to evaluating coating process and instructing the improvement of technique significant.
The preparation method of titanium-based surface coating section exemplar mainly contains resin embedding polishing method and focused ion beam patterning method.The step of resin embedding polishing method coats epoxy resin or PMMA resin in titanium base surface of test piece, after it solidifies completely, (as sample dimensions is comparatively large, available metal cutting machine cuts out the segment needing observation), be parallel to the direction sand papering of section, until section exposes.This method is the resinous protective coating layer utilizing solidification, by the method for mechanical grinding, coating section is exposed.The shortcoming of this method is that solidification process epoxy resin has certain contraction unavoidably; cause between epoxy resin and coating and produce the sightless space of naked eyes; can not play the effect of supercoat in the process of polishing well, when coat-thickness is less, coating is easy to be damaged.In addition, mechanical grinding can damage coating section microstructure originally, and the coating section microstructure in fact observed is different.
Focused ion beam (FIB) technology is the method for the most effective accurately location sample preparation now, utilizes the focused ion beam of high energy to carry out bombarding and cutting, the transverse section of coating is exposed, then carries out scanning electron microscope or transmission electron microscope observation.Focused ion beam equipment is expensive, and sample preparation expense is also very expensive, and time cost and equipment cost are all very high.
Why difficult the preparation of titanium-based surface coating section sample is, and mainly due to the existence of metal matrix, if the coating on the stripping titanium or titanium alloy surface that can can't harm, even if only obtain a fritter, the preparation of coating section will become simple.But often defining good combination between coating and matrix, this is the prerequisite that coating plays a role, and the coating of nondestructively peeling titanium-based surface is not easy very much.
Therefore develop a kind of method peeling off titanium-based surface coating and there is important Practical significance, provide new method by for the sample preparation of coating section, also for the detection of titanium-based surface coat-thickness and section microtexture provides new means.
Summary of the invention
For solving above technical problem, the object of this invention is to provide the method for coating on a kind of effective stripping Titanium base, and be used for preparing the scanning electron microscope example of coating section.
For achieving the above object, the method that the present invention adopts, is characterized in that, comprise the following steps:
(1) the pure titanium or titanium alloy test specimen of intending stripper surface coating are used acetone, dehydrated alcohol and deionized water ultrasonic cleaning, dry for standby successively;
(2) NH is taken
4f 5.2 grams, is dissolved in 40 ml deionized waters, then mixes with 360 ml glycerine or ethylene glycol, and magnetic agitation makes solution mix, obtained electrolytic solution; Under room temperature, the titanium test specimen crossed by cleaning-drying carries out anodic oxidation treatment in organic fluoride-containing electrolytic solution;
(3) to intend the titanium test specimen of stripper surface coating for anode, with titanium plate or titanium foil for negative electrode, titanium test specimen is immersed below liquid level of electrolyte, titanium test specimen and positive source wire is connected with the titanium material that shape is suitable, titanium test specimen can expose titanium metal face by the coating that sand paper grinds off contact position, makes it good contact.
(4) voltage-drop loading mode is gradient pressurization, slowly boosts with speed 2 ~ 5 V/min, when reaching 50 ~ 80 V, keeps this voltage until total oxidization time reaches 1.5 ~ 2.5 h.Oxidization time is too short, and coating can not be peeled off completely, and oxidization time is long, and coating can fall in electrolytic solution, cannot collect.
(5) after nanotube process terminates, take off test specimen gently, directly test specimen can not be rinsed with wash bottle, easily coating punching is taken off, should test specimen be soaked for a moment in the beaker filling deionized water, make the glycerine solution remaining in sample surfaces diffuse in deionized water, repeat one twice, then sample is dried.
Bake out temperature 50-60 DEG C, time 0.5-1h in described step (1).
Bake out temperature 50-60 DEG C, time 1-2h in described step (5).
Being applied as in the present invention prepares coating profile scanning electron microscopic sample, concrete grammar is for using the square aluminium block of fritter, conductive resin is stained with in certain one side, heating makes adhesive tape viscosity better in an oven, be stained with by the coating that sample surfaces has been peeled off by conductive resin, make the scanning electron microscope example of coating section, for observing the appearance structure feature of coat-thickness and coating section.
Heating temperature 60 DEG C in described baking oven, time 15-25min.
The square ratio juris of release coating provided by the invention is by nanotube process, the Nano tube array of titanium dioxide of 1-2 micrometer length is formed between Titanium base and coating, coating arches upward by this layer of nano-tube array, destroys original bonding force between Titanium base and coating interface simultaneously.And bonding force is very weak between coating and the nanotube layer newly formed.So just achieve the successful stripping of coating.Due in the forming process of nano-tube array, under current field condition, just oxonium ion and fluorion diffusion admittance that coating is served as, coating self substantially can not produce change.Therefore, the coating section sample of preparation remains the original structure of coating and topographical information completely really, and the coating section sample standby with focused ion beam legal system with existing resin embedding polishing method is compared, and has significant advantage.In addition, owing to being electrochemical treatment, the coating being soaked in all regions of the test specimen in electrolytic solution all can realize stripping effect, and the multiple spot being specially adapted to the top coat of the titanium part of geometric configuration complexity detects.The method can also be used for other application such as the removal of titanium or titanium alloy substrate top coat and transfer.
All features disclosed in this specification sheets, or the step in disclosed all methods or process, except mutually exclusive feature and/or step, all can combine by any way.
Arbitrary feature disclosed in this specification sheets (comprising any accessory claim, summary), unless specifically stated otherwise, all can be replaced by other equivalences or the alternative features with similar object.That is, unless specifically stated otherwise, each feature is an example in a series of equivalence or similar characteristics.
Accompanying drawing explanation
The scanning electron microscopic picture of the coating section that the pure titanium sample of accompanying drawing 1 sample that constant voltage 180V anodic oxidation treatment obtains in 1M sulfuric acid electrolyte adopts nanotube facture to prepare
Accompanying drawing 2 adopts MPCVD method to prepare diamond coatings at pure titanium plate surface, the scanning electron microscopic picture of the coating section adopting nanotube facture to prepare
The scanning electron microscopic picture of the coating section that the accompanying drawing 3 TC4 titanium alloy sample sample that constant voltage 150V anodic oxidation treatment obtains in 1M sulfuric acid electrolyte adopts nanotube facture to prepare
Embodiment
Below in conjunction with the specific examples that contriver provides, do invented processing method and further elaborate, specific embodiment is as follows:
Embodiment 1
Prepared by sample coatings: the pure titanium sheet of TA1 being of a size of 10 × 10 × 1 mm uses 400,600 successively, 800 order SiC sand papering polishings, and then with acetone, dehydrated alcohol, deionized water distinguishes ultrasonic cleaning 5 min; Constant voltage mode anodic oxidation in 1 M sulfuric acid electrolyte, whole voltage is 180V, after whole voltage, keep 1min.XRD detects and shows that the coating of this sample surfaces is the polycrystalline coating of titanium dioxide taking Rutile Type as principal crystalline phase and contain a small amount of Anatase.
Again the pure titanium sheet of TC4 after process is used acetone, dehydrated alcohol and deionized water ultrasonic cleaning, dry for standby, bake out temperature 50 DEG C, time 1h successively;
Sample nanotube release coating: take NH
4f 5.2 grams, is dissolved in 40 ml deionized waters, then mixes with 360 ml glycerine, and magnetic agitation makes solution mix, obtained electrolytic solution.With this titanium sheet for anode, with 200 × 25 × 1 mm titanium plate for negative electrode, this titanium sheet is immersed below liquid level of electrolyte, the titanium bar of 200 × 5mm is processed with the titanium plate that thickness is 1mm, process in one end of titanium bar the groove that width is slightly less than 1mm, be used for blocking this titanium sheet, slowly boost with the speed of 2 V/min, when reaching 50 V, keep this voltage until total oxidization time reaches 2 h.After nanotube process terminates, by the soft drip wash of deionized water, wash remaining electrolytic solution off, in baking oven, dry 2h for 50 DEG C.Visible sample surfaces has heaved a lot of bubble, conductive resin is bonded at the side of aluminium block, sample surfaces gently one glue, just coating can be glued.After metal spraying, SEM observes, and as shown in Figure 1, can see as smart as a new pin that complete coating section clearly can see the pore passage structure of coat inside.Adopt the coat-thickness at 10 places on image software test SEM picture, calculating mean value, obtains coat-thickness numerical value, is about 3.8 ± 0.3 microns.
Embodiment 2
Prepared by sample coatings: the pure titanium sheet of TC4 being of a size of 20 × 20 × 2 mm uses 400,600,800 successively, 1000 order abrasive paper for metallograph sanding and polishings, and then with acetone, dehydrated alcohol, deionized water distinguishes ultrasonic cleaning 5 min; Constant voltage mode anodic oxidation in 1 M sulfuric acid electrolyte, whole voltage is 150V, after whole voltage, keep 1min.Sample surfaces obtains bolarious coating of titanium dioxide.
Again pure for TC4 titanium sheet is used acetone, dehydrated alcohol and deionized water ultrasonic cleaning successively, dry for standby, bake out temperature 60 DEG C, time 0.5h;
Sample nanotube release coating: take NH
4f 5.2 grams, is dissolved in 40 ml deionized waters, then mixes with 360 ml glycerine, and magnetic agitation makes solution mix, obtained electrolytic solution.With this titanium alloy sheet for anode, take titanium foil as negative electrode, this titanium alloy sheet is immersed below liquid level of electrolyte, process the titanium bar of 200 × 5mm with the titanium plate that thickness is 1mm, process in one end of titanium bar the groove that width is slightly less than 2mm, be used for blocking this titanium alloy sheet, apply voltage, slowly boost with the speed of 3 V/min, when reaching 60 V, keep this voltage until total oxidization time reaches 2 h.After nanotube process terminates, by the soft drip wash of deionized water, wash remaining electrolytic solution off, dry in baking oven, temperature 60 C, time 1h.The bolarious coating of visible sample surfaces regional area is peeled off, and conductive resin is bonded at the side of aluminium block, toasts 15min in an oven under 60 DEG C of conditions, increase the stickiness of conductive resin, with conductive resin sample surfaces gently one glue, the coating of stripping is transferred on glue, makes scanning electron microscope example.Observe as under scanning electron microscope, morphological structure coating section clearly can be seen, and visible coat inside compact structure, piled up by the crystal grain of a lot of nano-scale and form.Adopt the coat-thickness at 10 places on software test SEM picture, obtain coat-thickness numerical value, be about 5.69 ± 0.3 microns.Observe coating cross-section morphology,
Embodiment 3
Prepared by sample coatings: the beta alloy sheet (trade mark) being of a size of 5 × 5 × 1 mm uses 400,600 successively, 800 order abrasive paper for metallograph sanding and polishings, and then with acetone, dehydrated alcohol, deionized water distinguishes ultrasonic cleaning 5 min; Constant voltage mode anodic oxidation in 1 M sulfuric acid electrolyte, whole voltage is 150V, after whole voltage, keep 1min.Sample surfaces obtains layer of titanium dioxide coating.
Again beta alloy sheet is used acetone, dehydrated alcohol and deionized water ultrasonic cleaning successively, dry for standby, bake out temperature 55 DEG C, time 0.8h;
Sample nanotube release coating: take NH
4f 5.2 grams, is dissolved in 40 ml deionized waters, then mixes with 360 ml glycerine, and magnetic agitation makes solution mix, obtained electrolytic solution.With this titanium alloy sheet for anode, take titanium foil as negative electrode, this titanium alloy sheet is immersed below liquid level of electrolyte, process the titanium bar of 200 × 5mm with the titanium plate that thickness is 1mm, process in one end of titanium bar the groove that width is slightly less than 1mm, be used for blocking this titanium alloy sheet, apply voltage, slowly boost with the speed of 2 V/min, when reaching 60 V, keep this voltage until total oxidization time reaches 2 h.After nanotube process terminates, by the soft drip wash of deionized water, wash remaining electrolytic solution off, dry in baking oven, temperature 52 DEG C, time 1.8h.The coating of visible sample surfaces regional area is peeled off, and conductive resin is bonded at the side of aluminium block, toasts 20min in an oven under 60 DEG C of conditions, increase the stickiness of conductive resin, with conductive resin sample surfaces gently one glue, the coating of stripping is transferred on glue, makes scanning electron microscope example.Observe as under scanning electron microscope, morphological structure coating section clearly can be seen, and visible coat inside contains a lot of micropore or pore passage structure.Adopt the coat-thickness at 10 places on software test SEM picture, obtain coat-thickness numerical value, be about 5 microns.
Embodiment 4:
Prepared by sample coatings: diameter is 15mm, and the pure titanium sheet of TA2 of thickness 1 mm uses 400,600 successively, 800 order SiC sand papering polishings, and then with acetone, dehydrated alcohol, deionized water distinguishes ultrasonic cleaning 5 min; Sample is immersed in the H of 30 wt.%
2o
2in solution, 80 DEG C of Water Under baths, process 8h, is then placed in 0.25 M dilute hydrochloric acid solution ageing 72 h.Layer of titanium dioxide coating has been prepared on surface.
Again pure titanium sheet is used acetone, dehydrated alcohol and deionized water ultrasonic cleaning successively, dry for standby, bake out temperature 50 DEG C, time 0.6h;
Sample nanotube release coating: take NH
4f 5.2 grams, is dissolved in 40 ml deionized waters, then mixes with 360 ml ethylene glycol, and magnetic agitation makes solution mix, obtained electrolytic solution.With this titanium sheet for anode, with 200 × 25 × 1 mm titanium plate for negative electrode, this titanium sheet is immersed below liquid level of electrolyte, the titanium bar of 200 × 5mm is processed with the titanium plate that thickness is 1mm, process in one end of titanium bar the groove that width is slightly less than 1mm, be used for blocking this titanium sheet, slowly boost with the speed of 2 V/min, when reaching 50 V, keep this voltage until total oxidization time reaches 2 h.After nanotube process terminates, by the soft drip wash of deionized water, wash remaining electrolytic solution off, in baking oven, 60 DEG C of oven dry, are bonded at the side of aluminium block by conductive resin, one sticky gently at sample surfaces, just coating can be glued.After metal spraying, SEM observes, and can see that as smart as a new pin complete coating section can see that coating has layered structure.Adopt the coat-thickness at 10 places on image software test SEM picture, calculating mean value, obtains coat-thickness numerical value, is about 0.78 ± 0.10 micron.
Embodiment 5
Prepared by sample coatings: the pure titanium sheet of TA1 being of a size of 10 × 10 × 1 mm uses 400,600 successively, 800 order SiC sand papering polishings, and then with acetone, dehydrated alcohol, deionized water distinguishes ultrasonic cleaning 5 min; Adopt microwave plasma CVD (MPCVD) equipment depositing diamond film in pure titanium sheet, frequency is 2.45 GHz, gas source is the mixed gas of CH4 and H2, its flow is respectively 20 sccm and 400 sccm, 5 h are processed under output rating is 1300 W, sample after process, through scanning electron microscope and X-ray diffractometer test, is defined as diamond film.
Again pure for TA1 titanium sheet is used acetone, dehydrated alcohol and deionized water ultrasonic cleaning successively, dry for standby, bake out temperature 58 DEG C, time 0.5h;
Sample nanotube release coating: take NH
4f 5.2 grams, is dissolved in 40 ml deionized waters, then mixes with 360 ml glycerine, and magnetic agitation makes solution mix, obtained electrolytic solution.With this titanium sheet for anode, with 200 × 25 × 1 mm titanium plate for negative electrode, this titanium sheet is immersed below liquid level of electrolyte, the titanium bar of 200 × 5mm is processed with the titanium plate that thickness is 1mm, process in one end of titanium bar the groove that width is slightly less than 1mm, be used for blocking this titanium sheet, slowly boost with the speed of 2 V/min, when reaching 50 V, keep this voltage until total oxidization time reaches 2 h.After nanotube process terminates, by the soft drip wash of deionized water, wash remaining electrolytic solution off, 60 DEG C of oven dry in baking oven.Visual inspection finds that the color of this sample there occurs change., conductive resin is bonded at the side of aluminium block, sample surfaces gently one glue, coating is adhered to aluminium block side, makes scanning electron microscope example.After metal spraying, SEM observes, and can see as smart as a new pin, complete coating section, and section structure is fine and close, and 50,000 times of lower imporosities, can not tell crystalline-granular texture.Software test coat-thickness is adopted to be about 0.4 micron.
Embodiment 6
Prepared by sample coatings: the pure titanium sheet of TA1 being of a size of 10 × 10 × 1 mm uses 400,600 successively, 800 order SiC sand papering polishings, and then with acetone, dehydrated alcohol, deionized water distinguishes ultrasonic cleaning 5 min; Constant voltage mode anodic oxidation in 1 M sulfuric acid electrolyte, whole voltage is 250V, after whole voltage, keep 1min.
Again pure titanium sheet is used acetone, dehydrated alcohol and deionized water ultrasonic cleaning successively, dry for standby, bake out temperature 52 DEG C, time 0.8h;
Sample nanotube release coating: take NH
4f 5.2 grams, is dissolved in 40 ml deionized waters, then mixes with 360 ml glycerine, and magnetic agitation makes solution mix, obtained electrolytic solution.With this titanium sheet for anode, with 200 × 25 × 1 mm titanium plate for negative electrode, this titanium sheet is immersed below liquid level of electrolyte, the titanium bar of 200 × 5mm is processed with the titanium plate that thickness is 1mm, process in one end of titanium bar the groove that width is slightly less than 1mm, be used for blocking this titanium sheet, slowly boost with the speed of 2 V/min, when reaching 50 V, keep this voltage until total oxidization time reaches 2 h.After nanotube process terminates, by the soft drip wash of deionized water, wash remaining electrolytic solution off, 55 DEG C of oven dry in baking oven.Visible sample surfaces has heaved a lot of bubble, conductive resin is bonded at the side of aluminium block, sample surfaces gently one glue, just coating can be glued.After metal spraying, SEM observes, and can see that as smart as a new pin complete coating section clearly can see the pore passage structure of coat inside.Adopt the coat-thickness at 10 places on image software test SEM picture, calculating mean value, obtains coat-thickness numerical value, is about 18.1 ± 0.3 microns.
Embodiment 7
Prepared by sample coatings: diameter is 15mm, and thickness is that the pure titanium sheet of TA1 of 1 mm uses 400,600 successively, 800 order SiC sand papering polishings, and then with acetone, dehydrated alcohol, deionized water distinguishes ultrasonic cleaning 5 min; Constant voltage mode anodic oxidation in 1 M water glass electrolytic solution, whole voltage is 180V, after whole voltage, keep 1min.After process terminates, naked eyes visible surface becomes coarse, presents black.
Again pure titanium sheet is used acetone, dehydrated alcohol and deionized water ultrasonic cleaning successively, dry for standby, bake out temperature 54 DEG C, time 0.7h;
Sample nanotube release coating: take NH
4f 5.2 grams, is dissolved in 40 ml deionized waters, then mixes with 360 ml glycerine, and magnetic agitation makes solution mix, obtained electrolytic solution.With this titanium sheet for anode, with 200 × 25 × 1 mm titanium plate for negative electrode, this titanium sheet is immersed below liquid level of electrolyte, processes the titanium bar of 200 × 5mm with the titanium plate that thickness is 1mm, process in one end of titanium bar the groove that width is slightly less than 1mm, polish off a certain pocket in disk edge, block this titanium sheet from this region, to ensure good contact, slowly boost with the speed of 10 V/min, when reaching 100 V, keep this voltage until total oxidization time reaches 1.5 h.After nanotube process terminates, by the soft drip wash of deionized water, wash remaining electrolytic solution off, 50 DEG C of oven dry in baking oven.Visible sample surfaces has heaved a lot of bubble, conductive resin is bonded at the side of aluminium block, sample surfaces gently one glue, just coating can be glued.After metal spraying, SEM observes, and can see that as smart as a new pin complete coating section clearly can see the pore passage structure that coat inside is huge.Adopt the coat-thickness at 10 places on image software test SEM picture, calculating mean value, obtains coat-thickness numerical value, is about 16.5 microns.
The method configuration organic fluoride-containing is used for electrolyte in carrying out the process of anodic oxidation nanotube to the titanium or titanium alloy substrate of intending release coating, the feature utilizing Nano tube array of titanium dioxide to be formed between Titanium base and former cated bonding interface and phenomenon, destroy the bonding force at original coating and Titanium base interface, and the bonding force at nano-tube array and original coating and Titanium base interface is between the two weak, result causes original coating nondestructively to open with matrix stripping.
Claims (6)
1. adopt nanotube facture to peel off a method for titanium top coat, it is characterized in that: specifically comprise following step:
(1) pure titanium or the titanium alloy test specimen acetone of stripper surface coating, dehydrated alcohol and deionized water ultrasonic cleaning, dry for standby will be intended;
(2) NH is taken
4f 5.2 grams, is dissolved in 40 ml deionized waters, then mixes with 360 ml glycerine or ethylene glycol, and magnetic agitation makes solution mix, obtained electrolytic solution;
(3) under room temperature, the titanium test specimen crossed by cleaning-drying carries out anodic oxidation treatment in organic fluoride-containing electrolytic solution, to intend the titanium test specimen of stripper surface coating for anode, with titanium plate or titanium foil for negative electrode, titanium test specimen is immersed below liquid level of electrolyte, connect titanium test specimen and positive source wire with the titanium material that shape is suitable, ensure that junction contact is good;
(4) voltage-drop loading mode is gradient pressurization, slowly boosts with speed 2 ~ 5 V/min, when reaching 50 ~ 80 V, keeps this voltage until total oxidization time reaches 1.5 ~ 2.5 h;
(5) after nanotube process terminates, take off test specimen gently, with the soft drip wash test specimen of deionized water, wash away the glycerine solution remaining in sample surfaces, then sample is dried.
2., according to a kind of method adopting nanotube facture to peel off titanium top coat described in claim 1, it is characterized in that: bake out temperature 50-60 DEG C, time 0.5-1h in described step (1).
3., according to a kind of method adopting nanotube facture to peel off titanium top coat described in claim 1, it is characterized in that: bake out temperature 50-60 DEG C, time 1-2h in described step (5).
4. according to a kind of application adopting nanotube method to peel off titanium top coat described in claim 1, it is characterized in that: be applied to preparation coating profile scanning electron microscopic sample.
5. according to a kind of application adopting nanotube method to peel off titanium top coat described in claim 4, it is characterized in that: described preparation method is specially and is stained with conductive resin in the one side of square aluminium block, heating makes adhesive tape stickiness better in an oven, be stained with by the coating that sample surfaces has been peeled off by conductive resin, make the scanning electron microscope example of coating section, for observing the appearance structure feature of coat-thickness and coating section.
6., according to a kind of application adopting nanotube method to peel off titanium top coat described in claim 5, it is characterized in that: Heating temperature 60 DEG C in described baking oven, time 15-25min.
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| CN104451824B (en) | 2017-01-18 |
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