CN101642972A - Stainless steel composite material and preparation method thereof - Google Patents
Stainless steel composite material and preparation method thereof Download PDFInfo
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- CN101642972A CN101642972A CN200810135480A CN200810135480A CN101642972A CN 101642972 A CN101642972 A CN 101642972A CN 200810135480 A CN200810135480 A CN 200810135480A CN 200810135480 A CN200810135480 A CN 200810135480A CN 101642972 A CN101642972 A CN 101642972A
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Abstract
The invention provides a stainless steel composite material. The composite material comprises a stainless steel base material, wherein the composite material also comprises a metallic titanium layer positioned on the surface of the stainless steel base material and a titanium oxide layer positioned on the surface of the metallic titanium layer. The invention also provides a preparation method forthe stainless steel composite material. According to the stainless steel composite material and the preparation method thereof, various required colors on the surface of the stainless steel compositematerial can be obtained, and the abrasion resistance is good. Through the preparation method, under the preferable condition and by adjusting the operation conditions, various required colors on thesurface of the stainless steel composite material can be obtained, and the stainless steel base material can obtain better decoration effect so as to improve the value of a product.
Description
Technical field
The present invention relates to a kind of stainless steel composite material, also relate to the preparation method of this stainless steel composite material.
Background technology
Traditional stainless steel surfaces is decorated methods such as adopting polishing, wire drawing, satin face and sandblast, and these class methods all can change stainless outward appearance to a certain extent, make stainless steel surfaces have certain aesthetic.Can also adopt the stainless steel coloring technology to make stainless steel surfaces have various colors, general stainless steel coloring technology can adopt technology such as direct oxidation stainless steel watch face colouring, film interference, spraying, silk-screen, though be colored stainless steel material but adopt direct oxidation stainless steel watch face colouring and adopt film interference can access the surface, the less stable of its technology, the difficult repeatability that realizes color.Adopt the wearability of the resulting stainless steel products of method such as spraying, silk-screen relatively poor, color and aesthetic property are all undesirable.
Summary of the invention
The objective of the invention is to overcome the relatively poor defective of wearability of above-mentioned stainless steel product of the prior art, a kind of wearability stainless steel composite material preferably is provided, the preparation method of this stainless steel composite material also is provided.
The invention provides a kind of stainless steel composite material, this composite comprises stainless steel substrate, and wherein, this composite also comprises the containing metal titanium layer that is positioned at this stainless steel substrate surface and is positioned at the titanium oxide layer that contains on containing metal titanium layer surface.
The present invention also provides a kind of preparation method of stainless steel composite material, and this method is included in the stainless steel substrate surface and forms the containing metal titanium layer, forms on described containing metal titanium layer surface to contain titanium oxide layer.
According to stainless steel composite material provided by the invention and preparation method thereof, make the color of the various needs of stainless steel composite material surface acquisition, and wearability is fine.And by preparation method of the present invention, in the preferred case,, can make the stainless steel composite material surface obtain the color of various needs, make stainless steel substrate can obtain better decorative effect, thereby can improve the value of product by regulating operating condition.
The specific embodiment
Stainless steel composite material provided by the invention comprises stainless steel substrate, and wherein, this composite also comprises the containing metal titanium layer that is positioned at this stainless steel substrate surface and is positioned at the titanium oxide layer that contains on containing metal titanium layer surface.
" stainless steel substrate " described herein expression stainless steel material, when described " stainless steel substrate " was present in the described stainless steel composite material, described " stainless steel substrate " was illustrated in the stainless steel material part of the not containing metal titanium behind the surface of stainless steel formation containing metal titanium layer; When described " stainless steel substrate " was present among the preparation method of described stainless steel composite material, described " stainless steel substrate " expression did not form the stainless steel material part of the initial stainless steel material or the not containing metal titanium after surface of stainless steel forms the containing metal titanium layer of containing metal titanium layer.
According to stainless steel composite material provided by the invention, under the preferable case, the thickness of described containing metal titanium layer is the 20-80 micron, and the described thickness that contains titanium oxide layer is the 0.05-1 micron.
According to stainless steel composite material provided by the invention, under the preferable case, described containing metal titanium layer is stainless metallic cementation titanium layer.Because this containing metal titanium layer is stainless metallic cementation titanium layer, so very good with the adhesion of stainless steel substrate in the stainless steel composite material of the present invention.
According to stainless steel composite material provided by the invention, under the preferable case, the described containing metal titanium layer of distance is at least 70 weight % with the 3 microns Ti contents with interior containing metal titanium layer of contact surface that contain titanium oxide layer, and the described titanium oxide content that contains titanium oxide layer is at least 85 weight %.
The preparation method of stainless steel composite material provided by the invention comprises, forms the containing metal titanium layer on the stainless steel substrate surface, forms on described containing metal titanium layer surface to contain titanium oxide layer.
According to preparation method provided by the invention, described containing metal titanium layer can adopt the whole bag of tricks to form, under the preferable case, the described method that forms the containing metal titanium layer on stainless steel substrate surface comprises carries out the ion implantation titanium to the stainless steel substrate surface, and the condition of ion implantation titanium to make the thickness of described containing metal titanium layer be the 20-81 micron.
According to preparation method provided by the invention, in the preferred case, the condition of ion implantation titanium makes described containing metal titanium layer surface 3-4 micron be at least 70 weight % with the Ti content of interior containing metal titanium layer, and the minimum titaniferous amount in 3 microns on the more preferably described containing metal titanium layer top layer is 85%; And the Ti content on preferred containing metal titanium layer surface is at least 95 weight %, and most preferably containing metal titanium layer surface is the simple metal titanium layer.
According to preparation method provided by the invention, the method for described ion implantation titanium is for well known to a person skilled in the art.Under the preferable case, the condition of ion implantation comprises that voltage is that 200-1000 volt, temperature are that 300-1200 ℃, the absolute pressure of inert gas are that 10-1000Pa, time are 3-15 hour.Described inert gas can adopt one or more in helium, neon, argon gas, krypton gas, xenon and the radon gas, and preferably adopts argon gas.
Described ion implantation method preferably adopts two brightness ion implantation methods, the detailed process of this method and method of operating become ion and atom for adopting the glow discharge of argon gas vacuum low-pressure that Titanium is stimulated, penetrate into the stainless steel substrate surface, form titanium alloy layer, and in the preferred case, along with constantly carrying out of ion titanizing, Titanium is deposited on the stainless steel substrate surface, thereby is that titanium alloy surface forms the simple metal titanium layer at stainless steel substrate.Under this preferable case of the present invention, titanium alloy layer and simple metal titanium layer are referred to as the containing metal titanium layer.
According to preparation method provided by the invention, the described titanium oxide layer that contains can adopt the various methods that well known to a person skilled in the art to form, preferred adopt anodised method to form, and anodised condition to make the described thickness that contains titanium oxide layer be the 0.05-1 micron.
According to preparation method provided by the invention, because anodic oxidation can not be carried out on stainless steel substrate, therefore the anodic oxidation that is formed with the containing metal titanium layer of 20-81 micron for the surface is that the Titanium in this containing metal titanium layer is carried out anodic oxidation, the present inventor finds, when being at least 70 weight % with 3 microns the titaniferous amounts of contact surface that contain titanium oxide layer with interior containing metal titanium layer by the described containing metal titanium layer of assurance distance, can effectively improve the adhesive force that contains titanium oxide layer, therefore, the present invention preferably is at least 70 weight % with the condition restriction of above-mentioned ion implantation in distance gained containing metal titanium layer and the 3 microns titaniferous amounts with interior containing metal titanium layer of contact surface that contain titanium oxide layer, more preferably is at least 85%.
According to preparation method provided by the invention, described anodised condition is for well known to a person skilled in the art.By controlling the titanium oxide layer that contains that anodised operating condition can obtain different-thickness, and because the titanium oxide layer that contains of different-thickness has different colors, thereby can make stainless steel composite material of the present invention obtain different colors.For example, when the thickness that contains titanium oxide layer was 0.78 micron left and right sides, stainless steel composite material of the present invention surface had reddish yellow; Thickness is a little increase again, and color becomes rose-red, and a little reduces thickness, and color becomes yellow or light yellow green.
For example, anodised condition can comprise that the stainless steel substrate that makes the surface be formed with the containing metal titanium layer contacts with electrolyte as anode, and to be not negative electrode with the conductive material of electrolyte reaction, voltage is the 1-110 volt, and current density is 0.05-0.8A/dm
2, the temperature of electrolyte is 15-35 ℃, the anodised time is 5-50 minute.Described negative electrode can adopt stainless steel, platinum, stereotype, graphite etc., preferably adopts stainless steel as negative electrode.Can contain the thickness of titanium oxide layer, thereby can obtain the color of needs by voltage, the time control of controlling in the above-mentioned condition.
According to preparation method provided by the invention, the employed electrolyte of described anodic oxidation can be generally acidic electrolysis bath for well known to a person skilled in the art various electrolyte.In the present invention, the preferred electrolyte that contains weak acid such as phosphoric acid, oxalic acid and hydrogen fluoride that adopts also can adopt strong acid such as sulfuric acid.For example, electrolyte of the present invention is the aqueous solution that contains phosphoric acid 50-180g/L, oxalic acid 5-20g/L, hydrogen fluoride 5-30g/L.
According to preparation method provided by the invention, obtain predetermined pattern if desired, mould with this pattern can be covered on the stainless steel material or and cover with the outside of mould with this pattern in surface of stainless steel, carry out ion implantation and anodic oxidation then successively, can obtain needed pattern.
According to preparation method provided by the invention, in the preferred case, preparation method of the present invention also comprises stainless steel material carried out pre-treatment, and the pre-treatment that stainless steel material carried out is generally included polishing and cleans or only clean.Polishing can be adopted and well known to a person skilled in the art and for example can adopt machine glazed finish, chemical polishing and electrobrightening by various finishing methods.Cleaning can be adopted and well known to a person skilled in the art the whole bag of tricks, can directly adopt the metal cleaner of producer's configuration, also can directly prepare, and for example can adopt and contain NaOH 10-15 grams per liter, Na
2CO
310-20 grams per liter, Na
3PO
412H
2The cleaning fluid of the aqueous solution of O50-70 grams per liter and waterglass 5-10 grams per liter cleans, and preferably can also cooperate ultrasonic vibration to clean.
Adopt the mode of embodiment that the present invention is described in further detail below.
Embodiment 1
Workpiece: stamping forming stainless steel (North America stainless steel company, 304) phone housing
1, pre-treatment
(1) machine glazed finish
Adopting rough polishing ointment (SBT-600 type) in the yellow that polishing machine (JM-101 type) that the brilliant close plant equipment of Dongguan City Co., Ltd produces produces with the outstanding sharp letter rubbing down in Jiangmen Materials Co., Ltd is under 2840 rev/mins the condition workpiece slightly to be thrown 10 minutes at the rotating speed of polishing wheel, is under 2840 rev/mins the condition workpiece to be carried out essence throwing 10 minutes at the rotating speed of polishing wheel with white smart throwing ointment (SBW-804 model) again.
(2) clean
Workpiece after the above-mentioned polishing is immersed in normal temperature successively removes La Shui, remove and carry out ultrasonic wave in the deionized water of oil-bound distemper solution and 70 ℃ and clean, scavenging period was followed successively by 5 minutes, 5 minutes, 10 minutes, and each all washed with water between the step.Wherein remove La Shui and remove oil-bound distemper and be wheat dolantin Fine Chemical Co., Ltd product.Oven dry after cleaning finishes.
2, ion implantation
Workpiece after the above-mentioned pre-treatment is put into ion metallizing device (multi-functional plasma surface modification equipment, Surface Engineering Co., Ltd runs initially in Wuhan, model LDMC-15A/LD-15A) carries out ion titanizing in, the voltage that is adopted is 500 ± 50 volts, the absolute pressure of argon gas is 30 ± 10 handkerchiefs, temperature is 300-650 ℃, and oozing the titanium time is 5 hours.
Metallographic structure detects (German ZEISS metallographic microscope, model Axio Imager.A 1m) tests out, obtain thickness on stainless steel substrate surface and be 50 microns containing metal titanium layer, test out the Ti content 90 weight % in 3 microns on the containing metal titanium layer surface with energy disperse spectroscopy check and analysis (Japanese ULVAC-PHI company 1800 type photoelectron spectrographs).
Then, the workpiece behind the gained ion implantation is slightly thrown and used ultrasonic wave to carry out oil removing and clean with ethanol (concentration 99.9 weight %, Tianjin chemical reagent factory).
3, anodic oxidation
The above-mentioned stainless steel substrate that carries out after the pre-treatment is immersed in the electrolyte of electrolytic cell, is anode with the workpiece, is negative electrode with the corrosion resistant plate, is 30V at voltage, and current density is 0.2A/dm
2, and be to carry out anodic oxidation under 25 ℃ the condition in the temperature of electrolyte, the anodised time is 20 minutes.
Electrolyte for contain phosphatase 11 00ml/L, oxalic acid 15g/L, proportion is 1.13g/cm
3Hydrofluoric acid 15ml/L, the pH value is 3 the aqueous solution.
Take out the clean and oven dry under 50-75 ℃ of workpiece cleaning, finally obtain the surface and be navy blue stainless steel phone housing product.
The thickness that contains titanium oxide layer that records this product is 0.5 micron, and titanium oxide content is 92 weight %, and the thickness of containing metal titanium layer is 50 microns, and the Ti content in 3 microns on the containing metal titanium layer top layer is 88%.
Embodiment 2
The corrosion resistant plate of workpiece: 300 * 60 * 0.5mm (general stainless steel alloy, 304)
1, pre-treatment
Clean
Workpiece after the above-mentioned polishing is immersed in normal temperature successively removes La Shui, remove and carry out ultrasonic wave in the deionized water of oil-bound distemper solution and 70 ℃ and clean, scavenging period was followed successively by 5 minutes, 5 minutes, 10 minutes, and each all washed with water between the step.Wherein remove La Shui and remove oil-bound distemper and be wheat dolantin Fine Chemical Co., Ltd product.Oven dry after cleaning finishes.
2, ion implantation
Steel plate after the above-mentioned pre-treatment is put into ion metallizing device (multi-functional plasma surface modification equipment, Surface Engineering Co., Ltd runs initially in Wuhan, model LDMC-15A/LD-15A) carries out ion titanizing in, the voltage that is adopted is 600 ± 50 volts, the absolute pressure of argon gas is 50 handkerchiefs, temperature is 750 ± 25 ℃, and oozing the titanium time is 8 ± 0.5 hours.
Metallographic structure detects (German ZEISS metallographic microscope, model Axio Imager.A 1m) tests out, obtain thickness on stainless steel substrate surface and be 30 microns containing metal titanium layer, be detected as (Japanese ULVAC-PHI company 1800 type photoelectron spectrographs) with energy disperse spectroscopy and test out, the Ti content 92% in 3 microns on the containing metal titanium layer surface.
Then, the workpiece behind the gained ion implantation is slightly thrown and used ultrasonic wave to carry out oil removing and clean with acetone (concentration 99.9 weight %, Tianjin chemical reagent factory).
3, anodic oxidation
The above-mentioned stainless steel substrate that carries out after the pre-treatment is immersed in the electrolyte of electrolytic cell, with the workpiece is anode, is negative electrode with the corrosion resistant plate, is 10V at voltage, and be to carry out anodic oxidation under 25 ℃ the condition in the temperature of electrolyte, the anodised time is 20 minutes.
Electrolyte is that concentration is that (proportion is 1.13g/cm for the hydrofluoric acid of 0.8 volume %
3) aqueous solution.
Take out the clean and oven dry under 65 ℃ of workpiece cleaning, finally obtain the surface and be flavous stainless steel composite material product.
The thickness that contains titanium oxide layer that records this product is 0.7 micron, and titanium oxide content is 94%, and the thickness of containing metal titanium layer is 30 microns, and the Ti content in 3 microns on the containing metal titanium layer top layer is 90 weight %.
Comparative Examples 1
The corrosion resistant plate of workpiece: 300 * 60 * 0.5mm (general stainless steel alloy, 304)
Method according to embodiment 1 is carried out pre-treatment.
Adopt spraying coating process then, spray distance is that 20cm, spray gun diameter are that 1.2mm, spray pressure are that 0.2MPa, baking temperature are that 150 ℃, stoving time are 18 minutes.Coating is polymethyl methacrylate baking vanish (2000 series, Dongguan prestige despot Industrial Co., Ltd., the collocation #201 of producer solvent dilution are to 40-60 volume %).The final thickness that obtains on the stainless steel substrate surface is 10 microns coating.
Performance test
1, adhesion
Test institute accepted standard: ISO 2409.
Testing procedure:
Mark the grid of 100 1mm * 1mm at sample surfaces to be tested, the degree of depth of drawing lattice is to exposing the sample ground, the model of producing with Minnesota Mining and Manufacturing Company is that 600 adhesive tape sticks on and draws on the good grid, and adhesive tape and grid are pasted fully, and phenomenons such as wrinkle bubble can not be arranged.Drag adhesive tape from adhesive tape is monolateral rapidly with 180 ° of horizontal directions then.
Evaluation criterion is:
The 5B cut edge is smooth fully, four jiaos of not distortion of grid;
There is little peeling off 4B overlay film inside, and the zone less than 5% is affected;
There is little peeling off 3B overlay film edge and inside, and the zone of quadrille 5-15% is affected;
The edge of 2B overlay film and part plane have and come off, and the zone of influence accounts for the 15-30% of grid;
Peel off the cut edge of 1B overlay film, and have large-area band to separate with monoblock, and the influence area is at 35-65%;
0B comes off and surpasses the requirement of 1B level with separating.
2, wearability
Use the RCA paper tape wear resistant instrument of model as F350008, the sample surfaces that rubs under 175 gram forces is milled to when show-through the number of turns that the record rubber wheel rotates to sample surfaces.
Adopt above-mentioned method of testing that embodiment 1-2 and Comparative Examples 1 resulting stainless steel composite material are carried out performance test, the results are shown in Table 1 for gained.
Table 1
| Embodiment 1 | Embodiment 2 | Comparative Examples 1 | |
| Adhesion | ?5B | ?5B | ?4B |
| Wearability | ?84 | ?75 | ?35 |
From the data of the foregoing description 1-2 and table 1 as can be seen, the resulting stainless steel composite material of the method according to this invention can have gay colours, wearability is fine, and also fine with the adhesion of stainless steel substrate in stainless steel composite material, in the decoration field of modern stainless steel material, very big application prospect is arranged.
Claims (11)
1, a kind of stainless steel composite material, this composite comprises stainless steel substrate, it is characterized in that, this composite also comprises the containing metal titanium layer that is positioned at this stainless steel substrate surface and is positioned at the titanium oxide layer that contains on containing metal titanium layer surface.
2, according to the composite described in the claim 1, wherein, the thickness of described containing metal titanium layer is the 20-80 micron, and the thickness that contains titanium oxide layer is the 0.05-1 micron.
3, composite according to claim 1 and 2, wherein, described containing metal titanium layer is stainless metallic cementation titanium layer.
4, composite according to claim 1 and 2, wherein, the described containing metal titanium layer of distance is at least 70 weight % with the 3 microns Ti contents with interior containing metal titanium layer of contact surface that contain titanium oxide layer, and the described titanium oxide content that contains titanium oxide layer is at least 85 weight %.
5, the preparation method of the described stainless steel composite material of claim 1 is characterized in that, this method is included in the stainless steel substrate surface and forms the containing metal titanium layer, forms on described containing metal titanium layer surface to contain titanium oxide layer.
6, method according to claim 5, wherein, the described method that forms the containing metal titanium layer on stainless steel substrate surface comprises carries out the ion implantation titanium to the stainless steel substrate surface, and the condition of ion implantation titanium to make the thickness of described containing metal titanium layer be the 20-81 micron.
7, method according to claim 6, wherein, the condition of ion implantation titanium makes described containing metal titanium layer surface 3-4 micron be at least 70 weight % with the Ti content of interior containing metal titanium layer.
8, according to claim 5 or 6 described methods, wherein, the condition of described ion implantation titanium comprises that voltage is that 200-1000 volt, temperature are that 300-1200 ℃, the absolute pressure of inert gas are that 10-1000Pa, time are 3-15 hour.
9, method according to claim 5, wherein, the described method that contains titanium oxide layer that forms on described containing metal titanium layer surface comprises anodic oxidation carried out on the surface of containing metal titanium layer, and anodised condition to make the described thickness that contains titanium oxide layer be the 0.05-1 micron.
10, method according to claim 9, wherein, described anodised condition comprises, the stainless steel substrate that makes the surface be formed with the containing metal titanium layer contacts with electrolyte as anode, being not negative electrode with the conductive material of electrolyte reaction, voltage is the 1-110 volt, and current density is 0.05-0.8A/dm
2, the temperature of electrolyte is 15-35 ℃, the anodised time is 5-50 minute.
11, method according to claim 10, wherein, described electrolyte is for containing phosphoric acid, oxalic acid and the hydrofluoric aqueous solution, and in this electrolyte, concentration of phosphoric acid is that the concentration of 50-180g/L, oxalic acid is that 5-20g/L, hydrofluoric concentration are 5-30g/L.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101992344A (en) * | 2010-11-11 | 2011-03-30 | 东北大学 | Preparation method of titanium-steel composite plate |
| CN102886929A (en) * | 2011-07-20 | 2013-01-23 | 鸿富锦精密工业（深圳）有限公司 | Film and preparation method thereof |
| CN103290417A (en) * | 2013-05-22 | 2013-09-11 | 太原理工大学 | Preparation method of titanium dioxide (TiO2) nanotube film on stainless steel surface |
| CN103895161A (en) * | 2012-12-28 | 2014-07-02 | 比亚迪股份有限公司 | Preparation method of stainless steel-resin composite and stainless steel-resin composite prepared by same |
| CN106363346A (en) * | 2015-07-24 | 2017-02-01 | 深圳市光峰光电技术有限公司 | Shell with identification piece and manufacturing method of shell |
| CN106521599A (en) * | 2016-11-03 | 2017-03-22 | 中国科学院兰州化学物理研究所 | Treatment method of coating surface modification |
| CN107981701A (en) * | 2016-10-26 | 2018-05-04 | 佛山市顺德区美的电热电器制造有限公司 | Titanium-based carries silver-colored titanium dioxide composite antibacterial base material and preparation method thereof and titanium-based cookware and preparation method thereof |
| CN108531961A (en) * | 2018-05-10 | 2018-09-14 | 中国科学院宁波材料技术与工程研究所 | Colour film and preparation method thereof, application |
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| CN101992344A (en) * | 2010-11-11 | 2011-03-30 | 东北大学 | Preparation method of titanium-steel composite plate |
| CN102886929A (en) * | 2011-07-20 | 2013-01-23 | 鸿富锦精密工业（深圳）有限公司 | Film and preparation method thereof |
| CN102886929B (en) * | 2011-07-20 | 2016-11-23 | 鸿富锦精密工业（深圳）有限公司 | Thin film and preparation method thereof |
| CN103895161A (en) * | 2012-12-28 | 2014-07-02 | 比亚迪股份有限公司 | Preparation method of stainless steel-resin composite and stainless steel-resin composite prepared by same |
| CN103290417A (en) * | 2013-05-22 | 2013-09-11 | 太原理工大学 | Preparation method of titanium dioxide (TiO2) nanotube film on stainless steel surface |
| CN106363346A (en) * | 2015-07-24 | 2017-02-01 | 深圳市光峰光电技术有限公司 | Shell with identification piece and manufacturing method of shell |
| CN107981701A (en) * | 2016-10-26 | 2018-05-04 | 佛山市顺德区美的电热电器制造有限公司 | Titanium-based carries silver-colored titanium dioxide composite antibacterial base material and preparation method thereof and titanium-based cookware and preparation method thereof |
| CN106521599A (en) * | 2016-11-03 | 2017-03-22 | 中国科学院兰州化学物理研究所 | Treatment method of coating surface modification |
| CN108531961A (en) * | 2018-05-10 | 2018-09-14 | 中国科学院宁波材料技术与工程研究所 | Colour film and preparation method thereof, application |
| CN108531961B (en) * | 2018-05-10 | 2020-06-09 | 中国科学院宁波材料技术与工程研究所 | Medical implant and method for producing the same |
| CN110042342A (en) * | 2019-04-23 | 2019-07-23 | 杭州阿牟文化艺术有限公司 | A kind of corrosion resistant type knife cuts the preparation method of material |
| CN113293421A (en) * | 2021-04-15 | 2021-08-24 | 光科真空科技(泰兴)有限公司 | Electrolytic process and electrolyte for inner wall protection plate of vacuum cavity |
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Application publication date: 20100210 |