CN101886247A - Preparation method of high transmission glass-based porous aluminum oxide substrate - Google Patents
Preparation method of high transmission glass-based porous aluminum oxide substrate Download PDFInfo
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- CN101886247A CN101886247A CN 201010229065 CN201010229065A CN101886247A CN 101886247 A CN101886247 A CN 101886247A CN 201010229065 CN201010229065 CN 201010229065 CN 201010229065 A CN201010229065 A CN 201010229065A CN 101886247 A CN101886247 A CN 101886247A
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Abstract
The invention provides a preparation method of a novel glass-based porous aluminum oxide substrate. The preparation method comprises the following steps of: firstly, preparing a high purity aluminum film by using glass as a substrate and adopting a vacuum thermal evaporation method; secondly, generating a porous aluminum oxide layer by using a primary anode oxidation method or a secondary anode oxidation method; thirdly, optimizing pore diameters of the porous aluminum oxide layer by using a pore expanding process; and fourthly, improving the transmission of the whole glass-based porous aluminum oxide substrate by using high temperature annealing treatment. The glass-based porous aluminum oxide substrate has favorable mechanical strength, ordered aluminum oxide pore heights and high transmission of visible light.
Description
Technical field
The present invention relates to a kind of preparation method of glass-based porous aluminum oxide substrate, particularly relate to a kind of vacuum thermal evaporation method and on glass substrate, be coated with rafifinal, as anode, adopt that anonizing preparation (assembling) has that performance is controlled, hole size and being evenly distributed and the preparation method of good stability, glass-based porous aluminum oxide substrate that transmission of visible light is high.
Background technology
Nanotechnology and nano material have begun to enter into from the laboratory industrial application and daily life, to one of also current the most popular scientific research forward position of the development of nano material and nano-device, and porous alumina has also obtained domestic many investigators' the concern that is as the first-selected template of preparation nano wire, nanometer rod, nano-wire array.
But common alumina formwork is substrate with aluminium or is stripped down from substrate, it is because the restriction of material itself, intensity is not high very easily broken, when particularly being applied to such as optics, photoelectricity, sun power, optical waveguide sensor, photoluminescence field, adhere in other substrates after porous alumina layer need being peeled off, this has not only increased the weight of process complexity, and combines bad with substrate or tackiness agent is selected can introduce other problems again when incorrect at film.In order to obtain the higher rete of the hole degree of order, also can adopt the glass that has been coated with transparent conductive film as substrate, be coated with aluminium on this basis and then adopt anonizing to prepare porous alumina layer, this has solved this problem to a certain extent, but the transmissivity of transparent conductive film layer itself is on the low side, has also limited the raising of its entire device optical property.Also have with semiconductor monocrystal or the polycrystalline silicon material method as template, this method need not be coated with nesa coating, but the base material cost is higher, is unfavorable for the reduction of industrial application and cost.Being coated with the aluminium film on base material more is to adopt magnetron sputtering method, this method helps preparing the big area aluminum membranous layer, but its homogeneity and thickness are wayward, accurately controls the Application Areas of porous alumina film thickness at needs, application as optical field just is restricted.
Bibliographical information is abroad arranged, and is template with the glass-based porous aluminum oxide, prepares OLED (Organic Light Emitting Diode) display device, can improve the light extraction efficiency of indicating meter, the life-span that can improve device to a certain extent; Glass-based porous aluminum oxide is a substrate, the preparation optical waveguide sensor, and the sensitivity that can improve transmitter reduces cost.
Summary of the invention
Technical problem to be solved by this invention is: provide a kind of preparation to have the method for the glass-based porous aluminum oxide substrate that high-sequential, transmissivity height, physical strength height, pore dimension can accurately control.
The technical solution adopted in the present invention is: substrate of glass is through after the clean, adopt thermal evaporation to be coated with high-purity aluminium lamination, high temperature annealing improves the crystallinity of rete, adopt anonizing to prepare porous alumina, the thickness of hole size and rete is is further optimized and revised in the process reaming, adopts high-temperature heat treatment to improve the transmissivity of rete at last.
The preparation method of described glass-based porous aluminum oxide substrate: after the glass substrate clean, vacuum thermal evaporation (resistance, electron beam) method deposits the rafifinal film on glass substrate; The said sample high temperature annealing is improved the crystal property of aluminium film; Adopt the two-step anodization method, utilize the self-assembly principle to generate multiaperture pellumina; Adopt chambering process, control reaming time and temperature are further optimized porous alumina layer aperture and thickness; Unnecessary metallic aluminium in the anneal, oxidation removal rete improves transmissivity.
Advantage of the present invention: with glass is substrate, the physical strength height, and drawing materials makes things convenient for cost low.Thermal evaporation AM aluminum metallization film, thickness and membrane uniformity are precisely controlled.The multiaperture pellumina degree of order height that two-step anodization obtains, transmissivity is good, and hole density, aperture, wall thickness are controlled, can obtain the rete of various specific surface areas.
Glass-based porous aluminum oxide substrate of the present invention, transmission of visible light can reach 75%, and the porous alumina layer thickness can be in nanometer to micron level, and controllable aperture is in 18～47nm scope.
Description of drawings
Fig. 1 is preparation technology's schema of glass-based porous aluminum oxide substrate of the present invention.
Fig. 2 is the cross section scanning electron microscope diagram sheet of glass-based porous aluminum oxide substrate of the present invention.
Fig. 3 is the surface scan electron microscope picture of glass-based porous aluminum oxide substrate of the present invention.
Fig. 4 is the transmittance graph of glass-based porous aluminum oxide substrate in the embodiments of the invention.
Embodiment
The present invention has mainly utilized the self-assembly performance of porous alumina, generates the porous alumina rete of high-sequential at glass basic surface.Because substrate is a glass, strengthened the physical strength of whole sample, keep transmissivity to a certain extent, and do not introduce other complicated technology, can be used as the substrate of devices such as other optics, photoelectricity, biochip, perhaps prepare the template of low-dimension nano materials such as nano wire, nanometer rod, nano-dot matrix.For removing metallic aluminium unnecessary in the rete, adopt high-temperature heat treatment, can guarantee the purity of the pellumina that generates, if then can introduce other impurity, can have influence on the follow-up performance of device with other chemical reactions (as replacing) with HgCl.
The preparation method of high transmission glass-based porous aluminum oxide substrate is: be substrate with glass earlier, adopt the vacuum thermal evaporation legal system to be equipped with the rafifinal film; Adopt once then or two-step anodization method generation porous alumina layer; Then adopt chambering process to optimize the aperture of porous alumina layer; Adopt The high temperature anneal at last, improve the transmissivity of whole glass-based porous aluminum oxide substrate.
The preparation method specifically comprises following steps:
1) the vacuum thermal evaporation legal system is equipped with the rafifinal film:
By vacuum resistance heating or electron beam heating heating rafifinal material, the controlled rafifinal film of deposit thickness on glass substrate;
2) step 1) gained glass-based aluminium film is carried out high-temperature heat treatment:
Be heated to 480 ℃ with stove, be incubated 1h then, furnace cooling again improves the crystallinity of rete;
3) to step 2) gained glass-based aluminium film carries out anodic oxidation:
To the rafifinal film of vacuum resistance evaporation preparation, it is transparent to sample to carry out an anodic oxidation, directly carries out reaming then and handles; To the rafifinal film of electron beam evaporation preparation, after carrying out an anodic oxidation, remove once anodised oxide film, under the once oxidation same process, carry out two-step anodization, transparent until sample;
Finish after the processing in this step, forming the surface is the transparent porous anodic aluminium oxide substrate of compact aluminum oxide for porous alumina, bottom;
4) glass-based porous aluminum oxide substrate after step 3) is handled carries out high-temperature heat treatment:
Be heated to 480 ℃ with stove, insulation 1h, furnace cooling to reduce the template internal stress, improves the crystallinity of rete and the transmissivity of substrate again;
Step 1) vacuum thermal evaporation legal system is equipped with the rafifinal film and specifically may further comprise the steps:
11) pre-treatment of rafifinal material:
Employing purity is 99.999% aluminium material, cleans roughly with deionized water, dehydrated alcohol; Be placed on then in the NaOH solution of 0.2mol/L and soak 5min, remove the natural oxide film on aluminium flake surface;
12) deposition of rafifinal film:
When adopting the vacuum resistance heating method, pretreated rafifinal material is placed on fritting in the conductivity ceramics boat, when adopting electron beam heating, then pretreated rafifinal material is placed on fritting in the plumbago crucible; Then the glass substrate that cleans up is placed on the substrate frame in the vacuum chamber, by the rafifinal film of crystal oscillator instrument control preparation different thickness.
Step 2) glass-based aluminium film carries out high-temperature heat treatment and specifically may further comprise the steps:
Be warming up to 480 ℃ with stove, be incubated 1h then, cool to room temperature again with the furnace,, can improve the order in follow-up porous alumina rete hole to improve the crystal property of aluminium lamination.
Step 3) electron beam evaporation preparation the anodic oxidation of rafifinal film specifically may further comprise the steps:
31) anodic oxidation:
Will be before the oxidation in step 2) the glass-based aluminium film handled the sodium hydroxide solution of putting into 0.2mol/l handles 5min, again analytically pure oxalic acid and deionized water are mixed with the oxalic acid solution of 0.3mol/l, as anodised electrolytic solution once, anode is a step 2) the glass-based aluminium film handled, negative electrode is the common aluminium flake that cleans up, anode and negative electrode are fixed on the oxidation support, distance between electrodes is 7cm, adopt constant voltage current stabilization pattern, oxidization time 10min, oxalic acid electrolytic solution oxidation voltage is 15～30V, adopt water-bath during the oxidizing reaction, the temperature in the reactive tank is controlled in 0 ℃ to 10 ℃ the interval range, after oxidization time reaches, take out sample this moment, cleans up with deionized water;
32) remove the once oxidation film:
With analytically pure phosphoric acid and chromic acid and deionized water, be mixed with the phosphoric acid solution of 6wt% and the chromic acid solution of 1.8wt% respectively, two kinds of solution are mixed, mixing solutions is heated to 80 ℃ then, immersion 10 or 15min at last are placed in one the sample after the once oxidation;
33) two-step anodization:
The parameter of two-step anodization is identical with anodised each parameter of the first step, and is transparent until sample during oxidation, cleans up with deionized water.
34) analytical pure phosphoric acid and deionized water are mixed with the phosphoric acid solution of 0.5mol/l, make reaming and handle the solution of usefulness, with step 33) the gained glass-based porous aluminum oxide substrate is immersed in the reaming solution, carry out reaming processing 20 or 60min, time reaches the back and takes out sample, cleans up with deionized water.
Anodic oxidation to the rafifinal film of vacuum resistance evaporation preparation only comprises above-mentioned steps 31) and 34), step 31 wherein) oxidizing reaction transparent until sample, step 34) the reaming treatment time be 100 or 120min.
Step 4) glass-based porous aluminum oxide template high-temperature heat treatment specifically comprises:
Be warming up to 480 ℃ with stove, be incubated 1 hour then, cool to room temperature with the furnace, aluminum oxide rete and film/remaining metallic aluminium in basic interface are oxidized to aluminum oxide.
Prepare high transmission glass-based porous aluminum oxide substrate of the present invention as stated above.
Be described further below in conjunction with the present invention, but do not limit the present invention form with embodiment.The present invention has promptly kept the ordered porous property and the structural controllability thereof of aluminum oxide in conjunction with physical vapor deposition and two kinds of technologies of anodic oxidation, chooses glass again and makees substrate, has strengthened its physical strength, and higher transmissivity is arranged simultaneously, has widened its potential Application Areas.
Embodiment 1: technical scheme
1) employing purity is 99.999% aluminium material, cleans roughly with deionized water, dehydrated alcohol; Be placed on then in the NaOH solution of 0.2mol/L and soak 5min, remove the natural oxide film on aluminium flake surface;
2) adopt the vacuum resistance heating method, pretreated rafifinal material is placed on fritting in the conductivity ceramics boat, then the glass substrate that cleans up is placed on the substrate frame in the vacuum chamber, by the rafifinal film of crystal oscillator instrument control preparation different thickness.
3) with the sample after the resistance evaporation, be warming up to 480 ℃ with stove, be incubated 1h then, cool to room temperature again with the furnace;
4) will handle 5min at the sodium hydroxide solution that the glass-based aluminium film that step 3) has been handled is put into 0.2mol/l before the oxidation, again analytically pure oxalic acid and deionized water are mixed with the oxalic acid solution of 0.3mol/l, as anodised electrolytic solution once, anode is the glass-based aluminium film that step 3) had been handled, negative electrode is the common aluminium flake that cleans up, anode and negative electrode are fixed on the oxidation support, distance between electrodes is 7cm, adopt constant voltage current stabilization pattern, oxidation voltage is 15V, adopts water-bath, oxidizing reaction temperature to be controlled in 0 ℃ to 10 ℃ the interval range during the oxidizing reaction, sample is taken out in the transparent back of sample, cleans up with deionized water;
5) analytical pure phosphoric acid and deionized water are mixed with the phosphoric acid solution of 0.5mol/l, make reaming and handle the solution of usefulness, step 4) gained glass-based porous aluminum oxide substrate is immersed in the reaming solution, handle 100min 14 ℃ of UR, time reaches the back and takes out sample, cleans up with deionized water;
6) be warming up to 480 ℃ with stove, be incubated 1 hour then, cool to room temperature again with the furnace, aluminum oxide rete and film/remaining metallic aluminium in basic interface are oxidized to aluminum oxide.
The microtexture and the transmission performance of the glass-based porous aluminum oxide substrate of embodiment 1 preparation:
The about 37nm of mean pore size; As shown in Figure 4, the visible light wave range transmissivity is greater than 60%, and maximum can reach 70%.
Embodiment 2: technical scheme
The step 5) reaming treatment time is 120min, and all the other are with embodiment 1.
The transmissivity of the glass-based porous aluminum oxide substrate of embodiment 2 preparations:
The about 47nm of mean pore size; As shown in Figure 4, the visible light wave range transmissivity is greater than 60%, and maximum can reach 70%.
Embodiment 3: technical scheme
1) employing purity is 99.999% aluminium material, cleans roughly with deionized water, dehydrated alcohol; Be placed on then in the NaOH solution of 0.2mol/L and soak 5min, remove the natural oxide film on aluminium flake surface;
2) adopt electron beam heating, pretreated rafifinal material is placed on fritting in the plumbago crucible, then the glass substrate that cleans up is placed on the substrate frame in the vacuum chamber, by the rafifinal film (this example evaporation time is 40s) of crystal oscillator instrument control preparation different thickness.
3) with the sample behind the electron beam evaporation plating, be warming up to 480 ℃ with stove, be incubated 1h then, cool to room temperature again with the furnace;
4) will be before the oxidation in step 2) the glass-based aluminium film handled the sodium hydroxide solution of putting into 0.2mol/l handles 5min, again analytically pure oxalic acid and deionized water are mixed with the oxalic acid solution of 0.3mol/l, as anodised electrolytic solution once, anode is the glass-based aluminium film that step 3) had been handled, negative electrode is the common aluminium flake that cleans up, anode and negative electrode are fixed on the oxidation support, distance between electrodes is 7cm, adopt constant voltage current stabilization pattern, oxidation voltage is 30V, adopts water-bath, oxidizing reaction temperature to be controlled in 0 ℃ to 10 ℃ the interval range during the oxidizing reaction, oxidization time 10min takes out sample and cleans up with deionized water;
5) with analytically pure phosphoric acid and chromic acid and deionized water, be mixed with the phosphoric acid solution of 6wt% and the chromic acid solution of 1.8wt% respectively, two kinds of solution are mixed, mixing solutions is heated to 80 ℃ then, the sample after the once oxidation is placed in one soaks 15min at last;
6) two-step anodization: the parameter of two-step anodization is identical with anodised each parameter of the first step, and oxidization time is adjusted according to actual needs, and sample is taken out in the transparent back of oxidised samples, cleans up with deionized water;
7) analytical pure phosphoric acid and deionized water are mixed with the phosphoric acid solution of 0.5mol/l, make reaming and handle the solution of usefulness, step 6) gained glass-based porous aluminum oxide substrate is immersed in the reaming solution, 20min is handled in reaming at room temperature, time reaches the back and takes out sample, cleans up with deionized water;
8) be warming up to 480 ℃ with stove, be incubated 1 hour then, cool to room temperature again with the furnace, aluminum oxide rete and film/remaining metallic aluminium in basic interface are oxidized to aluminum oxide.
The transmissivity of the glass-based porous aluminum oxide substrate of embodiment 3 preparations:
The about 40nm of mean pore size; As shown in Figure 4, see the optical band transmissivity greater than 65%, maximum can reach 74%.
Embodiment 4: technical scheme
Step 2) time of electron beam evaporation plating is 60s; The oxidation voltage of step 4) is 20V, and oxidizing reaction temperature is controlled in 0 ℃ to 10 ℃ the interval range; All the other are with embodiment 3.
The transmissivity of the glass-based porous aluminum oxide substrate of embodiment 4 preparations:
The about 24nm of mean pore size; As shown in Figure 4, the visible light wave range transmissivity is greater than 65%, and maximum can reach 73%.
Embodiment 5: technical scheme
Step 2) time of electron beam evaporation plating is 20s; The oxidation voltage of step 4) is 20V, and oxidizing reaction temperature is controlled in 3 ℃ to 10 ℃ the interval range; The soak time of step 5) is 10min; All the other are with embodiment 3.
The transmissivity of the glass-based porous aluminum oxide substrate of embodiment 5 preparations:
The about 23nm of mean pore size; As shown in Figure 4, the visible light wave range transmissivity is greater than 65%, and maximum can reach 75%.
Embodiment 6: technical scheme
Step 2) time of electron beam evaporation plating is 20s; The oxidation voltage of step 4) is 15V; The soak time of step 5) is 10min; The reaming treatment time of step 7) is 60min; All the other are with embodiment 3.
The transmissivity of the glass-based porous aluminum oxide substrate of embodiment 6 preparations:
The about 18nm of mean pore size; As shown in Figure 4, the visible light wave range transmissivity is greater than 67%, and maximum can reach 72%.
Claims (6)
1. the preparation method of high transmission glass-based porous aluminum oxide substrate is characterized in that: be substrate with glass earlier, adopt the vacuum thermal evaporation legal system to be equipped with the rafifinal film; Adopt once then or two-step anodization method generation porous alumina layer; Then adopt chambering process to optimize the aperture of porous alumina layer; Adopt The high temperature anneal at last, improve the transmissivity of whole glass-based porous aluminum oxide substrate.
2. glass-based porous aluminum oxide substrate preparation method according to claim 1 is characterized in that specifically may further comprise the steps:
1) the vacuum thermal evaporation legal system is equipped with the rafifinal film:
By vacuum resistance heating or electron beam heating heating rafifinal material, deposition rafifinal film on glass substrate;
2) step 1) gained glass-based aluminium film is carried out high-temperature heat treatment:
Earlier be heated to 480 ℃ with stove, insulation then, furnace cooling again improves the crystallinity of rete;
3) to step 2) gained glass-based aluminium film carries out anodic oxidation:
Rafifinal film to vacuum resistance evaporation preparation carries out an anodic oxidation, directly carries out reaming then and handles; To the rafifinal film of electron beam evaporation preparation, after carrying out an anodic oxidation, remove once anodised oxide film, under the once oxidation same process, carry out two-step anodization, transparent until sample;
Finish after the processing in this step, forming the surface is the transparent porous anodic aluminium oxide substrate of compact aluminum oxide for porous alumina, bottom;
4) glass-based porous aluminum oxide substrate after the step 3) processing is carried out high-temperature heat treatment:
Be heated to 480 ℃ with stove, be incubated 1 hour, furnace cooling reduces template internal stress and the transmissivity that improves template again;
3. preparation method according to claim 2 is characterized in that step 1) vacuum thermal evaporation legal system is equipped with the rafifinal film and specifically may further comprise the steps:
11) pre-treatment of rafifinal material:
Employing purity is 99.999% aluminium material, cleans roughly with deionized water, dehydrated alcohol; Be placed on then in the NaOH solution of 0.2mol/L and soak 5min, remove the natural oxide film on aluminium flake surface;
12) deposition of rafifinal film:
When adopting the vacuum resistance heating method, pretreated rafifinal material is placed on fritting in the conductivity ceramics boat; When adopting electron beam heating, then pretreated rafifinal material is placed on fritting in the plumbago crucible; Then the glass substrate that cleans up is placed on the substrate frame in the vacuum chamber, by the rafifinal film of crystal oscillator instrument control preparation different thickness.
4. preparation method according to claim 2 is characterized in that step 2) glass-based aluminium film carries out high-temperature heat treatment and specifically comprises: is warming up to 480 ℃ with stove, is incubated 1 hour then, cool to room temperature again with the furnace, improve the crystal property of aluminium lamination.
5. preparation method according to claim 2 is characterized in that step 3) specifically may further comprise the steps the rafifinal film anodic oxidation of electron beam evaporation preparation:
31) anodic oxidation:
Will be before the oxidation in step 2) the glass-based aluminium film handled the sodium hydroxide solution of putting into 0.2mol/l handles 5min, again analytically pure oxalic acid and deionized water are mixed with the oxalic acid solution of 0.3mol/l, as anodised electrolytic solution once, anode is a step 2) the glass-based aluminium film handled, negative electrode is the common aluminium flake that cleans up, anode and negative electrode are fixed on the oxidation support, distance between electrodes is 7cm, adopt constant voltage current stabilization pattern, oxidation voltage is 15～30V, adopt water-bath during the oxidizing reaction, oxidizing reaction temperature is controlled in 0 ℃ to 10 ℃ the interval range, cleans up with deionized water after the oxidizing reaction 10min;
32) remove the once oxidation film:
With analytically pure phosphoric acid and chromic acid and deionized water, be mixed with the phosphoric acid solution of 6wt% and the chromic acid solution of 1.8wt% respectively, two kinds of solution are mixed, mixing solutions is heated to 80 ℃ then, immersion 10 or 15min at last are placed in one the sample after the once oxidation;
33) two-step anodization:
The parameter of two-step anodization is identical with anodised each parameter of the first step, and sample is taken out in the transparent back of secondary oxidation sample, cleans up with deionized water;
34) analytical pure phosphoric acid and deionized water are mixed with the phosphoric acid solution of 0.5mol/l, make reaming and handle the solution of usefulness, with step 33) the gained glass-based porous aluminum oxide substrate is immersed in the reaming solution, carry out reaming processing 20 or 60min, time reaches the back and takes out sample, cleans up with deionized water;
Anodic oxidation to the rafifinal film of vacuum resistance evaporation preparation only comprises above-mentioned steps 31) and 34), step 31 wherein) react transparent, step 34 to sample) the reaming treatment time be 100 or 120min.
6. preparation method according to claim 2 is characterized in that the high-temperature heat treatment of step 4) glass-based porous aluminum oxide template specifically comprises:
Be warming up to 480 ℃ with stove, be incubated 1 hour then, cool to room temperature again with the furnace, aluminum oxide rete and film/remaining metallic aluminium in basic interface are oxidized to aluminum oxide.
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| CN102183629A (en) * | 2011-03-11 | 2011-09-14 | 中国科学院半导体研究所 | Manufacturing method of porous anodised aluminum oxide biochip |
| CN103668381A (en) * | 2012-09-04 | 2014-03-26 | 中国科学院宁波材料技术与工程研究所 | Method for preparing in-situ porous aluminum oxide membrane on insulated substrate |
| CN104846336A (en) * | 2015-03-20 | 2015-08-19 | 哈尔滨工业大学深圳研究生院 | Anti-reflective micro-nano structure of sapphire surface and preparation method thereof |
| CN108251877A (en) * | 2016-12-29 | 2018-07-06 | 北京有色金属研究总院 | A kind of Woelm Alumina film layer and preparation method thereof |
| CN109536885A (en) * | 2018-12-27 | 2019-03-29 | 广州海鸥住宅工业股份有限公司 | A kind of method of electron beam evaporation titanizing |
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| CN104846336B (en) * | 2015-03-20 | 2017-05-24 | 哈尔滨工业大学深圳研究生院 | Anti-reflective micro-nano structure of sapphire surface and preparation method thereof |
| CN108251877A (en) * | 2016-12-29 | 2018-07-06 | 北京有色金属研究总院 | A kind of Woelm Alumina film layer and preparation method thereof |
| CN109536885A (en) * | 2018-12-27 | 2019-03-29 | 广州海鸥住宅工业股份有限公司 | A kind of method of electron beam evaporation titanizing |
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Application publication date: 20101117 |