CN102173820B - Preparation method of YBa2Cu3O7-x(YBCO) high-temperature superconductive thick film - Google Patents
Preparation method of YBa2Cu3O7-x(YBCO) high-temperature superconductive thick film Download PDFInfo
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Abstract
The invention a preparation method of a YBa2Cu3O7-x(YBCO) high-temperature superconductive thick film. The preparation method comprises the following steps of: preparing precursor liquid; mixing yttrium acetate [Y(CH3COO)3], barium acetate [Ba(CH3COO)2] and copper acetate [Cu(CH3COO)2] according to the molar ratio of Y to Ba to Cu of 1:2:3; dissolving the mixture into aqueous solution of 10 to 30 molar percent trifluoroacetic acid; stirring uniformly and drying the solvent by evaporation under vacuum to obtain gel; adding methanol and stirring uniformly; drying the solvent by evaporation to obtain gel; adding a proper amount of methanol and terpineol to prepare solution, wherein the total concentration of three kinds of metal ions of Y, Ba and Cu is 1.5 to 3.0 mol/L; stirring the solution uniformly; adding titanium acetylacetonate in an amount which is 5 to 10 percent of the total molar concentration of the three kinds of metal ions to prepare precursor liquid; coating the precursor liquid on a substrate; perform low-temperature thermal treatment on the substrate coated with the precursor liquid at the temperature of between 300 and 500 DEG C to decompose trifluoroacetic acid salt; and performing high-temperature thermal treatment at the temperature of between 750 and 850 DEG C and annealing at the temperature of between 450 and 550 DEG C to form a nano titanium oxide-containing YBCO thick film. The critical current of the prepared YBCO thick film reaches 1,000 A/cm.
Description
Technical field
The present invention relates to the preparation method of superconducting layer in a kind of s-generation belt material of high temperature superconduct, particularly prepare the method for individual layer yttrium barium copper oxide high temperature superconductive thick film.
Background technology
S-generation belt material of high temperature superconduct refers to the rare earth class barium-copper oxide superconducting coating conductor based on the YBCO-123 series superconducting material.It is made of metal alloy base band, Seed Layer, blocking layer, cap layer, rare earth barium copper oxide superconducting layer, protective layer and stabilizing layer etc., is a kind of multilayered structure.Compare with first-generation Bi based high-temperature superconductive strip, s-generation belt material of high temperature superconduct has the ability of the high electric current of load under the upfield, can under higher temperature and magnetic field, use, and be the focus that various countries competitively research and develop in the high-temperature superconductor field.
At present, have at least 7 tame units all to prepare length in the world and surpass 100m, Ic surpasses the band of 150A.Especially the Superpower company of the U.S., it has been prepared and has reached 1311m, and Ic reaches the long band of km level of 153A, has stepped major step to batch process.But the cost for preparing the YBCO band now remains 50 times of copper cash, and the performance that must further improve the YBCO coating conductor could satisfy requirement widely.
YBCO as coating conductor can use in the forceful electric power field mainly be since it have can load current and the characteristic of not loss.Concerning the YBCO coating conductor with identical critical current density (Jc), the thickness that increases it has also just also just improved its current capacity.Therefore the current capacity that improves thick film is research focus in recent years.United States Air Force laboratory T.Haugan research group has reported pulsed laser deposition (PLD) method at Nature, and this method adopts two different target alternating deposit ybco films and non-superconducting Y mutually
2BaCuO
5(211)." 211 " nanoparticle size of deposition is 0.5~1.5nm, and density is 5~6 * 10
11/ cm
2These highdensity point defects have played the effect of flux pinning, make the 2-3MA/cm of critical current density by pure ybco film
2Bring up to 4MA/cm
2More than.They have finally prepared high performance YBCO coating by the mode with the multilayer film stack, have improved its current capacity.Although the United States Air Force laboratory adopts the PLD method to prepare the YBCO thick film by the mode of multilayer stack, but the pulsed laser deposition that this method adopts needs expensive vacuum system, sedimentation rate is lower, and the mode of this method employing multilayer film stack, and technology more complicated, cost are very high.The preparation method that the present domestic patent overwhelming majority about the YBCO superconducting film is ybco film.Have only Chinese patent CN 101719399A to mention the preparation of thick film in (open day on June 2nd, 2010 of application).This patent adopts chemical solution method to replace trifluoroacetic acid copper with vinylformic acid copper, and adding ethylene glycol amine in precursor liquid, to have prepared thickness be 1 micron YBCO thick film.Although this patent has prepared the YBCO thick film, thickness only is 1 micron, and is limited to the current capacity that improves the YBCO coating.The more important thing is for two most important index critical currents estimating superconducting material and critical current density in this patent, all not relate to, can't estimate its superconductivity.
Summary of the invention
The objective of the invention is to overcome the more weak shortcoming of YBCO superconducting thin film current capacity of prior art for preparing, a kind of preparation method with individual layer YBCO thick film of high current carrying capacity is provided.
The present invention is equipped with individual layer YBCO thick film by adopting trifluoroacetate-metal organic deposit (TFA-MOD) legal system, and the concrete steps order is as follows:
(1) according to Y: Ba: Cu=1: 2: 3 mol ratio is yttium acetate Y (CH
3COO)
3, barium acetate Ba (CH
3COO)
2With venus crystals Cu (CH
3COO)
2Mix, be dissolved in wiring solution-forming in the deionized water of the trifluoroacetic acid that contains 10-30mol% under room temperature, wherein the mol ratio of solute and solvent is 1: 100;
(2) solution that above-mentioned steps (1) is prepared adopted Rotary Evaporators to steam to desolventize again and obtains gel through magnetic stirrer 1-3 hour;
(3) gel that above-mentioned steps (2) is made adds in the methyl alcohol, gel in this step and the mol ratio of methyl alcohol are 1: 50, after magnetic stirrer 0.5-1.5 hour, adopt Rotary Evaporators to steam again and desolventize, with impurity such as further removal moisture, obtain very pure gel;
(4) gel that above-mentioned steps (3) is made joins in methyl alcohol and the Terpineol 350, the solution that to make three kinds of metal total ion concentrations of Y, Ba and Cu be 1.5-3.0mol/L, methyl alcohol in this step and the volume ratio of Terpineol 350 are 1: 1, the solution stirring that will contain described Y, Ba and Cu is even, add titanium acetylacetone again, the titanium acetylacetone that adds is the 5%-10% of described Y, Ba and three kinds of total ion volumetric molar concentrations of metal of Cu, is prepared into precursor liquid;
(5) the described precursor liquid that step (4) is made is coated on the substrate.Coating method can be spin coating (spin-coating) or lift (dipping) method, and described substrate can be that monocrystalline oxides such as lanthanum aluminate, strontium titanate or magnesium oxide single-crystal substrate or other are suitable for preparing the substrate of high-temperature superconducting thin film;
(6) substrate is placed the quartzy stove of high-temperature tubular, under 300 ℃~500 ℃ temperature, carry out 10 hours low-temperature heat treatment, decompose trifluoroacetate; The temperature rise rate of this step is 40 ℃/h; This step is in the mixed atmosphere of oxygen and water vapour, and the pressure of water vapour is to carry out under the condition of 100hPa-160hPa;
(7) will place under 750 ℃~850 ℃ the high temperature thermal treatment through the substrate that step (6) is handled 2~4 hours, generate the cubic phase YBCO film that contains nano-titanium oxide; The heat-up rate of this step can be 400 ℃/h; This step is in the atmosphere of moistening oxygen and argon gas, at the pressure of water vapour is to carry out under the condition of 160hPa-240hPa;
(8) will place through the substrate that step (7) is handled under 450 ℃~550 ℃ and the pure oxygen condition the film thermal treatment 0.5~1.5 hour of annealing, and be prepared into and contain nanometer Ti
2O
5YBCO high-temperature superconductor single layer thick film.
Compared with prior art, the present invention has following beneficial effect:
The present invention adds Terpineol 350 and titanium acetylacetone in traditional precursor liquid yttium acetate, barium acetate and venus crystals, by the concentration of control metal ion, after through low temperature thermal decomposition and high temperature sintering, prepared and contained nano-scale Ti
2O
5The YBCO superconducting thick-film.These have the Ti of nano-scale
2O
5And Ti
2O
5And the defective that forms between the YBCO film has well played the effect of flux pinning, has improved the critical current density of YBCO film.And the interpolation of Terpineol 350 can guarantee that the YBCO thick film for preparing does not ftracture, and can only apply a film and just can prepare the YBCO film that thickness reaches 2 μ m.The YBCO thick film critical current density J of preparation
CReach 5MA/cm
2, critical current arrives 1000A/cm, has improved the current capacity of YBCO thick film greatly, has reduced the production cost of coating conductor, has widened the range of application of YBCO coating conductor.
Description of drawings
Fig. 1 is the critical current density test picture of the YBCO film of embodiment 1 preparation;
Fig. 2 is the scanning electron microscope diagram sheet of the YBCO film of embodiment 1 preparation;
Fig. 3 is the critical current density test picture of the YBCO film of embodiment 2 preparations;
Fig. 4 is the scanning electron microscope diagram sheet of the YBCO film of embodiment 2 preparations;
Fig. 5 is the critical current density test picture of the YBCO film of embodiment 3 preparations;
Fig. 6 is the scanning electronic microscope mirror picture of the YBCO film of embodiment 3 preparations;
Fig. 7 a, Fig. 7 b are the X ray diffracting spectrums of the YBCO film of embodiment 3 preparations.
The specific embodiment mode
Embodiment 1
(1) takes by weighing yttium acetate, barium acetate and venus crystals and be respectively 0.005mol, 0.01mol and 0.015mol, be dissolved in wiring solution-forming in the 100ml deionized water of the trifluoroacetic acid that contains 10mol% after yttium acetate, barium acetate and venus crystals are mixed;
(2) solution that step (1) is made, adopts Rotary Evaporators to steam to desolventize again and obtains gel after 1 hour through magnetic stirrer;
(3) described gel is added 50ml methyl alcohol, adopt Rotary Evaporators to steam after 0.5 hour again to desolventize with impurity such as further removal moisture through magnetic stirrer again to obtain very pure gel;
(4) gel that step (4) is made joins in the mixed solution of 10ml methyl alcohol and 10ml Terpineol 350, and the volume ratio of described methyl alcohol and Terpineol 350 is 1: 1, the solution that to make three kinds of metal total ion concentrations of Y, Ba and Cu be 1.5mol/L.The methyl alcohol that contains Y, Ba and Cu and the terpineol solution of gained are stirred, add titanium acetylacetone again, the titanium acetylacetone that adds be in the described Y of containing, Ba and three kinds of metallic solutions of Cu Y, Ba and three kinds of total ion volumetric molar concentrations of metal of Cu 5%, be prepared into precursor liquid;
(5) precursor liquid that step (4) is made is spin-coated on the lanthanuma luminate single crystal substrate with 1500 rev/mins speed, and the spin coating time is 90 seconds;
(6) the coated substrate of step (5) that coating is good is placed on to send in the quartz boat in the quartzy stove of high-temperature tubular and carries out low-temperature heat treatment and high-temperature heat treatment, obtains containing nanometer Ti at last
2O
5YBCO high-temperature superconductor single layer thick film.
Low-temperature heat treatment is to carry out under the moistening oxygen condition, be through the vial that distilled water is housed water vapour to be brought the oxygen of 500sccm into reaction chamber, make that water vapour pressure is 100hPa in the reaction chamber, on average be warming up to 300 ℃ with the temperature rise rate of 40 ℃/h from room temperature, and then stove is chilled to room temperature.The purpose of low-temperature heat treatment is to decompose trifluoroacetate, forms unformed precursor film and discharges harmful residual substance.The whole resolving time is about 10h.
High-temperature heat treatment is to carry out under moistening oxygen and argon gas mixed atmosphere, the argon gas mixed gas that 500sccm is contained 500ppm oxygen is brought water vapour into reaction chamber through the vial that distilled water is housed, make that water vapour pressure is 160hPa in the reaction chamber, temperature rise rate with 400 ℃/h rose to 750 ℃ of the highest temperatures before this, directly feed the argon gas mixed gas that contains 500ppm oxygen after 2 hours 750 ℃ of insulations, be cooled to 450 ℃ with 100 ℃/h then, insulation made the YBCO oxygen uptake of cubic phase change the YBCO with superconductivity of quadrature phase in 0.5 hour in 450 ℃ purity oxygen atmosphere, and sample stove under the oxygen atmosphere is chilled to room temperature subsequently.With Lepi-system the YBCO thick film that prepared one-tenth contains nano-titanium oxide has been carried out the test of critical current density, the critical current maximum reaches 880A/cm, as shown in Figure 1.With field emission scanning electron microscope sample has been carried out the surface topography observation, the YBCO thick film surface is smooth, fine and close, as shown in Figure 2.
Embodiment 2
(1) takes by weighing yttium acetate, barium acetate and venus crystals and be respectively 0.01mol, 0.02mol and 0.03mol, be dissolved in wiring solution-forming in the 200ml deionized water of the trifluoroacetic acid that contains 20mol% after yttium acetate, barium acetate and venus crystals are mixed;
(2) the described solution that step (1) is made, adopts Rotary Evaporators to steam to desolventize again and obtains gel after 2 hours through magnetic stirrer;
(3) gel that step (2) made adds 50ml methyl alcohol, adopts Rotary Evaporators to steam after 1 hour again to desolventize with impurity such as further removal moisture through magnetic stirrer again to obtain very pure gel;
(4) gel that step (3) is made joins in the mixed solution of 15ml methyl alcohol and 15ml Terpineol 350, and the volume ratio of described methyl alcohol and Terpineol 350 is 1: 1, the solution that to make three kinds of metal total ion concentrations of Y, Ba and Cu be 2.0mol/L.The methyl alcohol that contains Y, Ba and Cu and the terpineol solution of gained are stirred, add titanium acetylacetone again, the titanium acetylacetone that adds be in the methyl alcohol of the described Y of containing, Ba and Cu and the terpineol solution Y, Ba and three kinds of total ion volumetric molar concentrations of metal of Cu 7.5%, be prepared into precursor liquid;
(5) precursor liquid that step (4) is made is spin-coated on the lanthanuma luminate single crystal substrate with 1500 rev/mins speed, and the spin coating time is 90 seconds;
(6) substrate that coating is good is placed on to send in the quartz boat in the quartzy stove of tubular type and carries out low-temperature heat treatment and high-temperature heat treatment, obtains containing nanometer Ti at last
2O
5YBCO high-temperature superconductor single layer thick film.
Low-temperature heat treatment is to carry out under the moistening oxygen condition, be through the vial that distilled water is housed water vapour to be brought the oxygen of 500sccm into reaction chamber, make that water vapour pressure is 130hPa in the reaction chamber, on average be warming up to 400 ℃ with the temperature rise rate of 40 ℃/h from room temperature, and then stove is chilled to room temperature.The purpose of low-temperature heat treatment is to decompose trifluoroacetate, forms unformed precursor film and discharges harmful residual substance.The whole resolving time is about 10 hours.
High-temperature heat treatment is to carry out under moistening oxygen and argon gas mixed atmosphere, the argon gas mixed gas that 500sccm is contained 500ppm oxygen is brought water vapour into reaction chamber through the vial that distilled water is housed, make that water vapour pressure is 200hPa in the reaction chamber, temperature rise rate with 400 ℃/h rose to 800 ℃ of the highest temperatures before this, directly feed the argon gas mixed gas that contains 500ppm oxygen after 3 hours 800 ℃ of insulations, be cooled to 500 ℃ with 100 ℃/h then, insulation made the YBCO oxygen uptake of cubic phase change the YBCO with superconductivity of quadrature phase in 1 hour in 500 ℃ purity oxygen atmosphere, and sample stove under the oxygen atmosphere is chilled to room temperature subsequently.With Lepi-system the YBCO thick film that prepared one-tenth contains nano-titanium oxide has been carried out the test of critical current density, the critical current maximum reaches 880A/cm, as shown in Figure 3.With field emission scanning electron microscope sample has been carried out the surface topography observation, the YBCO thick film surface is smooth, fine and close, as shown in Figure 4.
(1) takes by weighing yttium acetate, barium acetate and venus crystals and be respectively 0.015mol, 0.03mol and 0.045mol, be dissolved in wiring solution-forming in the 300ml deionized water of the trifluoroacetic acid that contains 30mol% after yttium acetate, barium acetate and venus crystals are mixed;
(2) solution that step (1) is made, adopts Rotary Evaporators to steam to desolventize again and obtains gel after 3 hours through magnetic stirrer;
(3) gel that step (2) made adds 50ml methyl alcohol, adopts Rotary Evaporators to steam after 1.5 hours again to desolventize with impurity such as further removal moisture through magnetic stirrer again to obtain very pure gel;
(4) gel that step (3) is made joins in the mixed solution of 15ml methyl alcohol and 15ml Terpineol 350, and the volume ratio of described methyl alcohol and Terpineol 350 is 1: 1, makes Y, Ba and Cu three metal ion species concentration are the solution of 3.0mol/L.The methyl alcohol that contains Y, Ba and Cu and the terpineol solution of gained are stirred, add titanium acetylacetone again, the titanium acetylacetone that adds be in the methyl alcohol of the described Y of containing, Ba and Cu and the terpineol solution Y, Ba and three kinds of total ion volumetric molar concentrations of metal of Cu 10%, be prepared into precursor liquid;
(5) speed of above-mentioned precursor liquid with 1500 rev/mins is spin-coated on the lanthanuma luminate single crystal matrix, the spin coating time is 90 seconds;
(6) sample that coating is good is placed on to send in the quartz boat in the quartzy stove of tubular type and carries out low-temperature heat treatment and high-temperature heat treatment, obtains containing nanometer Ti at last
2O
5YBCO high-temperature superconductor single layer thick film.Low-temperature heat treatment is to carry out under the moistening oxygen condition, be through the vial that distilled water is housed water vapour to be brought the oxygen of 500sccm into reaction chamber, make that water vapour pressure is 160hPa in the reaction chamber, on average be warming up to 500 ℃ with the temperature rise rate of 40 ℃/h from room temperature, and then stove is chilled to room temperature.The purpose of low-temperature heat treatment is to decompose trifluoroacetate, forms unformed precursor film and discharges harmful residual substance.The whole resolving time is about 10 hours.
High-temperature heat treatment is to carry out under moistening oxygen and argon gas mixed atmosphere, the argon gas mixed gas that 500sccm is contained 500ppm oxygen is brought water vapour into reaction chamber through the vial that distilled water is housed, make that water vapour pressure is 240hPa in the reaction chamber, temperature rise rate with 400 ℃/h rose to 850 ℃ of the highest temperatures before this, directly feed the argon gas mixed gas that contains 500ppm oxygen after 4 hours 850 ℃ of insulations, be cooled to 550 ℃ with 100 ℃/h then, insulation made the YBCO oxygen uptake of cubic phase change the YBCO with superconductivity of quadrature phase in 1.5 hours in 550 ℃ purity oxygen atmosphere, and sample stove under the oxygen atmosphere is chilled to room temperature subsequently.With Lepi-system the YBCO thick film that prepared one-tenth contains nano-titanium oxide has been carried out the test of critical current density, the critical current maximum reaches 1000A/cm, as shown in Figure 5.With field emission scanning electron microscope sample has been carried out the surface topography observation, the YBCO thick film surface is smooth, fine and close, as shown in Figure 6.Be that the sample of 7.5mol% and 10mol% has carried out analysis of components with X-ray diffractometer to titanium content, shown in Fig. 7 a.LAO (001) diffraction peak and YBCO (001) diffraction peak except matrix is arranged in the sample also have some more weak diffraction peaks in addition.In order more clearly to demarcate these faint diffraction peaks, we amplify sample X-ray diffraction θ-2 θ scanning spectra, and 2 θ useful ranges are 20 ° to 45 °, shown in Fig. 7 b.Can see significantly that at 2 θ be 20.711 °, 25.899 °, 26.620 °, 33.456 ° and 43.009 ° exist diffraction peak, through the retrieval of JCPDS card, and the corresponding Ti of diffraction peak difference that these intensity are more weak
3O
5(201), (202), (202), (203) and (204) diffraction peak is the corresponding BaF of diffraction peak of 24.853 ° and 28.775 ° existence at 2 θ
2(111) and (200) diffraction peak.The second that this explanation is added in precursor liquid is milled the acetone titanium and is generated Ti through after the follow-up thermal treatment
3O
5, therefore when the preparation of precursor liquid since the barium acetate of adding according to Y: Ba: Cu=1: (2+x): 3 stoichiometric ratio preparation, so barium acetate is excessive, these excessive barium acetate have generated BaF
2These titan oxide particles have played the effect of flux pinning just, and the critical current density of YBCO film is provided.
Claims (1)
1. the preparation method of a YBCO high temperature superconductive thick film is characterized in that, comprises the steps:
(1) according to the mol ratio of Y:Ba:Cu=1:2:3 Y (CH
3COO)
3, Ba (CH
3COO)
2And Cu (CH
3COO)
2Mix, under room temperature, be dissolved in the deionized water of the trifluoroacetic acid that contains 10-30mol%, wiring solution-forming, wherein the mol ratio of solute and solvent is 1:100;
(2) solution that step (1) is prepared adopted Rotary Evaporators to steam to desolventize again and obtains gel through magnetic stirrer 1-3 hour;
(3) gel that above-mentioned steps (2) is made adds in the methyl alcohol, gel in this step and the mol ratio of methyl alcohol are 1:50, after magnetic stirrer 0.5-1.5 hour, adopt Rotary Evaporators to steam again and desolventize, with impurity such as further removal moisture, obtain very pure gel;
(4) gel that above-mentioned steps (3) is made joins in methyl alcohol and the Terpineol 350, the solution that to make three kinds of metal total ion concentrations of Y, Ba and Cu be 1.5-3.0mol/L, the volume ratio of described methyl alcohol and Terpineol 350 is 1:1, the solution stirring that will contain described Y, Ba and Cu is even, add titanium acetylacetone again, the titanium acetylacetone that adds is Y, Ba in the described Y of containing, Ba and the Cu solution and the 5%-10% of three kinds of total ion volumetric molar concentrations of metal of Cu, is prepared into precursor liquid;
(5) precursor liquid of above-mentioned steps (4) being made adopts spin coating or method of pulling up to be coated on the substrate; Described substrate is lanthanum aluminate, strontium titanate or magnesium oxide single-crystal substrate;
(6) substrate after step (5) applies is placed the quartzy stove of high-temperature tubular, under 300 ℃~500 ℃ temperature, carry out 10 hours low-temperature heat treatment, decompose trifluoroacetate; The temperature rise rate of this step is 40 ℃/h; Described low-temperature heat treatment is carried out under the atmosphere of moistening oxygen and water vapour, and the water vapour pressure in the reaction chamber is 100hPa~160hPa;
(7) will place under 750 ℃~850 ℃ the high temperature thermal treatment through the substrate that step (6) is handled 2~4 hours, the heat-up rate of this step is 400 ℃/h; This step is carried out under moistening oxygen and argon gas condition, feeds the argon gas mixed gas that 500sccm contains 500ppm oxygen in reaction chamber, and the water vapour pressure in the reaction chamber is 160hPa~240hPa;
(8) will place through the substrate that step (7) is handled under 450 ℃~550 ℃ and the pure oxygen condition the film thermal treatment 0.5~1.5 hour of annealing, and be prepared into and contain nanometer Ti
3O
5YBCO high-temperature superconductor single layer thick film.
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CN102731083B (en) * | 2012-04-18 | 2014-02-26 | 中国科学院电工研究所 | Method for preparing yttrium-barium-copper-oxygen high-temperature superconducting film |
CN103130503A (en) * | 2012-12-07 | 2013-06-05 | 北京科技大学 | Bi (Zn1/2Zr1/2) O3-PbTiO3-based ferroelectric film with high Curie temperature large residual polarization and good fatigue property and preparation method thereof |
CN103641467A (en) * | 2013-11-06 | 2014-03-19 | 中国科学院电工研究所 | Method for preparing a high-temperature superconductive nanometer composite film |
TWI488994B (en) * | 2014-04-17 | 2015-06-21 | Ind Tech Res Inst | Method of repairing defect in superconducting film, method of coating superconducting film, and superconducting film formed by the method |
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CN101747031A (en) * | 2008-12-16 | 2010-06-23 | 北京有色金属研究总院 | High-temperature superconducting nanometer composite film and method for preparing same |
CN101752035A (en) * | 2008-12-16 | 2010-06-23 | 北京有色金属研究总院 | Method for preparing high temperature superconducting thin film by chemical process |
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