MgB2 superconducting material and preparation method thereof

Abstract

The invention discloses an MgB2 superconducting material and a preparation method thereof, and the preparation method of the MgB2 superconducting material comprises the following steps: (1) putting Mg (BH4) 2 powder into a crucible, and carrying out heating treatment to obtain a thermal decomposition product; (2) carrying out grinding treatment on the thermal decomposition product obtained in the step (1), and putting into a mold; (3) the filled mold is subjected to hot pressing treatment, and the heat preservation time is 0.5-2 h; and (4) cooling to room temperature, and taking out the material from the graphite mold to obtain the MgB2 superconducting material. The density of the MgB2 superconducting material prepared through the method exceeds 70% of the theoretical density, the problem that MgB2 prepared through Mg (BH4) 2 is low in density is solved, the critical transformation temperature (Tc) reaches 37.2 K, and the critical current density (Jc) under the 10K self-field reaches 2.58 * 10 < 5 > A / cm < 2 >.

Description

Technical Field

[0001] The present invention relates to the technical field of superconducting material preparation, and particularly to an MgB2 superconducting material and a preparation method thereof. Background Art

[0002] In 2001, the superconductor MgB2 with T c = 39K was first discovered, and this breakthrough triggered a research boom centered on MgB2 superconductors. Compared with low-temperature superconductors Nb3Ge or Nb3Sn, MgB2 can work in a liquid hydrogen cooling system (20K), directly reducing the operating cost of MgB2 superconducting devices. Compared with high-temperature superconducting materials, MgB2 has a large coherence length, weak anisotropy, and no grain weak connection, making it have good superconducting transport properties. These advantages enable MgB2 to show great potential in many application scenarios such as magnetic resonance imaging (MRI) coils, wind turbines, maglev propulsion systems, and superconducting permanent magnets.

[0003] However, the sintering temperature for preparing MgB2 is high (exceeding 800 °C), which may cause an interfacial reaction between the MgB2 precursor and the metal cladding material during the synthesis process, and is also a challenge to the stability of the external insulation material of the magnet and the stainless steel structural frame. Although undoped MgB2 has a high T c , at high magnetic fields, its J c drops sharply. This limitation is mainly due to the insufficient magnetic pinning centers inside the material. Under the increasing Lorentz force, the magnetic pinning centers cannot effectively fix the magnetic eddy currents. Therefore, J c decreases exponentially with the magnetic field strength, severely limiting its feasibility in high magnetic field applications such as MRI magnets or wind turbines.

[0004] Therefore, a new method for preparing MgB2 superconducting materials is needed. Summary of the Invention

[0005] In order to solve the problems of the prior art, the purpose of the present invention is to provide a method for preparing an MgB2 superconducting material. This method uses a method of first thermally decomposing and then hot pressing the Mg(BH4)2 precursor to prepare the MgB2 superconducting material, effectively improving the densification degree of MgB2, improving the grain boundary connectivity, and the prepared MgB2 exhibits excellent superconducting properties.

[0006] The technical solution of the present invention is as follows:

[0007] A method for preparing an MgB2 superconducting material, which includes the following steps:

[0008] (1) Heating the Mg(BH4)2 powder placed in a crucible to obtain a thermal decomposition product;

[0009] (2) Grind the thermal decomposition product obtained in step (1) and load it into a mold; the grinding treatment in this step is sufficient grinding;

[0010] (3) Perform hot pressing on the loaded mold, and the heat preservation time is 0.5 - 2 h;

[0011] (4) After cooling to room temperature, take out the material from the graphite mold to obtain the MgB2 superconducting material.

[0012] Among them, the atmosphere of the heating treatment in step (1) is flowing argon, vacuum or argon-hydrogen mixture.

[0013] Among them, the heating rate of the heating treatment in step (1) is 5 - 20 °C / min.

[0014] Among them, the temperature of the heating treatment in step (1) is 300 - 600 °C (preferably 520 - 600 °C), and the heat preservation time is 0.5 - 2 h.

[0015] Among them, the grinding duration in step (2) is 10 - 60 min.

[0016] Among them, the atmosphere of the hot pressing treatment in step (3) is vacuum, argon or argon-hydrogen mixture.

[0017] Among them, during the hot pressing treatment in step (3), the pressure is 30 - 100 MPa, the temperature of the hot pressing treatment is < 800 °C, and the heat preservation time of the hot pressing treatment is 0.5 - 2 h.

[0018] Among them, the temperature of the hot pressing treatment in step (3) is 500 - 750 °C, preferably 550 - 700 °C.

[0019] Among them, the cooling in step (4) is natural cooling.

[0020] A MgB2 superconducting material is prepared by using the above preparation method of the MgB2 superconducting material, and the superconducting transition temperature (T c ) of the superconducting material is 35 - 38 K, and the critical current density (J c ) at 10 K self-field is 1×10 5 - 3×10 5 A / cm 2 .

[0021] Preferably, the hot pressing method in step (3) includes uniaxial hot pressing and hot isostatic pressing.

[0022] Compared with the prior art, the present invention has the following beneficial effects:

[0023] (1) The method of the present invention prepares MgB2 bulk by two steps of thermal decomposition and hot pressing of Mg(BH4)2. First, the Mg(BH4)2 powder is heat-treated at different temperatures to achieve dehydrogenation to different degrees, and the intermediate process and mechanism of the decomposition of Mg(BH4)2 into MgB2 are analyzed in detail. Subsequently, the product is prepared into MgB2 bulk by hot pressing at a temperature of <800 °C.

[0024] (2) The MgB2 bulk prepared by the present invention exhibits a nanoscale grain structure, which is beneficial to providing more grain boundary pinning centers.

[0025] (3) The density of the MgB2 bulk prepared by the present invention is 50-80% of the theoretical density, and its density and grain connectivity are both significantly improved.

[0026] (4) The MgB2 bulk prepared by the present invention has excellent superconducting properties. The superconducting transition temperature (T c ) is 35-38 K, and the critical current density (J c ) at 10 K self-field is 1×10 5 - 3×10 5 A / cm 2 .

[0027] (5) The method of the present invention has the efficient characteristics of low heat treatment temperature and short time, avoiding the long sintering time for preparing MgB2. The combination of the two-step method of heat treatment first and then hot pressing realizes the ideal density and superconducting properties of the MgB2 bulk. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] Figure 1 is the reaction process and process flow chart for preparing the MgB2 superconducting material of the present invention;

[0029] Figure 2 is the TG-DSC combined thermal analysis curve of Mg(BH4)2;

[0030] Figure 3 is the XRD spectrum of the thermal decomposition products of Mg(BH4)2 at different temperatures;

[0031] Figure 4 is the scanning electron microscope (SEM) photograph of the cross-section of the MgB2 superconducting material (abbreviated as MB-550, MB-600, MB-650) prepared in Examples 1 to 4 of the present invention;

[0032] Figure 5 is the XRD spectrum of the MgB2 superconducting material prepared in Examples 1 to 4 of the present invention;

[0033] Figure 6It is the curve graph of the normalized magnetization intensity varying with temperature (M-T) of the MgB2 superconducting material prepared in Embodiments 1 to 4 of the present invention;

[0034] Figure 7 It is the curve graph of the critical current density of the MgB2 superconducting material prepared in Embodiments 1 to 4 of the present invention varying with the applied magnetic field (J c -H). Specific Embodiments

[0035] In order to make the objectives, technical solutions and advantages of the present invention clearer, the present invention will be further described in detail below with reference to the drawings and embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not used to limit the present invention. In addition, the technical features involved in the various embodiments of the present invention described below can be combined with each other as long as they do not conflict with each other.

[0036] To make the objectives, technical solutions and advantages of the present invention clearer, the embodiments of the present invention will be further described in detail below, but the scope of the present invention is not limited in any way.

[0037] The Mg(BH4)2 raw material used in the present invention includes Mg(BH4)2 obtained in any form.

[0038] As a borohydride complex, Mg(BH4)2 has the characteristics of high hydrogen storage density and low thermal decomposition temperature. The final thermal decomposition product of Mg(BH4)2 is MgB2, which provides a new idea for manufacturing MgB2 at a lower temperature. This method can reduce the sintering temperature by about 200 - 300 °C and refine the grain structure. However, currently, using Mg(BH4)2 as a precursor to prepare MgB2 usually results in many pores and low density (less than 50% of the theoretical density).

[0039] The inventors found that the large amount of hydrogen released during the pyrolysis of Mg(BH4)2 is the main reason for its many pores and low density. For this reason, the inventors analyzed the intermediate process and products of the decomposition of Mg(BH4)2, and the analysis results are as Figures 1 to 3 shown.

[0040] See Figure 1 , the pyrolysis process of Mg(BH4)2 generally goes through four stages. In the first stage, Mg(BH4)2 thermally decomposes to generate MgB 12 H 12 , MgH2 and H2; in the second stage, MgH2 further decomposes into Mg and H2; in the third stage, MgB 12 H 12 further decomposes into Mg, B and H2, and in the fourth stage, the decomposition products Mg and B combine to form MgB2.

[0041] Figure 2 TG-DSC coupled thermal analysis curve of Mg(BH4)2, where the DSC curve shows four endothermic peaks corresponding to the four stages of the thermal decomposition process of Mg(BH4)2. The TG curve shows that when the temperature reaches 500 °C, the thermal weight loss of Mg(BH4)2 reaches the theoretical decomposition value of 14.9 wt% for complete hydrogen release, indicating that the thermal decomposition reaction of Mg(BH4)2 has been completely completed.

[0042] Figure 3 XRD patterns of thermal decomposition products of Mg(BH4)2 at different temperatures (abbreviated as MBH-300, MBH-350, MBH-400, MBH-500, MBH-520, MBH-550). In the first stage, Mg(BH4)2 is decomposed into stable borohydrides MgB 12 H 12 and MgH2. MgB 12 H 12 is an amorphous compound and has no crystal diffraction peaks in XRD. Diffraction peaks of MgH2 are found in the XRD pattern at 350 °C. In the second stage, MgH2 is completely decomposed into Mg, which is confirmed by the XRD results at 400 °C, and crystal diffraction peaks of elemental Mg are detected, and the XRD peaks of MgH2 completely disappear. In the third stage, MgB 12 H 12 is confirmed to be decomposed into elemental Mg and elemental B. In the XRD of the products from 400 °C to 500 °C, the Mg diffraction peaks are more prominent, indicating a significant increase in Mg content, confirming that MgB 12 H 12 is decomposed into elemental Mg and elemental B. Diffraction peaks of MgB2 are already observed in the XRD at 500 °C, which is obtained by the reaction of Mg and B generated by decomposition. Finally, the presence of elemental Mg cannot be observed in the XRD pattern of MBH-550, proving that Mg and B have completely formed MgB2 at this temperature.

[0043] In view of this, the inventors considered that before preparing MgB2 by hot pressing Mg(BH4)2, it was first thermally decomposed to avoid the generation of voids during the subsequent hot pressing process by releasing the H2 generated during the decomposition process, that is, to generate MgB2 under the condition without H2 for Mg and B. The MgB2 bulk prepared by this method exhibits a nanoscale grain size, which is beneficial to providing grain boundary pinning centers. The density of the MgB2 bulk exceeds 70% of the theoretical density, improving the problem of low density in the preparation of MgB2 from Mg(BH4)2. The critical transition temperature (T c ) reaches 37.2 K, and the critical current density (J c ) at 10 K self-field reaches 2.58×10 5 A / cm 2。

[0044] Example 1

[0045] A preparation method of MgB2 superconducting material, comprising the following preparation steps:

[0046] (1) Put a certain amount of Mg(BH4)2 powder into an Al2O3 crucible, transfer the crucible to a tube furnace for heating, introduce flowing argon, the heating temperature is 520 °C, the heating rate is 10 °C / min, keep the temperature for 1 h, and obtain the thermal decomposition product of Mg(BH4)2, named MBH-520;

[0047] (2) Grind the thermal decomposition product MBH-520 of Mg(BH4)2 in a glove box with a mortar for 20 - 60 min, and put the ground powder into a cylindrical graphite mold with a diameter of 12.7 mm;

[0048] (3) Put the loaded graphite mold into a hot press and perform hot pressing under vacuum, the vacuum degree < 1×10 -1 Pa, apply a pressure of 80 MPa, keep the temperature at 550 °C for 1 h;

[0049] (4) After the heat preservation is completed, relieve the pressure, let the hot press cool naturally to room temperature, take out the material from the graphite mold, and polish the upper and lower surfaces to obtain the MgB2 superconducting material, named MB-550.

[0050] The density of the MgB2 superconducting material prepared in this example is 63%, T c = 36.1 K, J under a self-field of 10 K c = 1.58×10 5 A / cm 2 。

[0051] Example 2

[0052] A preparation method of MgB2 superconducting material, comprising the following preparation steps:

[0053] (1) Put a certain amount of Mg(BH4)2 powder into an Al2O3 crucible, transfer the crucible to a tube furnace for heating, introduce flowing argon, the heating temperature is 520 °C, the heating rate is 10 °C / min, keep the temperature for 1 h, and obtain the thermal decomposition product of Mg(BH4)2, named MBH-520;

[0054] (2) Grind the thermal decomposition product MBH-520 of Mg(BH4)2 in a glove box with a mortar for 20 - 60 min, and put the ground powder into a cylindrical graphite mold with a diameter of 12.7 mm;

[0055] (3) Place the loaded graphite mold into a hot press and perform hot pressing under vacuum. The vacuum degree is <1×10 -1 Pa, apply a pressure of 80 MPa, and keep the hot pressing temperature at 600 °C for 1 h;

[0056] (4) After the heat preservation is completed, release the pressure, let the hot press cool naturally to room temperature, take out the material from the graphite mold, and polish the upper and lower surfaces to obtain the MgB2 superconducting material, named MB-600.

[0057] The density of the MgB2 superconducting material prepared in this example is 66%, T c = 36.3 K, and J c = 1.60×10 5 A / cm 2 .

[0058] Example 3

[0059] A preparation method of an MgB2 superconducting material, comprising the following preparation steps:

[0060] (1) Put a certain amount of Mg(BH4)2 powder into an Al2O3 crucible, transfer the crucible to a tube furnace for heating, introduce flowing argon, the heating temperature is 520 °C, the heating rate is 10 °C / min, and keep it for 1 h to obtain the Mg(BH4)2 thermal decomposition product at different temperatures, named MBH-520;

[0061] (2) Grind the Mg(BH4)2 thermal decomposition product MBH-520 in a glove box with a mortar for 20 - 60 min, and load the ground powder into a cylindrical graphite mold with a diameter of 12.7 mm;

[0062] (3) Place the loaded graphite mold into a hot press and perform hot pressing under vacuum. The vacuum degree is <1×10 -1 Pa, apply a pressure of 80 MPa, and keep the hot pressing temperature at 650 °C for 1 h;

[0063] (4) After the heat preservation is completed, release the pressure, let the hot press cool naturally to room temperature, take out the material from the graphite mold, and polish the upper and lower surfaces to obtain the MgB2 superconducting material, named MB-650.

[0064] The density of the MgB2 superconducting material prepared in this example is 71%, T c = 37.2 K, and J c = 2.58×10 5 A / cm 2 .

[0065] Example 4

[0066] A preparation method of MgB2 superconducting material, comprising the following preparation steps:

[0067] (1) Put a certain amount of Mg(BH4)2 powder into an Al2O3 crucible, transfer the crucible to a tube furnace for heating, introduce flowing argon gas, the heating temperature is 520 °C, the heating rate is 10 °C / min, keep the temperature for 1 h, and obtain the thermal decomposition product of Mg(BH4)2, named MBH-520;

[0068] (2) Grind the Mg(BH4)2 thermal decomposition product MBH-520 in a glove box with a mortar for 20 - 60 min, and put the ground powder into a cylindrical graphite mold with a diameter of 12.7 mm;

[0069] (3) Put the loaded graphite mold into a hot press and perform hot pressing under vacuum, the vacuum degree < 1×10 -1 Pa, apply a pressure of 80 MPa, and keep the temperature at 700 °C for 1 h;

[0070] (4) After the heat preservation is completed, release the pressure, let the hot press cool naturally to room temperature, take out the material from the graphite mold, and polish the upper and lower surfaces to obtain the MgB2 superconducting material, named MB-700.

[0071] The density of the MgB2 superconducting material prepared in this example is 71%, T c = 37.1 K, J c = 2.63×10 5 A / cm 2 .

[0072] Example 5

[0073] A preparation method of MgB2 superconducting material, comprising the following preparation steps:

[0074] (1) Put a certain amount of Mg(BH4)2 powder into an Al2O3 crucible, transfer the crucible to a tube furnace for heating, introduce flowing argon gas, the heating temperature is 300 °C, the heating rate is 5 °C / min, keep the temperature for 1 h, and obtain the thermal decomposition product of Mg(BH4)2 at different temperatures, named MBH-300;

[0075] (2) Grind the Mg(BH4)2 heat treatment product MBH-300 in a glove box with a mortar for 20 - 60 min, and put the ground powder into a cylindrical graphite mold with a diameter of 12.7 mm;

[0076] (3) Put the loaded graphite mold into a hot press and perform hot pressing under vacuum, the vacuum degree < 1×10 -1 Pa, apply a pressure of 100 MPa, and keep the temperature at 500 °C for 0.5 h;

[0077] (4) After the heat preservation is completed, relieve the pressure, let the hot press cool naturally to room temperature, take out the material from the graphite mold, and polish the upper and lower surfaces to obtain the MgB2 superconducting material, named MB-500.

[0078] The density of the MgB2 superconducting material prepared in this example is 64%, T c = 36.2 K, and J c = 1.13×10 5 A / cm 2 .

[0079] Example 6

[0080] A preparation method of an MgB2 superconducting material, comprising the following preparation steps:

[0081] (1) Put a certain amount of Mg(BH4)2 powder into an Al2O3 crucible, transfer the crucible to a tube furnace for heating, introduce flowing argon, the heating temperature is 600 °C, the heating rate is 20 °C / min, and keep the temperature for 1 h to obtain the Mg(BH4)2 thermal decomposition products at different temperatures, named MBH-600;

[0082] (2) Grind the Mg(BH4)2 heat treatment product MBH-600 in a glove box with a mortar for 20 - 60 min, and load the ground powder into a cylindrical graphite mold with a diameter of 12.7 mm;

[0083] (3) Put the loaded graphite mold into a hot press for hot pressing under vacuum, the vacuum degree < 1×10 -1 Pa, apply a pressure of 30 MPa, and keep the temperature at 750 °C for 2 h;

[0084] (4) After the heat preservation is completed, relieve the pressure, let the hot press cool naturally to room temperature, take out the material from the graphite mold, and polish the upper and lower surfaces to obtain the MgB2 superconducting material, named MB-750.

[0085] The density of the MgB2 superconducting material prepared in this example is 61%, T c = 36.4 K, and J c = 1.05×10 5 A / cm 2 .

[0086] Comparative Example 1

[0087] A method for preparing an MgB2 superconducting material from Mg(BH4)2, comprising the following preparation steps:

[0088] A certain amount of Mg(BH4)2 powder was mechanically pressed axially in a mold under a hydrostatic pressure of about 1.8 GPa to form a block with a diameter of 12.7 mm. The Mg(BH4)2 block was placed in an Al2O3 crucible and heated in a tubular furnace under a flowing Ar gas atmosphere. The temperature in the furnace was raised to 500 °C at a rate of 10 °C·min -1 , and held for 2 h to obtain the MgB2 superconducting material, named MB-500-0.

[0089] The density of the MgB2 superconducting material prepared in this comparative example was 49%, and T c = 34.8 K. At 20 K under self-field, J c = 0.176×10 5 A / cm 2 .

[0090] Figure 4 These are the scanning electron microscope (SEM) photos of the cross-sections of the MgB2 superconducting materials (abbreviated as MB-550, MB-600, MB-650, MB-700) prepared in Examples 1 to 4 of the present invention. The structure of MB-550 is relatively loose with many pores. Compared with MB-550, the grain connectivity of MB-600 is significantly improved and the number of voids is significantly reduced. Compared with the previous two blocks, MB-650 has a higher density, the fewest voids, and the best grain connectivity. The density and connectivity of the MB-700 sample are similar to those of MB-650, without particularly obvious improvement.

[0091] Figure 5 These are the XRD patterns of the MgB2 superconducting materials prepared in Examples 1 to 4 of the present invention. The images show that the main phase of the hot-pressed samples at different temperatures is MgB2, with a small amount of MgO. No crystal diffraction peaks of elemental Mg were observed in the XRD, indicating that at a hot-pressing temperature of 550 °C, Mg has completely reacted to form MgB2.

[0092] Figure 6 These are the curves of the normalized magnetization intensity versus temperature (M-T) of the MgB2 superconducting materials prepared in Examples 1 to 4 of the present invention. All the MgB2 blocks show obvious superconducting transitions. The T c of the MgB2 obtained by hot pressing at 550 °C reaches 36.1 K, and the T c of MB-650 is the highest, reaching 37.2 K. The T c of MgB2 is roughly positively correlated with the hot-pressing temperature, which can be attributed to more complete reactions and better crystallinity at higher processing temperatures.

[0093] Figure 7 These are the curves of the critical current density versus the applied magnetic field (J c-H) curve, J of MgB2 bulk material hot pressed at 550℃ for 1h under 10K self-field c Up to 1.58×10 5 A / cm 2 , J of MB-650 under the same conditions c The value is 2.58×10 5 A / cm 2 MgB2 sample J obtained at hot pressing temperature of 650℃ c The value is the highest, which is related to the effect of temperature increase on the connectivity and density of the material grains. Low temperature and short holding time lead to insufficient grain connectivity, limiting the superconducting properties of the sample sintered at 550℃.

[0094] Table 1 shows the preparation conditions and performance parameters of the MgB2 superconducting materials prepared in Examples 1 to 4 of the present invention and Comparative Example 1, T c , J c The density of MB-500-0 without heat treatment and pressure is only 49%, and the density reaches more than 60% after pressure is applied. Applying pressure during the sintering process can effectively increase the density of MgB2.

[0095] Table 1

[0096] It will be easily understood by those skilled in the art that the above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

[0097] The parts not described in detail in the present description belong to the known technology in the art. The above embodiments are provided only for the purpose of describing the present invention, and are not intended to limit the scope of the present invention. The scope of the present invention is defined by the appended claims. Various equivalent substitutions and modifications made without departing from the spirit and principle of the present invention should be included within the scope of the present invention.

Claims

1. A method for preparing MgB2 superconducting material, characterized in that, It includes the following steps: (1) Heat the Mg(BH4)2 powder placed in a crucible to obtain a thermal decomposition product; (2) Grind the thermal decomposition product obtained in step (1) and load it into a mold; (3) Perform hot pressing on the loaded mold, and the heat preservation time is 0.5 - 2 h; (4) After cooling to room temperature, take out the material from the graphite mold to obtain the MgB2 superconducting material.

2. The preparation method of the MgB2 superconducting material according to claim 1, wherein The atmosphere of the heat treatment in step (1) is flowing argon, vacuum or argon-hydrogen mixture.

3. The preparation method of the MgB2 superconducting material according to claim 1, characterized in that, The heating rate of the heat treatment in step (1) is 5 - 20 °C / min.

4. The preparation method of the MgB2 superconducting material according to claim 1, characterized in that, The temperature of the heat treatment in step (1) is 300 - 600 °C, and the heat preservation time is 0.5 - 2 h.

5. The preparation method of the MgB2 superconducting material according to claim 1, characterized in that, The grinding duration in step (2) is 10 - 60 min.

6. The preparation method of the MgB2 superconducting material according to claim 1, characterized in that, The atmosphere of the hot pressing treatment in step (3) is vacuum, argon or argon-hydrogen mixture.

7. The preparation method of the MgB2 superconducting material according to claim 1, characterized in that, During the hot pressing treatment in step (3), the pressure is 30 - 100 MPa, the temperature of the hot pressing treatment is < 800 °C, and the heat preservation time of the hot pressing treatment is 0.5 - 2 h.

8. The preparation method of the MgB2 superconducting material according to claim 1, characterized in that, The temperature of the hot pressing treatment in step (3) is 500 - 750 °C.

9. The preparation method of the MgB2 superconducting material according to claim 1, characterized in that, The cooling in step (4) is natural cooling.

10. A MgB2 superconducting material, characterized in that, Prepared by the method for preparing MgB2 superconducting material according to any one of claims 1 to 9, the superconducting transition temperature (T c ) of the superconducting material is 35 to 38 K, and the critical current density (J c ) at 10 K self-field is 1×10 5 to 3×10 5 A / cm 2 .

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