Titanium indium gallium oxide target as well as preparation method and application thereof

Abstract

The invention belongs to the technical field of oxide target materials, and particularly discloses an indium gallium titanium oxide target material and a preparation method and application thereof. The indium gallium titanium oxide target material is prepared from the following raw materials in parts by mass: 95 to 99 parts of indium oxide, 0.5 to 2 parts of gallium oxide and 0.6 to 3 parts of titanium dioxide. According to the preparation method, gallium oxide and titanium dioxide in a proper proportion are doped in the indium oxide-based target material, so that an oxide film prepared from the target material has excellent light transmittance on the premise of keeping relatively low resistivity of the target material, and the oxide film prepared from the target material has relatively good mechanical flexibility, and can be applied to the field of organic light-emitting devices, such as organic light-emitting devices, organic light-emitting devices, organic light-emitting devices, organic light-emitting devices, organic light-emitting devices and organic light-emitting devices. And the method can be better applied to flexible OLEDs. The invention also provides a preparation method of the indium gallium titanium oxide target material.

Description

Technical Field

[0001] The present invention relates to the technical field of oxide target materials, and in particular to an indium gallium titanium oxide target material and a preparation method and application thereof. Background Art

[0002] In recent years, flexible organic light-emitting diodes (OLEDs) have attracted widespread attention due to their unique properties. The design flexibility brought by flexible properties has opened up new possibilities for the application of light-emitting diodes. The deformation of the curved or foldable screen has produced innovative foldable or bendable products, which have been applied in foldable mobile phones and large-area curved screens. Foldable smartphones with flexible screens have expanded the screen size without affecting the convenience of users. The technical effect of screen flexibility can be attributed to the advancement of flexible electrodes, which is crucial to achieving the flexibility required for OLEDs. Given the great potential of flexible transparent electrodes in applications such as flexible or foldable OLEDs, it is imperative to develop transparent electrodes with low sheet resistance, excellent optical transmittance, and outstanding mechanical flexibility.

[0003] Currently, many flexible transparent electrode materials have been proposed as alternatives to traditional ITO films, however, thin ITO electrodes continue to be used as the bottom electrode of flexible OLEDs, mainly driven by the advantageous properties of ITO, including low sheet resistance, high transmittance, and a sound manufacturing process. Although other materials have been extensively explored, the above qualities and characteristics make the use of thin ITO electrodes the first choice to ensure the best performance of flexible OLEDs. However, with the growing interest in flexible displays, the demand for transparent conductors that can overcome the challenges of flexible configurations continues to grow. Current ITO-based electrodes exhibit lower mechanical strain tolerance than other layers in the device, which is increasingly difficult to meet the needs of the industry and the market.

[0004] Therefore, there is an urgent need to develop a transparent conductor material that can replace ITO, which has good mechanical flexibility while ensuring good conductivity and transparency under large mechanical strain. Summary of the invention

[0005] The present invention aims to solve at least one of the technical problems existing in the prior art. To this end, the present invention provides an indium gallium titanium oxide target. The indium gallium titanium oxide target of the present invention has a low resistivity, and the oxide film prepared therefrom has excellent light transmittance and mechanical flexibility, and can be well applied to flexible OLEDs.

[0006] The present invention also provides a method for preparing an indium gallium titanium oxide target material.

[0007] The invention also provides a flexible oxide film.

[0008] The invention also provides a flexible OLED.

[0009] The present invention also proposes the application of indium gallium titanium oxide target in the field of display.

[0010] In a first aspect of the present invention, an indium gallium titanium oxide target is provided, wherein the raw materials for preparing the target include 95-99 parts by weight of indium oxide, 0.5-2 parts by weight of gallium oxide, and 0.6-3 parts by weight of titanium dioxide.

[0011] According to a specific embodiment of the present invention, the indium gallium titanium oxide target provided by the present invention has at least the following beneficial effects:

[0012] The indium gallium titanium oxide target material of the present invention has a relatively high relative density and a relatively small average grain size, and can make the oxide film prepared by the target material have excellent light transmittance and mechanical flexibility while maintaining a relatively low resistivity of the target material;

[0013] The present invention uses amorphous gallium and titanium to co-dope indium oxide, wherein Ga (62 p.m.) and Ti (60.5 p.m.) have ionic radii similar to In (80 p.m.), so compared with other doped oxides, Ga and Ti doping produce less stress, resulting in a smaller decrease in the electron mobility of the target material, and Ga and Ti have higher metal oxygen bonding capacity (Ga-O, Ti-O), which can reduce the presence of oxygen vacancies in the indium oxide matrix, and titanium doping can make Ti 4+ Replace In 3+ Additional free electrons are provided. Ti doping also has a strong Lewis acid strength, which leads to strong polarization of electrons away from the O2p valence band, thereby causing charge screening, reducing the electron scattering effect, and ultimately increasing the electron mobility and improving the conductivity of the target material and oxide film;

[0014] The present invention further optimizes the doping amount and doping ratio of gallium oxide and titanium dioxide in the indium oxide target material, further improves the comprehensive performance of the target material and the oxide film, especially improves the flexibility of the oxide film prepared by the present invention, so that it can maintain conductivity and transparency under large mechanical strain, so that it can be better applied to the field of flexible OLED and flexible display.

[0015] According to some embodiments of the present invention, the preparation raw materials include 96.12 to 98.48 parts of indium oxide, 0.67 to 1.34 parts of gallium oxide and 0.85 to 2.54 parts of titanium dioxide in parts by mass.

[0016] According to some embodiments of the present invention, the preparation raw materials include 96.12 to 97.64 parts of indium oxide, 0.67 to 1.34 parts of gallium oxide and 1.69 to 2.54 parts of titanium dioxide in parts by mass.

[0017] According to some embodiments of the present invention, the preparation raw material further comprises 1 to 5 parts of a dispersant and 1 to 5 parts of a binder.

[0018] According to some embodiments of the present invention, the preparation raw materials further include 2 to 4 parts of a dispersant and 2 to 4 parts of a binder.

[0019] According to some embodiments of the present invention, the dispersant includes at least one of polyvinyl pyrrolidone, polyacrylamide, polyethylene glycol or hydrogenated nitrile rubber.

[0020] According to some embodiments of the present invention, the binder includes at least one of polyvinyl alcohol, sodium polyacrylate, butyl rubber or cyanoacrylate.

[0021] The second aspect of the present invention provides a method for preparing the indium gallium titanium oxide target material according to the first aspect of the present invention, comprising the following steps:

[0022] S1, mixing the indium oxide, the gallium oxide and the titanium dioxide, and then adding water, a dispersant and a binder to mix and grind;

[0023] S2, spray drying and granulation to obtain mixed powder;

[0024] S3, cold isostatic pressing and sintering to obtain indium gallium titanium oxide target.

[0025] According to some embodiments of the present invention, the grinding in step S1 is ball milling.

[0026] According to some embodiments of the present invention, the ball milling in step S1 is divided into three steps, specifically, ball milling the indium oxide, gallium oxide and titanium dioxide for the first time after mixing, adding water and a dispersant for the second time after ball milling, and adding a binder for the third time after ball milling.

[0027] According to some embodiments of the present invention, the cold isostatic pressing pressure in step S3 is 100-400 MPa, and the holding time is 2-10 min.

[0028] According to some embodiments of the present invention, the sintering in step S3 is sequentially carried out by keeping at 500-600° C. for 1-3 h, keeping at 900-1100° C. for 3-5 h, keeping at 1350-1400° C. for 6-8 h in an oxygen atmosphere, and keeping at 900-1100° C. for 1-3 h.

[0029] According to some embodiments of the present invention, the sintering in step S3 is to place the statically pressed embryo body in a sintering furnace, heat the temperature to 500-600°C at a heating rate of 2-4°C / min, keep the temperature for 1-3 hours, heat the temperature to 900-1100°C at a heating rate of 0.5-2°C / min, keep the temperature for 3-5 hours, introduce oxygen, heat the temperature to 1350-1390°C at a heating rate of 0.2-1°C / min in an oxygen atmosphere, keep the temperature for 4-6 hours, heat the temperature to 1390-1420°C at a heating rate of 0.2-1°C / min in an oxygen atmosphere, keep the temperature for 1-3 hours, stop introducing oxygen, cool the temperature to 900-1100°C at a cooling rate of 0.5-2°C / min, keep the temperature for 1-3 hours, and finally cool the temperature to room temperature at a cooling rate of 0.5-2°C / min.

[0030] A third aspect of the present invention provides a flexible oxide film, which is made from the indium gallium titanium oxide target material described in the first aspect of the present invention, and the light transmittance of the oxide film is 92% to 99%.

[0031] A fourth aspect of the present invention provides a flexible OLED, comprising the flexible oxide film described in the third aspect of the present invention.

[0032] The fifth aspect of the present invention provides applications of the indium gallium titanium oxide target described in the first aspect of the present invention, the flexible oxide film described in the third aspect of the present invention, and the flexible OLED described in the fourth aspect of the present invention in the field of displays.

[0033] Other features and advantages of the present invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the present invention. DETAILED DESCRIPTION

[0034] The following will be combined with the embodiments to clearly and completely describe the concept of the present invention and the technical effects produced, so as to fully understand the purpose, characteristics and effects of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, other embodiments obtained by those skilled in the art without creative work are all within the scope of protection of the present invention.

[0035] If the specific conditions are not specified in the examples, the experiments were carried out under conventional conditions or conditions recommended by the manufacturer. If the manufacturers of the reagents or instruments are not specified, they are all conventional products that can be purchased commercially.

[0036] Example 1

[0037] This embodiment provides an indium gallium titanium oxide target material and a preparation method thereof.

[0038] The oxide raw material composition of the indium gallium titanium oxide target material of this embodiment is calculated by weight: indium oxide (In 2 O 3 ) 98.48 parts, gallium oxide (Ga 2 O 3 )0.67 parts and titanium dioxide (TiO 2 ) 0.85 parts, in addition to the preparation of raw materials, there are 1.33 parts of deionized water, 3 parts of dispersant, and 3.385 parts of binder;

[0039] The dispersant is polyvinyl pyrrolidone (the dispersant may also be polyacrylamide, polyethylene glycol, or hydrogenated nitrile rubber), and the binder is polyvinyl alcohol (the binder may also be sodium polyacrylate, butyl rubber, or cyanoacrylate).

[0040] This embodiment also provides a method for preparing the indium gallium titanium oxide target material, and the specific steps are as follows:

[0041] 1) Indium oxide powder, gallium oxide powder and titanium dioxide powder are mixed, added to a ball mill and ball milled for 1 hour to make the oxide powders uniformly mixed, wherein the ball milling speed is 400 r / min, and the zirconium bead particle size is 2.0 mm; then 1.33 parts of deionized water and a dispersant are added, and a second ball milling is performed for 40 hours, wherein the ball milling speed is 1100 r / min, and the zirconium bead particle size is 0.65 mm; a binder is added to the mixed slurry, and a third ball milling is performed for 1 hour, wherein the ball milling speed is 1100 r / min, and the zirconium bead particle size is 0.3 mm;

[0042] 2) After the ball milling, the slurry is spray dried and granulated to obtain a mixed powder;

[0043] 3) injecting the mixed powder into a mold, performing molding (80 MPa, 5 min) and cold isostatic pressing, and maintaining the cold isostatic pressing pressure at 220 MPa for 5 min to obtain a target blank;

[0044] 4) The green blank is placed in a sintering furnace for sintering. In the first step, the temperature is increased to 550°C at a heating rate of 3°C / min and kept at this temperature for 2 hours. In the second step of sintering, the temperature is increased to 1000°C at a heating rate of 1°C / min and kept at this temperature for 4 hours. In the third step of sintering, oxygen is introduced and the temperature is increased to 1380°C at a heating rate of 0.5°C / min and kept at this temperature for 5 hours in an oxygen atmosphere. Then, the temperature is increased to a maximum temperature of 1400°C at a rate of 0.5°C / min and kept at this temperature for 2 hours. After the insulation is completed, the oxygen is stopped and the temperature is decreased to 1000°C at a rate of 1°C / min and kept at this temperature for 2 hours. Finally, the temperature is decreased to room temperature at a rate of 1°C / min. After sintering and cooling, an indium gallium titanium oxide target is obtained.

[0045] In this embodiment, further processing steps of the indium gallium titanium oxide target are also included for subsequent practical use or measurement. Specifically:

[0046] The sintered target material is processed and polished according to size requirements to obtain a finished target material.

[0047] Example 2

[0048] This embodiment provides an indium gallium titanium oxide target material and a preparation method thereof.

[0049] The difference between this embodiment and embodiment 1 is only that the mass fractions of the metal oxide raw material components of the two are different: this embodiment uses 97.81 parts of indium oxide, 1.34 parts of gallium oxide and 0.85 parts of titanium dioxide, and the remaining raw material components and preparation methods are consistent with those of embodiment 1.

[0050] Example 3

[0051] This embodiment provides an indium gallium titanium oxide target material and a preparation method thereof.

[0052] The difference between this embodiment and embodiment 1 is only that the mass fractions of the metal oxide raw material components of the two are different: this embodiment uses 97.64 parts of indium oxide, 0.67 parts of gallium oxide and 1.69 parts of titanium dioxide, and the remaining raw material components and preparation methods are consistent with those of embodiment 1.

[0053] Example 4

[0054] This embodiment provides an indium gallium titanium oxide target material and a preparation method thereof.

[0055] The difference between this embodiment and embodiment 1 is only that the mass fractions of the metal oxide raw material components of the two are different: this embodiment uses 96.97 parts of indium oxide, 1.34 parts of gallium oxide and 1.69 parts of titanium dioxide, and the remaining raw material components and preparation methods are consistent with those of embodiment 1.

[0056] Example 5

[0057] This embodiment provides an indium gallium titanium oxide target material and a preparation method thereof.

[0058] The difference between this embodiment and embodiment 1 is only that the mass fractions of the metal oxide raw material components of the two are different: this embodiment uses 96.79 parts of indium oxide, 0.67 parts of gallium oxide and 2.54 parts of titanium dioxide, and the remaining raw material components and preparation methods are consistent with those of embodiment 1.

[0059] Example 6

[0060] This embodiment provides an indium gallium titanium oxide target material and a preparation method thereof.

[0061] The difference between this embodiment and embodiment 1 is only that the mass fractions of the metal oxide raw material components of the two are different: this embodiment uses 96.12 parts of indium oxide, 1.34 parts of gallium oxide and 2.54 parts of titanium dioxide, and the remaining raw material components and preparation methods are consistent with those of embodiment 1.

[0062] Comparative Example 1

[0063] This comparative example provides a conventional tin-doped indium oxide (ITO) target material and provides a preparation method thereof.

[0064] The difference between this comparative example and Example 1 is that the metal oxide raw materials of the two are different: this comparative example uses 90.00 parts of indium oxide and tin oxide (SnO 2 ) 10.00 parts, and the remaining raw material components and preparation method are consistent with Example 1.

[0065] Comparative Example 2

[0066] This comparative example provides a gallium-doped indium oxide target material and a preparation method thereof.

[0067] The difference between this comparative example and Example 1 is that the metal oxide raw materials of the two are different: this comparative example uses 98.66 parts of indium oxide and 1.34 parts of gallium oxide, and the other raw material components and preparation methods are consistent with Example 1.

[0068] Comparative Example 3

[0069] This comparative example provides a titanium-doped indium oxide target material and a preparation method thereof.

[0070] The difference between this comparative example and Example 1 is that the metal oxide raw materials of the two are different: this comparative example uses 97.46 parts of indium oxide and 2.54 parts of titanium dioxide, and the other raw material components and preparation methods are consistent with Example 1.

[0071] Comparative Example 4

[0072] This comparative example provides an indium gallium titanium oxide target material and a preparation method thereof.

[0073] The difference between this comparative example and Example 1 is only that the mass fractions of the metal oxide raw material components of the two are different: this example uses 95.94 parts of indium oxide, 0.67 parts of gallium oxide and 3.39 parts of titanium dioxide, and the remaining raw material components and preparation methods are consistent with Example 1.

[0074] Comparative Example 5

[0075] This comparative example provides an indium gallium titanium oxide target material and a preparation method thereof.

[0076] The difference between this comparative example and Example 1 is only that the mass fractions of the metal oxide raw material components of the two are different: this example uses 95.27 parts of indium oxide, 1.34 parts of gallium oxide and 3.39 parts of titanium dioxide, and the remaining raw material components and preparation methods are consistent with Example 1.

[0077] Performance Test:

[0078] 1. The performance test was performed on the finished products of the doped indium oxide targets prepared in the above embodiments and comparative examples, wherein the density was measured by the Archimedes drainage method, and the relative density was the ratio of the actual density of the target measured by the drainage method to the theoretical density; the target samples were subjected to metallographic analysis, and the average grain size was measured by the intercept method; the resistivity was measured using a resistivity meter using a four-point probe method; and each target was then sputtered using a magnetron sputtering machine to form a 100nm thick oxide film, and the substrate was a 10*10mm plastic substrate, and the transmittance was measured using a double-beam UV-visible photometer. The results of the oxide raw materials used and the performance parameters in the embodiments and comparative examples are shown in Table 1.

[0079] Table 1 Oxide raw material usage and performance parameter results in each embodiment and comparative example

[0080]

[0081]

[0082] From the test results in Table 1, it can be seen that the multi-doping of gallium oxide and titanium dioxide in the indium oxide-based target material of the present invention has a great influence on the performance of the target material and the oxide film prepared therefrom. By changing the doping components and proportions, the comprehensive performance of the target material and the oxide film is improved. Compared with the traditional ITO target material, the indium gallium titanium oxide target material of the present invention can maintain a low resistivity while the prepared oxide film has excellent light transmittance, and the target material of the present invention has a higher relative density and a smaller average grain size.

[0083] By comparing Examples 1 and 2, Examples 3 and 4, and Comparative Example 2, it can be seen that the doping of gallium in the scheme of the present invention has different degrees of influence on the relative density, resistivity, and transmittance of the target material. With the increase of the doping amount of gallium, the relative density and transmittance of the target material are improved, but its resistivity also tends to increase, which is not conducive to electron migration. Therefore, the doping of gallium in the scheme of the present invention cannot be excessive. By comparing Examples 1, 3 and Examples 2, 4, 6 and Comparative Example 2, it can be seen that the doping of titanium in the scheme of the present invention has a greater influence on the resistivity of the target material and the transmittance of the prepared oxide film. Increasing the doping ratio of titanium dioxide helps to reduce the resistivity of the target material, and the transmittance of the film is also improved. However, by comparing Examples 1, 3, 5, and Comparative Example 4 with Examples 2, 4, 6, and Comparative Example 5, it can be seen that after the titanium element is doped to a greater than a certain value, the resistivity instead shows an increasing trend. This is because when the titanium element is doped in excess, the element cannot be well mixed with the matrix, but will agglomerate and cause abnormal grain growth during sintering, resulting in an increase in resistivity instead of a decrease. At the same time, the average grain size of the target material will also increase, while the relative density will significantly decrease. Therefore, the doping amount of the titanium element needs to be within a certain range.

[0084] It can be seen from the performance test results of Comparative Example 3 that only a certain amount of titanium dioxide is doped in Comparative Example 3, resulting in a relative density of the prepared target material of less than 90%. Too low a relative density will reduce the life of the target material, resulting in poor heat dissipation performance, and the target sputtering process is prone to instability, affecting the quality of the prepared oxide film.

[0085] It can be seen from Comparative Examples 4 and 5 that with the increase of the doping ratio, the relative performance of the target material does not show a trend of getting better and better. This is probably because the doping ratio is too large, and the doping elements and the indium oxide base cannot be evenly mixed and sintered, resulting in reduced performance. In addition, the average grain size of the target material is large, which also leads to low strength of the target material.

[0086] From the above analysis, it can be seen that the doping of gallium oxide and titanium dioxide will affect the resistivity of the target material. As the doping ratio of gallium oxide increases, the resistivity of the target material will show an increasing trend, but the effect of the increase in the doping ratio of titanium dioxide on the resistivity is opposite to that of gallium oxide. It can be seen from the test results that the effect of titanium dioxide on the resistivity is better than that of gallium oxide, and the increase in the doping amount of titanium dioxide can reverse the trend of gallium oxide reducing the resistivity of the target material. Therefore, Examples 4 and 6 of the present invention have achieved very low technical effects of target resistivity, and the oxide film prepared by the target material has excellent light transmittance, but the target material of Example 6 has a lower relative density. It is believed that the combination of Ga-O and Ti-O can prevent In 2 O 3The presence of oxygen vacancies in the matrix and the electrostatic force of oxygen vacancies on electrons produce ion scattering centers in the IGTO film. The reduction of oxygen vacancies increases the total performance of carrier mobility and light transmittance. 4+ Replace In 3+ It can provide more free electrons to make up for the defect of low carrier concentration. The high mobility caused by titanium and the low oxygen vacancy concentration caused by doping make the target material of the present invention and the film prepared by it have two advantages: low resistivity and high transmittance.

[0087] 2. Use a bending tester to perform bending fatigue test on oxide film;

[0088] The target material of Example 4 of the present invention and the traditional ITO target material of Comparative Example 1 were subjected to the aforementioned sputtering process to be made into thin films and then subjected to thousands of bending fatigue tests at different bending radii. The results are shown in Table 2.

[0089] Table 2 Bending fatigue test results of oxide films

[0090] Serial number Film Type Bending times Bending radius / mm Resistivity increase (%) 1 IGTO 5000 3 0 2 IGTO 5000 4 5.6 3 ITO 5000 3 3.4 4 ITO 5000 4 187 5 ITO 2500 3 0

[0091] From the above test results, it can be seen that when the number of bends is 5000 times and the bending radius is 3mm or 4mm, the resistance of the ITO film is more likely to increase after the bending fatigue test, and the increase is more obvious, while the resistance of the film made by the target material of the present invention does not change much, and the resistivity increase is greatly reduced compared with the ITO film. This shows that compared with the oxide film prepared by the traditional ITO target material, the IGTO film of the present invention has better flexibility and durability. At the same time, the IGTO target material of the present invention can be formed into an IGTO film using a damage-free deposition technology, which reduces the damage to the substrate when the film is formed, so that it can perform its performance more effectively.

[0092] The above is a detailed description of the embodiments of the present invention, but the present invention is not limited to the above embodiments. Various changes can be made within the knowledge of ordinary technicians in the relevant technical field without departing from the purpose of the present invention. In addition, the embodiments of the present invention and the features in the embodiments can be combined with each other without conflict.

Claims

1. An indium gallium titanium oxide target, characterized in that: The raw materials for preparation include 95-99 parts of indium oxide, 0.5-2 parts of gallium oxide and 0.6-3 parts of titanium dioxide by weight.

2. The indium gallium titanium oxide target according to claim 1, characterized in that: The preparation raw materials include 96.12-98.48 parts of indium oxide, 0.67-1.34 parts of gallium oxide and 0.85-2.54 parts of titanium dioxide by weight.

3. The indium gallium titanium oxide target according to claim 1 or 2, characterized in that: The preparation raw materials also include 1 to 5 parts of a dispersant and 1 to 5 parts of a binder.

4. The indium gallium titanium oxide target according to claim 3, characterized in that: The dispersant includes at least one of polyvinyl pyrrolidone, polyacrylamide, polyethylene glycol or hydrogenated nitrile rubber, and / or the binder includes at least one of polyvinyl alcohol, sodium polyacrylate, butyl rubber or cyanoacrylate.

5. The method for preparing an indium gallium titanium oxide target according to any one of claims 1 to 4, characterized in that: The following steps are involved: S1, mixing the indium oxide, the gallium oxide and the titanium dioxide, and then adding water, a dispersant and a binder to mix and grind; S2, spray drying and granulation to obtain mixed powder; S3, cold isostatic pressing and sintering to obtain indium gallium titanium oxide target.

6. The preparation method according to claim 5, characterized in that: The cold isostatic pressing pressure in step S3 is 100-400 MPa, and the holding time is 2-10 min.

7. The preparation method according to claim 5, characterized in that: The sintering in step S3 is sequentially carried out at 500-600° C. for 1-3 hours, at 900-1100° C. for 3-5 hours, at 1350-1400° C. for 6-8 hours in an oxygen atmosphere, and at 900-1100° C. for 1-3 hours.

8. A flexible oxide film, characterized in that: The oxide film is made of the indium gallium titanium oxide target material according to any one of claims 1 to 4, and the light transmittance of the oxide film is 92% to 99%.

9. A flexible OLED, characterized in that: Comprising the flexible oxide film as claimed in claim 8.

10. Use of the indium gallium titanium oxide target material according to any one of claims 1 to 4, the flexible oxide film according to claim 8, or the flexible OLED according to claim 9 in the field of displays.

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