Silver plane target material, preparation method and application thereof

Abstract

The application discloses a silver plane target material and a preparation method and application thereof, and belongs to the technical field of target materials, and comprises the following steps: (1) placing silver ingots in a continuous casting furnace, completely melting the silver ingots, and then continuously casting to obtain silver blanks; (2) heat-treating the silver blanks to obtain silver plates; (3) coarsely rolling the silver plates, and finely rolling the silver plates; (4) heat-treating the rolled silver plates to obtain the silver plane target material; the coarse rolling comprises 6-8 passes, and the deformation of a single pass is 10-15%; the fine rolling comprises 7-9 passes, and the deformation of a single pass is 2-9.9%; and the total deformation of the coarse rolling and the fine rolling is 71.25-77.50%. The silver ingots are completely melted, continuously cast, heat-treated, coarsely rolled, finely rolled and heat-treated, so that the average grain size of the target material is effectively reduced, the internal organization of the target material is uniformly distributed, and the target material is free of internal defects; and the method is suitable for preparing large-size silver plane target materials, has high utilization rate and low cost.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of target material, in particular to a silver plane target material and a preparation method and application thereof. BACKGROUND

[0002] Low-e glass has high visible light transmittance, low ultraviolet transmittance, ultralow emissivity and low heat transfer performance, and is often used in the fields of building material glass and automobile glass.

[0003] The main functional layer of the Low-e film is a silver layer, and a silver target material is plated on the surface of the glass in the form of a nanometer-level silver layer through a magnetron sputtering method. Silver is one of the materials with the lowest emissivity in nature, and can reduce the emissivity of the glass from 0.84 to 0.02-0.12. The film coating technology of Low-e glass is the key, and the target material used for film coating is the key consumable that determines success or failure.

[0004] With a substantial increase in market demand, higher requirements are put forward for the purity, quality, size and utilization rate of the target material. The target material has no cracks, inclusions and holes on the surface, has no defects in the interior, has fine and uniformly distributed grain structures, can obtain a silver film with uniform thickness and stable performance, and the utilization rate is relatively improved as the size of the target material is larger, and the total length of the Low-e glass target material can reach 4 meters.

[0005] In view of this, the present application is proposed. SUMMARY

[0006] The present application aims to overcome the deficiencies in the prior art and provide a silver plane target material and a preparation method and application thereof, which effectively reduce the average grain size of the target material, make the internal organization uniformly distributed and have no defects in the interior. The method is suitable for preparing a large-size silver plane target material, has high utilization rate, low cost and wide application prospect.

[0007] To achieve the above object, the technical scheme adopted by the present application is as follows:

[0008] A preparation method of a silver plane target material, comprising the following steps:

[0009] (1) placing a silver ingot in a continuous casting furnace, completely melting the silver ingot and then continuously casting to obtain a silver blank;

[0010] (2) heat treating the silver blank to obtain a silver plate;

[0011] (3) rough rolling and finish rolling the silver plate;

[0012] (4) heat treating the rolled silver plate to obtain a silver plane target material;

[0013] The rough rolling includes 6-8 passes, and the deformation of a single pass is 10-15%, for example, 10%, 11%, 12%, 13%, 14%, 15%, or a range formed by any two of the above values.

[0014] The fine rolling includes 7-9 passes, and the deformation of a single pass is 2-9.9%, for example, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 9.9%, or a range formed by any two of the above values.

[0015] The total deformation of the rough rolling and the fine rolling is 71.25-77.50%, for example, 60%, 62%, 65%, 68%, 70%, 72%, 75%, or a range formed by any two of the above values.

[0016] The present application creatively melts the silver ingot completely, and then performs continuous casting, heat treatment, rough rolling, fine rolling, and heat treatment, effectively reduces the average grain size of the target material, makes the internal structure uniform, and has no internal defects. The method is suitable for preparing large-size silver plane target material, has high utilization rate, low cost, and wide application prospect.

[0017] The heat treatment after the continuous casting can effectively eliminate the continuous casting defects and reduce the internal stress generated in the continuous casting process. The rough rolling and the fine rolling, and the strict control of the parameters of the rough rolling and the fine rolling can effectively refine the grains, ensure the uniformity of the internal structure of the silver target, and make the grains elongated after the rolling to be recovered and recrystallized, thereby refining the grains, eliminating the rolling stress, and avoiding abnormal growth of the grains.

[0018] As a preferred embodiment of the present application, the thickness reduction of the rough rolling is 57.5-66.25%, for example, 57.5%, 58%, 59%, 60%, 62%, 65%, 66%, 66.25%, or a range formed by any two of the above values.

[0019] As a preferred embodiment of the present application, the thickness reduction of the rough rolling is 57.5-61.25%.

[0020] As a preferred embodiment of the present application, the thickness reduction of the fine rolling is 32.20-35.50%.

[0021] As a preferred embodiment of the present application, the thickness reduction of the fine rolling is 18-36%, for example, 18%, 20%, 22%, 25%, 28%, 30%, 32%, 35%, 36%, or a range formed by any two of the above values.

[0022] As a preferred embodiment of the present invention, the rough rolling speed is 0.25 to 0.35 m / s, for example, it can be 0.25 m / s, 0.26 m / s, 0.28 m / s, 0.3 m / s, 0.32 m / s, 0.35 m / s or a range consisting of any two values ​​therein.

[0023] As a preferred embodiment of the present invention, the finishing rolling speed is 0.45 to 0.55 m / s, for example, it can be 0.45 m / s, 0.46 m / s, 0.48 m / s, 0.5 m / s, 0.52 m / s, 0.55 m / s or a range consisting of any two values ​​therein.

[0024] The rolling is carried out along the length direction without changing the direction.

[0025] As a preferred embodiment of the present invention, the purity of the silver ingot is ≥3N, for example, it can be 3N (99.9%), 3N2 (99.92%), 3N5 (99.95%), 3N8 (99.98%), 4N (99.99%), 5N (99.999), 6N (99.9999%) or a range consisting of any two of these values.

[0026] As a preferred embodiment of the present invention, the melting temperature of the silver ingot is 1000-1100°C, for example, it can be 1000°C, 1020°C, 1050°C, 1080°C, 1100°C or a range consisting of any two values ​​therein.

[0027] As a preferred embodiment of the present invention, the continuous casting stretching speed is 0.5 to 0.6 m / min.

[0028] As a preferred embodiment of the present invention, the temperature of the heat treatment in step (2) is 700-800°C, for example, it can be 700°C, 720°C, 750°C, 780°C, 800°C or a range consisting of any two values ​​therein.

[0029] As a preferred embodiment of the present invention, the heat treatment time in step (2) is 1h, 1.2h, 1.5h, 1.8h, 2h, 2.2h, 2.5h, 2.8h, 3h or a range consisting of any two of these values.

[0030] As a preferred embodiment of the present invention, the continuous casting stretching speed is 0.5 to 0.6 m / min, for example, it can be 0.5 m / min, 0.52 m / min, 0.55 m / min, 0.58 m / min, 0.6 m / min or a range consisting of any two values ​​therein.

[0031] As a preferred embodiment of the present application, the temperature of the heat treatment in step (4) is 300-400℃, for example, it can be 300℃, 320℃, 350℃, 380℃, 400℃ or a range between any two of the above values.

[0032] As a preferred embodiment of the present application, the time of the heat treatment in step (4) is 1h, 1.2h, 1.5h, 1.8h, 2h or a range between any two of the above values.

[0033] The present application also provides a silver plane target prepared by the above method.

[0034] The present application also provides an application of the plane target in preparing Low-e glass.

[0035] The present application has the advantages that: the silver ingot is completely melted, then continuous casting, heat treatment, rough rolling, finish rolling and heat treatment are performed, which effectively reduces the average grain size of the target material, makes the internal structure distribution uniform, and has no internal defects, the method is suitable for preparing large-size silver plane target, has high utilization rate, low cost and wide application prospect. BRIEF DESCRIPTION OF DRAWINGS

[0036] Figure 1 The silver plane target prepared by Example 1. DETAILED DESCRIPTION

[0037] In order to make the purpose, technical scheme and advantages of the embodiments of the present application more clear, the technical scheme of the embodiments of the present application will be described clearly and completely below. Obviously, the described embodiments are some embodiments of the present application, but not all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor fall within the scope of protection of the present application.

[0038] In the present application, the technical features described in an open way include both the closed technical scheme consisting of the listed features and the open technical scheme containing the listed features.

[0039] In the present application, when referring to a numerical interval, the above numerical interval is considered to be continuous and includes the minimum value and the maximum value of the range and each value between the minimum value and the maximum value, unless otherwise specified. Further, when a range is referred to as an integer, each integer between the minimum value and the maximum value of the range is included. In addition, when multiple ranges are provided to describe a feature or a characteristic, the ranges can be combined. In other words, unless otherwise specified, all the ranges disclosed herein should be understood to include any and all sub-ranges falling within the range.

[0040] In the present application, the specific dispersion, stirring treatment method is not particularly limited.

[0041] The components raw materials or instruments used in the embodiments and comparative examples of the present application are commercially available raw materials or instruments unless otherwise specified, and the component raw materials used in each parallel experiment are the same.

[0042] Example 1

[0043] A method for preparing a silver plane target material, comprising the following steps:

[0044] (1) After cleaning and drying silver ingots with a purity of 3N5 (99.95%), the silver ingots are put into a crucible and placed in a continuous casting furnace. After complete melting of the silver ingots at 1050℃, continuous casting is performed at a continuous casting stretching rate of 0.5 m / min, and the continuous casting billet size is 1100*250*80 mm, to obtain a silver billet;

[0045] (2) The silver billet is placed in a heating furnace and heat treated at 750℃ for 1 h to obtain a silver plate;

[0046] (3) The silver plate is rough-rolled and finish-rolled according to the parameters in Table 1. After rolling, the size of the target billet is 3738*255*23 mm, and the total deformation amount of rolling is 71.25%.

[0047] In Table 1, (S represents the length direction, and X represents the width direction)

[0048]

[0049]

[0050] (4) The silver plate after rolling is placed in a heating furnace and heat treated at 300℃ for 1 h. The obtained target billet is flattened and machined according to the drawing requirements to obtain a large-size silver plane target material with a size of 3720*248*20 mm. The grain size and distribution of the target material are as shown in Figure 1

[0051] Example 2

[0052] A method for preparing a silver plane target material, comprising the following steps:

[0053] (1) After cleaning and drying silver ingots with a purity of 3N5 (99.95%), the silver ingots are put into a crucible and placed in a continuous casting furnace. After complete melting of the silver ingots at 1050℃, continuous casting is performed at a continuous casting stretching rate of 0.5 m / min, and the continuous casting billet size is 1100*250*80 mm, to obtain a silver billet;

[0054] (2) The silver billet is placed in a heating furnace and heat treated at 750℃ for 1 h to obtain a silver plate;

[0055] ​(3) The silver plate is rough-rolled and finish-rolled according to the parameters in Table 2, and the size of the target blank after rolling is 3730*256*20mm, and the total deformation amount of rolling is 75%.

[0056] Table 2 (S represents the length direction, and X represents the width direction)

[0057]

[0058]

[0059] (4) The silver plate after rolling is placed into a heating furnace, and heat-treated at 300℃ for 1h, and the obtained target blank is flattened, and mechanically processed according to the drawing requirements, to obtain a large-size silver flat target material with a size of 3710*245*18mm.

[0060] Example 3

[0061] A method for preparing a silver flat target material, comprising the following steps:

[0062] (1) A silver ingot with a purity of 3N5 (99.95%) is cleaned and dried, and then put into a crucible and placed in a continuous casting furnace, and after the silver ingot is completely melted at 1050℃, continuous casting is performed at a continuous casting stretching rate of 0.5m / min, and the size of the continuous casting blank is 1100*250*80mm, to obtain a silver blank;

[0063] (2) The silver blank is placed into a heating furnace, and heat-treated at 750℃ for 1h, to obtain a silver plate;

[0064] (3) The silver plate is rough-rolled and finish-rolled according to the parameters in Table 3, and the size of the target blank after rolling is 3720*256*18mm, and the total deformation amount of rolling is 77.5%.

[0065] Table 3 (S represents the length direction, and X represents the width direction)

[0066]

[0067]

[0068] (4) The silver plate after rolling is placed into a heating furnace, and heat-treated at 300℃ for 1h, and the obtained target blank is flattened, and mechanically processed according to the drawing requirements, to obtain a large-size silver flat target material with a size of 3700*248*16mm.

[0069] Example 4

[0070] A method for preparing a silver flat target material, comprising the following steps:

[0071] (1) The silver ingot with purity of 3N5 (99.95%) is washed and dried, and then is put into a crucible and placed in a continuous casting furnace. The silver ingot is completely melted at 1050°C, and then is continuously cast at a drawing speed of 0.5 m / min. The size of the continuously cast billet is 1100*250*80 mm, and a silver billet is obtained.

[0072] (2) The silver billet is put into a heating furnace and is heat treated at 750°C for 1 h, and a silver plate is obtained.

[0073] (3) The silver plate is rough-rolled and finish-rolled according to the parameters in Table 4. The size of the target billet after rolling is 3738*255*23 mm, and the total deformation amount of rolling is 71.25%.

[0074] In Table 4, (S represents the length direction, and X represents the width direction)

[0075]

[0076] (4) The silver plate after rolling is put into a heating furnace and is heat treated at 400°C for 1 h. The target billet obtained is flattened, and is mechanically processed according to the drawing requirements, and a large-size silver flat target material with a size of 3720*248*20 mm is obtained.

[0077] Comparative Example 1

[0078] A method for preparing a silver flat target material, comprising the following steps:

[0079] (1) The silver ingot with purity of 3N5 (99.95%) is washed and dried, and then is put into a crucible and placed in a continuous casting furnace. The silver ingot is completely melted at 1050°C, and then is continuously cast at a drawing speed of 0.5 m / min. The size of the continuously cast billet is 1100*250*80 mm, and a silver billet is obtained.

[0080] (2) The silver billet is put into a heating furnace and is heat treated at 750°C for 1 h, and a silver plate is obtained.

[0081] (3) The silver plate is rough-rolled and finish-rolled according to the parameters in Table 5. The size of the target billet after rolling is 3738*255*23 mm, and the total deformation amount of rolling is 71.25%, and a large-size silver flat target material is obtained.

[0082] In Table 5, (S represents the length direction, and X represents the width direction)

[0083]

[0084] Comparative Example 2

[0085] A method for preparing a silver flat target material, comprising the following steps:

[0086] (1) The silver ingot with purity of 3N5 (99.95%) is washed and dried, and then is put into a crucible and placed in a continuous casting furnace. The silver ingot is completely melted at 1050°C, and then is continuously cast at a drawing speed of 0.5 m / min. The size of the continuously cast billet is 1100*250*80 mm, and a silver billet is obtained;

[0087] (2) The silver billet is put into a heating furnace and is heat treated at 750°C for 1 h, and a silver plate is obtained;

[0088] (3) The silver plate is rough-rolled and finish-rolled according to the parameters in Table 6. The size of the target billet after rolling is 3738*255*23 mm, and the total deformation amount of rolling is 71.25%.

[0089] In Table 6, (S represents the length direction, and X represents the width direction)

[0090]

[0091] (4) The silver plate after rolling is put into a heating furnace and is heat treated at 450°C for 1 h. The target billet obtained is flattened, and is mechanically processed according to the requirements of the drawing, and a large-size silver flat target material with a size of 3720*248*20 mm is obtained.

[0092] Comparative Example 3

[0093] A method for preparing a silver flat target material, comprising the following steps:

[0094] (1) The silver ingot with purity of 3N5 (99.95%) is washed and dried, and then is put into a crucible and placed in a continuous casting furnace. The silver ingot is completely melted at 1050°C, and then is continuously cast at a drawing speed of 0.5 m / min. The size of the continuously cast billet is 1100*250*80 mm, and a silver billet is obtained;

[0095] (2) The silver billet is put into a heating furnace and is heat treated at 750°C for 1 h, and a silver plate is obtained;

[0096] (3) The silver plate is rough-rolled according to the parameters in Table 7. The size of the target billet after rolling is 3738*255*23 mm, and the total deformation amount of rolling is 71.25%.

[0097] In Table 7, (S represents the length direction, and X represents the width direction)

[0098]

[0099] (4) The silver plate after rolling is put into a heating furnace and is heat treated at 300°C for 1 h. The target billet obtained is flattened, and is mechanically processed according to the requirements of the drawing, and a large-size silver flat target material with a size of 3720*248*20 mm is obtained.

[0100] Comparative Example 4

[0101] A method for preparing a silver plane target material, comprising the following steps:

[0102] (1) After cleaning and drying silver ingots with a purity of 3N5 (99.95%), the silver ingots are put into a crucible and placed in a continuous casting furnace. After the silver ingots are completely melted at 1050°C, continuous casting is performed at a casting speed of 0.5 m / min, and the size of the continuous casting billet is 1100*250*80 mm, to obtain a silver billet;

[0103] (2) The silver billet is placed in a heating furnace and heat treated at 750°C for 1 h to obtain a silver plate;

[0104] (3) The silver plate is rough-rolled and finish-rolled according to the parameters in Table 8. After rolling, the size of the target billet is 3735*256*23 mm, and the total deformation of rolling is %.

[0105] In Table 8, (S represents the length direction, and X represents the width direction)

[0106]

[0107]

[0108] (4) The silver plate after rolling is placed in a heating furnace and heat treated at 300°C for 1 h. The obtained target billet is flattened and machined according to the drawing requirements to obtain a large-size silver plane target material with a size of 3720*248*20 mm.

[0109] Test Example

[0110] The target materials of the examples and comparative examples are subjected to water immersion ultrasonic C scanning to observe whether there are defects in the interior of the target materials.

[0111] The target materials of the examples and comparative examples are subjected to metallographic analysis to determine whether the internal structure of the target materials is uniform and the average grain size.

[0112] Table 10

[0113]

[0114]

[0115] Finally, it should be noted that the above examples are only used to illustrate the technical solutions of the present application and not to limit the protection scope of the present application. Although the present application has been described in detail with reference to the preferred embodiments, those skilled in the art should understand that the technical solutions of the present application can be modified or replaced by equivalents without departing from the essence and scope of the technical solutions of the present application.

Claims

1. A method for preparing a silver planar target, characterized in that: The following steps are involved: (1) Placing the silver ingot in a continuous casting furnace, melting the silver ingot completely and then continuously casting it to obtain a silver billet; (2) heat treating the silver blank to obtain a silver plate; (3) Rough rolling and finish rolling of the silver plate; (4) heat treating the rolled silver plate to obtain a silver flat target; The rough rolling process includes 6 to 8 passes, and the deformation of each pass is 10 to 15%; The finishing rolling process includes 7 to 9 passes, and the deformation of each pass is 2 to 9.9%; The total deformation of the rough rolling and the finish rolling is 71.25-77.50%; The heat treatment temperature in step (4) is 300-400° C., and the heat treatment time is 1-2 hours.

2. The method for preparing a silver planar target according to claim 1, wherein: The thickness reduction during the rough rolling is 57.5-66.25%; and / or The thickness reduction during the finish rolling is 18-36%.

3. The method for preparing a silver planar target according to claim 1, wherein: The rough rolling speed is 0.25-0.35 m / s; and / or The speed of the finish rolling is 0.45-0.55 m / s.

4. The method for preparing a silver planar target according to claim 1, wherein: The purity of the silver ingot is ≥3N.

5. The method for preparing a silver planar target according to claim 1, wherein: The melting temperature of the silver ingot is 1000-1100°C.

6. The method for preparing a silver planar target according to claim 1, wherein: The continuous casting stretching speed is 0.5-0.6 m / min.

7. The method for preparing a silver planar target according to claim 1, wherein: The heat treatment temperature in step (2) is 700-800° C., and the heat treatment time is 1-3 hours.

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