A method for preparing a sputtering planar silver-indium alloy target

Abstract

The invention relates to the technical field of low-radiation coated glass, and provides a method for preparing a sputtering plane silver-indium alloy target material. The radiation coated glass adopts silver-indium alloy to form infrared reflection, and compared with pure silver, the moisture resistance and water vapor resistance are significantly improved, and the white spot defects caused by the agglomeration of silver atoms are avoided, and strong infrared reflection ability and low emissivity can be maintained, and the silver-indium alloy target material is resistant to heat bending, tempering and processing. The density and uniformity of the silver-indium alloy target material structure are effectively improved by adopting smelting and pouring treatment; the composition of the alloy target material ingot is homogenized by adopting homogenization annealing treatment, and the component segregation and structural inhomogeneity are eliminated; and the target material composition is uniform and the grain distribution is uniform by rolling and low-temperature annealing.

Description

Technical Field

[0001] The invention relates to the technical field of low-radiation coated glass, and in particular to a method for preparing a sputtering planar silver-indium alloy target material. Background Art

[0002] Low-E coated glass, also known as Low-E glass, is a new type of high-end low-E glass. It is a film product composed of multiple layers of metals and other compounds, including a silver layer, coated on the glass surface. Due to the low-radiation characteristics of the silver layer, Low-E glass has a high transmittance to visible light, a high reflectivity to infrared rays, and excellent heat insulation and thermal insulation properties.

[0003] In the existing technology, low-emissivity films are all prepared by magnetron sputtering. Traditional low-emissivity coated glass is based on a very thin single or double silver film layer. It is sandwiched between two anti-reflective metal oxide protective layers to prevent oxidation, sulfidation and other performance requirements of the silver layer, so as to stabilize the performance of the product and meet the requirements of the product color. In addition, in order to further protect the silver film layer and avoid erosion of the silver film layer during the subsequent sputtering reaction process, a "barrier layer" is added to one side of the silver film layer. Therefore, a method for preparing a sputtering planar silver-indium alloy target is required. Summary of the invention

[0004] In view of this, the purpose of the present invention is to provide a method for preparing a sputtering planar silver-indium alloy target material to solve the problems arising in the background technology.

[0005] Based on the above purpose, the present invention provides a method for preparing a sputtering planar silver-indium alloy target, wherein the target comprises the following components in weight percentage: 0.1%-0.6% indium and 99.4%-99.9% silver;

[0006] The method comprises the following steps:

[0007] Step 1, melting silver and indium in a protective atmosphere to obtain a liquid alloy;

[0008] Step 2, casting the liquid alloy to obtain a silver-indium alloy ingot;

[0009] Step three, subjecting the silver-indium alloy ingot to homogenization treatment, forging, rolling, low-temperature annealing, CNC machining, binding, flaw detection, and post-treatment in sequence to obtain a silver-indium alloy target.

[0010] Preferably, the smelting in step 1 is as follows:

[0011] Under a protective atmosphere, silver block and indium block raw materials are placed in a crucible for smelting to obtain a silver-indium alloy ingot.

[0012] Preferably, the vacuum degree during the smelting process in step 1 is ≤6×10 -2 mmH, melting temperature 1000℃-1200℃, melting time 0.5~1h, pour the alloy melt into a heated mold, and the mold temperature is below 700℃.

[0013] Preferably, the temperature of the homogenization annealing in step three is 600° C. to 800° C., and the holding time is 1 to 2 hours.

[0014] Preferably, the forging in step three is hot forging, the hot forging heating temperature is 600° C.-800° C., and the forging ratio is 3.5-4.5.

[0015] Preferably, the step three of rolling includes hot rolling and cold rolling in sequence.

[0016] Preferably, the hot rolling heating temperature is 600° C.-700° C., the hot rolling is performed for 6 passes, the deformation amount per pass is 25%-25%-25%-25%-20%-3%, the total deformation amount is 86%, and the first 5 passes of the 6 passes are subjected to reversing rolling.

[0017] Preferably, the alloy billet obtained after hot rolling is cold rolled with a deformation amount of 17%, and then reversed and flattened.

[0018] Preferably, the obtained cold-rolled alloy billet is subjected to annealing heat treatment, the heat treatment temperature is 350° C.-400° C., and the holding time is 1 h to 3 h.

[0019] Beneficial effects of the present invention: The radiation coated glass of the present invention adopts silver-indium alloy to form infrared reflection, which significantly improves the resistance to moisture and water vapor compared with pure silver, avoids white spot defects caused by silver atom agglomeration, and can still maintain strong infrared reflection ability and low emissivity, and is resistant to heat bending, tempering and processing. The target material of the present invention can provide a AgIn alloy barrier layer for high-quality low-radiation coated glass with high transmittance, stable performance, lower shading coefficient, excellent optical and thermal properties, and color closer to natural color, and can ensure that the silver layer is not oxidized and discolored as much as possible during the tempering process, and the performance of each film layer is more stable, ensuring that the product performance remains consistent before and after tempering. The present invention effectively improves the density and uniformity of the silver-indium alloy target material structure by using smelting and pouring treatment; the alloy target material ingot composition is homogenized by using homogenization annealing treatment, and the component segregation and structural inhomogeneity are eliminated; the target material composition is uniform and the grain distribution is uniform by rolling and low-temperature annealing. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] In order to more clearly illustrate the technical solutions in the present invention or the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings in the following description are only for the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0021] Figure 1 It is a process flow chart of the present invention;

[0022] Figure 2 It is a metallographic structure diagram of the silver-indium alloy target material obtained by implementing the present invention;

[0023] Figure 3 It is a schematic diagram of the silver-indium alloy target material prepared by the implementation of the present invention. DETAILED DESCRIPTION

[0024] In order to make the objectives, technical solutions and advantages of the present invention more clearly understood, the present invention is further described in detail below in conjunction with specific embodiments.

[0025] It should be noted that, unless otherwise defined, the technical terms or scientific terms used in the present invention should be understood by people with ordinary skills in the field to which the present invention belongs. The "first", "second" and similar words used in the present invention do not indicate any order, quantity or importance, but are only used to distinguish different components. "Include" or "comprise" and similar words mean that the elements or objects appearing before the word include the elements or objects listed after the word and their equivalents, without excluding other elements or objects. "Connect" or "connected" and similar words are not limited to physical or mechanical connections, but may include electrical connections, whether direct or indirect. "Up", "down", "left", "right" and the like are only used to indicate relative positional relationships. When the absolute position of the described object changes, the relative positional relationship may also change accordingly.

[0026] This embodiment provides a method for preparing a sputtering planar silver-indium alloy target, wherein the target material is selected from indium with a purity of 99.99% and silver with a purity of 99.99%, in accordance with a ratio of 99.46% by mass of indium and 0.54% by mass of indium. The alloy target obtained by adding indium element to pure silver increases the strength of silver, thereby producing a grain refinement effect. Secondly, the indium added during the annealing process can play a role in solid solution strengthening, which can greatly improve the adhesion of the silver alloy film and improve its surface roughness while maintaining good conductivity and reflectivity of the film.

[0027] like Figure 1 As shown, the preparation method comprises the following steps:

[0028] S1, adding silver and indium into a vacuum medium frequency induction melting furnace, and starting to power on and heat up when the vacuum degree reaches 0.6 Pa, and melting into liquid alloy when the temperature reaches 1178°C;

[0029] S2, in an argon atmosphere, heat preservation for 30 minutes, pouring and depositing the liquid alloy, breaking the vacuum and cooling to obtain a silver-indium alloy ingot, wherein the inert gas pressure is set to 0.8 Pa;

[0030] S3, high temperature homogenization annealing of the silver-indium alloy ingot, the temperature is controlled at 650°C, and the temperature is kept for 1.5 hours;

[0031] S4, hot forging the obtained alloy ingot, wherein the hot forging heating temperature is 600° C. and the forging ratio is 4.0;

[0032] S5, the rough ingot is subjected to 6 passes of reciprocating rolling in a two-roll mill, and subjected to low-temperature annealing treatment in the middle, the annealing temperature is 500°C, the holding time is 1.5h, the pass deformation is 25%-25%-25%-25%-20%-3%, and the total deformation is 86%. In these six passes, the first five passes are subjected to reversing rolling;

[0033] S6, the alloy billet obtained after hot rolling is cold rolled with a deformation amount of 17%, and then reversed and flattened;

[0034] S7, performing recrystallization annealing, controlling the temperature to 390°C, and keeping the temperature for 1 hour to obtain a silver-indium alloy crude ingot,

[0035] S8, the silver-indium alloy rough ingot is subjected to CNC machining, binding, flaw detection, and post-processing in sequence to obtain a silver-indium alloy target material, and the average grain size of the silver-indium alloy target material is 26um. The CNC machining performs milling on the surface of the rough ingot, and the processing amount of the milling process is 0.5mm to 2mm, and more preferably 0.7mm. The present invention has no special limitation on the specific operation of the milling process, and the conventional CNC machining process in the field can be used.

[0036] Binding is to bind the silver-indium alloy target to the copper backing plate. The binding process needs to be pre-treated first, the purpose is to make the target and the backing plate fit together fully, and then use the contact material filler to bond the target and the backing plate, that is, configure the molten bonding material on each heated surface, and apply the bonding material while applying ultrasonic vibration using an ultrasonic soldering iron equipped with a heater. Metallization can promote the removal of dirt on each surface, the reduction of oxide film, the removal of bubbles, etc., and can make the bonding material fuse to each surface, so that the target and the backing plate can be fully bound together.

[0037] The bound silver-indium alloy target material needs to be inspected for flaws. A flat metal target ultrasonic flaw detector is used to inspect the welding rate of the bound target material. The welding rate is ≥95%.

[0038] The silver-indium alloy target after flaw detection needs to be post-processed. The surface is treated with a scouring pad and the roughness of the target surface is tested using a roughness tester. The Ra is 0.45.

[0039] like Figure 2 and 3 As shown, a silver-indium alloy target material is finally obtained, and the average grain size of the silver-indium alloy target material is 26 um. Figure 2 It can be seen that the grains are evenly distributed, the composition is uniform, and the density is high.

[0040] It should be understood by those skilled in the art that the discussion of any of the above embodiments is merely exemplary and is not intended to imply that the scope of the present invention is limited to these examples; under the concept of the present invention, the technical features in the above embodiments or different embodiments may also be combined, the steps may be implemented in any order, and there are many other variations of the different aspects of the present invention as described above, which are not provided in detail for the sake of simplicity. Any omissions, modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention shall be included in the scope of protection of the present invention.

Claims

1. A method for preparing a sputtering planar silver-indium alloy target, characterized in that: The target material comprises the following components in weight percentage: 0.1%-0.6% indium and 99.4%-99.9% silver; The method comprises the following steps: Step 1, melting silver and indium in a protective atmosphere to obtain a liquid alloy; Step 2, casting the liquid alloy to obtain a silver-indium alloy ingot; Step three, subjecting the silver-indium alloy ingot to homogenization treatment, forging, rolling, low-temperature annealing, CNC machining, binding, flaw detection, and post-treatment in sequence to obtain a silver-indium alloy target.

2. The method for preparing a sputtering planar silver-indium alloy target according to claim 1, characterized in that: The smelting in step 1 is as follows: in a protective atmosphere, silver block and indium block raw materials are placed in a crucible for smelting to obtain a silver-indium alloy ingot.

3. The method for preparing a sputtering planar silver-indium alloy target according to claim 2, characterized in that: The vacuum degree during the smelting process in step 1 is ≤6×10 -2 mmH, melting temperature 1000℃-1200℃, melting time 0.5~1h, pour the alloy melt into a heated mold, and the mold temperature is below 700℃.

4. The method for preparing a sputtering planar silver-indium alloy target according to claim 1, characterized in that: The temperature of the homogenization annealing in step three is 600° C. to 800° C., and the holding time is 1 to 2 hours.

5. The method for preparing a sputtering planar silver-indium alloy target according to claim 1, characterized in that: The forging in step three is hot forging, the hot forging heating temperature is 600° C.-800° C., and the forging ratio is 3.5-4.

5.

6. The method for preparing a sputtering planar silver-indium alloy target according to claim 1, characterized in that: The step three of rolling includes hot rolling and cold rolling in sequence.

7. The method for preparing a sputtering planar silver-indium alloy target according to claim 6, characterized in that: The hot rolling heating temperature is 600° C.-700° C., the hot rolling is performed for 6 passes, the deformation amount of each pass is 25%-25%-25%-25%-20%-3%, and the total deformation amount is 86%. Among the six passes, the first 5 passes are all subjected to reversing rolling.

8. The method for preparing a sputtering planar silver-indium alloy target according to claim 7, characterized in that: The alloy billet obtained after hot rolling is cold rolled with a deformation amount of 17%, and then reversed and flattened.

9. The method for preparing a sputtering planar silver-indium alloy target according to claim 8, characterized in that: The obtained cold-rolled alloy billet is subjected to annealing heat treatment, the heat treatment temperature is 350° C.-400° C., and the heat preservation time is 1 h to 3 h.

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