Plane target material sintering tool and sintering process thereof

Abstract

The invention relates to the technical field of target material sintering, and provides a planar target material sintering tool which comprises at least two placing frames, and the placing frames are stacked one by one to form a plurality of bearing positions used for placing planar target materials; the placing frame consists of a pair of symmetrically arranged supporting blocks, at least one beam arranged on the pair of supporting blocks and a boron plate lapped on the upper end surfaces of the supporting blocks; the upper end face of the supporting block and the upper end face of the beam are located on the same horizontal plane. A gap exists between the lower end face of the beam and the upper end face of the plane target material, the sintering tool forms a plurality of bearing positions used for containing the formed biscuits by stacking the containing frames, the containing frames are high in strength at the high temperature, not prone to deformation and capable of stably supporting the formed biscuits, meanwhile, the space of the bearing positions is reasonable, all layers are evenly heated, and the sintering quality is good; the invention further discloses a planar target material sintering process based on the sintering tool. The planar target material sintering process has the advantages that a plurality of formed biscuits can be sintered at a time, and the quality of sintered target materials is high.

Description

Technical Field

[0001] The invention relates to the technical field of target material sintering, in particular to a planar target material sintering tool and a sintering process thereof. Background Art

[0002] Indium tin oxide thin film has the advantages of high transparency and good conductivity. It is widely used in transparent electrodes for flat panel display devices, window materials for solar cells and anti-static conductive films. At present, the methods for forming indium tin oxide thin films mainly include chemical methods such as thermal spray decomposition and chemical vapor deposition, as well as physical methods such as electron beam deposition and sputtering deposition. Among them, sputtering deposition is easy to be applied to large areas, and high-performance films can be formed efficiently, and are widely used in many fields. The formation of high-quality indium tin oxide thin films by sputtering deposition requires high-density indium tin oxide targets. These high-density indium tin oxide targets are usually made of powders with a certain size and composition. After the molded body is manufactured, the molded body is sintered at high temperature in a sintering furnace.

[0003] When a conventional loading rack is used to sinter an ITO molded body, due to the high sintering temperature, a weak loading rack will be trapped, which will cause the ITO sintered body to deform, thereby increasing the subsequent processing amount of the ITO sintered body.

[0004] CN117105634A discloses a method for sintering ITO planar targets by stacking, which includes raw material selection, slurry preparation, spray granulation, primary molding, secondary molding, and target sintering. The target sintering of the above patent adopts stacking, which increases the number of secondary blanks processed in a single process, thereby reducing the sintering cost, and the target prepared by stacking is less in curvature than the target prepared without stacking. The stacking of the method uses zirconium oxide particles to separate the secondary blanks. Due to the lack of stable support, it is still difficult to ensure that the secondary blanks do not deform during the sintering process in actual work, and even the deformation of the lower secondary blanks causes all processed secondary blanks to be defective. In addition, the ITO planar target needs to continuously introduce oxygen during sintering to suppress the volatilization of indium oxide and tin oxide during sintering. The stacking method of the above patent makes it difficult for the target to maintain a good oxidizing atmosphere, resulting in the volatilization of indium oxide and tin oxide and deformation.

[0005] Based on this, the technical problem solved in this case is: how to solve the problem that the current stacked sintered green billets cause deformation of the formed green billets. Summary of the invention

[0006] In order to solve the above technical problems, the present invention provides a planar target sintering tool. The sintering tool forms a plurality of bearing positions for placing formed blanks by stacking placement racks. The placement racks have high strength at high temperatures and are not easily deformed. The placement racks have a stable structure and can stably support the formed blanks. A planar target sintering process based on the above sintering tool is also disclosed, which has the advantages of being able to sinter multiple formed blanks at a single time and having high quality sintered targets.

[0007] The technical solution of the present invention is:

[0008] A planar target sintering tool comprises at least two placement racks, which are stacked one by one to form a plurality of bearing positions for placing planar targets; the placement racks are composed of a pair of symmetrically arranged support blocks, at least one beam arranged on the pair of support blocks, and a boron plate overlapped on the upper end surface of the support block; the upper end surface of the support block and the upper end surface of the beam are located on the same horizontal plane; there is a gap between the lower end surface of the beam and the upper end surface of the planar target.

[0009] The present invention mainly solves the problem of deformation of the planar target due to deformation of the boron plate at high temperature by optimizing the structural design of the support block and the beam, and significantly improves the flatness of the planar target. In addition, the gap design of the present invention is more conducive to the contact between oxygen and the target blank, and multiple planar targets can be sintered at one time, and each layer of the planar target can maintain extremely high uniformity.

[0010] In the above-mentioned planar target sintering tooling, the support block is provided with at least one groove; the two ends of the beam are respectively overlapped in the grooves of a pair of support blocks.

[0011] In the above-mentioned planar target sintering tool, the gap between the lower end surface of the beam and the upper end surface of the planar target is not less than twice the thickness of the target.

[0012] In the above-mentioned planar target sintering tool, the boron plate is made of aluminum oxide or recrystallized silicon carbide.

[0013] In the above-mentioned planar target sintering tool, the support block is made of aluminum oxide or recrystallized silicon carbide.

[0014] In the above-mentioned planar target sintering tool, the beam is made of recrystallized silicon carbide.

[0015] A planar target sintering process is also disclosed. Based on any of the planar target sintering tools described above, the green blank is formed into an indium tin oxide target blank, comprising the following steps:

[0016] Step 1, laying aluminum oxide powder on the bearing position of the placement rack, and placing the indium tin oxide target blank on the bearing position;

[0017] Step 2, stack another placement rack on the above-mentioned carrying position, return to step 1, and enter step 3 until the preset single sintering quantity is reached;

[0018] Step 3, sintering the flat target sintering tooling with the indium tin oxide target blank placed thereon, introducing oxygen at a rate of 10 to 15 L / min, and at a rate of 0.5 to 1.5 ° C / min, including but not limited to 0.5 ° C / min, 0.6 ° C / min, 0.7 ° C / min, 0.8 ° C / min, 0.9 ° C / min, 1.0 ° C / min, 1.1 ° C / min, 1.2 ° C / min, 1.3 ° C / min, 1 .4°C / min, 1.5°C / min heating rate to the sintering temperature, the sintering temperature is 1200°C to 1600°C, including but not limited to 1200°C, 1250°C, 1300°C, 1350°C, 1400°C, 1450°C, 1500°C, 1550°C, 1600°C, and heat preservation for 8 to 15 hours, including but not limited to 8h, 9h, 10h, 11h, 12h, 13h, 14h, 15h;

[0019] Step 4: Cool down to room temperature to obtain an ITO planar target.

[0020] In the above-mentioned planar target sintering process, the particle size of the aluminum oxide powder is 100 to 700 μm.

[0021] In the above-mentioned planar target sintering process, during the planar target sintering process, the number of layers of the placement rack does not exceed 8 layers.

[0022] In the above-mentioned planar target sintering process, the sintering temperature in step 3 is 1300℃~1500℃, including but not limited to 1300℃, 1350℃, 1400℃, 1450℃, 1500℃, and the temperature is kept for 10~12h, including but not limited to 10h, 11h, 12h.

[0023] One of the above technical solutions of the present invention has at least one of the following advantages or beneficial effects:

[0024] The sintering tool of the present invention forms a plurality of bearing positions for placing the formed blanks by stacking the placing racks, the placing racks have high strength at high temperatures, are not easily deformed, and the structure of the placing racks is stable and can stably support the formed blanks, while the space of the bearing positions is reasonable, the heating of each layer is uniform, and the sintering quality is good. In addition, the design of the beam can make the supporting structure more stable, the thickness requirement of the boron plate can be reduced, and the problem of large deviation of the flatness of the planar target caused by the deformation of the boron plate is avoided.

[0025] Also disclosed is a planar target sintering process based on the sintering tooling, which has the advantages of being able to sinter a plurality of formed green blanks at a single time and having high quality of sintered target materials. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] Figure 1 This is a schematic diagram of the three-dimensional structure of the sintering tooling of Example 1 of the present application;

[0027] Figure 2 It is a front view schematic diagram of the sintering tooling of Example 1 of the present application;

[0028] Figure 3 This is a front view schematic diagram of the sintering tooling of Comparative Example 2 of the present application.

[0029] Description of reference numerals:

[0030] 1. Placement rack; 11. Support block; 12. Beam; 13. Boron plate; a. Load-bearing position; b. Forming blank. DETAILED DESCRIPTION

[0031] The technical solutions in the embodiments of the present invention are described clearly and completely below. 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, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0032] Example 1

[0033] refer to Figure 1 , 2 A planar target sintering tool comprises five placement racks 1, which are stacked one by one to form five bearing positions a for placing planar targets; the placement racks 1 are composed of a pair of symmetrically arranged support blocks 11, three beams 12 arranged on the pair of support blocks 11, and a boron plate 13 overlapped on the upper end surface of the support block 11; the upper end surface of the support block 11 and the upper end surface of the beam 12 are located on the same horizontal plane; there is a gap between the lower end surface of the beam 12 and the upper end surface of the planar target.

[0034] In the above-mentioned planar target sintering tooling, the support block 11 is provided with three equally spaced grooves; the two ends of the three beams 12 are respectively overlapped in the grooves of a pair of support blocks 11 .

[0035] Specifically, in this embodiment, the height of the support block 11 is 10 cm, the height of the beam 12 is 5 cm, and the thickness of the formed blank b is 2 cm; therefore, in this embodiment, when the beam 12 is placed in the groove, the distance between the lower end surface of the beam 12 and the formed blank b is 3 cm. More specifically, in this embodiment, the thickness of the boron plate 13 is 1 cm.

[0036] Under the above design, a wind cavity through which oxygen can pass is formed between the formed blank b and the boron plate 13. Specifically, Figure 1As shown, in this embodiment, four air cavities are formed by stacking five placement racks 1, and the topmost formed blank b is completely exposed.

[0037] More specifically, the boron plate 13, the support block 11, and the beam 12 are all made of recrystallized silicon carbide.

[0038] A planar target sintering process, based on the above-mentioned planar target sintering tooling, forms a blank b into an indium tin oxide target blank, comprising the following steps:

[0039] Step 1: Use a 40-mesh screen to lay aluminum oxide powder on the bearing position a of the placement rack 1, and at least make the aluminum oxide powder cover the bearing position a. As for the laying thickness of the aluminum oxide powder, this application does not make a specific limitation. Specifically in this embodiment, the thickness of the aluminum oxide powder is 0.5 mm. After the laying is completed, the indium tin oxide target blank is placed on the bearing position a;

[0040] Step 2, stack another placement rack 1 on the above-mentioned carrying position a, and return to step 1 until the stacking reaches 5 layers;

[0041] Step 3, sintering the planar target sintering tool, introducing oxygen at a rate of 10 L / min, heating to 1500° C. at a heating rate of 1.5° C. / min, and keeping warm for 10 hours;

[0042] Step 4: Cool down to room temperature to obtain an ITO planar target.

[0043] By observing the sintering tools of each layer of planar target, the boron plates 13 of each layer are not deformed, the warpage of the top ITO planar target is 1.0 mm, and the relative density is 99.2%, and the average warpage of the remaining lower ITO planar targets is 1.2 mm, and the relative density is 98.5%.

[0044] Example 2

[0045] It is basically the same as the sintering tooling of Example 1, except that the height of the support block 11 is 10 cm, the height of the beam 12 is 4 cm, and the thickness of the formed blank b is 2 cm; therefore, in this embodiment, when the beam 12 is placed in the groove, the distance between the lower end surface of the beam 12 and the formed blank b is 4 cm.

[0046] The sintering tool of this embodiment is used to carry out the sintering process which is completely the same as that of the above-mentioned embodiment 1 to obtain an ITO planar target;

[0047] By observing the sintering fixtures of each layer of the planar target material, it was found that the boron plates 13 of each layer were not deformed, the warpage of the ITO planar target material was 1.0 mm, and the relative density was 99.2%.

[0048] Example 3

[0049] It is basically the same as the sintering tooling of Example 1, except that the height of the support block 11 is 10 cm, the height of the beam 12 is 3 cm, and the thickness of the formed blank b is 2 cm; therefore, in this embodiment, when the beam 12 is placed in the groove, the distance between the lower end surface of the beam 12 and the formed blank b is 5 cm.

[0050] The sintering tool of this embodiment is used to carry out the sintering process which is completely the same as that of the above-mentioned embodiment 1 to obtain an ITO planar target;

[0051] By observing the sintering fixtures of each layer of the planar target material, it was found that the boron plates 13 of each layer were not deformed, the warpage of the ITO planar target material was 1.0 mm, and the relative density was 99.2%.

[0052] Example 4

[0053] It is basically the same as Example 1, except that the height of the support block 11 is 10 cm, the height of the beam 12 is 6 cm, and the thickness of the formed blank b is 2 cm; therefore, in this embodiment, when the beam 12 is placed in the groove, the distance between the lower end surface of the beam 12 and the formed blank b is 2 cm.

[0054] The sintering tool of this embodiment is used to carry out the sintering process which is completely the same as that of the above-mentioned embodiment 1 to obtain an ITO planar target;

[0055] By observing the sintering tooling of each layer of planar target, the boron plate 13 is not deformed, and the relative density of the topmost ITO planar target is not significantly different from that of Examples 1 to 3, but the average warpage of the ITO planar target in the lower layer is 1.6 mm, and the relative density is 97.2%. Compared with Examples 1 to 3, the warpage of the ITO planar target in the lower layer is higher and the relative density is lower. It is speculated that the reason is that the reduction in the volume of the wind cavity causes oxygen to be unable to fully contact the ITO planar target, causing the volatilization of indium oxide and tin oxide.

[0056] Example 5

[0057] It is basically the same as Example 2, except that oxygen is introduced at a rate of 15 L / min during the sintering process, and the temperature is heated to the sintering temperature at a heating rate of 0.5°C / min. The sintering temperature is 1200°C and kept for 15 hours to obtain an ITO planar target.

[0058] There is no significant difference with the results of Example 1.

[0059] Example 6

[0060] It is basically the same as Example 2, except that oxygen is introduced at a rate of 12 L / min during the sintering process, and the temperature is heated to the sintering temperature at a heating rate of 1.0°C / min. The sintering temperature is 1600°C and kept at this temperature for 8 hours to obtain an ITO planar target.

[0061] There is no significant difference with the results of Example 1.

[0062] Comparative Example 1

[0063] The sintering tooling is basically the same as that of Example 4, but the lower end surface of the beam 12 contacts the upper end surface of the planar target.

[0064] The sintering tool of comparative example 1 is used to carry out the same sintering process as that of the above embodiment 1 to obtain an ITO planar target;

[0065] By observing the sintering tools of each layer of planar target material, it can be seen that beam 12 fuses with the ITO planar target material during the sintering process.

[0066] Comparative Example 2

[0067] like Figure 3 The planar target sintering tool shown lacks a supporting structure similar to the beam 12 compared with Example 1, which is equivalent to placing the boron plate 13 directly on the supporting block 11, and the distance between the indium tin oxide target blank and the boron plate 13 is the same as that in Example 1.

[0068] The sintering tool of comparative example 2 is used to carry out the same sintering process as that of the above embodiment 1 to obtain an ITO planar target;

[0069] By observing the sintering tooling of each layer of the planar target, it is found that the boron plate 13 of each layer is deformed, specifically, the center collapses downward, and the maximum difference with the plane reaches 0.5mm. The warping of the ITO planar target is 2.5mm.

[0070] Result analysis:

[0071] The boron plates 13 of each layer of Examples 1 to 3 are not deformed, except that the ITO planar target of the lower layer of Example 1 has a slightly increased warpage and a slightly decreased relative density compared to the ITO planar target of the top layer and the ITO planar targets of Examples 2 and 3. It is speculated that the reason is that the volume of the wind cavity is too small, resulting in insufficient oxygen contact with the ITO planar target, causing the volatilization of indium oxide and tin oxide. Similarly, after further reducing the volume of the wind cavity in Example 4, the results are consistent with the speculated reasons.

[0072] The beam 12 of comparative example 1 fuses with the ITO planar target during the sintering process.

[0073] In Comparative Example 2 compared with Examples 1 to 3, the downward collapse of the boron plate 13 causes the warping of the ITO planar target to increase. Obviously, in the absence of the beam 12, the sintering tooling cannot use the boron plate 13 of the same thickness to achieve stable support.

[0074] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the claims and their equivalents.

Claims

1. A planar target sintering tool, comprising at least two placement racks, characterized in that: The placement racks are stacked one by one to form a plurality of bearing positions for placing planar targets; the placement racks are composed of a pair of symmetrically arranged support blocks, at least one beam arranged on the pair of support blocks, and a boron plate overlapped on the upper end surface of the support block; the upper end surface of the support block and the upper end surface of the beam are located on the same horizontal plane; there is a gap between the lower end surface of the beam and the upper end surface of the planar target.

2. A planar target sintering tool according to claim 1, characterized in that: The support block is provided with at least one groove; the two ends of the beam are respectively overlapped in the grooves of a pair of support blocks.

3. A planar target sintering tool according to claim 1, characterized in that: The gap between the lower end surface of the beam and the upper end surface of the planar target is not less than twice the thickness of the target.

4. A planar target sintering tool according to claim 1, characterized in that: The boron plate is made of aluminum oxide or recrystallized silicon carbide.

5. The planar target sintering tool according to claim 1, characterized in that: The support block is made of alumina or recrystallized silicon carbide.

6. The planar target sintering tool according to claim 1, characterized in that: The beam is made of recrystallized silicon carbide.

7. A planar target sintering process, characterized in that: Based on the planar target sintering tool as described in any one of claims 1 to 6, the formed blank is an indium tin oxide target blank, comprising the following steps: Step 1, laying aluminum oxide powder on the bearing position of the placement rack, and placing an indium tin oxide target blank on the bearing position; Step 2, stack another placement rack on the above-mentioned carrying position, return to step 1, and enter step 3 until the preset single sintering quantity is reached; Step 3, sintering the flat target sintering tooling with the indium tin oxide target blank placed thereon, introducing oxygen at a rate of 10 to 15 L / min, heating to a sintering temperature at a heating rate of 0.5 to 1.5°C / min, the sintering temperature is 1200°C to 1600°C, and keeping the temperature for 8 to 15 hours; Step 4: Cool down to room temperature to obtain an ITO planar target.

8. The planar target sintering process according to claim 7, characterized in that: The particle size of the aluminum oxide powder is 100 to 700 μm.

9. The planar target sintering process according to claim 7, characterized in that: During the sintering process of planar targets, the number of layers of the placement rack shall not exceed 8.

10. The planar target sintering process according to claim 7, characterized in that: The sintering temperature in step 3 is 1300° C. to 1500° C., and the temperature is kept for 10 to 12 hours.

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