A target material for a blue light storage dielectric layer and a method of manufacturing the same

Abstract

This invention provides a target material for a dielectric layer of blue light storage and its preparation method. The preparation method includes: weighing In2O3 and ZrO2 according to a preset stoichiometric ratio and dry grinding them in a ball mill for 4-8 hours; then adding SiO2, binder, dispersant, defoamer, and deionized water; ball milling to form a homogenate; centrifuging to remove bubbles; and spray granulation to obtain a high-flowability powder material; loading the high-flowability powder material into a mold; cold isostatic pressing; then transferring it to a degreasing furnace for low-temperature degreasing; then transferring it to an oxygen-containing atmosphere for sintering; after furnace shutdown and cooling, demolding and machining are performed to obtain the target material for a dielectric layer of blue light storage. This invention, through a combination of dry grinding and wet grinding slurry preparation processes, combined with secondary particle size shaping technology, significantly improves the uniformity of the mixing of In2O3, ZrO2, and SiO2 powders. Combined with subsequent cold isostatic pressing, low-temperature degreasing, and atmosphere sintering processes, it ensures a consistent internal component distribution of the target material, solving the problems of low density and uneven composition in traditional preparation methods.

Description

Technical Field

[0001] This invention relates to the field of magnetron sputtering target materials and their preparation technology, and particularly to a target material for blue light storage dielectric layers and its preparation method. Background Technology

[0002] The dielectric sputtering target for Blu-ray storage is a core material for constructing the multilayer thin-film structure of high-performance optical discs. Its quality directly determines the performance of the dielectric layer, thus affecting the data recording accuracy, long-term stability, and lifespan of the optical disc. As a key functional layer for physical protection and optical control, the dielectric layer not only needs to possess excellent thermal stability, chemical inertness, and mechanical strength, but also must be able to precisely control the laser energy distribution and suppress the degradation of the recording layer material. This places almost stringent requirements on the density, purity, microstructure uniformity, and phase structure of its source material—the sputtering target.

[0003] The dielectric layer fabrication scheme can adopt the indirect path of single-component target co-sputtering, that is, multiple single oxide targets are installed on independent sputtering sources, and the composition ratio is achieved by synchronously controlling parameters such as multi-source power, gas flow rate, and sputtering time. This scheme is not only difficult to operate and requires extremely high parameter coordination, but also prone to deviation of film composition from the design value due to fluctuations in a certain sputtering source. Moreover, multi-source sputtering is difficult to adapt to large-area substrates, and the film thickness and composition uniformity are poor, which cannot meet the stringent requirements of high-density blue light storage for dielectric layer consistency.

[0004] Currently, ZrO2-based doped dielectric materials have become the mainstream choice. However, existing preparation methods suffer from problems such as uneven mixing of multiple components, low target density, and imprecise control of process parameters. This results in the target purity, resistivity, and other properties failing to meet the requirements, making them unsuitable for the high-density blue light storage needs of eight layers or more. Therefore, there is an urgent need for a process-controllable and stable target preparation method for blue light storage dielectric layers. Summary of the Invention

[0005] To address the problems existing in the background art, the present invention provides a target material for blue light storage dielectric layer and its preparation method, so as to achieve the preparation of a multi-component target material with density, purity and resistivity that meet the requirements for sputtering.

[0006] The specific details of the invention are as follows: In a first aspect, the present invention provides a method for preparing a target material for a blue light storage dielectric layer, the method comprising: S1. Weigh In2O3 and ZrO2 according to the preset stoichiometric ratio and dry grind them in a ball mill jar for 4-8 hours. Then add SiO2, binder, dispersant, defoamer and deionized water. Continue to ball mill the resulting slurry with a solid content of 35 wt%-45 wt% to form a homogenate. After centrifugation and defoaming, spray granulation is performed to obtain a high-flowability powder material. S2. The high-flowability powder material is loaded into a mold and cold isostatically pressed. Then it is transferred to a degreasing furnace for low-temperature degreasing treatment, and then transferred to an oxygen-containing atmosphere for sintering treatment. After the furnace is stopped and cooled, the material is demolded and processed to obtain the target material for the blue light storage dielectric layer.

[0007] Optionally, in step S1, by atomic percentage, the In2O3 accounts for 45 at% to 75 at%, the ZrO2 accounts for 15 at% to 35 at%, and the SiO2 accounts for 10 at% to 30 at%.

[0008] Optionally, the adhesive is selected from one or more of polyvinyl alcohol, polyethylene / polyacrylic acid, polymethacrylic acid, polyacrylic acid, and polyvinyl butyral, and is used in an amount of 10 wt% to 20 wt% of the total solid content. The dispersant is selected from one or more of polyethylene glycol, polyvinylpyrrolidone, triethanolamine, and trioleic acid glyceride, and is used in an amount of 2 wt% to 5 wt% of the total solid content. The defoaming agent is selected from diethylhexanol and / or organosilicon, and the amount used is 0.5 wt% to 1 wt% of the total solid content.

[0009] Optionally, the spray granulation system is configured with an inlet temperature of 220 ℃~240 ℃, an outlet temperature of 120 ℃~140 ℃, and a peristaltic pump speed of 30 Hz~70 Hz.

[0010] Optionally, the mass flow rate of the high-flowability powder material obtained by spray granulation is 105 g / min to 125 g / min, and the D50 is 25 μm to 35 μm.

[0011] Optionally, the density of the green body obtained by the cold isostatic pressing is 60%~68%.

[0012] Optionally, the cold isostatic pressing includes: The mold containing the material is placed in a cold isostatic pressing device, and the pressure is increased to 20 MPa~50 MPa within 30 s. After holding the pressure for 10 s~30 s, the pressure is further increased to 120 MPa~200 MPa within 180 s. After holding the pressure for 30 s~300 s, the pressure is released.

[0013] Optionally, the low-temperature degreasing treatment is performed at a temperature of 400 ℃-500 ℃ for a time of 6 h-10 h.

[0014] Optionally, the pressure of the sintering process is controlled at 0.1 MPa to 0.3 MPa, and the temperature is controlled using a gradient heating method, including: The temperature is raised to 900℃~1100℃ within 6h~9h, held for 1h, then raised to 1250℃ within 1h, held for 1h~5h, then raised to 1500℃, held for 5h~8h, and then allowed to cool naturally.

[0015] In a second aspect, the present invention provides a target material for a blue light storage dielectric layer, wherein the target material for a blue light storage dielectric layer is obtained by the preparation method described in the first aspect above; The target material used for the blue light storage dielectric layer has a purity of 99.9%, a density greater than 98%, and a resistivity less than 1 Ω·cm.

[0016] This invention provides a method for preparing a target material for a blue light storage dielectric layer. The preparation method includes: S1, dry grinding In2O3 and ZrO2 in a ball mill jar for 4 h to 8 h according to a preset stoichiometric ratio, then adding SiO2, binder, dispersant, defoamer and deionized water, and continuing to ball mill the resulting slurry with a solid content of 35 wt% to 45 wt% to form a homogeneous slurry, followed by spray granulation to obtain a high-flowability powder material; S2, loading the high-flowability powder material into a mold, performing cold isostatic pressing, then transferring it to a degreasing furnace for low-temperature degreasing, then transferring it to an oxygen atmosphere sintering furnace for atmosphere sintering, then cooling after furnace shutdown, demolding and material removal, and machining to obtain the target material for the blue light storage dielectric layer. Compared with the prior art, this invention has the following advantages: This invention constructs an In2O3 / ZrO2 / SiO2 ternary oxide system. By combining dry grinding and wet grinding slurry processes with secondary particle size shaping technology, the uniformity of In2O3, ZrO2, and SiO2 powder mixing is significantly improved. Combined with subsequent cold isostatic pressing, low-temperature debinding, and atmosphere sintering processes, the internal composition distribution of the target material is ensured to be consistent, solving the problem of uneven composition in traditional preparations. The preparation process of this invention has a clear range of control over powder particle size, granulation parameters, sintering atmosphere, and pressure increase rate, resulting in uniform microstructure, small performance fluctuations, and high finished product qualification rate of the target material. Attached Figure Description

[0017] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0018] Figure 1 A flowchart illustrating the preparation method of the target material for blue light storage dielectric layer provided in an embodiment of the present invention is shown; Figure 2A physical image of the target material for the dielectric layer of blue light storage provided in an embodiment of the present invention is shown; Figure 3 The microstructure of the target material for the dielectric layer of blue light storage provided in the embodiments and comparative examples of the present invention is shown. Detailed Implementation

[0019] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. The following description of at least one exemplary embodiment is merely illustrative and is in no way intended to limit the present invention or its application or use. Based on the embodiments of the present invention, any product that is the same as or similar to the present invention, derived by any person under the guidance of the present invention or by combining the features of the present invention with other prior art, falls within the protection scope of the present invention. Furthermore, all other embodiments obtained by those skilled in the art without inventive effort are within the protection scope of the present invention.

[0020] Specific experimental steps or conditions are not specified in the embodiments; they can be performed according to the conventional experimental steps or conditions described in the prior art. Reagents and other instruments used, unless otherwise specified, are all commercially available conventional reagent products. Furthermore, the accompanying drawings are merely illustrative diagrams of the embodiments of the present invention and are not necessarily drawn to scale. The same reference numerals in the drawings denote the same or similar parts, and therefore, repeated descriptions of them will be omitted. Some block diagrams shown in the drawings are functional entities and do not necessarily correspond to physically or logically independent entities.

[0021] Techniques, methods, and devices known to those skilled in the art may not be discussed in detail, but where appropriate, such techniques, methods, and devices should be considered part of this specification.

[0022] Furthermore, the technical features involved in the different embodiments of the present invention described below can be combined with each other as long as they do not conflict with each other.

[0023] Breakthroughs in the fabrication technology of high-performance dielectric layer targets are key to achieving a leapfrog improvement in the capacity and security of blue light storage. This invention provides a high-density, uniformly composed multi-component In2O3 / ZrO2 / SiO2 blue light storage dielectric layer target, which solves the problem of uneven composition in traditional target coatings and achieves uniform control of the blue light storage target composition. Specific implementation details are as follows: In a first aspect, the present invention provides a method for preparing a target material for a blue light storage dielectric layer. Figure 1 A flowchart illustrating the fabrication method of the target material for blue light storage dielectric layer provided in an embodiment of the present invention is shown, as follows: Figure 1 As shown, the preparation method includes: S1. According to the preset stoichiometric ratio, In2O3 and ZrO2 are dry-milled in a ball mill jar for 4 h to 8 h, and then mixed with SiO2, binder, dispersant, defoamer and deionized water. The resulting slurry with a solid content of 35 wt% to 45 wt% is further ball-milled to form a homogenate. After centrifugation and defoaming, it is spray-granulated to obtain a high-flowability powder material. This step begins with the premixing of In2O3 and ZrO2. The mechanical impact of dry milling breaks down the original agglomerates of In2O3 (micron-sized) and ZrO2 (nano-sized) powders, allowing the two core oxide particles to come into full contact and achieve preliminary molecular-level mixing. This avoids component segregation caused by differences in density and particle size when mixing with SiO2 and additives later. Furthermore, the collisions and friction between particles during dry milling refine the particle size of both powders and activate the particle surface, improving the interfacial compatibility with SiO2, binders, etc., during subsequent wet milling, thus laying the foundation for the uniformity of the overall slurry. Furthermore, after dry grinding and mixing In2O3 and ZrO2, the mixture is then mixed with low-density SiO2 (D50 30~100 nm), binder, dispersant, defoamer, and deionized water, and wet-milled for 4-8 h to improve the uniformity of the multi-component powder mixing. By controlling the amount of each material, a slurry with a solid content of 35 wt%~45 wt% is obtained. The slurry is defoamed by centrifugation to improve the uniformity of the powder. By controlling the feed and discharge temperatures and creep rate through spray granulation, a secondary particle size shaping powder with high flowability is obtained, which is convenient for molding.

[0024] In some implementations, In2O3, ZrO2 and SiO2 are weighed according to atomic percentage (total 100%): In2O3 accounts for 45 at%~75 at%, ZrO2 accounts for 15 at%~35 at%, and SiO2 accounts for 10 at%~30 at%.

[0025] In some embodiments, the binder may be selected from one or more of polyvinyl alcohol, polyethylene / polyacrylic acid, polymethacrylic acid, polyacrylic acid, and polyvinyl butyral, and the amount of binder is 10 wt% to 20 wt% of the total solid content; the dispersant may be selected from one or more of polyethylene glycol, polyvinylpyrrolidone, triethanolamine, and trioleic acid glyceride, and the amount is 2 wt% to 5 wt% of the total solid content; the defoamer may be selected from diethylhexanol and / or organosilicon, and the amount is 0.5 wt% to 1 wt% of the total solid content.

[0026] In some embodiments, the solid particles in the homogenate formed after dry and wet ball milling have a D50 particle size of 0.5 μm to 0.9 μm.

[0027] In some embodiments, during the spray granulation process, the inlet temperature can be set to 220 ℃~240 ℃, the outlet temperature to 120 ℃~140 ℃, and the peristaltic pump speed to 30 Hz~70 Hz, in order to obtain a highly fluid powder material (mass flow rate of 105 g / min~125 g / min), and the D50 of the highly fluid powder material is maintained at 20 μm~35 μm.

[0028] S2. The high-flowability powder material is loaded into a mold and cold isostatically pressed. Then it is transferred to a degreasing furnace for low-temperature degreasing treatment, and then transferred to an oxygen-containing atmosphere for sintering treatment. After the furnace is stopped and cooled, the material is demolded and processed to obtain the target material for the blue light storage dielectric layer.

[0029] In this step, the high-flowability powder material with high fluidity is formed into a green body with a density of 60%~68% by using the cold isostatic pressing process. The green body is then subjected to low-temperature (400℃-500℃) degreasing and high-temperature (900℃~1500℃) calcination in a synergistic process to form a target material with high density, high purity and low resistivity.

[0030] In some embodiments, the cold isostatic pressing process includes: placing a mold containing highly fluid powder material in a cold isostatic pressing apparatus, raising the pressure to 20-50 MPa within 30 seconds, holding the pressure for 10-30 seconds, then further raising the pressure to 120-200 MPa within 180 seconds, holding the pressure for 30-300 seconds, and then releasing the pressure. The cold isostatic pressing mold can be cylindrical, cylindrical, square, or round depending on the size requirements of the target material, and the prepared green body can be a disc, rod, cylindrical, or square block.

[0031] In some embodiments, the low-temperature degreasing treatment is controlled at a temperature of 400 ℃-500 ℃ for a time of 6 h-10 h.

[0032] In some embodiments, the pressure of the sintering process is controlled at 0.1 MPa to 0.3 MPa, and the temperature is controlled using a gradient heating method, including: The temperature is raised to 900℃~1100℃ within 6h~9h, held for 1h, then raised to 1250℃ within 1h, held for 1h~5h, then raised to 1500℃, held for 5h~8h, and then allowed to cool naturally.

[0033] It should be noted that before sintering, a 3mm~8mm thick layer of material with a particle density of 5.7g / cm³ is spread on the firing plate. 3 ~6.8g / cm 3The In2O3 particles can prevent the target material from sticking to the sintering plate at high temperatures, protecting the integrity of the target material while avoiding the increase in resistivity and fluctuation in dielectric properties caused by impurities.

[0034] In a second aspect, the present invention provides a target material for a blue light storage dielectric layer, wherein the target material for a blue light storage dielectric layer is obtained by the preparation method described in the first aspect above; The target material used for the blue light storage dielectric layer has a purity of 99.9%, a density greater than 98%, and a resistivity less than 1 Ω·cm.

[0035] The target material for blue light storage dielectric layers provided by this invention uses various oxide powders (including zirconium oxide powder, indium oxide powder, and silicon dioxide powder) as raw materials, formulated according to stoichiometric ratios. A secondary particle size shaping process combined with pressureless sintering technology is employed, and a staged heating and holding process is used to achieve precise and controllable densification of the target material in an oxygen sintering furnace. This preparation method involves ball milling and granulating multi-component oxide powders with stoichiometric ratios to obtain a highly fluid powder with a D50 of 25 μm to 35 μm. This powder is then cold isostatically pressed into a green body with a density of 60% to 68%, and finally densified by micro-positive pressure sintering in an oxygen atmosphere, resulting in a blue light storage recording layer target material with a density of over 98%.

[0036] The thin film obtained by the In2O3 / ZrO2 / SiO2 ternary oxide target film constructed in this invention can balance dielectric constant and insulation. In2O3 helps to improve dielectric layer capacitance density, reduce driving voltage, and meet the low power consumption requirements of optical disc. ZrO2 provides good electrical insulation and field breakdown capability, and SiO2 improves film uniformity and inhibits crystallization of high-k materials.

[0037] To enable those skilled in the art to more clearly understand the present invention, the following embodiments will be used to provide a detailed description of a target material for a blue light storage dielectric layer and its preparation method.

[0038] Example 1 The In2O3:ZrO2:SiO2 stoichiometric ratio was 50 at%:23 at%:27 at%; In2O3 powder (D50=14µm) and nano ZrO2 powder (D50=600 nm) were mixed in a ball mill and dry-milled for 8 h, followed by the addition of nano SiO2 powder (D50=30nm); at the same time, 10 wt% polyvinyl alcohol binder, 2.5 wt% polyethylene glycol dispersant, and 0.5 wt% diethylhexanol defoamer were added to deionized water to prepare a slurry with a solid content of 40 wt%, and ball milling was continued for 8 h to obtain a homogeneous slurry; the D50 particle size of the solid particles in the slurry was 0.5 µm.

[0039] The slurry was spray-granulated in a centrifugal spray granulator with an inlet temperature of 220 ℃ and a peristaltic pump speed of 60 Hz to obtain a high-flowability secondary particle size-shaped powder with a D50 of 20 μm and a mass flow rate of 105 g / min.

[0040] The secondary particle size-shaped powder was loaded into a 100 mm diameter cold isostatic pressing mold. The mold was placed in a cold isostatic pressing apparatus, and the pressure was increased to 30 MPa in 30 seconds, held for 20 seconds, and then further increased to 200 MPa in 180 seconds, pressing for 100 seconds to obtain a green body with a density of 65%. The green body was then placed in a degreasing furnace for low-temperature degreasing at 450 °C for 8 hours. The degreased material was then placed in an oxygen sintering furnace for sintering (the alumina sintering plate was covered with approximately 5 mm thick In₂O₃ particles with a particle density of 5.86 g / cm³). 3 The heating process was as follows: the temperature was raised to 1050℃ in 6 hours, held for 1 hour, then raised to 1250℃ in 1 hour, held for 2 hours, and finally raised to 1500℃ and held for 6 hours, followed by natural cooling. An oxygen sintering atmosphere was maintained during the sintering process, with an atmosphere pressure of 0.2 MPa slightly positive. Natural cooling was performed to obtain a ceramic target for the In2O3(50)ZrO2(23)SiO2(27) dielectric layer.

[0041] Example 2 The In2O3:ZrO2:SiO2 stoichiometric ratio was 45 at%:28 at%:27 at%; In2O3 powder (D50=60µm) and nano ZrO2 powder (D50=300nm) were mixed in a ball mill and dry-milled for 8 h. Then, nano SiO2 powder (D50=50nm) was added, along with 10 wt% solids content polyacrylic acid binder, 2.5 wt% solids content triethanolamine dispersant, and 0.5 wt% solids content diethylhexanol defoamer in deionized water to prepare a slurry with a solid content of 40 wt%. The slurry was ball-milled for another 8 h to obtain a homogeneous slurry; the D50 particle size of the solid particles in the slurry was 0.5 µm.

[0042] The slurry was spray-granulated in a centrifugal spray granulator with an inlet temperature of 220 ℃ and a peristaltic pump speed of 60 Hz to obtain a highly fluid secondary particle size-shaped powder with a D50 of 20 μm and a mass flow rate of 115 g / min.

[0043] The secondary particle size-shaped powder was loaded into a 100 mm diameter cold isostatic pressing mold. The mold was placed in a cold isostatic pressing apparatus, and the pressure was increased to 50 MPa in 30 seconds, held for 10 seconds, and then further increased to 150 MPa in 180 seconds, pressing for 200 seconds to obtain a green body with a density of 65%. The green body was then placed in a degreasing furnace for low-temperature degreasing at 450 °C for 8 hours. The degreased material was then sintered in an oxygen sintering furnace using ZrO2 plates, achieving a density of 6.21 g / cm³. 3 In2O3 particles were laid on a ZrO2 sintering plate, followed by the degreased material. The sintering heating process was as follows: the temperature was raised to 1050 ℃ for 6 h, held for 1 h, raised to 1250 ℃ for 1 h, held for 2 h, and finally raised to 1500 ℃ for 6 h, followed by natural cooling. An oxygen sintering atmosphere was maintained during the sintering process, with an atmosphere pressure of 0.2 MPa slightly positive. Natural cooling was performed to obtain a ceramic target for the In2O3 (45)ZrO2 (28)SiO2 (27) dielectric layer.

[0044] Example 3 According to the stoichiometric ratio of In2O3:ZrO2:SiO2 of 48 at%:25 at%:27 at%, In2O3 powder (D50=20um) and nano ZrO2 powder (D50=800 nm) were mixed in a ball mill and dry-milled for 5 h. Then, nano SiO2 powder (D50=30 nm) was added. At the same time, 10 wt% solids content of polyvinyl alcohol binder, 2.5 wt% solids content of polyethylene glycol dispersant, and 0.5 wt% solids content of diethylhexanol defoamer were added to deionized water to prepare a slurry with a solids content of 43 wt%. The slurry was ball-milled for another 6 h to obtain a slurry with uniform composition.

[0045] A slurry with a solid content of 43 wt% was spray-granulated in a centrifugal spray granulator with an inlet temperature of 220 ℃ and a peristaltic pump speed of 50 Hz to obtain a highly fluid secondary particle size-shaped powder with a D50 of 32 μm and a mass flow rate of 120 g / min.

[0046] The secondary particle size-shaped powder was loaded into a 60 mm diameter cold isostatic pressing mold. The mold was placed in a cold isostatic pressing apparatus, and the pressure was increased to 50 MPa in 30 seconds, held for 10 seconds, and then increased to 150 MPa in 180 seconds, and pressed for 200 seconds to obtain a green body with a density of 60%. The green body was then placed in a degreasing furnace for low-temperature degreasing at 450 °C for 8 hours. The degreased material was then placed in an oxygen sintering furnace for sintering. The heating process was as follows: heating to 1050 °C in 6 hours, holding for 1 hour, then heating to 1250 °C in 1 hour, holding for 2 hours, then heating to 1500 °C, holding for 8 hours, and then naturally cooled. An oxygen sintering atmosphere was maintained during the sintering process, with a pressure of 0.1 MPa slightly positive. Natural cooling yielded a ceramic target for an In2O3(48)ZrO2(25)SiO2(27) dielectric layer; see physical image. Figure 2 .

[0047] Example 4 According to the stoichiometric ratio of In2O3:ZrO2:SiO2 of 35 at%:35 at%:30 at%, In2O3 powder (D50=14um) and nano ZrO2 powder (D50=600 nm) were mixed in a ball mill and dry-milled for 8 h. Then, nano SiO2 powder (D50=30nm) was added. At the same time, 10 wt% solid content polyvinyl alcohol binder, 2.5 wt% solid content polyethylene glycol dispersant, and 0.5 wt% solid content diethylhexanol defoamer were added to deionized water to prepare a slurry with a solid content of 40 wt%. The slurry was ball-milled for another 8 h to obtain a slurry with uniform composition.

[0048] A slurry with a solid content of 40 wt% was spray-granulated in a centrifugal spray granulator with an inlet temperature of 220℃ and a peristaltic pump speed of 60 Hz to obtain a high-flowability secondary particle size-shaped powder with a D50 of 20 μm.

[0049] The secondary particle size-shaped powder was loaded into a 100 mm diameter cold isostatic pressing mold. The mold was placed in a cold isostatic pressing machine and pressed at 200 MPa for 100 s to obtain a green body with a density of 65%. The green body was then placed in a degreasing furnace for low-temperature degreasing at 450 ℃ for 8 h. The degreased material was then placed in an oxygen sintering furnace for sintering. An alumina sintering plate was covered with In₂O₃ particles approximately 5 mm thick, with a particle density of 5.9 g / cm³. 3The heating process was as follows: the temperature was raised to 1050 ℃ in 6 hours, held for 1 hour, then raised to 1250 ℃ in 1 hour, held for 2 hours, and finally raised to 1500 ℃ and held for 6 hours, followed by natural cooling. An oxygen sintering atmosphere was maintained during the sintering process, with an atmosphere pressure of 0.2 MPa slightly positive. Natural cooling was performed to obtain a ceramic target for the In2O3(35)ZrO2(35)SiO2(30) dielectric layer.

[0050] Comparative Example 1 Unlike Example 1, the three raw material powders with a stoichiometric ratio of In2O3:ZrO2:SiO2 of 48at%:25at%:27at% were ground in a ball mill for 8 h and then prepared into a slurry with a solid content of 60wt% in deionized water. After drying, the slurry was placed in a hot press mold and kept at 1100 °C and 40 MPa for 2 h to obtain an In2O3 (48)ZrO2 (25)SiO2 (27) dielectric layer target.

[0051] Comparative Example 2 The difference from Example 1 is that the stoichiometric ratio of In2O3:ZrO2:SiO2 is 25 at%:50 at%:25 at%, and all other process conditions are the same. The final target material is labeled as In2O3(25)ZrO2(50)SiO2(25).

[0052] Comparative Example 3 Compared with Example 1, the difference is that the stoichiometric ratio of In2O3:ZrO2:SiO2 is 80 at%:10 at%:10 at%, and the other process conditions are the same. The final target material is labeled as In2O3(80)ZrO2(10)SiO2(10).

[0053] The dielectric target materials obtained in Examples 1-4 and Comparative Examples 1-3 all achieved a purity of 99.9%. Other performance test parameters are shown in Table 1. Table 1. Test parameters for dielectric layer target material performance

[0054] The target material prepared in Comparative Example 1 has a non-dense porous structure, which makes it prone to uneven sputtering composition and sputtering spots during subsequent magnetron sputtering.

[0055] By comparing the microscopic morphology photographs of the target material provided in Example 3 (see...) Figure 3 a)) It can be observed that the morphology of the target material prepared by the traditional hot pressing sintering technology is ( Figure 3b) has a loose, porous structure with low density, and the indium oxide in its composition is highly susceptible to oxygen loss during sintering in a vacuum / inert atmosphere. The target material prepared in the embodiments of this invention has high density and no obvious sintering shrinkage pores are visible at the microscopic level.

[0056] Furthermore, the targets obtained in Examples 1-4 and Comparative Examples 1-3 were used for sputtering to form dielectric layers. The coating results showed that the films formed by sputtering using the targets provided in Examples 1-4 were dense and uniform with high thickness uniformity (film thickness deviation between 1.1% and 1.7%). The films formed by sputtering using the target provided in Comparative Example 1 showed sputtering spots on the surface, indicating uneven sputtering and poor film thickness uniformity (film thickness deviation of 13.2%). The sputtered film layer with the target provided in Comparative Example 2 showed increased film resistance, which may increase the driving voltage and power consumption. The target provided in Comparative Example 3 had poor electrical insulation, making the optical disc prone to electrical breakdown failure.

[0057] In the description of this specification, the references to terms such as "one embodiment," "some embodiments," "example," "specific example," or "some examples," etc., indicate that a specific feature, structure, material, or characteristic described in connection with that embodiment or example is included in at least one embodiment or example of the invention. In this specification, the illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples. In addition, those skilled in the art can combine and integrate the different embodiments or examples described in this specification.

[0058] For the sake of simplicity, the method embodiments are described as a series of actions. However, those skilled in the art should understand that the present invention is not limited to the described order of actions, as some steps can be performed in other orders or simultaneously according to the present invention. Furthermore, those skilled in the art should also understand that the embodiments described in the specification are preferred embodiments, and the actions and components involved are not necessarily essential to the present invention.

[0059] The above provides a detailed description of the target material for blue light storage dielectric layer and its preparation method. Specific examples have been used to illustrate the principle and implementation of the present invention. The description of the above embodiments is only for the purpose of helping to understand the method and core idea of ​​the present invention. At the same time, for those skilled in the art, there will be changes in the specific implementation and application scope based on the idea of ​​the present invention. Therefore, the content of this specification should not be construed as a limitation of the present invention.

Claims

1. A method of producing a target material for a blue light storage dielectric layer, characterized by, The preparation method includes: S1. Weigh In2O3 and ZrO2 according to the preset stoichiometric ratio and dry grind them in a ball mill jar for 4-8 hours. Then add SiO2, binder, dispersant, defoamer and deionized water. Continue to ball mill the resulting slurry with a solid content of 35 wt%-45 wt% to form a homogenate. After centrifugation and defoaming, spray granulation is performed to obtain a high-flowability powder material. S2. The high-flowability powder material is loaded into a mold and cold isostatically pressed. Then it is transferred to a degreasing furnace for low-temperature degreasing treatment, and then transferred to an oxygen-containing atmosphere for sintering treatment. After the furnace is stopped and cooled, the material is demolded and processed to obtain the target material for the blue light storage dielectric layer.

2. The method of claim 1, wherein the target material for a blue-ray storage dielectric layer is prepared by the steps of: In step S1, by atomic percentage, In2O3 accounts for 45 at% to 75 at%, ZrO2 accounts for 15 at% to 35 at%, and SiO2 accounts for 10 at% to 30 at%. ​ 3. The method for preparing the target material for the blue light storage dielectric layer according to claim 1, characterized in that, The adhesive is selected from one or more of polyvinyl alcohol, polyethylene / polyacrylic acid, polymethacrylic acid, polyacrylic acid, and polyvinyl butyral, and is used in an amount of 10 wt% to 20 wt% of the total solid content. The dispersant is selected from one or more of polyethylene glycol, polyvinylpyrrolidone, triethanolamine, and trioleic acid glyceride, and is used in an amount of 2 wt% to 5 wt% of the total solid content. The defoaming agent is selected from diethylhexanol and / or organosilicon, and the amount used is 0.5 wt% to 1 wt% of the total solid content.

4. The method for preparing the target material for the blue light storage dielectric layer according to claim 1, characterized in that, The spray granulation system is configured with an inlet temperature of 220 ℃~240 ℃, an outlet temperature of 120 ℃~140 ℃, and a peristaltic pump speed of 30 Hz~70 Hz.

5. The method for preparing the target material for the blue light storage dielectric layer according to claim 1 or 4, characterized in that, The mass flow rate of the high-flowability powder material obtained by spray granulation is 105 g / min to 125 g / min, and the D50 is 25 μm to 35 μm.

6. The method for preparing the target material for the blue light storage dielectric layer according to claim 1, characterized in that, The density of the green body obtained by the cold isostatic pressing is 60%~68%.

7. The method for preparing the target material for the blue light storage dielectric layer according to claim 1 or 6, characterized in that, The cold isostatic pressing process includes: The mold containing the material is placed in a cold isostatic pressing device, and the pressure is increased to 20 MPa~50 MPa within 30 s. After holding the pressure for 10 s~30 s, the pressure is further increased to 120 MPa~200 MPa within 180 s. After holding the pressure for 30 s~300 s, the pressure is released.

8. The method for preparing the target material for the blue light storage dielectric layer according to claim 1, characterized in that, The low-temperature degreasing treatment is carried out at a temperature of 400 ℃-500 ℃ for a time of 6 h-10 h.

9. The method for preparing the target material for the blue light storage dielectric layer according to claim 1, characterized in that, The sintering process is controlled at pressure between 0.1 MPa and 0.3 MPa, and the temperature is controlled using a gradient heating method, including: The temperature is raised to 900℃~1100℃ within 6h~9h, held for 1h, then raised to 1250℃ within 1h, held for 1h~5h, then raised to 1500℃, held for 5h~8h, and then cooled naturally.

10. A target material for a dielectric layer of blue light storage, characterized in that, The target material for the blue light storage dielectric layer is obtained by the preparation method described in any one of claims 1-9 above; The target material used for the blue light storage dielectric layer has a purity of 99.9%, a density greater than 98%, and a resistivity less than 1 Ω·cm.

Images