Lithium cobalt oxide ceramic target material, and preparation method and application thereof
By using slurry casting and atmospheric pressure sintering processes, large-size lithium cobalt oxide ceramic targets are prepared by utilizing the water absorption of gypsum molds. This solves the problem of cost-effectiveness in preparing large-size lithium cobalt oxide ceramic targets in existing technologies, achieving high density and regularity, and making it suitable as a cathode material for solid-state thin-film batteries.
Patent Information
- Application Number
- CN202510141523.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-02-08
- Publication Date
- 2025-11-04
- Estimated Expiration
- 2045-02-08
AI Technical Summary
Existing technologies make it difficult to prepare large-size lithium cobalt oxide ceramic targets with good uniformity and high density at low cost and high efficiency.
Lithium cobalt oxide ceramic targets were prepared by using slurry casting and atmospheric pressure sintering processes, taking advantage of the water absorption of gypsum molds. The density and regularity of the targets were improved by controlling the holding pressure and sintering temperature and time.
This technology enables the efficient preparation of large-size lithium cobalt oxide ceramic targets, reducing production costs, simplifying processes, shortening molding cycles, and facilitating mass production.
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Abstract
Description
Technical Field
[0001] This invention belongs to the field of lithium cobalt oxide material technology, and relates to a lithium cobalt oxide ceramic target, its preparation method and application. Background Technology
[0002] The advent of batteries has reduced our dependence on non-renewable resources. With the rapid development of the electronics industry, electronic products are becoming smaller, thinner, and more portable, which places new demands on batteries. Lithium-ion solid-state batteries, with their higher energy density, longer cycle life, and higher operating voltage, have attracted considerable attention. Compared to liquid lithium-ion batteries, all-solid-state batteries offer higher safety, greater energy density, and a wider operating temperature range, and have become the latest area of development in lithium-ion battery technology.
[0003] The earliest cathode material for thin-film batteries was TiS2. With the successful development of the high-performance solid-state electrolyte LiPON, lithium cobalt oxide has attracted widespread research as a cathode material for LiPON-type solid-state thin-film batteries. Lithium cobalt oxide not only possesses high voltage, high specific energy density, and good cycle performance, but also has a simple fabrication process, making it the mainstream cathode material for lithium-ion batteries. With the development of thin-film solid-state batteries, higher requirements are being placed on lithium cobalt oxide targets for magnetron sputtering of all-solid-state thin-film batteries.
[0004] Slip casting refers to a method in which appropriate additives are selected to suspend powdered raw materials evenly in a solution, forming a fluid slurry. This slurry is then poured into an absorbent plaster mold to remove excess water, and the molded material is shaped to obtain a green body with a certain strength. This method is often used to manufacture large-sized, complex-shaped ceramic targets, and it offers advantages such as regular green body shape, ease of mass production, short molding cycle, and low cost.
[0005] The lithium cobalt oxide ceramic targets prepared by existing technologies are relatively small in size. Therefore, how to prepare large-size lithium cobalt oxide ceramic targets with good uniformity and high density at low cost and high efficiency has become an urgent problem to be solved. Summary of the Invention
[0006] To address the aforementioned technical problems, this invention provides a lithium cobalt oxide ceramic target, its preparation method, and its application. This invention employs slip casting and atmospheric pressure sintering processes. Through slip casting, utilizing the water absorption of gypsum molds, lithium cobalt oxide ceramic targets with regular shapes, high density, and large dimensions can be prepared. The use of atmospheric pressure sintering reduces production steps and lowers production costs, offering advantages such as simplicity, high efficiency, low cost, short molding cycle, and ease of mass production.
[0007] To achieve this objective, the present invention adopts the following technical solution:
[0008] In a first aspect, the present invention provides a method for preparing a lithium cobalt oxide ceramic target, the method comprising the following steps: (1) mixing a binder, a dispersant, a solvent and lithium cobalt oxide to obtain a lithium cobalt oxide slurry; (2) subjecting the lithium cobalt oxide slurry to defoaming, slurry casting and drying in sequence to obtain a lithium cobalt oxide green body; (3) subjecting the lithium cobalt oxide green body to degreasing and atmospheric pressure sintering in sequence to obtain the lithium cobalt oxide ceramic target.
[0009] This invention employs slip casting and atmospheric pressure sintering processes. Through slip casting, the water absorption of the gypsum mold is utilized to prepare lithium cobalt oxide ceramic targets with regular shapes, high density, and large dimensions. The use of atmospheric pressure sintering reduces production steps and costs, and has the advantages of being simple, efficient, low-cost, having a short molding cycle, and being easy to mass-produce.
[0010] Preferably, the adhesive in step (1) comprises polyvinyl alcohol.
[0011] Preferably, the amount of the binder is 2wt% to 5wt% of the total amount of binder, dispersant and lithium cobalt oxide, for example, it can be 2wt%, 2.5wt%, 3wt%, 4wt%, 4.5wt% or 5wt%, but is not limited to the listed values, and other unlisted values within the range are also applicable.
[0012] Preferably, the dispersant comprises any one or a combination of at least two of polyacrylic acid, polyacrylamide, sodium hexametaphosphate, or sodium acrylate. Typical but non-limiting combinations include a combination of polyacrylic acid and polyacrylamide, a combination of sodium hexametaphosphate and sodium acrylate, or a combination of polyacrylamide, sodium hexametaphosphate, and sodium acrylate.
[0013] Preferably, the amount of the dispersant is 0.5wt% to 3wt% of the total amount of binder, dispersant and lithium cobalt oxide, for example, it can be 0.5wt%, 1wt%, 1.5wt%, 2wt%, 2.5wt% or 3wt%, but is not limited to the listed values, and other unlisted values within the range are also applicable.
[0014] Preferably, the solvent includes deionized water.
[0015] Preferably, the mixing in step (1) includes three stages of mixing.
[0016] Preferably, the mixing stage includes: mixing a solvent and a dispersant to obtain a mixture.
[0017] Preferably, the mixing time is 0.5h to 3h, for example, it can be 0.5h, 1h, 1.5h, 2h, 2.5h or 3h, but is not limited to the listed values. Other unlisted values within the range are also applicable.
[0018] Preferably, the two-stage mixing includes: mixing a primary mixture and lithium cobalt oxide powder in two stages to obtain a two-stage mixture.
[0019] Preferably, the mixing time for the two stages is 12h to 24h, for example, it can be 12h, 16h, 18h, 20h, 22h or 24h, but is not limited to the listed values. Other unlisted values within the range are also applicable.
[0020] Preferably, the three-stage mixing includes: mixing two-stage mixtures and a binder in three stages to obtain a mixed lithium cobalt oxide slurry.
[0021] Preferably, the mixing time for the three segments is 12h to 24h, for example, it can be 12h, 16h, 18h, 20h, 22h or 24h, but is not limited to the listed values. Other unlisted values within the range are also applicable.
[0022] Preferably, the defoaming in step (2) includes vacuum defoaming.
[0023] Preferably, the vacuum degree of the vacuum degassing is -0.98 MPa to -0.90 MPa, for example, it can be -0.98 MPa, -0.96 MPa, -0.95 MPa, -0.94 MPa, -0.92 MPa or -0.90 MPa, but is not limited to the listed values. Other unlisted values within the range are also applicable.
[0024] Preferably, the defoaming device includes a defoaming tank.
[0025] Preferably, after vacuum degassing and before grouting, gas is injected into the degassing pot to pressurize it.
[0026] Preferably, the gas includes nitrogen and / or air.
[0027] Preferably, the pressurized pressure is 0.1 MPa to 1 MPa, for example, it can be 0.1 MPa, 0.2 MPa, 0.4 MPa, 0.5 MPa, 0.7 MPa or 1 MPa, but is not limited to the listed values. Other unlisted values within the range are also applicable.
[0028] Preferably, the dimensions of the gypsum mold used in step (2) are length (40cm~60cm) × width (70cm~90cm) × thickness (10cm~30cm). For example, it can be length 40cm × width 70cm × thickness 10cm, length 50cm × width 80cm × thickness 20cm, length 40cm × width 90cm × thickness 30cm, length 60cm × width 70cm × thickness 30cm, length 60cm × width 90cm × thickness 10cm or length 60cm × width 90cm × thickness 30cm, but it is not limited to the listed values. Other unlisted values within the range are also applicable.
[0029] Preferably, after the grouting process is completed and before drying, pressure is maintained.
[0030] Preferably, the pressure for holding the pressure is 0.1 MPa to 1 MPa, for example, it can be 0.1 MPa, 0.2 MPa, 0.4 MPa, 0.5 MPa, 0.7 MPa or 1 MPa, but is not limited to the listed values. Other unlisted values within the range are also applicable.
[0031] Preferably, the pressure holding time is 3h to 12h, for example, it can be 3h, 6h, 9h, 10h, 11h or 12h, but is not limited to the listed values. Other unlisted values within the range are also applicable.
[0032] This invention further improves the integrity and uniformity of the lithium cobalt oxide ceramic target by further controlling the holding pressure and time. Within the preferred holding pressure and time range, the prepared lithium cobalt oxide ceramic target has an intact blank, full utilization of raw materials, and facilitates the smooth progress of subsequent drying steps.
[0033] Preferably, the drying temperature in step (2) is 40℃~50℃, for example, it can be 40℃, 42℃, 44℃, 46℃, 48℃ or 50℃, but is not limited to the listed values. Other unlisted values within the range are also applicable.
[0034] Preferably, the drying and heat preservation time in step (2) is 20h to 48h, for example, it can be 20h, 24h, 30h, 35h, 40h or 48h, but is not limited to the listed values. Other unlisted values within the range are also applicable.
[0035] Preferably, the drying device includes a constant temperature and humidity chamber.
[0036] Preferably, the heat preservation temperature for degreasing in step (3) is 500℃~600℃, for example, it can be 500℃, 520℃, 540℃, 560℃, 580℃ or 600℃, but is not limited to the listed values. Other unlisted values within the range are also applicable.
[0037] Preferably, the heat preservation time for degreasing in step (3) is 1h to 5h, for example, it can be 1h, 2h, 3h, 4h, 4.5h or 5h, but is not limited to the listed values. Other unlisted values within the range are also applicable.
[0038] Preferably, the degreasing apparatus includes a lifting furnace.
[0039] Preferably, the holding temperature for atmospheric pressure sintering in step (3) is 950℃~1000℃, for example, it can be 950℃, 960℃, 970℃, 980℃, 990℃ or 1000℃, but is not limited to the listed values. Other unlisted values within the range are also applicable.
[0040] Preferably, the holding time for atmospheric pressure sintering is 1h to 5h, for example, it can be 1h, 2h, 3h, 4h, 4.5h or 5h, but is not limited to the listed values. Other unlisted values within the range are also applicable.
[0041] This invention further improves the density of the lithium cobalt oxide ceramic target by further controlling the holding temperature and holding time during atmospheric pressure sintering. Within the preferred range of atmospheric pressure sintering holding temperature and holding time, the density of the prepared lithium cobalt oxide ceramic target is further improved.
[0042] Preferably, the atmosphere for atmospheric pressure sintering is an oxygen-containing atmosphere.
[0043] Preferably, the oxygen-containing atmosphere includes air and / or oxygen.
[0044] Preferably, the apparatus for atmospheric pressure sintering includes an atmospheric pressure sintering furnace.
[0045] As a preferred technical solution of the present invention, the preparation method includes the following steps:
[0046] (1) Add solvent and dispersant, mix for 0.5h to 3h; then add lithium cobalt oxide powder, mix for 12h to 24h; finally add binder, mix for 12h to 24h to obtain lithium cobalt oxide slurry.
[0047] (2) Pour the lithium cobalt oxide slurry into the degassing tank for vacuum degassing. After degassing, pressurize the degassing tank by filling it with gas. The pressurization pressure is 0.1MPa to 1MPa. Connect the outlet to the plaster mold. The lithium cobalt oxide slurry is automatically filled into the plaster mold. After filling, maintain the pressure at 0.1MPa to 1MPa for 3h to 12h. Remove the mold and place it in a constant temperature and humidity chamber at 40℃ to 50℃ for 20h to 48h to obtain the lithium cobalt oxide green blank.
[0048] (3) The lithium cobalt oxide green billet is placed in a lifting furnace for degreasing. The degreasing temperature is 500℃~600℃ and the degreasing time is 1h~5h to obtain the degreased lithium cobalt oxide green billet.
[0049] (4) The degreased lithium cobalt oxide green blank is placed in an atmospheric pressure sintering furnace for atmospheric pressure sintering. The atmospheric pressure sintering temperature is 950℃~1000℃ and the atmospheric pressure sintering holding time is 1h~5h to obtain the lithium cobalt oxide ceramic target.
[0050] In a second aspect, the present invention provides a lithium cobalt oxide ceramic target, which is prepared by the preparation method described in the first aspect.
[0051] Preferably, the dimensions of the lithium cobalt oxide ceramic target are length (40cm~60cm) × width (70cm~90cm) × thickness (8cm~28cm), for example, it can be length 40cm × width 70cm × thickness 8cm, length 50cm × width 80cm × thickness 20cm, length 40cm × width 90cm × thickness 28cm, length 60cm × width 70cm × thickness 28cm, length 60cm × width 90cm × thickness 8cm or length 60cm × width 90cm × thickness 28cm, but it is not limited to the listed values, and other unlisted values within the range are also applicable.
[0052] Thirdly, the present invention provides an application of the lithium cobalt oxide ceramic target as described in the second aspect, wherein the lithium cobalt oxide target is used as the positive electrode of a solid-state thin-film battery.
[0053] Compared with the prior art, the present invention has at least the following beneficial effects:
[0054] This invention employs slip casting and atmospheric pressure sintering processes. By using slip casting and the water absorption of the gypsum mold, lithium cobalt oxide ceramic targets with regular shapes, high density, and large dimensions can be prepared. By using atmospheric pressure sintering, production steps are reduced while production costs are lowered. This invention has the advantages of being simple, efficient, low-cost, having a short molding cycle, and being easy to mass-produce. Detailed Implementation
[0055] To facilitate understanding of the present invention, the following embodiments are provided. Those skilled in the art should understand that these embodiments are merely illustrative and should not be construed as limiting the scope of the invention.
[0056] Example 1
[0057] This embodiment provides a method for preparing a lithium cobalt oxide ceramic target, the method comprising the following steps:
[0058] (1) Add 2 parts of polyacrylic acid and 200 parts of water to a mixing tank and mix for 2 hours; then add 95 parts of lithium cobalt oxide powder and mix for 12 hours; finally add 3 parts of polyvinyl alcohol solution and mix for 12 hours to obtain lithium cobalt oxide slurry.
[0059] (2) The lithium cobalt oxide slurry is poured into a degassing tank and vacuum degassed at a vacuum degree of -0.95MPa. After degassing, nitrogen gas is introduced into the degassing tank for pressurization at a pressure of 0.5MPa. The outlet is connected to a gypsum mold with dimensions of 50cm long × 80cm wide × 20cm thick. The lithium cobalt oxide slurry is automatically filled into the gypsum mold. After filling, the pressure is maintained at 0.5MPa for 9 hours. The mold is then removed and placed in a constant temperature and humidity chamber at 45℃ for drying for 36 hours to obtain a lithium cobalt oxide green blank.
[0060] (3) The lithium cobalt oxide green billet is placed in a lifting furnace for degreasing. The degreasing temperature is 550℃ and the degreasing time is 3h to obtain the degreased lithium cobalt oxide green billet.
[0061] (4) The degreased lithium cobalt oxide green blank is placed in an atmospheric pressure sintering furnace for atmospheric pressure sintering. The atmospheric pressure sintering temperature is 980℃ and the atmospheric pressure sintering holding time is 3h to obtain the lithium cobalt oxide ceramic target.
[0062] The lithium cobalt oxide ceramic target prepared in this embodiment has dimensions of 50cm in length × 80cm in width × 18cm in thickness.
[0063] Example 2
[0064] This embodiment provides a method for preparing a lithium cobalt oxide ceramic target, the method comprising the following steps:
[0065] (1) Add 0.5 parts of sodium polyacrylate and 200 parts of water to the powder mixture and mix for 0.5 hours; then add 97.5 parts of lithium cobalt oxide powder and mix for 12 hours; add 2 parts of polyvinyl alcohol solution and mix for 12 hours to obtain a mixed liquid slurry.
[0066] (2) The lithium cobalt oxide slurry is poured into a degassing tank and vacuum degassed at a vacuum degree of -0.90MPa. After degassing, nitrogen gas is introduced into the degassing tank for pressurization at a pressure of 0.1MPa. The outlet is connected to a gypsum mold with dimensions of 40cm long × 70cm wide × 10cm thick. The lithium cobalt oxide slurry is automatically filled into the gypsum mold. After filling, the pressure is maintained at 0.1MPa for 12 hours. The mold is then removed and placed in a constant temperature and humidity chamber at 50℃ for drying for 20 hours to obtain a lithium cobalt oxide green blank.
[0067] (3) The lithium cobalt oxide green billet is placed in a lifting furnace for degreasing. The degreasing temperature is 600℃ and the degreasing time is 1h to obtain the degreased lithium cobalt oxide green billet.
[0068] (4) The degreased lithium cobalt oxide green blank is placed in an atmospheric pressure sintering furnace for atmospheric pressure sintering. The atmospheric pressure sintering temperature is 1000℃ and the atmospheric pressure sintering holding time is 1h to obtain the lithium cobalt oxide ceramic target.
[0069] The lithium cobalt oxide ceramic target prepared in this embodiment has dimensions of 40cm in length × 70cm in width × 9cm in thickness.
[0070] Example 3
[0071] This embodiment provides a method for preparing a lithium cobalt oxide ceramic target, the method comprising the following steps:
[0072] (1) Add 3 parts of polyacrylamide and 200 parts of water to the powder mixture and mix for 3 hours; then add 92 parts of lithium cobalt oxide powder and mix for 24 hours; add 5 parts of polyvinyl alcohol solution and mix for 24 hours to obtain a mixed liquid slurry.
[0073] (2) The lithium cobalt oxide slurry is poured into a degassing machine and degassed under a vacuum of -0.98MPa. After degassing, nitrogen gas is introduced into the degassing tank for pressurization. The pressurization pressure is 1MPa. The outlet is connected to a gypsum mold with dimensions of 60cm long × 90cm wide × 30cm thick. The lithium cobalt oxide slurry is automatically filled into the gypsum mold. After filling, the pressure is maintained at 1MPa for 3 hours. The mold is then removed and placed in a 40℃ constant temperature and humidity chamber for drying for 48 hours to obtain a lithium cobalt oxide green blank.
[0074] (3) The lithium cobalt oxide green billet is placed in a lifting furnace for degreasing. The degreasing temperature is 500℃ and the degreasing time is 5h to obtain the degreased lithium cobalt oxide green billet.
[0075] (4) The degreased lithium cobalt oxide green blank is placed in an atmospheric pressure sintering furnace for atmospheric pressure sintering. The atmospheric pressure sintering temperature is 950℃ and the atmospheric pressure sintering holding time is 5h to obtain the lithium cobalt oxide ceramic target.
[0076] The lithium cobalt oxide ceramic target prepared in this embodiment has dimensions of 60cm in length × 90cm in width × 27cm in thickness.
[0077] Example 4
[0078] The only difference between this embodiment and embodiment 1 is that, except that the pressure for holding pressure in step (2) is 0.08 MPa, everything else is the same as in embodiment 1.
[0079] Example 5
[0080] The only difference between this embodiment and embodiment 1 is that, except that the pressure for holding pressure in step (2) is 1.1 MPa, everything else is the same as in embodiment 1.
[0081] Example 6
[0082] The only difference between this embodiment and embodiment 1 is that, except that the pressure holding time in step (2) is 2.5 hours, everything else is the same as in embodiment 1.
[0083] Example 7
[0084] The only difference between this embodiment and embodiment 1 is that, except that the pressure holding time in step (2) is 12.5h, everything else is the same as in embodiment 1.
[0085] Example 8
[0086] The only difference between this embodiment and embodiment 1 is that, except that the holding temperature for atmospheric pressure sintering in step (4) is 900°C, everything else is the same as in embodiment 1.
[0087] Example 9
[0088] The only difference between this embodiment and embodiment 1 is that, except that the holding temperature for atmospheric pressure sintering in step (4) is 1050°C, everything else is the same as in embodiment 1.
[0089] Comparative Example 1
[0090] The only difference between this comparative example and Example 1 is that, except that the mold in step (2) is a rubber mold, everything else is the same as in Example 1.
[0091] Comparative Example 2
[0092] This comparative example provides a method for preparing a lithium cobalt oxide ceramic target, the method comprising the following steps:
[0093] (1) Add 2 parts of polyacrylic acid and 200 parts of water to a mixing tank and mix for 2 hours; then add 95 parts of lithium cobalt oxide powder and mix for 12 hours; finally add 3 parts of polyvinyl alcohol solution and mix for 12 hours to obtain lithium cobalt oxide slurry.
[0094] (2) The lithium cobalt oxide slurry is spray-granulated, and then dry-pressed and cold isostatically pressed in sequence. The pressure of the cold isostatic pressing is 300 MPa and the holding time is 50 min to obtain the lithium cobalt oxide green blank.
[0095] (3) The lithium cobalt oxide green billet is placed in a lifting furnace for degreasing. The degreasing temperature is 550℃ and the degreasing time is 3h to obtain the degreased lithium cobalt oxide green billet.
[0096] (4) The degreased lithium cobalt oxide green blank is placed in an atmospheric pressure sintering furnace for atmospheric pressure sintering. The atmospheric pressure sintering temperature is 980℃ and the atmospheric pressure sintering holding time is 3h to obtain the lithium cobalt oxide ceramic target.
[0097] Test methods
[0098] The lithium cobalt oxide ceramic targets prepared in Examples 1-9 and Comparative Examples 1-2 were subjected to density testing. The density of the lithium cobalt oxide ceramic targets was tested using an AKD-220A density instrument from Yangzhou Aike Ruide Instrument Co., Ltd. The test method was the water displacement method, and the test results were recorded in Table 1.
[0099] Table 1
[0100]
[0101]
[0102] The test results show that:
[0103] (1) As can be seen from Examples 1-9 and Comparative Examples 1-2, the present invention adopts slurry casting and atmospheric pressure sintering process. By slurry casting, the water absorption of the gypsum mold can be used to prepare lithium cobalt oxide ceramic targets with regular shape, high density and large size. By adopting atmospheric pressure sintering, the production process is reduced and the production cost is reduced. It has the advantages of being simple and efficient, low cost, short molding cycle and easy to mass-produce.
[0104] (2) As can be seen from Examples 1 and 4-5, the density of the lithium cobalt oxide ceramic target prepared by the present invention is further improved by further controlling the holding pressure after slurry molding.
[0105] (3) As can be seen from Examples 1 and 6-7, the density of the lithium cobalt oxide ceramic target prepared by the present invention is further improved by further controlling the holding time after slurry molding.
[0106] (4) As can be seen from Examples 1 and 8-9, the density of the lithium cobalt oxide ceramic target prepared by the present invention is further improved by further controlling the temperature of atmospheric pressure sintering.
[0107] In summary, this invention employs slip casting and atmospheric pressure sintering processes. By using slip casting and the water absorption of the gypsum mold, lithium cobalt oxide ceramic targets with regular shapes, high density, and large dimensions can be prepared. By using atmospheric pressure sintering, production steps are reduced, and production costs are lowered. This invention has the advantages of being simple, efficient, low-cost, having a short molding cycle, and being easy to mass-produce.
[0108] The applicant declares that the above description is only a specific embodiment of the present invention, but the protection scope of the present invention is not limited thereto. Those skilled in the art should understand that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope disclosed in the present invention fall within the protection and disclosure scope of the present invention.
Claims
1. A method for preparing a lithium cobalt oxide ceramic target, characterized in that, The preparation method includes the following steps: (1) Mix the binder, dispersant, solvent and lithium cobalt oxide to obtain lithium cobalt oxide slurry; The binder is polyvinyl alcohol; the amount of the binder accounts for 2wt% to 5wt% of the total amount of binder, dispersant and lithium cobalt oxide. The dispersant comprises any one or a combination of at least two of polyacrylic acid, polyacrylamide, sodium hexametaphosphate, or sodium acrylate; the amount of the dispersant is 0.5 wt% to 3 wt% of the total amount of binder, dispersant, and lithium cobalt oxide. The mixing process includes three stages. The first stage of mixing includes: mixing the solvent and the dispersant to obtain a first-stage mixture; the time for the first stage of mixing is 0.5h to 3h. The two-stage mixing process includes: mixing the first-stage mixture and lithium cobalt oxide powder in a two-stage process to obtain a two-stage mixture; the two-stage mixing time is 12h~24h. The three-stage mixing process includes: mixing the two-stage mixture and the binder in three stages to obtain a mixed lithium cobalt oxide slurry; the three-stage mixing time is 12h~24h. (2) The lithium cobalt oxide slurry is subjected to defoaming, slurry casting and drying in sequence to obtain lithium cobalt oxide green blank; The defoaming process includes vacuum defoaming; after vacuum defoaming and before grouting, gas is injected into the defoaming pot for pressurization; the pressurization pressure is 0.1 MPa to 1 MPa. After the grouting process is completed and before drying, pressure must be maintained. The pressure for holding the pressure is 0.1 MPa to 1 MPa; The pressure holding time is 3h~12h; The drying temperature is 40℃~50℃; the drying time is 20h~48h. (3) The lithium cobalt oxide green blank is degreased and sintered under normal pressure in sequence to obtain the lithium cobalt oxide ceramic target; The degreasing temperature is 500℃~600℃; the degreasing time is 1h~5h. The holding temperature for atmospheric pressure sintering is 950℃~1000℃; the holding time for atmospheric pressure sintering is 1h~5h.
2. The preparation method according to claim 1, characterized in that, The solvent includes deionized water.
3. The preparation method according to claim 1, characterized in that, The vacuum degree of the vacuum degassing is -0.98 MPa to -0.90 MPa.
4. The preparation method according to claim 1, characterized in that, The dimensions of the gypsum mold used in step (2) are length (40cm~60cm) × width (70cm~90cm) × thickness (10cm~30cm).
Citation Information
Patent Citations
Lithium cobalt oxide target material and preparation method thereof
CN102181840A
Method for preparing oxide ceramic target material green body
CN108046767A
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