Spliced die-pressed graphite anode pot and preparation method thereof

By introducing a combination of phosphorus-doped graphite powder, β-Si3N4 whiskers, and composite reinforcing phases into the graphite sagger, the problems of thermal shock resistance and uneven heating of traditional graphite saggers are solved, achieving high durability and uniform heating, and improving the service life and performance of the graphite sagger.

CN120736901BActive Publication Date: 2025-11-18CHANGSHA ZHONGCI NEW MATERIAL TECH CO LTD
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Patent Information

Application Number
CN202511237483.1
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2025-09-01
Publication Date
2025-11-18
Estimated Expiration
2045-09-01

AI Technical Summary

Technical Problem

Traditional graphite saggers have poor thermal shock resistance and oxidation resistance, uneven heating, and short service life. Existing improved methods, such as those using silicon nitride and phenolic resin, produce saggers with insufficient durability.

Method used

The system employs a combination of phosphorus-doped graphite powder, β-Si3N4 whiskers, and a composite reinforcing phase (boron nitride nanotubes and zirconium oxide). Phosphorus doping enhances oxidation resistance, β-Si3N4 whiskers enhance strength, the composite reinforcing phase constructs an efficient thermally conductive network, and zirconium oxide toughens the system to improve thermal shock resistance. The partition is made of flake graphite, carbon fiber, and aluminum nitride, which synergistically improve thermal conductivity.

Benefits of technology

It achieves high durability and uniform heating of the keg body, with a thermal shock resistance of over 200 cycles, a flexural strength of over 19 MPa, and a thermal conductivity of 410~430 W/(m·K) for the partition, significantly improving the service life and heating uniformity of the graphite keg.

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Abstract

The application discloses spliced die-pressed graphite anode baking furnace, and a preparation method thereof, and relates to the technical field of graphite anode baking furnace, which comprises a baking furnace body and a partition plate. The baking furnace body comprises the following raw materials in parts by mass: 70-90 parts of phosphorus-doped graphite powder, 3-5 parts of silicon nitride whisker, and 5-8 parts of composite reinforcing phase. The partition plate comprises the following raw materials in parts by mass: 50-80 parts of flaky graphite, 5-20 parts of carbon fiber, and 4-10 parts of aluminum nitride. The composite reinforcing phase is boron nitride nanotube and zirconium oxide. The preparation method of the spliced die-pressed graphite anode baking furnace comprises the following steps: S1. wet mixing of the raw materials of the baking furnace body after ball milling to obtain a baking furnace body precursor, die pressing and heat treatment of the baking furnace body precursor to obtain the baking furnace body; S2. ball milling of the raw materials of the partition plate to obtain a partition plate precursor, die pressing and heat treatment of the partition plate precursor to obtain the partition plate; and S3. preparation of the spliced die-pressed graphite anode baking furnace.
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Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of graphite ladle, and particularly relates to a spliced mould-pressed graphite ladle and a preparation method thereof. BACKGROUND

[0002] The graphite ladle and the partition plate are key consumables in high-temperature industries (such as lithium battery material sintering, photovoltaic silicon wafer heat treatment, semiconductor process, etc.), and are mainly used for carrying and protecting heated materials. The poor thermal shock resistance and oxidation resistance of the ladle body of the traditional graphite ladle lead to short service life of the ladle, and the ladle depends on high-VOC pitch binder.

[0003] In the prior art, the ladle body is made of silicon nitride to improve oxidation, and the ladle body prepared from phenolic resin is beneficial to the improvement of mechanical properties, but has poor durability. In addition, when the ladle body carries too much material, the material in the middle and around the ladle body is not uniformly heated. SUMMARY

[0004] The application is to overcome the above technical problems, and therefore provides a spliced mould-pressed graphite ladle and a preparation method thereof. The spliced mould-pressed graphite ladle has good durability and good heat conduction capacity, and can make the heated material more uniform.

[0005] The application solves the above technical problems through the following technical scheme.

[0006] The application discloses a spliced mould-pressed graphite ladle, which comprises a ladle body and a partition plate.

[0007] The ladle body comprises the following preparation raw materials in mass parts: 70-90 parts of phosphorus-doped graphite powder, 3-5 parts of silicon nitride whisker and 5-8 parts of composite reinforcing phase.

[0008] Preferably, the ladle body comprises the following preparation raw materials in mass parts: 75-85 parts of phosphorus-doped graphite powder, 3.5-4.5 parts of silicon nitride whisker and 5.5-7.0 parts of composite reinforcing phase.

[0009] The partition plate comprises the following preparation raw materials in mass parts: 50-80 parts of flaky graphite, 5-20 parts of carbon fiber and 4-10 parts of aluminum nitride.

[0010] Preferably, the partition plate comprises the following preparation raw materials in mass parts: 55-75 parts of flaky graphite, 8-12 parts of carbon fiber and 5-8 parts of aluminum nitride.

[0011] The composite reinforcing phase is boron nitride nanotube and zirconium oxide.

[0012] In the application, the mass ratio of the boron nitride nanotube to the zirconium oxide in the composite reinforcing phase is 2-4:1. The boron nitride nanotube in the composite reinforcing phase constructs a rapid heat conduction channel, and the ZrO2 can buffer thermal stress, so that the ladle remains stable in structure under rapid cooling and rapid heating.

[0013] The preparation method of the phosphorus-doped graphite powder is as follows: graphite powder is immersed in a 3-7wt% diammonium hydrogen phosphate solution, and then activated at 750-850 DEG C to form the phosphorus-doped graphite powder; wherein, the phosphorus doping can improve the oxidation resistance of graphite, improve the durability of the sagger, and the phosphorus doping can optimize the heat conduction performance of the sagger; therefore, the sagger prepared from the ordinary graphite can be used for a longer service life at high temperature.

[0014] Further, the feed liquid ratio of the graphite powder / the diammonium hydrogen phosphate solution is 1 / 2-1 / 5 g / L.

[0015] In the present application, the silicon nitride whisker is β -Si3N4; wherein, β -Si3N4 will not undergo phase transition at high temperature, and β -Si3N4 can effectively hinder crack propagation and improve the strength of the sagger; β The Si-N bond on the surface of -Si3N4 is easy to react with the defect carbon in graphite to form a Si-C-N transition layer.

[0016] In the present application, the specific surface area of the silicon nitride whisker is greater than or equal to 15 m 2 / g;

[0017] In the present application, the bending strength of the silicon nitride whisker is greater than or equal to 1.0 GPa;

[0018] In the present application, the specific surface area of the boron nitride nanotube is greater than or equal to 50 m 2 / g, preferably 50-70 m 2 / g.

[0019] In the present application, the thermal conductivity of the boron nitride nanotube is greater than or equal to 3000 W / (m·k), preferably 3000-3200 W / (m·k).

[0020] In the present application, the mechanical strength of the boron nitride nanotube is greater than or equal to 1.8 TPa, preferably 1.8-2.0 TPa.

[0021] In the present application, the composite reinforcing phase is formed by ball milling the boron nitride nanotube and zirconium oxide.

[0022] In the present application, the particle size of the flaky graphite is 800-1000 mesh;

[0023] In the present application, the tensile strength of the carbon fiber is greater than or equal to 4100 MPa, preferably 4100-4200 MPa.

[0024] In the present application, the preparation raw material of the sagger further includes 4-6 parts of a binder;

[0025] The preparation raw materials of the partition plate further include 8-12 parts of a binder.

[0026] Further, the binder is at least one of polyvinyl butyral (PSZ, CAS No.: 63148-65-2) and polysilazane (PVB, CAS No.: 89535-60-4).

[0027] Further, 0.1-0.3wt% of aluminum acetylacetonate can be added to the binder.

[0028] In the application, the pot body is composed of the following mass parts of preparation raw materials: 70-90 parts of phosphorus-doped graphite powder, 3-5 parts of silicon nitride whiskers, 5-8 parts of a composite reinforcing phase, and 4-6 parts of a binder.

[0029] In the application, the partition plate is composed of the following mass parts of preparation raw materials: 55-75 parts of flake graphite, 8-12 parts of carbon fiber, 5-8 parts of aluminum nitride, and 8-12 parts of a binder.

[0030] In the application, the partition plate is in the shape of a cross and is placed in the pot body to divide the internal space of the pot body into four independent areas.

[0031] In the application, the thermal shock resistance of the pot body is ≥200 times.

[0032] In the application, the folding strength of the pot body is 19-23 MPa.

[0033] In the application, the thermal conductivity of the partition plate is 400-430 W / (m·K).

[0034] The application further discloses a preparation method of the spliced die-pressed graphite pot.

[0035] S1. Preparing the pot body: wet mixing the preparation raw materials of the pot body after ball milling to obtain a pot body precursor, and die-pressing and heat treating the pot body precursor to obtain the pot body.

[0036] S2. Preparing the partition plate: ball milling the preparation raw materials of the partition plate to obtain a partition plate precursor, and die-pressing and heat treating the partition plate precursor to obtain the partition plate.

[0037] S3. Preparing the spliced die-pressed graphite pot: assembling the pot body and the partition plate to obtain the spliced die-pressed graphite pot.

[0038] In S1, the solid content of the pot body precursor is 50-70%.

[0039] In S1, the die-pressing pressure is 5-15 MPa, and the die-pressing time is 5-15 min.

[0040] In S1, the heat treatment is sintering at 1000-1200℃ for 70-80h in nitrogen atmosphere;

[0041] In S2, the molding pressure is 5-15MPa, and the molding time is 5-15min.

[0042] In S2, the heat treatment is sintering at 1000-1200℃ for 15-30h in nitrogen atmosphere.

[0043] The spliced molding graphite saggar as described above, or the spliced molding graphite saggar prepared by the preparation method of the spliced molding graphite saggar as described above, is applied in the field of high-temperature heating and chemical reaction.

[0044] On the basis of common knowledge in the art, the above-mentioned preferred conditions can be combined arbitrarily, thereby obtaining each preferred example of the present application.

[0045] Compared with the prior art, the present application has the following beneficial effects:

[0046] The saggar body of the present application adopts phosphorus-doped graphite powder, β -Si3N4 whiskers and a composite reinforcing phase. The oxidation resistance of the graphite powder is improved by phosphorus doping, β The Si3N4 whiskers can improve the strength of the saggar body, the composite reinforcing phase constructs an efficient three-dimensional heat conduction network, and the zirconia toughening effect improves the thermal shock resistance. Therefore, the thermal shock resistance of the saggar body of the present application is ≥200 times, and in some preferred embodiments, it can reach 200-250 times; the saggar body has a bending strength ≥19MPa, and in some preferred embodiments, it can reach 19-23MPa.

[0047] The present application adopts flaky graphite, carbon fiber and aluminum nitride as the core, and the thermal conductivity of flaky graphite and the radial reinforcing effect of carbon fiber cooperatively solve the technical problem of insufficient heat conduction of graphite material, and the introduction of aluminum nitride further optimizes the interface thermal resistance, and the obtained partition plate has a thermal conductivity of 410-430 W / (m·k). BRIEF DESCRIPTION OF DRAWINGS

[0048] Figure 1 It is a structural assembly diagram of the spliced molding graphite saggar. DETAILED DESCRIPTION

[0049] In order to facilitate the understanding of the present application, the present application will be described more fully below in conjunction with preferred embodiments, but the scope of protection of the present application is not limited to the following specific embodiments.

[0050] Unless otherwise defined, all professional terms used herein have the same meaning as commonly understood by those skilled in the art. The professional terms used herein are only for the purpose of describing specific embodiments, and are not intended to limit the scope of protection of the present application.

[0051] The ranges disclosed herein are intended to include both endpoints and also any and all intervening ranges, unless otherwise indicated. For example, a range of "between a and b" is intended to include "a and b" and also the term "a-b." Unless otherwise indicated, the use of "or" in the disclosed aspects herein shall be considered the inclusive, "and / or," unless the context clearly indicates otherwise. It is further understood that the use of relational terms such as first, second, third, and the like, if any, are used solely to distinguish one from another entity, item, or action without necessarily giving rise to a corresponding "first," "second" or "third" entities, items or actions unless otherwise indicated. The disclosed "ranges" are defined herein in terms of their lower and upper limits, given that a range is defined by selecting a lower limit and an upper limit, the selected lower limit and upper limit define the boundaries of the particular range. Ranges defined in this manner can be inclusive or exclusive of the endpoints, and can be combined in any manner, i.e., any lower limit can be combined with any upper limit to form a range. For example, if ranges of 60-120 and 80-110 are listed for a particular parameter, it is understood that ranges of 60-110 and 80-120 are also contemplated. Further, if minimum range values of 1 and 2 are listed, and if maximum range values of 3, 4, and 5 are listed, then the following ranges are all contemplated: 1-3, 1-4, 1-5, 2-3, 2-4, and 2-5. In the present disclosure, unless otherwise indicated, a numerical range "a-b" indicates a shorthand manner of describing all of the individual integers between and including a and b, where a and b are both integers. For example, the numerical range "0-5" indicates that all of the integers between and including 0 and 5 have been listed herein, and "0-5" is merely a shorthand manner of describing those numerical combinations. Also, when a parameter is stated to be an integer ≥ 2, it is equivalent to disclose that the parameter is, for example, an integer 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, etc.

[0052] Unless otherwise indicated, all embodiments and optional embodiments of the present disclosure can be combined with each other to form new technical solutions.

[0053] Unless otherwise indicated, all technical features and optional technical features of the present disclosure can be combined with each other to form new technical solutions.

[0054] Unless otherwise indicated, all steps of the present disclosure can be performed in sequence or randomly, and are preferably performed in sequence. For example, the method comprises steps (a) and (b), which means that the method can comprise steps (a) and (b) performed in sequence, or steps (b) and (a) performed in sequence. For example, the method further comprises step (c), which means that step (c) can be added to the method in any order, for example, the method can comprise steps (a), (b) and (c), or steps (a), (c) and (b), or steps (c), (a) and (b), etc.

[0055] Unless otherwise indicated, the "includes" and "contains" mentioned in the present disclosure are open-ended and can also be closed. For example, the "includes" and "contains" can mean that other components not listed can also be included or contained, or only the listed components can be included or contained.

[0056] If not otherwise specifically stated, the term "or" in this application is inclusive. For example, the phrase "A or B" means "A, B, or both A and B." More specifically, any of the following conditions can satisfy the condition "A or B": A is true (or present) and B is false (or not present); A is false (or not present) and B is true (or present); or both A and B are true (or present).

[0057] The raw material information used in the following examples is as follows:

[0058] The graphite powder was purchased from Qingdao Dongkai Graphite Co., Ltd., and the particle size was 800 mesh;

[0059] The flake graphite was purchased from Qingdao Pingdu Fukang Graphite Processing Factory, and the particle size was 1000 mesh;

[0060] The silicon nitride whisker was purchased from Shandong Sitaili Metal Material Co., Ltd. β The silicon nitride whisker has a bending strength of 1.0 GPa, a thermal expansion coefficient of 3.2x10 -6 / ℃, and a specific surface area of 15 m 2 / g;

[0061] The boron nitride nanotube was purchased from Zhongke Leiming Technology Co., Ltd., and had an average diameter of 50 nm, a specific surface area of 50 m 2 / g, a thermal conductivity of 3000 W / (m·k), an expansion coefficient of 1x10 -6 / ℃, and a mechanical strength of 1.8 TPa;

[0062] The D50 of zirconium oxide was 48 μm;

[0063] The carbon fiber was a chopped carbon fiber, purchased from Weihai Guangwei Composite Material Co., Ltd. TZ50J, and had a tensile strength of 4120 MPa, a tensile modulus of 475 GPa, and a bulk density of 1.88 g / cm 3 ;

[0064] Including but not limited to the above manufacturers and models.

[0065] Example 1

[0066] The spliced graphite mold graphite pot of this embodiment is composed of a pot body and a partition plate.

[0067] The pot body is composed of the following mass parts of the prepared raw materials: 80 parts of phosphorus-doped graphite powder, 4.5 parts of silicon nitride whisker, 6.3 parts of composite reinforcing phase, and 5.4 parts of binder.

[0068] The preparation method of the phosphorus-doped graphite powder is as follows: the graphite powder is immersed in a 6.4wt% diammonium hydrogen phosphate solution with a material-to-liquid ratio of 1 / 3 g / L, and then activated at 800℃ to form the phosphorus-doped graphite powder.

[0069] The mass ratio of boron nitride nanotube to zirconium oxide is 3:1, and the composite reinforcing phase is obtained by ball milling boron nitride nanotube and zirconium oxide.

[0070] The binder is polyvinyl butyral (PSZ), and the adhesive further adds 0.2wt% acetylacetone aluminum.

[0071] The separator is composed of the following mass parts of raw materials for preparation: 70 parts of flake graphite, 10 parts of carbon fiber, 6.3 parts of aluminum nitride and 11.4 parts of binder.

[0072] The preparation method of the spliced mold pressing graphite graphite crucible of the embodiment is as follows:

[0073] S1. Preparation of the pot body: the raw materials for preparing the pot body are ball milled and wet mixed to obtain a pot body precursor with a solid content of 65%, and the pot body precursor is molded at 10Mpa for 12min, and then sintered at 1100℃ in a nitrogen atmosphere for 75h heat treatment to obtain the pot body;

[0074] S2. Preparation of the separator: the raw materials for preparing the separator are ball milled to obtain a separator precursor, the separator precursor is molded at 10Mpa for 10min, and then sintered at 1150℃ in a nitrogen atmosphere for 20h heat treatment to obtain the separator;

[0075] S3. Assemble the pot body and the separator to obtain a spliced mold pressing graphite graphite crucible as shown in Figure 1 .

[0076] The spliced mold pressing graphite graphite crucible prepared in this embodiment is subjected to thermal shock resistance test and thermal conductivity test;

[0077] The thermal conductivity test method refers to GB / T 8722;

[0078] The thermal shock resistance test method refers to GB / T 30873, and the specific process is to heat the sample to 1200℃, then quench the sample in water for 3min, and repeat the process of alternating cold and hot until the test is stopped when the heated end face of the sample is damaged by half and the number of times is recorded as the thermal shock resistance cycle number;

[0079] The thermal shock resistance cycle number of the pot body of this embodiment is 240 times, and the bending strength of the pot body is 22.5MPa;

[0080] The thermal conductivity of the separator is 423 W / (m·K).

[0081] Example 2

[0082] The difference between this embodiment and Example 1 is that:

[0083] The pot body is composed of the following mass parts of raw materials for preparation: 80 parts of phosphorus doped graphite powder, 6 parts of silicon nitride whisker, 4.2 parts of composite reinforcing phase and 5.6 parts of binder.

[0084] Other raw materials, steps and parameters are the same as in Example 1.

[0085] The heat shock resistance cycle number of the pot body of this example is 203 times, and the bending strength of the pot body is 19.7 MPa.

[0086] Example 3

[0087] The difference between this example and Example 1 is that:

[0088] The pot body is composed of the following mass parts of the preparation raw materials: 80 parts of phosphorus-doped graphite powder, 4.8 parts of silicon nitride whisker, 5.7 parts of composite reinforcing phase and 5.1 parts of binder.

[0089] The preparation method of the phosphorus-doped graphite powder is: the graphite powder is immersed in a 5wt% diammonium hydrogen phosphate solution, the solid-liquid ratio is 1 / 5 g / L, and the phosphorus-doped graphite powder is formed after activation at 830℃.

[0090] The heat shock resistance cycle number of the pot body of this example is 215 times, and the bending strength of the pot body is 21.6 MPa.

[0091] Example 4

[0092] The difference between this example and Example 1 is that:

[0093] The pot body is composed of the following mass parts of the preparation raw materials: 80 parts of phosphorus-doped graphite powder, 4.8 parts of silicon nitride whisker, 7.2 parts of composite reinforcing phase and 4.8 parts of binder.

[0094] The mass ratio of boron nitride nanotube to zirconia in the composite reinforcing phase is 2.4:1.

[0095] The heat shock resistance cycle number of the pot body of this example is 225 times, and the bending strength of the pot body is 22.8 MPa.

[0096] Example 5

[0097] The difference between this example and Example 1 is that:

[0098] The separator is composed of the following mass parts of the preparation raw materials: 65 parts of flake graphite, 11.7 parts of carbon fiber, 5.7 parts of aluminum nitride and 8.4 parts of binder.

[0099] The binder is polysilazane and polyvinyl butyral, and the mass ratio of polysilazane to polyvinyl butyral is 4.5:1.

[0100] The thermal conductivity of the separator of this example is 416 W / (m·K).

[0101] Example 6

[0102] The difference between this example and Example 1 is that:

[0103] The mass ratio of boron nitride nanotube: zirconia in the composite reinforcing phase is 1:1.

[0104] The number of thermal shock resistance cycles of the pot body of this example is 194, and the bending strength of the pot body is 18.1 MPa.

[0105] The other raw materials, steps and parameters are the same as in Example 1.

[0106] Comparative Example 1

[0107] The difference between this example and Example 1 is that:

[0108] The graphite powder in the pot body is not phosphorus-doped, and this undoped phosphorus graphite powder is replaced by phosphorus-doped graphite powder;

[0109] The number of thermal shock resistance cycles of the pot body of this example is 182, and the bending strength of the pot body is 16.1 MPa. The graphite of this example is not phosphorus-doped, so the strength of the pot body is low, and the thermal conductivity is poor, and the thermal shock resistance is also reduced accordingly.

[0110] The other raw materials, steps and parameters are the same as in Example 1.

[0111] Comparative Example 2

[0112] The difference between this example and Example 1 is that:

[0113] Silicon nitride is used in the pot body instead of silicon nitride whiskers, and the silicon nitride is purchased from Jiangxi Silicon Nitride New Material Co., Ltd. (D50≤10 μm);

[0114] The number of thermal shock resistance cycles of the pot body of this example is 176, and the bending strength of the pot body is 17.9 MPa. Silicon nitride whiskers inhibit crack propagation through bridging effect, increase fracture toughness, and can promote the formation of continuous thermal conduction path. ZrO2 phase change energy absorption needs to rely on the stress transfer of the whisker, and the granular silicon nitride cannot effectively buffer thermal stress due to short-range effect, so the thermal shock resistance is poor.

[0115] The other raw materials, steps and parameters are the same as in Example 1.

[0116] Comparative Example 3

[0117] The difference between this example and Example 1 is that:

[0118] The separator is composed of the following mass parts of the prepared raw materials: 70 parts of flake graphite, 6.2 parts of aluminum nitride and 8.4 parts of binder;

[0119] The thermal conductivity of the separator of this example is 374 W / (m·K).

[0120] Other raw materials, steps and parameters are the same as in Example 1.

[0121] Comparative Example 4

[0122] The difference between this comparative example and Example 1 is that:

[0123] The separator is composed of the following mass parts of the preparation raw materials: 80 parts of flake graphite, 10 parts of carbon fiber and 10 parts of binder.

[0124] The thermal conductivity of the separator of this comparative example is 388 W / (m·K).

[0125] Other raw materials, steps and parameters are the same as in Example 1.

[0126] Application Example

[0127] Lithium iron phosphate was prepared by a solid phase method, with the spliced die-pressed graphite pot of Example 1 as the experimental object. The specific process is as follows: iron compounds, lithium compounds and phosphorus compounds were placed in the pot, and sintering was carried out at 750℃ for 12h, as the experimental group. The control group removed the separator of the spliced die-pressed graphite pot, and only used the pot body as the container, and the other conditions were the same as the experimental group.

[0128] After sintering, samples of lithium iron phosphate were taken from the experimental group and the control group, respectively. The sampling method was to take 5 samples from the four corners and the center of the pot, respectively, to prepare half-cells, and then detect the discharge specific capacity of each sample. The variance was used to measure the difference in discharge specific capacity of the lithium iron phosphate samples at the center and the four corners of the pot.

[0129]

[0130] Unless otherwise specified, various raw materials, reagents, instruments and equipment used in the present application can be purchased from the market or can be prepared by existing methods. The above specific examples further illustrate the purpose, technical solutions and beneficial effects of the present application. It should be understood that the above description is only a specific embodiment of the present application and is not intended to limit the present application. Any modification, equivalent replacement, improvement, etc. made within the spirit and principles of the present application should be included in the protection scope of the present application.

Claims

1. A spliced ​​molded graphite sagger, characterized in that, Includes the bowl body and partitions; The bowl body comprises the following raw materials in parts by weight: 70-90 parts phosphorus-doped graphite powder, 3-5 parts silicon nitride whiskers, and 5-8 parts composite reinforcing phase; The partition comprises the following raw materials in parts by weight: 50-80 parts flake graphite, 5-20 parts carbon fiber and 4-10 parts aluminum nitride; The preparation method of the phosphorus-doped graphite powder is as follows: graphite powder is impregnated with a 3-7 wt% diammonium hydrogen phosphate solution and activated at 750-850℃ to form phosphorus-doped graphite powder. The composite reinforcing phase consists of boron nitride nanotubes and zirconium oxide.

2. The spliced ​​molded graphite sagger as described in claim 1, characterized in that, The ratio of graphite powder to diammonium hydrogen phosphate solution is 1 / 2 to 1 / 5 g / L.

3. The spliced ​​molded graphite sagger as described in claim 1, characterized in that, At least one of the following conditions a to b must be met: a. The silicon nitride whiskers are β -Si3N4; b. The mass ratio of boron nitride nanotubes to zirconium oxide in the composite reinforcing phase is 2~4:

1.

4. The spliced ​​molded graphite sagger as described in claim 3, characterized in that, At least one of the following conditions a to c must be met: a. The specific surface area of ​​the silicon nitride whiskers is ≥15m². 2 / g; b. The specific surface area of ​​the boron nitride nanotubes is ≥50 m². 2 / g; c. The thermal conductivity of the boron nitride nanotubes is ≥3000 W / (m·K).

5. The spliced ​​molded graphite sagger as described in claim 1, characterized in that, At least one of the following conditions a to b must be met: a. The particle size of the flake graphite is 800~1000 mesh; b. The tensile strength of the carbon fiber is ≥4100MPa.

6. The spliced ​​molded graphite sagger as described in claim 1, characterized in that, The raw materials for preparing the bowl also include 4 to 6 parts of binder; And / or, the raw materials for preparing the partition also include 8 to 12 parts of binder; The adhesive is at least one of polyvinyl butyral and polysilazane.

7. The spliced ​​molded graphite sagger as described in claim 1, characterized in that, The partition is cross-shaped and placed inside the bowl, which can divide the internal space of the bowl into four independent areas.

8. The method for preparing the spliced ​​molded graphite sagger as described in any one of claims 1 to 7, characterized in that, Includes the following steps: S1. Preparation of the bowl body: The raw materials for preparing the bowl body are ball-milled and wet-mixed to obtain a bowl body precursor. The bowl body precursor is then molded and heat-treated to obtain the bowl body. S2. Preparation of the partition: The raw materials for preparing the partition are ball-milled to obtain a partition precursor, and the partition precursor is molded and heat-treated to obtain the partition; S3. Preparation of spliced ​​molded graphite sagger: The spliced ​​molded graphite sagger is obtained by assembling the sagger body and partition.

9. The method for preparing the spliced ​​molded graphite sagger as described in claim 8, characterized in that, At least one of the following conditions a to d must be met: In a.S1, the molding pressure is 5MPa~15MPa, and the molding time is 5~15min; In b.S1, the heat treatment is sintering at 1000~1200℃ for 70~80h in a nitrogen atmosphere; In c.S2, the molding pressure is 5MPa~15MPa, and the molding time is 5~15min; In d.S2, the heat treatment is sintering at 1000~1200℃ for 15~30h in a nitrogen atmosphere.

Citation Information

Patent Citations

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