CN111037710A - Forming method of sagger for lithium battery positive electrode material - Google Patents
Forming method of sagger for lithium battery positive electrode material Download PDFInfo
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- CN111037710A CN111037710A CN201911278502.XA CN201911278502A CN111037710A CN 111037710 A CN111037710 A CN 111037710A CN 201911278502 A CN201911278502 A CN 201911278502A CN 111037710 A CN111037710 A CN 111037710A
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- Prior art keywords
- sagger
- pressure
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- finished
- forming
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B3/00—Producing shaped articles from the material by using presses; Presses specially adapted therefor
- B28B3/003—Pressing by means acting upon the material via flexible mould wall parts, e.g. by means of inflatable cores, isostatic presses
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B11/00—Apparatus or processes for treating or working the shaped or preshaped articles
- B28B11/24—Apparatus or processes for treating or working the shaped or preshaped articles for curing, setting or hardening
- B28B11/243—Setting, e.g. drying, dehydrating or firing ceramic articles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B3/00—Producing shaped articles from the material by using presses; Presses specially adapted therefor
- B28B3/02—Producing shaped articles from the material by using presses; Presses specially adapted therefor wherein a ram exerts pressure on the material in a moulding space; Ram heads of special form
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B7/00—Moulds; Cores; Mandrels
- B28B7/34—Moulds, cores, or mandrels of special material, e.g. destructible materials
- B28B7/348—Moulds, cores, or mandrels of special material, e.g. destructible materials of plastic material or rubber
Abstract
The invention relates to the technical field of sagger kiln furniture preparation, in particular to a forming method of a sagger for a lithium battery anode material, which comprises the following steps: powder preliminary treatment, die filling pre-compaction, drying, die filling, shaping, the shaping specifically is: placing the sealed elastic die tightly wrapped with the semi-finished sagger blank into a high-pressure cylinder and suspending the elastic die in the high-pressure cylinder in the air by using a high-pressure resistant rope; then covering a high-pressure cylinder sealing cover; and continuously injecting liquid between the interior of the high-pressure cylinder and the elastic mold for pressurization, keeping the pressure for 12 hours when the internal pressure reaches 5000kgf/cm2, then discharging the liquid for slow pressure relief, taking out the container after the pressure relief is finished, opening the container, and removing the elastic mold to obtain the finished sagger blank. The sagger blank obtained by pressing by the method has the advantages of uniform tissue structure, high density, small sintering shrinkage rate, low mold cost, high production efficiency, and capability of forming slender products with complex shapes, large-size products and precise-size products, and is suitable for automatic operation.
Description
Technical Field
The invention relates to the technical field of sagger kiln furniture preparation, in particular to a forming method of a sagger for a lithium battery positive electrode material.
Background
The sagger used in the process of synthesizing the lithium ion battery anode material is generally a corundum-based, mullite-based, quartz-based and cordierite-based high-temperature resistant sagger. Cordierite and corundum sagger are the most used. However, the raw materials used for synthesizing the lithium ion cathode material can be decomposed in the synthesis process to generate lithium oxide with strong permeability and reactivity to corrode the high-temperature resistant sagger, and on the other hand, when the sagger material is rapidly cooled after high temperature, cracks are easily generated on the sagger along with the increase of the using times, the thermal shock stability of the sagger is damaged, and the service life of the high-temperature resistant sagger can be greatly reduced. In view of the above disadvantages, a new sagger using recrystallized silicon carbide is being gradually substituted for the sagger. The sagger is prepared by adopting recrystallized silicon carbide material, and the sagger is prepared by mixing and molding raw materials to prepare a sagger green body and then calcining the raw material.
The forming method of the recrystallized silicon carbide material mainly adopts two types of slip casting and extrusion forming in the industrial production at present. The grouting forming can prepare any thin-wall injection piece with complex appearance and large size, and the blank body has uniform structure. The extrusion molding method has the advantages of continuous production, high efficiency, wide application range and the like. However, the requirements of the two methods on the particle size of the material are relatively high, the particle size of the material particles is not suitable to be too large, and the blanks prepared by the two methods have the following defects: the shrinkage rate is large, and the thermal stability is reduced; the green body has low molding density, and the high-temperature mechanical strength of the green body is influenced; in addition, although slip casting is suitable for blanks in various shapes, the slip casting is not suitable for automatic production and has low production efficiency; the extrusion molding is suitable for automated production and has high production efficiency, but is only suitable for manufacturing tubular blanks, and saggars used for lithium ion battery anode materials are usually square block-shaped bodies.
Disclosure of Invention
In view of the above problems, an object of the present invention is to provide a method for forming a sagger for a lithium battery positive electrode material, which has a wide range of applicable particle sizes, a high green body forming density, a low green body shrinkage rate, is suitable for forming a sagger green body for a lithium battery positive electrode material, has a high production efficiency, and is suitable for automated operation. The specific technical scheme is as follows:
a forming method of a sagger for a lithium battery positive electrode material comprises the following steps:
s1, pretreating powder: adding a binder and a coupling agent into the silicon carbide powder and uniformly mixing to obtain the premix.
S2, die filling and prepressing: the premix is filled in a hard die, and is pre-pressed and molded by an automatic hydraulic machine (similar to an automatic hydraulic brick press) to obtain a semi-finished sagger blank.
S3, drying: and (3) putting the semi-finished sagger blank into a drying chamber with the temperature of 45-55 ℃ for air drying for 18-22 hours, and taking out.
S4, die filling: wrapping and sealing the semi-finished sagger blank processed in the step S3 by using an elastic die; and (3) uniformly coating a release agent in the elastic mould before mould filling.
S5, forming: placing the sealed elastic die tightly wrapped with the semi-finished sagger blank into a high-pressure cylinder and suspending the elastic die in the high-pressure cylinder in the air by using a high-pressure resistant rope; then covering a high-pressure cylinder sealing cover; and continuously injecting liquid between the interior of the high-pressure cylinder and the elastic mold for pressurization, keeping the pressure for 10-20 hours when the internal pressure reaches 4500-5500kgf/cm2, then releasing the liquid at the speed of reducing 800kgf/cm2 per hour for slow pressure release, taking out the elastic mold after pressure release is finished, putting the elastic mold into a drying chamber at 55-60 ℃ for air drying for 30-60 minutes, taking out the elastic mold, opening the elastic mold, and removing the elastic mold to obtain the finished sagger blank.
Further, in step S2, the hard mold is a steel mold, preferably a stainless steel mold.
Further, the pressure of the automatic hydraulic press acting on the hard die is 300-600kgf/cm 2. More preferably, the pressure applied to the hard mold by the automatic hydraulic press is 500kgf/cm 2.
Further, the temperature of the drying chamber in step S3 was 50 ℃.
Further, the elastic mold of step S4 is made of one of silicone rubber, polyurethane, and vinyl chloride. Silicone rubber molds are preferred.
Further, the pressure holding time of step S5 is 12 hours.
Further, the coupling agent in step S1 is silane.
The invention has the following advantages:
the sagger blank obtained by pressing by the method has the outstanding advantages of uniform tissue structure, high density, small sintering shrinkage rate, low mould cost, high production efficiency, capability of forming long and thin products with complex shapes, large-size products and precise-size products, suitability for automatic operation and the like.
Detailed Description
The present invention will be described in further detail with reference to examples.
The first embodiment is as follows:
a forming method of a sagger for a lithium battery positive electrode material comprises the following steps:
s1, pretreating powder: adding a binder and a coupling agent into the silicon carbide powder and uniformly mixing to obtain the premix.
S2, die filling and prepressing: the premix was filled in a stainless steel mold and an automatic hydraulic press (pre-press molding to obtain a semi-finished sagger blank, the pressure of the automatic hydraulic press on the hard mold was 500kgf/cm 2.
S3, drying: and (3) putting the semi-finished sagger blank into a drying chamber at 50 ℃, air-drying for 20 hours, and taking out.
S4, die filling: wrapping and sealing the semi-finished sagger blank processed in the step S3 by using a silicon rubber mold; and (3) uniformly coating a release agent in the silicon rubber mold before mold filling.
S5, forming: placing the sealed silicon rubber mold tightly wrapped with the semi-finished sagger blank into a high-pressure cylinder and suspending the silicon rubber mold in the high-pressure cylinder in the air by using a high-pressure resistant rope; then covering a high-pressure cylinder sealing cover; and continuously injecting liquid between the interior of the high-pressure cylinder and the silicon rubber mold for pressurization, keeping the pressure for 12 hours when the internal pressure reaches 5000kgf/cm2, then releasing the liquid at the speed of reducing 800kgf/cm2 per hour for slow pressure release, taking out the silicon rubber mold after pressure release is finished, putting the silicon rubber mold into a drying chamber at the temperature of 55 ℃ for air drying for 40 minutes, taking out the silicon rubber mold, opening the silicon rubber mold, and removing the silicon rubber mold to obtain the finished sagger blank.
Example two:
a forming method of a sagger for a lithium battery positive electrode material comprises the following steps:
s1, pretreating powder: adding a binder and a coupling agent into the silicon carbide powder and uniformly mixing to obtain the premix.
S2, die filling and prepressing: filling the premix in a hard die, and performing pre-pressing forming by adopting an automatic hydraulic press to obtain a semi-finished sagger blank; the pressure of the automatic hydraulic press on the hard mold was 350kgf/cm 2.
S3, drying: and (3) putting the semi-finished sagger blank into a drying chamber with the temperature of 55 ℃ for air drying for 22 hours, and taking out.
S4, die filling: covering the semi-finished sagger blank processed in the step S3 by a polyurethane mould and sealing; and (3) uniformly coating a release agent in the polyurethane mold before mold filling.
S5, forming: placing the sealed polyurethane mold tightly wrapped with the semi-finished sagger blank into a high-pressure cylinder and suspending the polyurethane mold in the high-pressure cylinder in the air by using a high-pressure resistant rope; then covering a high-pressure cylinder sealing cover; and continuously injecting liquid between the interior of the high-pressure cylinder and the polyurethane mold for pressurization, maintaining the pressure for 16 hours when the internal pressure reaches 4600kgf/cm2, then reducing the internal pressure in the high-pressure cylinder by 800kgf/cm2 per hour to release the liquid for slow pressure release, taking out the polyurethane mold after pressure release is finished, putting the polyurethane mold into a drying chamber at the temperature of 60 ℃ for air drying for 35 minutes, taking out the polyurethane mold, opening the polyurethane mold, and removing the polyurethane mold to obtain the finished sagger blank.
Example three:
a forming method of a sagger for a lithium battery positive electrode material comprises the following steps:
s1, pretreating powder: adding a binder and a coupling agent into the silicon carbide powder and uniformly mixing to obtain the premix.
S2, die filling and prepressing: filling the premix in a hard die, and performing pre-pressing forming by adopting an automatic hydraulic press to obtain a semi-finished sagger blank; the pressure of the automatic hydraulic press on the hard mold was 400kgf/cm 2. .
S3, drying: and (3) putting the semi-finished sagger blank into a drying chamber with the temperature of 45 ℃, air-drying for 22 hours, and taking out.
S4, die filling: wrapping the semi-finished sagger blank processed in the step S3 by using a vinyl chloride mould and sealing; and (3) uniformly coating a release agent in the vinyl chloride mould before filling.
S5, forming: placing a vinyl chloride mould tightly wrapped with semi-finished sagger blanks and sealed into a high-pressure cylinder and suspending the vinyl chloride mould in the high-pressure cylinder in the air by using a high-pressure resistant rope; then covering a high-pressure cylinder sealing cover; and continuously injecting liquid between the interior of the high-pressure cylinder and the vinyl chloride mold for pressurization, maintaining the pressure for 10 hours when the internal pressure reaches 5500kgf/cm2, then releasing the liquid at the speed of reducing 800kgf/cm2 per hour for slow pressure release, taking out the vinyl chloride mold after pressure release is finished, putting the vinyl chloride mold into a drying chamber at 55 ℃ for air drying for 50 minutes, taking out the vinyl chloride mold, opening the vinyl chloride mold, and removing the vinyl chloride mold to obtain the finished sagger blank.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (8)
1. A forming method of a sagger for a lithium battery positive electrode material is characterized by comprising the following steps:
s1, pretreating powder: adding a binder and a coupling agent into the silicon carbide powder and uniformly mixing to obtain a premix;
s2, die filling and prepressing: filling the premix in a hard die, and performing pre-pressing forming by adopting an automatic hydraulic press to obtain a semi-finished sagger blank;
s3, drying: putting the semi-finished sagger blank into a drying chamber with the temperature of 45-55 ℃ for air drying for 18-22 hours, and taking out;
s4, die filling: wrapping and sealing the semi-finished sagger blank processed in the step S3 by using an elastic die; uniformly coating a release agent in the elastic mould before mould filling;
s5, forming: placing the sealed elastic die tightly wrapped with the semi-finished sagger blank into a high-pressure cylinder and suspending the elastic die in the high-pressure cylinder in the air by using a high-pressure resistant rope; then covering a high-pressure cylinder sealing cover; and continuously injecting liquid between the interior of the high-pressure cylinder and the elastic mold for pressurization, keeping the pressure for 10-20 hours when the internal pressure reaches 4500-5500kgf/cm2, then releasing the liquid at the speed of reducing 800kgf/cm2 per hour for slow pressure release, taking out the elastic mold after pressure release is finished, putting the elastic mold into a drying chamber at 55-60 ℃ for air drying for 30-60 minutes, taking out the elastic mold, opening the elastic mold, and removing the elastic mold to obtain the finished sagger blank.
2. The method for forming a sagger for a positive electrode material of a lithium battery as claimed in claim 1, wherein: and step S2, the hard die is a steel die.
3. The method for forming a sagger for a positive electrode material of a lithium battery as claimed in claim 1, wherein: the pressure of the automatic hydraulic press acting on the hard die is 300-600kgf/cm 2.
4. The method for forming a sagger for a positive electrode material of a lithium battery as claimed in claim 3, wherein: the pressure of the automatic hydraulic press on the hard mold was 500kgf/cm 2.
5. The method for forming a sagger for a positive electrode material of a lithium battery as claimed in claim 1, wherein: the temperature of the drying chamber in step S3 was 50 ℃.
6. The method for forming a sagger for a positive electrode material of a lithium battery as claimed in claim 1, wherein: step S4 the elastic mold is made of one of silicone rubber, polyurethane, and vinyl chloride.
7. The method for forming a sagger for a positive electrode material of a lithium battery as claimed in claim 1, wherein: the dwell time is 12 hours at step S5.
8. The method for forming a sagger for a positive electrode material of a lithium battery as claimed in claim 1, wherein: step S1 the coupling agent is silane.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911278502.XA CN111037710A (en) | 2019-12-12 | 2019-12-12 | Forming method of sagger for lithium battery positive electrode material |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911278502.XA CN111037710A (en) | 2019-12-12 | 2019-12-12 | Forming method of sagger for lithium battery positive electrode material |
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| Publication Number | Publication Date |
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| CN111037710A true CN111037710A (en) | 2020-04-21 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201911278502.XA Pending CN111037710A (en) | 2019-12-12 | 2019-12-12 | Forming method of sagger for lithium battery positive electrode material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114161547A (en) * | 2021-12-13 | 2022-03-11 | 湖南太子新材料科技有限公司 | Forming method of sagger for lithium battery positive electrode material |
Citations (5)
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| JPH08302403A (en) * | 1995-05-10 | 1996-11-19 | Kobe Steel Ltd | Press molding method |
| CN101100384A (en) * | 2007-07-20 | 2008-01-09 | 浙江大学 | Nanometer composite silicon carbide ceramic and preparation method thereof |
| CN104386670A (en) * | 2014-04-23 | 2015-03-04 | 天津锦美碳材科技发展有限公司 | Isostatic-pressure high-purity graphite material and preparation method thereof |
| CN108484188A (en) * | 2018-05-07 | 2018-09-04 | 武汉科技大学 | A kind of silicon carbide sagger and preparation method thereof for anode material of lithium battery roasting |
| CN109192946A (en) * | 2018-08-28 | 2019-01-11 | 大同新成新材料股份有限公司 | A kind of preparation method of titanium-based ion cathode material lithium |
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2019
- 2019-12-12 CN CN201911278502.XA patent/CN111037710A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08302403A (en) * | 1995-05-10 | 1996-11-19 | Kobe Steel Ltd | Press molding method |
| CN101100384A (en) * | 2007-07-20 | 2008-01-09 | 浙江大学 | Nanometer composite silicon carbide ceramic and preparation method thereof |
| CN104386670A (en) * | 2014-04-23 | 2015-03-04 | 天津锦美碳材科技发展有限公司 | Isostatic-pressure high-purity graphite material and preparation method thereof |
| CN108484188A (en) * | 2018-05-07 | 2018-09-04 | 武汉科技大学 | A kind of silicon carbide sagger and preparation method thereof for anode material of lithium battery roasting |
| CN109192946A (en) * | 2018-08-28 | 2019-01-11 | 大同新成新材料股份有限公司 | A kind of preparation method of titanium-based ion cathode material lithium |
Non-Patent Citations (1)
| Title |
|---|
| 李瑛娟、宋群玲: "《炭素生产机械设备》", 30 September 2017 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114161547A (en) * | 2021-12-13 | 2022-03-11 | 湖南太子新材料科技有限公司 | Forming method of sagger for lithium battery positive electrode material |
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Application publication date: 20200421 |
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| RJ01 | Rejection of invention patent application after publication |