CN114361637A - Method for separating electrode material and foil of lithium battery - Google Patents
Method for separating electrode material and foil of lithium battery Download PDFInfo
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- CN114361637A CN114361637A CN202210042729.XA CN202210042729A CN114361637A CN 114361637 A CN114361637 A CN 114361637A CN 202210042729 A CN202210042729 A CN 202210042729A CN 114361637 A CN114361637 A CN 114361637A
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Abstract
The invention provides a method for separating an electrode material and a foil of a lithium battery, which comprises the following steps: and mixing the positive pole piece and/or the negative pole piece with the ball-milled beads, vibrating and roasting in sections, and separating to obtain a positive pole material and/or a negative pole material, and an aluminum foil and/or a copper foil. The invention adopts a simple method to effectively separate the anode/cathode material and the foil, can obtain electrode materials with different grades, has controllable aluminum and/or copper impurity content, and has the advantages of safe and environment-friendly whole recovery process, simple process, low energy consumption, good economy and the like.
Description
Technical Field
The invention relates to the field of treatment and recovery of waste materials of lithium ion batteries, in particular to a method for separating electrode materials and foils of lithium ion batteries.
Background
Owing to the advantages of high voltage, high energy density, good cyclicity and the like, the lithium ion battery is widely applied to the fields of mobile intelligent terminals, small-sized electric equipment, power grid energy storage, electric automobiles and the like. According to statistics, in 2019, as many as 157.2 hundred million lithium ion batteries are produced in China. With the increase of the usage amount of the lithium ion battery, the retirement amount of the lithium ion battery is increased. It is estimated that over 1100 million tons of decommissioned lithium ion batteries are expected to be produced globally during 2017-2030 years.
A large amount of Li, Ni, Co, Mn, Fe, Cu, Al and other metals are used in the lithium ion battery, and the retired lithium ion battery is a rich valuable technology mineral deposit. The recovery of the lithium ion battery has important economic and environmental protection significance.
And carrying out pretreatment such as discharging and disassembling on the waste lithium ion battery to obtain the anode/cathode material containing the foil. For the separation of the anode/cathode material and the foil material, an alkali solution dissolving method, an organic solvent dissolving method and high-temperature pyrolysis are mainly adopted. The alkali solution dissolution method has the disadvantages of serious heat release, difficult reaction control, hydrogen generation, serious corrosion to equipment and high treatment cost. The organic solvent dissolution method has the disadvantages of serious solvent volatilization, poor recycling and toxicity. High-temperature pyrolysis, large energy consumption, and generation of a large amount of harmful waste gas containing fluorine, which is easy to cause secondary pollution.
Disclosure of Invention
In order to solve the problems existing in the prior art of separating the positive/negative electrode material and the foil, the invention provides a method for separating the electrode material and the foil of the lithium battery.
In order to achieve the above object, an embodiment of the present invention provides a method for separating an electrode material from a foil of a lithium battery, the method comprising the steps of:
s1: mixing a primary positive pole piece and/or a primary negative pole piece obtained after disassembly of a retired lithium battery with ball-milled beads, roasting and vibrating to respectively obtain a primary recovered positive pole material and/or a primary recovered negative pole material, and a secondary positive pole piece and/or a secondary negative pole piece;
s2: mixing the secondary positive pole piece and/or the secondary negative pole piece with the ball-milled beads, roasting and vibrating to respectively obtain a secondary recovered positive pole material and/or a secondary recovered negative pole material, and a tertiary positive pole piece and/or a tertiary negative pole piece;
s3: mixing the three-stage positive pole piece and/or negative pole piece with the ball-milled beads, roasting and vibrating to respectively obtain a three-stage recovered positive pole material and/or negative pole material, and a four-stage positive pole piece and/or negative pole piece;
s4: and mixing the four-stage positive pole piece and/or negative pole piece with the ball-milled beads, roasting and vibrating to respectively obtain four-stage recycled positive pole material and/or negative pole material, waste aluminum foil and/or copper foil.
Further, in the step S1, the mass ratio of the primary positive electrode sheet and/or negative electrode sheet to the ball-milled beads is 1: 1 to 10.
Further, the roasting temperature in the step S1 is 100-150 ℃, the roasting time is 2-30min, and the vibration frequency of the ball milling beads is 20-300 times/min.
Further, in the step S2, the mass ratio of the secondary positive electrode sheet and/or negative electrode sheet to the ball-milled beads is 1: 5 to 12.
Further, the roasting temperature in the step S2 is 150-.
Further, in the step S3, the mass ratio of the three-stage positive electrode piece and/or negative electrode piece to the ball-milling beads is 1: 10 to 20.
Further, the roasting temperature in the step S3 is 200-.
Further, in the step S4, the mass ratio of the four-stage positive electrode sheet and/or negative electrode sheet to the ball-milled beads is 1: 5 to 25.
Furthermore, the roasting temperature in the step S4 is 250-350 ℃, the vibration frequency of the ball milling beads is 30-200 times/min, and the roasting time is 1-20 min.
Further, in the step S1, the material of the ball milling beads is one or more of zirconia, alumina, polyurethane and stainless steel, in the step S2, the material of the ball milling beads is one or more of zirconia, alumina and stainless steel, in the step S3, the material of the ball milling beads is one or two of zirconia and alumina, and in the step S4, the material of the ball milling beads is zirconia.
The invention mixes the anode pole piece and/or the cathode pole piece obtained after the decommissioned lithium battery with ball-milling beads, then carries out roasting in sections and simultaneously vibrates, so that the ball-milling beads bounce and the anode pole piece and/or the cathode pole piece are fully contacted, and the anode material and/or the cathode material are separated from the aluminum foil and/or the copper foil by utilizing the mechanical force generated when the ball-milling beads are contacted with the anode pole piece and/or the cathode pole piece.
The scheme of the invention has the following beneficial effects:
1) the separation method of the scheme of the invention is a method for mixing the positive pole piece and/or the negative pole piece with the ball milling beads, vibrating and roasting in sections to obtain the recycled materials with different grades in sections: the aluminum content in the primary and secondary recovered anode materials is 0; the copper content in the first-stage and second-stage recycled negative electrode materials is 0; the aluminum content in the three-level recovered positive electrode material is 10ppm, the copper content in the three-level recovered negative electrode material is 10ppm, the aluminum content in the four-level recovered positive electrode material is 100ppm, and the copper content in the four-level recovered negative electrode material is 30 ppm;
2) the invention mixes the anode plate and/or the cathode plate with the ball milling beads, and then vibrates and calcinates the mixture in sections, thereby reducing the processing cost and avoiding the harm to the environment and human body caused by the prior alkali liquor, organic solvent and high-temperature pyrolysis technology.
Drawings
Fig. 1 is a process flow chart of a method for separating a positive/negative electrode material and a foil of a lithium battery according to an embodiment of the present invention.
Detailed Description
In order to make the technical problems, technical solutions and advantages of the present invention more apparent, the following detailed description is given with reference to the accompanying drawings and specific embodiments.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention, and unless otherwise specifically indicated, various starting materials, reagents, equipment and devices, etc. used in the present invention may be commercially available or may be prepared by conventional methods.
Aiming at the existing problems, the invention provides a method for separating an electrode material and a foil material of a lithium battery.
As shown in fig. 1, the embodiment of the present invention provides a process flow chart of a method for separating an electrode material from a foil material of a lithium battery.
Example 1
And (3) taking the waste lithium ion battery, cleaning the shell of the waste lithium ion battery, and completely drying the shell at 20 ℃. And (3) disassembling the dried waste lithium ion battery in a protective atmosphere to obtain a shell and a battery core package, and randomly cutting the battery core package into pieces to obtain a mixed piece containing the anode/cathode material and the foil.
Mixing a first-stage negative pole piece and zirconia ball grinding beads according to the mass ratio of 1: 10, mixing, roasting at a first interval temperature of 150 ℃ for 30min, and vibrating at a frequency of 300 times/min to separate the negative electrode material from the copper foil to obtain a first-stage recycled negative electrode material and a second-stage negative electrode piece;
and (3) mixing the secondary negative pole piece with zirconia ball grinding beads according to the mass ratio of 1: 12, mixing, roasting for 60min at the temperature of 200 ℃ in a second interval, and vibrating at the frequency of 200 times/min to separate the negative electrode material from the copper foil to obtain a secondary recovered negative electrode material and a tertiary negative electrode plate;
and (3) grinding the three-stage negative pole piece and zirconia ball according to the mass ratio of 1: 20, mixing, roasting at 250 ℃ in a third interval for 40min, vibrating at the frequency of 200 times/min, and separating the negative electrode material from the copper foil to obtain a three-level recycled negative electrode material and a four-level negative electrode plate;
and (3) grinding the four-level negative pole piece and zirconia ball according to the mass ratio of 1: 25, then roasting for 20min at the temperature of 350 ℃ in a fourth interval, vibrating at the frequency of 200 times/min, and separating the negative electrode material from the copper foil to obtain a four-stage recycled negative electrode material and waste copper foil.
Table 1 copper content in recycled negative electrode material obtained in example 1 of the present invention
Example 2
And (3) taking the waste lithium ion battery, cleaning the shell of the waste lithium ion battery, and completely drying the shell at 20 ℃. And (3) disassembling the dried waste lithium ion battery in a protective atmosphere to obtain a shell and a battery core package, and randomly cutting the battery core package into pieces to obtain a mixed piece containing the anode/cathode material and the foil.
Mixing a primary positive/negative electrode mixed pole piece with zirconium oxide or stainless steel ball grinding beads according to a mass ratio of 1: 5, mixing, roasting for 15min at the temperature of 125 ℃ in a first interval, and vibrating at the frequency of 150 times/min to separate the positive electrode material and the negative electrode material from the aluminum foil and the copper foil respectively to obtain a first-stage positive/negative electrode mixed material and a second-stage positive/negative electrode mixed pole piece;
mixing the secondary positive/negative electrode mixed pole piece with zirconium oxide and stainless steel ball grinding beads according to the mass ratio of 1: 10, mixing, roasting at 175 ℃ in a second interval for 30min, and vibrating at 150 times/min to separate the anode material and the cathode material from the aluminum foil and the copper foil respectively to obtain a second-stage anode/cathode mixed material and a third-stage anode/cathode mixed pole piece;
mixing a three-stage positive/negative electrode mixed pole piece with zirconium oxide and aluminum oxide balls, and grinding the three-stage positive/negative electrode mixed pole piece with the zirconium oxide and aluminum oxide balls according to a mass ratio of 1: 15, then roasting for 20min at a third interval temperature of 225 ℃, and simultaneously vibrating according to the frequency of 100 times/min to separate the anode material and the cathode material from the aluminum foil and the copper foil respectively to obtain a three-level anode/cathode mixed material and a four-level anode/cathode mixed pole piece;
mixing a four-stage positive/negative electrode mixed pole piece with zirconia and alumina ball grinding beads according to the mass ratio of 1: 20, mixing, roasting at 275 ℃ in a fourth interval for 10min, and vibrating at the frequency of 100 times/min to separate the positive electrode material and the negative electrode material from the aluminum foil and the copper foil respectively to obtain a four-level positive/negative electrode mixed material and a waste positive/negative electrode mixed pole piece;
example 3
And (3) taking the waste lithium ion battery, cleaning the shell of the waste lithium ion battery, and completely drying the shell at 20 ℃. And (3) disassembling the dried waste lithium ion battery in a protective atmosphere to obtain a shell and a battery core package, and randomly cutting the battery core package into pieces to obtain a mixed piece containing the anode/cathode material and the foil.
Mixing a first-stage positive pole piece with zirconia and polyurethane ball-milling beads according to a mass ratio of 1: 1, mixing, roasting at the first interval temperature of 100 ℃ for 7.5min, and vibrating at the frequency of 75 times/min to separate the anode material from the aluminum foil to obtain a primary recovered anode material and a secondary anode plate;
and (3) mixing the secondary positive pole piece with the alumina ball grinding beads according to the mass ratio of 1: 5, mixing, roasting for 15min at the temperature of 150 ℃ in a second interval, and vibrating at the frequency of 75 times/min to separate the positive electrode material from the aluminum foil to obtain a secondary recovered positive electrode material and a tertiary positive electrode plate;
and (3) mixing the three-stage positive pole piece with zirconia or alumina ball grinding beads according to the mass ratio of 1: 10, mixing, roasting at the temperature of 200 ℃ in a third interval for 10min, and vibrating at the frequency of 50 times/min to separate the positive electrode material from the aluminum foil to obtain a three-level recovered positive electrode material and a four-level positive electrode plate;
grinding four-stage positive pole pieces and zirconia balls according to a mass ratio of 1: 15, then roasting for 5min at the temperature of 250 ℃ in a fourth interval, and simultaneously vibrating for 50 times/min to separate the anode material from the aluminum foil so as to obtain a four-stage recovered anode material and a waste aluminum foil;
table 3 content of aluminum in recovered positive electrode material obtained in example 3 of the present invention
Table 4 recovery rate of recovered positive electrode material obtained in example 3 of the present invention
Comparative example 1
And (3) taking the waste lithium ion battery, cleaning the shell of the waste lithium ion battery, and completely drying the shell at 20 ℃. And (3) disassembling the dried waste lithium ion battery in a protective atmosphere to obtain a shell and a battery core package, and randomly cutting the battery core package into pieces to obtain a mixed piece containing the anode/cathode material and the foil.
Mixing a first-stage negative pole piece and zirconia ball grinding beads according to the mass ratio of 1: 10, mixing, roasting at a first interval temperature of 150 ℃ for 30min, and vibrating at a frequency of 300 times/min to separate the negative electrode material from the copper foil to obtain a first-stage recycled negative electrode material and a second-stage negative electrode piece;
and (3) mixing the secondary negative pole piece with zirconia ball grinding beads according to the mass ratio of 1: 12, mixing, roasting at the temperature of 150 ℃ in a first interval for 60min, and vibrating at the frequency of 200 times/min to separate the negative electrode material from the copper foil to obtain a secondary recovered negative electrode material and a tertiary negative electrode piece;
and (3) grinding the three-stage negative pole piece and zirconia ball according to the mass ratio of 1: 20, mixing, roasting at a first interval temperature of 150 ℃ for 40min, vibrating at a frequency of 200 times/min, and separating the negative electrode material from the copper foil to obtain a three-level recycled negative electrode material and a four-level negative electrode plate;
and (3) grinding the four-level negative pole piece and zirconia ball according to the mass ratio of 1: 25, then roasting for 20min at the temperature of 150 ℃ in the first interval, vibrating at the frequency of 200 times/min, and separating the negative electrode material from the copper foil to obtain a four-stage recycled negative electrode material and waste copper foil.
Table 5 copper content in recovered anode material obtained in comparative example 1 of the present invention
Table 6 recovery rate of recovered anode material obtained in comparative example 1 of the present invention
Comparative example 2
And (3) taking the waste lithium ion battery, cleaning the shell of the waste lithium ion battery, and completely drying the shell at 20 ℃. And (3) disassembling the dried waste lithium ion battery in a protective atmosphere to obtain a shell and a battery core package, and randomly cutting the battery core package into pieces to obtain a mixed piece containing the anode/cathode material and the foil.
Mixing a first-stage negative pole piece and zirconia ball grinding beads according to the mass ratio of 1: 10, mixing, roasting at a first interval temperature of 150 ℃ for 30min, and vibrating at a frequency of 300 times/min to separate the negative electrode material from the copper foil to obtain a first-stage recycled negative electrode material and a second-stage negative electrode piece;
and (3) mixing the secondary negative pole piece with zirconia ball grinding beads according to the mass ratio of 1: 12, mixing, roasting for 60min at the temperature of 200 ℃ in a second interval, and vibrating at the frequency of 200 times/min to separate the negative electrode material from the copper foil to obtain a secondary recovered negative electrode material and a tertiary negative electrode plate;
and (3) grinding the three-stage negative pole piece and zirconia ball according to the mass ratio of 1: 20, mixing, roasting at 250 ℃ in a third interval for 40min, vibrating at the frequency of 200 times/min, and separating the negative electrode material from the copper foil to obtain a three-level recycled negative electrode material and a four-level negative electrode plate;
and (3) grinding the four-level negative pole piece and zirconia ball according to the mass ratio of 1: 25, then roasting for 20min at the temperature of 250 ℃ in a third interval, vibrating at the frequency of 200 times/min, and separating the negative electrode material from the copper foil to obtain a four-stage recycled negative electrode material and waste copper foil.
Table 7 copper content in recovered anode material obtained in comparative example 2 of the present invention
Table 8 recovery rate of recovered anode material obtained in comparative example 2 of the present invention
Comparative example 3
And (3) taking the waste lithium ion battery, cleaning the shell of the waste lithium ion battery, and completely drying the shell at 20 ℃. And (3) disassembling the dried waste lithium ion battery in a protective atmosphere to obtain a shell and a battery core package, and randomly cutting the battery core package into pieces to obtain a mixed piece containing the anode/cathode material and the foil.
Mixing a first-stage positive pole piece with zirconia and polyurethane ball-milling beads according to a mass ratio of 1: 1, mixing, roasting at the first interval temperature of 100 ℃ for 7.5min, and vibrating at the frequency of 75 times/min to separate the anode material from the aluminum foil to obtain a primary recovered anode material and a secondary anode plate;
and (3) mixing the secondary positive pole piece with the alumina ball grinding beads according to the mass ratio of 1: 5, mixing, roasting for 15min at the first interval temperature of 100 ℃, and vibrating at the frequency of 75 times/min to separate the anode material from the aluminum foil to obtain a secondary recovered anode material and a tertiary anode plate;
and (3) mixing the three-stage positive pole piece with zirconia or alumina ball grinding beads according to the mass ratio of 1: 10, mixing, roasting at 100 ℃ in a first interval for 10min, and vibrating at the frequency of 50 times/min to separate the positive electrode material from the aluminum foil to obtain a three-level recovered positive electrode material and a four-level positive electrode plate;
grinding four-stage positive pole pieces and zirconia balls according to a mass ratio of 1: 15, then roasting for 5min at the first interval temperature of 100 ℃, and simultaneously vibrating according to the frequency of 50 times/min to separate the anode material from the aluminum foil, thereby obtaining a four-stage recovered anode material and a waste aluminum foil;
table 9 content of aluminum in recovered positive electrode material obtained in comparative example 3 of the present invention
Table 10 recovery rate of recovered positive electrode material obtained in comparative example 3 of the present invention
Comparative example 4
This example is a comparative example. And (3) taking the waste lithium ion battery, cleaning the shell of the waste lithium ion battery, and completely drying the shell at 20 ℃. And (3) disassembling the dried waste lithium ion battery in a protective atmosphere to obtain a shell and a battery core package, and randomly cutting the battery core package into pieces to obtain a mixed piece containing the anode/cathode material and the foil.
Mixing a first-stage positive pole piece with zirconia and polyurethane ball-milling beads according to a mass ratio of 1: 1, mixing, roasting at the first interval temperature of 100 ℃ for 7.5min, and vibrating at the frequency of 75 times/min to separate the anode material from the aluminum foil to obtain a primary recovered anode material and a secondary anode plate;
and (3) mixing the secondary positive pole piece with the alumina ball grinding beads according to the mass ratio of 1: 5, mixing, roasting for 15min at the temperature of 150 ℃ in a second interval, and vibrating at the frequency of 75 times/min to separate the positive electrode material from the aluminum foil to obtain a secondary recovered positive electrode material and a tertiary positive electrode plate;
and (3) mixing the three-stage positive pole piece with zirconia or alumina ball grinding beads according to the mass ratio of 1: 10, mixing, roasting at the temperature of 200 ℃ in a third interval for 10min, and vibrating at the frequency of 50 times/min to separate the positive electrode material from the aluminum foil to obtain a three-level recovered positive electrode material and a four-level positive electrode plate;
grinding four-stage positive pole pieces and zirconia balls according to a mass ratio of 1: 15, then roasting for 5min at the temperature of 200 ℃ in a third interval, and simultaneously vibrating for 50 times/min to separate the anode material from the aluminum foil so as to obtain a four-stage recovered anode material and a waste aluminum foil;
table 11 content of aluminum in recovered positive electrode material obtained in comparative example 4 of the present invention
Table 12 recovery rate of recovered positive electrode material obtained in comparative example 4 of the present invention
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (10)
1. A method for separating an electrode material and a foil of a lithium battery is characterized by comprising the following steps:
s1: mixing a primary positive pole piece and/or a primary negative pole piece obtained after disassembly of a retired lithium battery with ball-milled beads, roasting and vibrating to respectively obtain a primary recovered positive pole material and/or a primary recovered negative pole material, and a secondary positive pole piece and/or a secondary negative pole piece;
s2: mixing the secondary positive pole piece and/or the secondary negative pole piece with the ball-milled beads, roasting and vibrating to respectively obtain a secondary recovered positive pole material and/or a secondary recovered negative pole material, and a tertiary positive pole piece and/or a tertiary negative pole piece;
s3: mixing the three-stage positive pole piece and/or negative pole piece with the ball-milled beads, roasting and vibrating to respectively obtain a three-stage recovered positive pole material and/or negative pole material, and a four-stage positive pole piece and/or negative pole piece;
s4: and mixing the four-stage positive pole piece and/or negative pole piece with the ball-milled beads, roasting and vibrating to respectively obtain four-stage recycled positive pole material and/or negative pole material, waste aluminum foil and/or copper foil.
2. The separation method according to claim 1, wherein the mass ratio of the primary positive electrode sheet and/or negative electrode sheet to the ball-milled beads in the step S1 is 1: 1 to 10.
3. The separation method as claimed in claim 1, wherein the calcination temperature in step S1 is 100-150 ℃, the calcination time is 2-30min, and the vibration frequency of the ball milling beads is 20-300 times/min.
4. The separation method according to claim 1, wherein the mass ratio of the secondary positive electrode sheet and/or negative electrode sheet mixed with the ball-milled beads in the step S2 is 1: 5 to 12.
5. The separation method as claimed in claim 1, wherein the calcination temperature in step S2 is 150 ℃ to 200 ℃, the vibration frequency of the ball milling beads is 60-300 times/min, and the calcination time is 5-60 min.
6. The separation method according to claim 1, wherein the mass ratio of the three-stage positive electrode sheet and/or negative electrode sheet to the ball-milled beads in the step S3 is 1: 10 to 20.
7. The separation method as claimed in claim 1, wherein the calcination temperature in step S3 is 200-250 ℃, the vibration frequency of the ball-milling beads is 20-200 times/min, and the calcination time is 2-40 min.
8. The separation method according to claim 1, wherein the mass ratio of the four-stage positive electrode sheet and/or negative electrode sheet to the ball-milled beads in the step S4 is 1: 5 to 25.
9. The separation method as claimed in claim 1, wherein the calcination temperature in step S4 is 250-350 ℃, the vibration frequency of the ball-milling beads is 30-200 times/min, and the calcination time is 1-20 min.
10. The separation method according to claim 1, wherein the ball milling beads in the step S1 are made of one or more of zirconia, alumina, polyurethane and stainless steel, the ball milling beads in the step S2 are made of one or more of zirconia, alumina and stainless steel, the ball milling beads in the step S3 are made of one or more of zirconia and alumina, and the ball milling beads in the step S4 are made of zirconia.
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| CN107785631A (en) * | 2017-09-14 | 2018-03-09 | 河南易成新能源股份有限公司 | The recovery method of graphite cathode material |
| CN108832216A (en) * | 2018-06-14 | 2018-11-16 | 合肥工业大学 | A kind of pre-treating method of waste power lithium battery recycling |
| CN209076871U (en) * | 2018-09-25 | 2019-07-09 | 荆门市格林美新材料有限公司 | A kind of broken recovery system of old and useless battery |
| CN109786882A (en) * | 2019-02-25 | 2019-05-21 | 上海毅信环保科技有限公司 | A kind of dry-type pulverizing recovery method of waste and old lithium ion battery |
| CN110148801A (en) * | 2019-05-08 | 2019-08-20 | 株洲冶炼集团股份有限公司 | A kind of vacuum separation method of waste lithium iron phosphate battery positive plate |
| CN110661055A (en) * | 2019-10-14 | 2020-01-07 | 赣州有色冶金研究所 | Method for efficiently stripping waste lithium ion battery material |
| US20210288359A1 (en) * | 2020-09-22 | 2021-09-16 | Huazhong University Of Science And Technology | Method for recycling positive plate of lithium-ion battery |
| CN113690501A (en) * | 2021-07-23 | 2021-11-23 | 广东邦普循环科技有限公司 | Recycling process of battery pole piece without pickling |
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