JPH01320228A - Production of hexa vanadium tridecyloxide - Google Patents
Production of hexa vanadium tridecyloxideInfo
- Publication number
- JPH01320228A JPH01320228A JP63152156A JP15215688A JPH01320228A JP H01320228 A JPH01320228 A JP H01320228A JP 63152156 A JP63152156 A JP 63152156A JP 15215688 A JP15215688 A JP 15215688A JP H01320228 A JPH01320228 A JP H01320228A
- Authority
- JP
- Japan
- Prior art keywords
- positive electrode
- nh4vo3
- discharge capacity
- heating
- vanadium
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000004519 manufacturing process Methods 0.000 title claims description 12
- XPTBREFNLXCPSN-UHFFFAOYSA-N C(CCCCCCCCCCCC)OCCCCCCCCCCCCC.[V].[V].[V].[V].[V].[V] Chemical compound C(CCCCCCCCCCCC)OCCCCCCCCCCCCC.[V].[V].[V].[V].[V].[V] XPTBREFNLXCPSN-UHFFFAOYSA-N 0.000 title abstract 2
- 238000010438 heat treatment Methods 0.000 claims abstract description 20
- 239000012298 atmosphere Substances 0.000 claims abstract description 11
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims abstract description 8
- 239000011261 inert gas Substances 0.000 claims abstract description 4
- -1 hexavanadium hexaoxide Chemical compound 0.000 claims 1
- 239000007774 positive electrode material Substances 0.000 abstract description 14
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 abstract description 6
- 229910003206 NH4VO3 Inorganic materials 0.000 abstract description 4
- 229910052786 argon Inorganic materials 0.000 abstract description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 2
- 229910001873 dinitrogen Inorganic materials 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 16
- 229910052744 lithium Inorganic materials 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 10
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000011255 nonaqueous electrolyte Substances 0.000 description 4
- 238000011056 performance test Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 239000012212 insulator Substances 0.000 description 2
- 239000007773 negative electrode material Substances 0.000 description 2
- 229910052720 vanadium Inorganic materials 0.000 description 2
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 2
- SPEUIVXLLWOEMJ-UHFFFAOYSA-N 1,1-dimethoxyethane Chemical compound COC(C)OC SPEUIVXLLWOEMJ-UHFFFAOYSA-N 0.000 description 1
- JWUJQDFVADABEY-UHFFFAOYSA-N 2-methyltetrahydrofuran Chemical compound CC1CCCO1 JWUJQDFVADABEY-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- MHCFAGZWMAWTNR-UHFFFAOYSA-M lithium perchlorate Chemical compound [Li+].[O-]Cl(=O)(=O)=O MHCFAGZWMAWTNR-UHFFFAOYSA-M 0.000 description 1
- 229910001486 lithium perchlorate Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
Description
【発明の詳細な説明】
[産業上の利用分野]
本発明は、リチウム等の軽金属を負極とする非水電解液
電池において高放電容量、かつ電位平坦性の優れた正極
材料である十三酸化穴バナジウム(V6O13)の製造
方法に関する。[Detailed Description of the Invention] [Industrial Application Field] The present invention is directed to 13 oxide, which is a positive electrode material with high discharge capacity and excellent potential flatness in non-aqueous electrolyte batteries using light metals such as lithium as negative electrodes. The present invention relates to a method for producing hollow vanadium (V6O13).
電解質に非水電解液を用いた電池用正極材料としてMn
O2や(CF)n等を用いたリチウム電池が市場化され
ているが、更に高放電容量かつ電位平坦性の向上を目指
して正極材料としてV60□3を用いたリチウム電池の
研究が行われている。ところが、例えば’Jornal
of theelectrocheilcal 5o
ciety 、 12月号(1981年)、r Rec
hargeable Lith1um/ Vanadl
ui 0xide CellsUtilizing 2
Me−THF / L I A s F a J、K
、M、Abrahaa+ et al ’に見られる製
造方法によって得られるV6O13を用いたリチウム電
池の放電容量および電位平坦性については、未だ十分満
足の行くものではなかった。Mn as a positive electrode material for batteries using non-aqueous electrolyte as electrolyte
Lithium batteries using O2, (CF)n, etc. are on the market, but research is being conducted on lithium batteries using V60□3 as the positive electrode material with the aim of achieving even higher discharge capacity and improved potential flatness. There is. However, for example, 'Journal
of the electrocheilcal 5o
ciety, December issue (1981), r Rec
Hargeable Lith1um/Vanadl
ui Oxide Cells Utilizing 2
Me-THF/LIAsFa J,K
The discharge capacity and potential flatness of a lithium battery using V6O13 obtained by the manufacturing method described in , M., Abrahaa+ et al.' have not yet been fully satisfactory.
また、米国特許第4.488,400号公報には、バナ
ジウム酸アンモニウムを窒素雰囲気中で一定時間昇温し
た後、保持し、次いで特定の雰囲気でさらに加熱するV
6O13の製造方法が開示されているが、製造工程が繁
雑であり、また特定の雰囲気を用いるため、雰囲気の条
件設定に労力や設備を必要とするという課題を有する。Further, US Pat. No. 4,488,400 discloses that ammonium vanadate is heated in a nitrogen atmosphere for a certain period of time, held, and then further heated in a specific atmosphere.
Although a method for manufacturing 6O13 has been disclosed, the manufacturing process is complicated, and since a specific atmosphere is used, there are problems in that labor and equipment are required to set the atmosphere conditions.
本発明はかかる従来技術の課題を解決すべくなされたも
ので、高放電容量、かつ電位平坦性の優れた電池の正極
材料であるV6O13の簡便な製造方法を提供すること
を目的とするものである。The present invention has been made to solve the problems of the prior art, and aims to provide a simple method for producing V6O13, which is a positive electrode material for batteries with high discharge capacity and excellent potential flatness. be.
[課題を解決するための手段]
本発明のこの目的は次に示すV8O13の製造方法によ
って達成される。[Means for Solving the Problems] This object of the present invention is achieved by the following method for producing V8O13.
すなわち、本発明の電池用V6O13の製造方法は、バ
ナジウム酸アンモニウム(NH4VO3)を不活性ガス
中で400〜450℃、10〜20時間加熱処理するこ
とを特徴とするものである。That is, the method for producing V6O13 for batteries of the present invention is characterized by heat-treating ammonium vanadate (NH4VO3) in an inert gas at 400 to 450°C for 10 to 20 hours.
以下、本発明の製造方法をさらに具体的に説明する。The manufacturing method of the present invention will be explained in more detail below.
本発明においては、v80□3を製造するための原料と
して、バナジウム酸アンモニウム(NH4vo3)を用
いる。このバナジウム酸アンモニウムは、通常、−15
0メツシュ程度に粉砕して用いられる。In the present invention, ammonium vanadate (NH4vo3) is used as a raw material for producing v80□3. This ammonium vanadate is usually -15
It is used after being crushed to about 0 mesh.
次いで、粉砕されたバナジウム酸アンモニウムは、不活
性雰囲気中で加熱される。不活性雰囲気としては、アル
ゴン、水素ガス、窒素ガス雰囲気等が例示される。The ground ammonium vanadate is then heated in an inert atmosphere. Examples of the inert atmosphere include argon, hydrogen gas, and nitrogen gas atmospheres.
加熱条件は、400〜450℃、10〜20時間が採用
される。加熱温度または加熱時間が、450℃を超える
時または20時間を超える時には、放電容量が小さい。The heating conditions are 400 to 450°C and 10 to 20 hours. When the heating temperature or heating time exceeds 450° C. or exceeds 20 hours, the discharge capacity is small.
これは生成したV8O13の部分的な分解反応が起って
いるためと考えられる。また、加熱温度または加熱時間
が、400℃未満の時または10時間未満の時にも、放
電容量が小さい。これはVaO+tの生成が充分進まず
V2O5が一部生成しているためと考えられる。This is considered to be due to a partial decomposition reaction of the generated V8O13. Further, the discharge capacity is also small when the heating temperature or heating time is less than 400° C. or less than 10 hours. This is considered to be because the generation of VaO+t did not progress sufficiently and some V2O5 was generated.
このように、本発明の製造方法においては、前記した文
献に示される従来技術と比較し、特に加熱処理において
低温で長時間加熱することを特徴とする。例えば前記し
た文献では、高温(550’C)で短時間(1時間)加
熱処理することが示されているが、このような高温では
生成したV80+iの部分的な分解反応がおこり、これ
が電池性能に悪影響を及ぼすと考えられる。As described above, the manufacturing method of the present invention is characterized in that heating is performed at a low temperature for a long time in the heat treatment, in particular, compared to the conventional technology shown in the above-mentioned literature. For example, the above-mentioned literature indicates that heat treatment is performed at a high temperature (550'C) for a short time (1 hour), but at such a high temperature, a partial decomposition reaction of the generated V80+i occurs, which deteriorates the battery performance. is thought to have a negative impact on
これに対して本発明では、上記したように加熱処理にお
いて、加熱温度と加熱時間とを特定することにより、非
水電解液電池の正極材料として、放電容量、電位平坦性
の著しく優れたV6O13が得られたものである。In contrast, in the present invention, by specifying the heating temperature and heating time in the heat treatment as described above, V6O13, which has extremely excellent discharge capacity and potential flatness, can be used as a positive electrode material for non-aqueous electrolyte batteries. This is what was obtained.
[実施例] 以下、本発明を実施例等に基づき具体的に説明する。[Example] Hereinafter, the present invention will be specifically explained based on Examples and the like.
実施例1
試薬特級のNH4vo3を50g粉砕し、粒度を=15
0メツシュとし、これをアルゴンガス気流中にて、第1
表に示すように450℃、15時間加熱処理を行いv、
、013を得た。得られたV[1O13のX線回折図を
第2図に示す。Example 1 50g of reagent special grade NH4vo3 was crushed to a particle size of 15
0 mesh, and in an argon gas flow,
Heat treatment was performed at 450°C for 15 hours as shown in the table.
, 013 was obtained. The X-ray diffraction pattern of the obtained V[1O13 is shown in FIG.
このV8O13を正極活物質として以下に示すリチウム
電池を構成した(第1図)。A lithium battery shown below was constructed using this V8O13 as a positive electrode active material (FIG. 1).
第1図のリチウム電池は、負極端子1、絶縁物2、負極
集電板3、負極材(リチウム)4、セパレータ5、正極
合剤6、正極端子7で構成されている。The lithium battery shown in FIG. 1 is composed of a negative electrode terminal 1, an insulator 2, a negative electrode current collector plate 3, a negative electrode material (lithium) 4, a separator 5, a positive electrode mixture 6, and a positive electrode terminal 7.
正極合剤6としては、V 60.190mgに対し、黒
鉛6mg、四フッ化エチレン樹脂4mgを混合し、加重
2トンで加圧成型して、直径1.O,Gmのペレットと
したものを用いた。The positive electrode mixture 6 was prepared by mixing 60.190 mg of V, 6 mg of graphite, and 4 mg of tetrafluoroethylene resin, and press-molding the mixture under a load of 2 tons to obtain a diameter of 1. Pellets of O and Gm were used.
また、電解液としては、プロピレンカーボネートと 1
.2−ジメトキシエタンが1=1の混合溶媒に過塩素酸
リチウム(LICJOs)を溶解したものを使用した。In addition, as an electrolyte, propylene carbonate and 1
.. A solution of lithium perchlorate (LICJOs) in a 1=1 mixed solvent of 2-dimethoxyethane was used.
得られたリチウム電池の電池性能試験は2.5にΩの定
抵抗にて放電を行い、終止電圧1,7Vまでの放電時間
を測定し、結果を第1表に示した。A battery performance test of the obtained lithium battery was performed by discharging at a constant resistance of 2.5Ω and measuring the discharge time until the final voltage was 1.7V.The results are shown in Table 1.
実施例2
加熱温度と加熱時間を第1表に示すように、425℃、
15時間として不活性ガスにH2を用いた他は、実施例
1と同様にしてV[1013を得た。Example 2 As shown in Table 1, the heating temperature and heating time were 425°C,
V[1013 was obtained in the same manner as in Example 1 except that H2 was used as the inert gas for 15 hours.
得られたV80+iを正極材料として実施例1と同様に
リチウム電池を構成し、その電池性能試験を行い結果を
第1表に示した。A lithium battery was constructed in the same manner as in Example 1 using the obtained V80+i as a positive electrode material, and the battery performance test was conducted and the results are shown in Table 1.
実施例3〜5および比較例1〜4
加熱温度と加熱時間を変化させた他は実施例1と同様に
してV8O13を得た。Examples 3 to 5 and Comparative Examples 1 to 4 V8O13 was obtained in the same manner as in Example 1 except that the heating temperature and heating time were changed.
得られたVa o□、を正極材料として実施例1と同様
にリチウム電池を構成し、その電池性能試験を行い結果
を第1表に示した。A lithium battery was constructed in the same manner as in Example 1 using the obtained Vao□ as a positive electrode material, and the battery performance test was conducted and the results are shown in Table 1.
また、比較例1.比較例4で得られたV6013のX線
回折図を第3図および第4図にそれぞれ示す。Also, Comparative Example 1. The X-ray diffraction diagram of V6013 obtained in Comparative Example 4 is shown in FIGS. 3 and 4, respectively.
上記した実施例1に加えて実施例3および比較例1,4
の経時における放電性能試験結果を第5図に示した。In addition to the above-mentioned Example 1, Example 3 and Comparative Examples 1 and 4
Figure 5 shows the results of the discharge performance test over time.
第 1 表
第1表に示されるように、実施例1〜5により得られた
Van、3を正極材料としたリチウム電池は、比較例1
〜4で得られたV8O13を正極材料としたリチウム電
池に比較して、放電容量(放電時間)が非常に優れてい
ることがわかる。Table 1 As shown in Table 1, the lithium batteries using Van, 3 obtained in Examples 1 to 5 as positive electrode materials were as follows: Comparative Example 1
It can be seen that the discharge capacity (discharge time) is very superior compared to the lithium battery using the V8O13 obtained in 4 as the positive electrode material.
また、第5図に示した放電曲線より、実施例1゜3によ
り得られたV6O13を正極材料としたリチウム電池は
、比較例1.4で得られたV8O13を正極材料とした
リチウム電池に比較して2V付近での電位平坦性も非常
に優れていることがわかる。Furthermore, from the discharge curve shown in Figure 5, the lithium battery using V6O13 obtained in Example 1.3 as the positive electrode material was compared to the lithium battery using V8O13 obtained in Comparative Example 1.4 as the positive electrode material. It can be seen that the potential flatness near 2V is also very excellent.
さらに、第2〜4図のX線回折図より、実施例1(第2
図)で得られたVex、3は、比較例]。Furthermore, from the X-ray diffraction diagrams in Figures 2 to 4, Example 1 (2nd
Vex, 3 obtained in Figure) is a comparative example].
(第3図)に比較してV2O5等の生成物が少なく、ま
た比較例4(第4図)に比較してV6O13のピークが
シャープで高く、結晶が十分に発達しており、またV2
o、、等の生成物も少ないことがわかる。Compared to Comparative Example 4 (Fig. 3), there are fewer products such as V2O5, and compared to Comparative Example 4 (Fig. 4), the peak of V6O13 is sharp and high, and the crystals are sufficiently developed.
It can be seen that there are also fewer products such as o, , etc.
[発明の効果]
以上説明したように、本発明の製造方法によって、簡便
に得られた十三酸化穴バナジウム(Veoo、)を正極
材料として用いることにより、リチウム電池等の非水電
解液電池の電池性能を著しく向上することができる。[Effects of the Invention] As explained above, by using 13-oxide porous vanadium (Veoo), which is easily obtained by the manufacturing method of the present invention, as a positive electrode material, it can be used for non-aqueous electrolyte batteries such as lithium batteries. Battery performance can be significantly improved.
第1図は、本発明に係わるリチウム電池の側断面図、
第2〜4図は、実施例1、比較例1、比較例4でそれぞ
れ得られた反応生成物のX線回折図、および
第5図は実施例1,3および比較例1,4の経時におけ
る放電曲線を示すグラフ。
1:負極端子、 2:絶縁物、
3:負極集電板、 4:負極材、
5;セパレータ、 6:正極合剤、
7:正極端子。
特許出願人 三井金属鉱業株式会社
代理人 弁理士 伊 東 辰 雄
代理人 弁理士 伊 東 哲 也
第1図FIG. 1 is a side cross-sectional view of a lithium battery according to the present invention, and FIGS. 2 to 4 are X-ray diffraction diagrams and FIG. 5 is a graph showing the discharge curves of Examples 1 and 3 and Comparative Examples 1 and 4 over time. 1: negative electrode terminal, 2: insulator, 3: negative electrode current collector plate, 4: negative electrode material, 5: separator, 6: positive electrode mixture, 7: positive electrode terminal. Patent applicant Mitsui Kinzoku Mining Co., Ltd. Agent Patent attorney Tatsuo Ito Agent Patent attorney Tetsuya Ito Figure 1
Claims (1)
不活性ガス雰囲気中で400〜450℃、10〜20時
間加熱することを特徴とする電池用十三酸化六バナジウ
ムの製造方法。1. A method for producing hexavanadium hexaoxide for batteries, which comprises heating ammonium vanadate (NH_4VO_3) at 400 to 450°C for 10 to 20 hours in an inert gas atmosphere.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP63152156A JPH01320228A (en) | 1988-06-22 | 1988-06-22 | Production of hexa vanadium tridecyloxide |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP63152156A JPH01320228A (en) | 1988-06-22 | 1988-06-22 | Production of hexa vanadium tridecyloxide |
Publications (1)
Publication Number | Publication Date |
---|---|
JPH01320228A true JPH01320228A (en) | 1989-12-26 |
Family
ID=15534247
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP63152156A Pending JPH01320228A (en) | 1988-06-22 | 1988-06-22 | Production of hexa vanadium tridecyloxide |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPH01320228A (en) |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5453261A (en) * | 1994-06-21 | 1995-09-26 | Saidi; M. Yazid | Method of synthesizing high surface area vanadium oxides |
US6042805A (en) * | 1994-11-29 | 2000-03-28 | Danionics A/S | Method for synthesizing an essentially V2 O5 -free vanadium oxide |
KR100433626B1 (en) * | 2001-11-28 | 2004-06-02 | 한국전자통신연구원 | Method of synthesizing amorphous vanadium oxides, lithium secondary batteries comprising the same, and method of manufacturing the same |
-
1988
- 1988-06-22 JP JP63152156A patent/JPH01320228A/en active Pending
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5453261A (en) * | 1994-06-21 | 1995-09-26 | Saidi; M. Yazid | Method of synthesizing high surface area vanadium oxides |
US6042805A (en) * | 1994-11-29 | 2000-03-28 | Danionics A/S | Method for synthesizing an essentially V2 O5 -free vanadium oxide |
KR100433626B1 (en) * | 2001-11-28 | 2004-06-02 | 한국전자통신연구원 | Method of synthesizing amorphous vanadium oxides, lithium secondary batteries comprising the same, and method of manufacturing the same |
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