JPS6119075A - Charge-discharge method of solid electrolyte secondary battery - Google Patents
Charge-discharge method of solid electrolyte secondary batteryInfo
- Publication number
- JPS6119075A JPS6119075A JP59140881A JP14088184A JPS6119075A JP S6119075 A JPS6119075 A JP S6119075A JP 59140881 A JP59140881 A JP 59140881A JP 14088184 A JP14088184 A JP 14088184A JP S6119075 A JPS6119075 A JP S6119075A
- Authority
- JP
- Japan
- Prior art keywords
- charge
- discharge
- solid electrolyte
- battery
- charging
- 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.)
- Granted
Links
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0561—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of inorganic materials only
- H01M10/0562—Solid materials
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/44—Methods for charging or discharging
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Secondary Cells (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
Description
【発明の詳細な説明】
産業上の利用分野
本発明は、固体電解質二次電池の充・放電方式従来例の
構成とその問題点
一般に二次電池は、用いられる正極活物質、負極活物質
、電解質の可逆性、過電圧１分解電圧等の電気化学的性
質により決定されるその電池系特有の、その電圧値ある
いは電気量を越えるとくり返し充・放電特性が極端に低
下する充・放電限界電圧あるいは電気量を有している。DETAILED DESCRIPTION OF THE INVENTION Field of Industrial Application The present invention relates to the structure of a conventional charging/discharging system for solid electrolyte secondary batteries and its problems. The charge/discharge limit voltage, which is determined by the electrochemical properties such as electrolyte reversibility, overvoltage, and decomposition voltage, and which is unique to the battery system and whose repeated charge/discharge characteristics deteriorate extremely when the voltage value or quantity of electricity is exceeded. It has electricity.
すなわち、従来の二次電池の代表例であるニッケルーカ
ドミウム電池とか鉛蓄電池とかも、長年にわたる検討が
加えられ、それぞれの電池系に固有の充・放電限界電圧
あるいは電気量を見定め現在の充・放電方式をとるに至
っている。In other words, nickel-cadmium batteries and lead-acid batteries, which are typical examples of conventional secondary batteries, have been studied for many years, and the current charging and discharging limit voltage or amount of electricity unique to each battery system has been determined. A discharge method has been adopted.
新しい正極活物質、負極活物質、電解質により構成され
る二次電池を実用に供するためには、この電池系固有の
充・放電限界電圧あるいは電気量を３ベージ
見定め、この電池系固有の充・放電方式を与えることは
必須の要件となる。In order to put into practical use a secondary battery composed of a new positive electrode active material, negative electrode active material, and electrolyte, the charging/discharging limit voltage or the amount of electricity unique to this battery system must be determined on three basis. Providing a discharge method is an essential requirement.
一方、在来の液体電解質を用いるニッケル・カドミウム
電池等とは異なり、固体状の電解質を用いる固体電解質
二次電池は、原理的に液もれがなく小形・うす形化がき
わめて簡便にできることから、近年発展が著しい省電力
・省エネルギーが達成されるマイクロエレクトロニクス
分野の小結電源として注目されるに至っている。この固
体電解質二次電池の中でも、Ｃｕ！ＴｉＳ２とかＣｕ
ＴＩＣｒｙＳ２＋１．６７ 等の眉間化合物を正極活物
質とし、Ｃｕ■イオン導電性固体電解質を用いる二次電
池は、正極活物質の可逆性が優れ、固体電解質のイオン
伝導度は有機電解液電解質に匹適するくらい高くかつ化
学的に安定であることから優れた電池特性が期待できる
固体電解質二次電池として注目されるに至っている。On the other hand, unlike conventional nickel-cadmium batteries that use liquid electrolytes, solid electrolyte secondary batteries that use solid electrolytes do not leak in principle and can be made smaller and thinner very easily. It has been attracting attention as a small power source for the microelectronics field, which has achieved remarkable power and energy savings in recent years. Among these solid electrolyte secondary batteries, Cu! TiS2 or Cu
A secondary battery that uses a eyebrow compound such as TICryS2+1.67 as a positive electrode active material and a Cu ion conductive solid electrolyte has excellent reversibility of the positive electrode active material, and the ionic conductivity of the solid electrolyte is comparable to that of an organic electrolyte. It is attracting attention as a solid electrolyte secondary battery that can be expected to have excellent battery characteristics because of its high chemical stability and chemical stability.
該固体電解質二次電池の電池反応は
と表されるが、負極の反応は、銅（Ｃｕ ）の溶解析出
反応であり、その可逆性については特別な制限はない。The battery reaction of the solid electrolyte secondary battery is expressed as follows; however, the reaction at the negative electrode is a dissolution precipitation reaction of copper (Cu), and there is no particular restriction on its reversibility.
正極の反応については、Ｃｕ■がＴｉＳ２あるいはＴｉ
ＣｒｙＳ２＋１．６Ｖ のＳとＳの層間を出入りする反
応であるが、その可逆性については全く知られておらず
、したがって該電池の良好なくり返し特性を与える充・
放電限′界を定め難く、該固体電解質二次電池を実用に
供するだめの障害となっている。Regarding the reaction at the positive electrode, Cu■ is TiS2 or Ti
CryS2+1.6V is a reaction that moves between S and S layers, but its reversibility is completely unknown.
It is difficult to determine the discharge limit, which is an obstacle to putting the solid electrolyte secondary battery into practical use.
発明の目的
本発明は、固体電解質二次電池について、良好なくり返
し充・放電特性を与える充・放電方式を提供することを
目的とする。OBJECTS OF THE INVENTION An object of the present invention is to provide a charging/discharging method that provides good repeated charging/discharging characteristics for a solid electrolyte secondary battery.
発明の構成
５ページ
本発明を適用する固体電解質二次電池は、Ｃｕを主体と
゛する負極、Ｃｕ ｘＴ Ｉ Ｓ２ ＋ Ｃｕ ｘＴ
＊ Ｃｒ ｙＳ２ｃ 、５ｙ（Ｏ＜！＜０．２．０．０
１ ＜ｙ＜０．２）の一群より選ばれる化合物を主体と
する正極、ＲｂＣｕ４Ｉ １．５ＣＩ３．５゜ＲｂＣｕ
４１１．２．Ｃ１３，７６等のＣｕ■イオン導電性固体
電解質により構成される。そして、該電池の使用に際し
ては、充電限界電池電圧として、０．６５＋ｔ、、ｎｏ
（ボルト）以下、放電限界電池電圧として０ 、３３−
１ ｄ−Ｒｃ１（ボルト）以上の条件を満足するように
充・放電をくり返し行うようにする。Structure of the Invention Page 5 A solid electrolyte secondary battery to which the present invention is applied has a negative electrode mainly composed of Cu, Cu xT I S2 + Cu xT
* Cr yS2c , 5y (O<!<0.2.0.0
1<y<0.2), a positive electrode mainly composed of a compound selected from the group of RbCu4I 1.5CI3.5°RbCu
411.2. It is composed of a Cu ion conductive solid electrolyte such as C13,76. When using the battery, the charging limit battery voltage is 0.65+t, no.
(Volt) Below, the discharge limit battery voltage is 0,33-
Charge and discharge are repeated so that the condition of 1 d-Rc1 (volt) or more is satisfied.
ここで、ｉ、、ｉｄは、それぞれ充電９．放電電流値−
ム。電池の充電中あるいは放電中に、約１００ミリ秒間
、充電電流あるいは放電電流を１０分の９にしたときの
電池の電圧■。。、Ｖｄｃと、電流を減じる直前の電池
電圧Ｖ。ｏ、ＶｄｃからＲｏ＝１０・（ｖｃｃ −ｖｃ
ｏ ）／ ｔ。Here, i, , id are respectively charging 9. Discharge current value -
Mu. Battery voltage ■ when the charging or discharging current is reduced to 9/10 for approximately 100 milliseconds while the battery is being charged or discharged. . , Vdc, and the battery voltage V immediately before reducing the current. o, Vdc to Ro=10・(vcc −vc
o)/t.
Ｒｄ＝１０・（Ｖｄｏ−Ｖｄｃ）／ｉｄで求められる値
である。This is a value determined by Rd=10.(Vdo-Vdc)/id.
６ペーノ
ここで言う、充電限界電池電圧とは、充電はこの電圧値
以下で行うという意味での限界電圧であり、放電限界電
池電圧とは、放電は、この電圧以上で行うという意味で
の限界電圧である。The charging limit battery voltage mentioned here is the limit voltage in the sense that charging is performed below this voltage value, and the discharge limit battery voltage is the limit in the sense that discharging is performed above this voltage value. It is voltage.
実施例の説明
下記に示した構成の固体電解質二次電池を構成し、本発
明を適用する。Description of Examples A solid electrolyte secondary battery having the configuration shown below is constructed and the present invention is applied thereto.
〔実施例１〕
電解質： ＲｂＣｕ４Ｉ １．５Ｃｔ３．６を０．０５
ｇｒ負極合剤：Ｃｕ粉８０重量％とＣｕ２Ｓ２０重量％
の混合物４．７５重量部と前記電解
質１．２５重量部の混合物を０．２ｇ ｒ正極合剤：Ｃ
ｕｏ、１ＴｉＳ２２重量部と前記電解質３重量部の混合
物を０．０６ｇｒ
上記の材料を２トン／−の圧力で三層に加圧成型して直
径７ ｗ＋、厚さ約１ｍ＋の電池を組み立てた。[Example 1] Electrolyte: RbCu4I 1.5Ct3.6 to 0.05
gr negative electrode mixture: Cu powder 80% by weight and Cu2S 20% by weight
0.2 g of a mixture of 4.75 parts by weight of the mixture and 1.25 parts by weight of the electrolyte.
0.06 gr of a mixture of 22 parts by weight of 1TiS and 3 parts by weight of the electrolyte.The above materials were pressure molded into three layers at a pressure of 2 tons/- to assemble a battery with a diameter of 7 W+ and a thickness of about 1 m+.
これらの電池を室温で通常は１００μＡで、６０秒間に
１回１００ミリ秒間９ｏｐＡとなる定電流パルスで、次
表に示す９種類の充・放電サイクル試験ａ−ｈを行なっ
た。同表に、第１サイクル目７ヘーノ
充電中、放電中共に変化はほとんどなく、試験した全サ
イクルに渡り常温でほぼ同じＲ３’：： Ｒｄ：２２０
Ω第１図は、ａ−ｈの各サイクル試験における、サイク
ル数と放電末電圧（実線）、充電末電圧（破線）との関
係を示しており、本発明の充・放電方式に従い、充電限
界電圧が、０ 、６０＋１０””・２２０＝０．６２２
ボルト以下でかつ放電限界電圧が、０．３３−１０””
’ ＠２２０＝０．３０８ボルト以上である充・放電サ
イクル試験、ａ、ｂ、ｃ、ｄ、ｅでは実用に耐える良好
なくり返し充・放電特性を与えることがわかる。These batteries were subjected to nine types of charge/discharge cycle tests a-h shown in the following table at room temperature with a constant current pulse of 9 opA for 100 milliseconds once every 60 seconds, typically at 100 μA. In the same table, there is almost no change during the first cycle 7 during charging and discharging, and R3':: Rd: 220 is almost the same at room temperature over all the cycles tested.
Ω Figure 1 shows the relationship between the number of cycles, the end-of-discharge voltage (solid line), and the end-of-charge voltage (broken line) in each cycle test of a to h, and according to the charge/discharge method of the present invention, the charge limit The voltage is 0, 60+10''・220=0.622
volt or less and the discharge limit voltage is 0.33-10""
It can be seen that the charge/discharge cycle tests a, b, c, d, and e, where @220 = 0.308 volts or more, give good repeated charge/discharge characteristics that can withstand practical use.
また、ｄ、ｅにおいてサイクル試験の末期になって充電
電圧あるいは放電電圧が本発明により示される限界電圧
を越えると、急激にくり返し充・放電特性が劣化するこ
とがわかる。Furthermore, it can be seen that when the charging voltage or the discharging voltage exceeds the limit voltage indicated by the present invention at the end of the cycle test in d and e, the charging/discharging characteristics repeatedly deteriorate rapidly.
〔実施例２〕
電解質：Ｒｂ Ｃｕ ４Ｉ １．ｓ ＣＺａ 、ｓを０
．０５ｇｒ負極合剤：Ｃｕ粉８０重量％とＣｕ２Ｓ ２
０重量％の混合物４．７６重量部と前記電解
質１．２５重量部の混合物０，２ｑｒ
正極合剤：ＣｕＯ００６ＴｉＣｒｏ、０２６Ｓ２．０３
７６２重量部と前記電解質３重量部の混合
物を０．０６ｇｒ
上記の材料を２トン／ ｃｄの圧力で三層に加圧成型９
ページ
し２直径７咽、厚さ約１閣の電池を組み立てた。[Example 2] Electrolyte: Rb Cu 4I 1. s CZa, s is 0
．． 05gr negative electrode mixture: 80% by weight of Cu powder and Cu2S2
A mixture of 4.76 parts by weight of 0% by weight mixture and 1.25 parts by weight of the electrolyte 0.2qr Positive electrode mixture: CuO006TiCro, 026S2.03
A mixture of 762 parts by weight and 3 parts by weight of the electrolyte was press-molded into three layers with 0.06 gr of the above materials at a pressure of 2 tons/cd9.
I made a page and assembled a battery that was 2 inches in diameter and about 1 inch thick.
これらの電池を室温で、通常は１００μＡで６０秒間に
１回１ｏｏミリ秒間９０μＡとなる定電流パルスで、次
表に示す９種類の充・放電サイクル試験ａ′〜ｈ′を行
った。同表に、第１サイクル目充電中、放電中共に変化
はほとんどなく、試験した全サイクルに渡Ｖ、常温でほ
ぼ同じＲ８二Ｒｄ二２２０Ωである。These batteries were subjected to nine types of charge/discharge cycle tests a' to h' shown in the following table at room temperature, using a constant current pulse of 90 μA for 10 milliseconds once every 60 seconds at 100 μA. In the same table, there is almost no change during charging and discharging in the first cycle, and V and Rd2220Ω are almost the same at room temperature over all the cycles tested.
１０−・
第２図は、ａ′〜ｈ′各サイクル試験における、サイク
ル数と放電末電圧（実線）、充電末電圧（破線）との関
係を示しており、本発明の充・放電方式に従い、充電限
界電圧が、０．６０ ＋ １０”−’・２２０＝０．６
２２ボルト以下でかつ放電限界電圧が、０．３３−１０
””−２２０＝０．３０８ポル）以上である充・放電サ
イクル試験ａ、ｂ、Ｃ，ｄ、 ｅでは実用に耐える良好
なくり返し充・放電特性を与えることがわかる。10-. Figure 2 shows the relationship between the number of cycles, the end-of-discharge voltage (solid line), and the end-of-charge voltage (dashed line) in each cycle test from a' to h'. , the charging limit voltage is 0.60 + 10"-'・220=0.6
22 volts or less and the discharge limit voltage is 0.33-10
It can be seen that in the charge/discharge cycle tests a, b, C, d, and e, which are equal to or higher than ""-220=0.308 pol), good repeated charge/discharge characteristics that can withstand practical use are provided.
また、ｄ、ｅにおいて、サイクル試験の末期になって充
電電圧あるいは放電電圧が本発明により示される限界電
圧を越えると、急激にくり返し充・放電特性が劣化する
ことがわかる。Furthermore, in d and e, it can be seen that when the charging voltage or the discharging voltage exceeds the limit voltage indicated by the present invention at the end of the cycle test, the charging/discharging characteristics repeatedly deteriorate rapidly.
発明の効果
本発明によれば、固体電解質二次電池に良好なくり返し
充・放電特性を発揮させることができる。Effects of the Invention According to the present invention, a solid electrolyte secondary battery can exhibit good repeated charge/discharge characteristics.
第１図は本発明の一実施例の充・放電方式の効果を示す
充・放電サイクル数と、充電時の電池電圧特性図、第２
図は同放電時の電池電圧との関係１１ベー〕ｆ
図である。
代理人の氏名 弁理士 中 尾 敏 男 ほか１名−―
凭嚇−号
城
手続補正書
昭和６９年１１月ユ２日Figure 1 shows the number of charging/discharging cycles and battery voltage characteristics during charging, showing the effects of the charging/discharging method of an embodiment of the present invention.
The figure shows the relationship with the battery voltage at the time of discharge. Name of agent: Patent attorney Toshio Nakao and one other person --
凭凭 - Gojo Procedures Amendment Book November 2, 1986
Claims (1)
＿ｘＴｉＣｒ＿ｙＳ＿２＿＋＿１＿．＿５＿ｙ（０＜ｘ
＜０．２、０．０１＜ｙ＜０．２）の一群より選ばれる
化合物を主体とする正極と、Ｃｕ＾■イオン導電性固体
電解質で構成される固体電解質二次電池の充放電を、充
電限界電池電圧が０．６０＋ｉ＿ｃＲ＿ｃ以下、放電限
界電池電圧が０．３３−ｉ＿ｄＲ＿ｄ以上とすることを
特徴とする固体電解質二次電池の充・放電方式。 ただし、ｉ＿ｃ、ｉ＿ｄはそれぞれ充電放電電流値、Ｒ
＿ｃ、Ｒ＿ｄはそれぞれ充電、放電時の電池の直流内部
抵抗値であり、 Ｒ＿ｃ＝１０・（Ｖ＿ｃ＿ｃ−Ｖ＿ｃ＿ｏ）／ｉ＿ｃＲ
＿ｄ＝１０・（Ｖ＿ｄ＿ｏ−Ｖ＿ｄ＿ｃ）／ｉ＿ｄで与
えられる値、Ｖ＿ｃ＿ｏ、Ｖ＿ｄ＿ｏは、充電中、放電
中に、約１００ミリ秒間、充電電流値あるいは放電電流
値を１０分の９に減じた際の電池電圧であり、Ｖ＿ｃ＿
ｃ、Ｖ＿ｄ＿ｃは減じる前の電池電圧である。[Claims] A negative electrode mainly made of metallic copper, Cu_xTiS_2, Cu
_xTiCr_yS_2_+_1_. _5_y(0<x
<0.2, 0.01<y<0.2) A positive electrode mainly composed of a compound selected from the group of A charging/discharging method for a solid electrolyte secondary battery, characterized in that a charge limit battery voltage is 0.60+i_cR_c or less and a discharge limit battery voltage is 0.33-i_dR_d or more. However, i_c and i_d are charging and discharging current values, R
_c and R_d are the DC internal resistance values of the battery during charging and discharging, respectively, R_c=10・(V_c_c−V_c_o)/i_cR
The value given by _d=10・(V_d_o−V_d_c)/i_d, V_c_o, V_d_o, is the value when the charging current value or discharging current value is reduced to 9/10 for about 100 milliseconds during charging and discharging. is the battery voltage, V_c_
c and V_d_c are the battery voltages before being reduced.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59140881A JPS6119075A (en) | 1984-07-06 | 1984-07-06 | Charge-discharge method of solid electrolyte secondary battery |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59140881A JPS6119075A (en) | 1984-07-06 | 1984-07-06 | Charge-discharge method of solid electrolyte secondary battery |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6119075A true JPS6119075A (en) | 1986-01-27 |
| JPH0534788B2 JPH0534788B2 (en) | 1993-05-24 |
Family
ID=15278935
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP59140881A Granted JPS6119075A (en) | 1984-07-06 | 1984-07-06 | Charge-discharge method of solid electrolyte secondary battery |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6119075A (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57107568A (en) * | 1980-12-25 | 1982-07-05 | Matsushita Electric Ind Co Ltd | Reversible copper electrode |
| JPS599875A (en) * | 1982-07-08 | 1984-01-19 | Japan Storage Battery Co Ltd | Lead storage battery |
-
1984
- 1984-07-06 JP JP59140881A patent/JPS6119075A/en active Granted
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57107568A (en) * | 1980-12-25 | 1982-07-05 | Matsushita Electric Ind Co Ltd | Reversible copper electrode |
| JPS599875A (en) * | 1982-07-08 | 1984-01-19 | Japan Storage Battery Co Ltd | Lead storage battery |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0534788B2 (en) | 1993-05-24 |
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