CN109921155A - The chemical synthesizing method of multisection type capacitor batteries - Google Patents
The chemical synthesizing method of multisection type capacitor batteries Download PDFInfo
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- CN109921155A CN109921155A CN201910068482.7A CN201910068482A CN109921155A CN 109921155 A CN109921155 A CN 109921155A CN 201910068482 A CN201910068482 A CN 201910068482A CN 109921155 A CN109921155 A CN 109921155A
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- 239000003990 capacitor Substances 0.000 title claims abstract description 89
- 238000000034 method Methods 0.000 title claims abstract description 24
- 239000000126 substance Substances 0.000 title claims abstract description 24
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 18
- 230000005684 electric field Effects 0.000 claims description 12
- 238000012360 testing method Methods 0.000 description 20
- 230000000052 comparative effect Effects 0.000 description 12
- 238000006243 chemical reaction Methods 0.000 description 7
- 229910001416 lithium ion Inorganic materials 0.000 description 5
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 4
- 230000005611 electricity Effects 0.000 description 4
- 230000033228 biological regulation Effects 0.000 description 3
- 238000001595 flow curve Methods 0.000 description 3
- 239000000178 monomer Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
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- 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
The invention discloses a kind of chemical synthesizing methods of multisection type capacitor batteries, comprising the following steps: Step 1: under normal temperature and pressure conditions, first with I1The voltage of electric current constant-current charge to capacitor batteries is V1, then with I2The voltage of electric current constant-current charge to capacitor batteries is V2, wherein I1<I2, V1<V2；Step 2: with I3The voltage of electric current constant-current charge to capacitor batteries is V3, then power off standing, wherein I1<I3<I2, V2<V3；Step 3: with I4The voltage of electric current constant-current charge to capacitor batteries is V4, then with V4Voltage constant-voltage charge, finally power-off is stood, wherein I2<I4, V3<V4, V4For capacitor batteries limiting voltage.The chemical synthesizing method of multisection type capacitor batteries provided by the invention can significantly reduce the self discharge of capacitor batteries, reduce leakage current, extend battery life.
Description
Technical field
The present invention relates to capacitor batteries fields.It is more particularly related to a kind of chemical conversion of multisection type capacitor batteries
Method.
Background technique
Existing mature application by the double electric layers supercapacitor of electrode material of active carbon there is excellent pulse to fill
Discharge performance and fast charging and discharging performance, the power density with superelevation, and have extended cycle life, is comparatively safe, but its energy is close
Spend lower (general≤6wh/kg)；Lithium ion battery operating voltage is high, has advantage in terms of energy density, is most to have hair at present
The secondary cell of potentiality is opened up, however power-performance is poor, low-temperature characteristics is poor (generally in -20 DEG C or so discharge capacitances
Less than 50%), cycle life it is short (several hundred thousands of secondary cycle lives).With aerospace, defence and military, electric vehicle, electronics
The development in the fields such as information and instrument and meter and its needs to high-energy density and high power density energy storage device, will be super
The research that capacitor and lithium ion battery carry out " internal chiasma " is gradually risen, i.e., lithium is added in double layer capacitor positive and negative anodes
Ion battery material forms new capacitor batteries.This new capacitor batteries are similar with the preparing craft of lithium ion battery,
Need to carry out chemical conversion treatment in the production process, however existing lithium ion battery chemical synthesis technology is not able to satisfy this new electricity
Hold the high performance demands of battery, capacitor batteries self discharges is high after usually there is chemical conversion, and leakage current is big, service life short disadvantage.
Summary of the invention
It is an object of the invention to solve at least the above problems, and provide the advantages of at least will be described later.
It is a still further object of the present invention to provide a kind of chemical synthesizing methods of multisection type capacitor batteries, can significantly reduce capacitor electricity
The self discharge in pond reduces leakage current, extends battery life.
In order to realize these purposes and other advantages according to the present invention, a kind of chemical conversion of multisection type capacitor batteries is provided
Method, comprising the following steps:
Step 1: under normal temperature and pressure conditions, first with I1The voltage of electric current constant-current charge to capacitor batteries is V1, then with I2
The voltage of electric current constant-current charge to capacitor batteries is V2, wherein I1<I2, V1<V2；
Step 2: with I3The voltage of electric current constant-current charge to capacitor batteries is V3, then power off standing, wherein I1<I3<I2, V2
<V3；
Step 3: with I4The voltage of electric current constant-current charge to capacitor batteries is V4, then with V4Voltage constant-voltage charge, finally breaks
Electricity is stood, wherein I2<I4, V3<V4, V4For capacitor batteries limiting voltage.
Preferably, the capacity of the capacitor batteries is C, I1Range in 0.016~0.023CmA, V1Range exist
72.5%~77%V4。
Preferably, I2Range in 0.056~0.064C, V2Range in 80%~87.5%V4。
Preferably, I3Range in 0.034~0.042C, V3Range in 90%~95%V4。
Preferably, I4Range in 0.096~0.103C.
Preferably, when a length of 28~33min of standing is powered off in step 2.
Preferably, in step 3 constant-voltage charge when a length of 26~40min.
Preferably, when a length of 23~27h of standing is powered off in step 3.
Preferably, the capacitor batteries are before carrying out step 1, be first placed under 40~50 DEG C of atmospheric pressure environments and stand 22~
26h。
Preferably, comprising the following steps:
Step 1: under normal temperature and pressure conditions, first with the voltage of 0.02C electric current constant-current charge to capacitor batteries for 75%
V4, while being aided with ultrasound-magnetic field-electric field Combined Treatment, the frequency of ultrasonic wave is 40~45KHz, magnetic direction and battery axis
Direction is parallel, and magnetic field strength is pressedVariation, H unit are T, t1Unit is min, direction of an electric field and battery shaft
Line direction is vertical, and electric field strength presses E=0.03t2+ 0.12 variation, E unit are V/m, t2Unit is min, then permanent with 0.06C electric current
The voltage of current charge to capacitor batteries is 85%V4；
Step 2: being 92.5%V with the voltage of 0.04C electric current constant-current charge to capacitor batteries4, while being aided with ultrasound-magnetic
The frequency of field-electric field Combined Treatment, ultrasonic wave is 28~33KHz, and magnetic direction is parallel with battery axis direction, and magnetic field strength is pressedVariation, H unit are T, t3Unit is min, and direction of an electric field is vertical with battery axis direction, electric field strength
By E=0.05t4+ 0.07 variation, E unit are V/m, t4Unit is min, then powers off and stand 30min；
Step 3: being V with the voltage of 0.1C electric current constant-current charge to capacitor batteries4, then with V4Voltage constant-voltage charge 30min
Duration, finally power-off is stood for 24 hours.
The present invention is include at least the following beneficial effects: by design multisection type charging current and voltage, respectively be melted into
The SEI film reaction that journey each stage occurs matches, and electric current is intensive uniform when inside battery charges when can effectively improve chemical conversion
Property, more stable SEI film is generated, and then significantly reduce the self discharge of capacitor batteries, reduce leakage current, extend battery life.
Further advantage, target and feature of the invention will be partially reflected by the following instructions, and part will also be by this
The research and practice of invention and be understood by the person skilled in the art.
Detailed description of the invention
Fig. 1 is the leakage current value time history plot in present invention electric leakage current test；
Fig. 2 is the final leakage current histogram in present invention electric leakage current test；
Fig. 3 is the voltage value time history plot in self discharge of the present invention test.
Specific embodiment
Present invention will be described in further detail below with reference to the accompanying drawings, to enable those skilled in the art referring to specification text
Word can be implemented accordingly.
It should be noted that experimental method described in following embodiments is unless otherwise specified conventional method, institute
Reagent and material are stated, unless otherwise specified, is commercially obtained, therefore be not considered as limiting the invention.
It is below 100mAh with capacity, limiting voltage is the chemical conversion work that the present invention will be described in detail for the capacitor batteries of 4V
Skill.
<embodiment 1>
Capacitor batteries are first placed under 40 DEG C of atmospheric pressure environments and stand 22h, then followed the steps below:
Step 1: be first 2.9V with the voltage of 1.6mA electric current constant-current charge to capacitor batteries under normal temperature and pressure conditions,
It is again 3.2V with the voltage of 5.6mA electric current constant-current charge to capacitor batteries；
Step 2: being 3.6V with the voltage of 3.4mA electric current constant-current charge to capacitor batteries, then powers off and stand 28min；
Step 3: being 4V with the voltage of 9.6mA electric current constant-current charge to capacitor batteries, then with 4V voltage constant-voltage charge
26min, finally power-off stands 23h.
<embodiment 2>
Capacitor batteries are first placed under 45 DEG C of atmospheric pressure environments and are stood for 24 hours, then followed the steps below:
Step 1: be first 3V with the voltage of 2mA electric current constant-current charge to capacitor batteries under normal temperature and pressure conditions, then with
The voltage of 6mA electric current constant-current charge to capacitor batteries is 3.4V；
Step 2: being 3.7V with the voltage of 4mA electric current constant-current charge to capacitor batteries, then powers off and stand 30min；
Step 3: being 4V with the voltage of 10mA electric current constant-current charge to capacitor batteries, then with 4V voltage constant-voltage charge
30min, finally power-off is stood for 24 hours.
<embodiment 3>
Capacitor batteries are first placed under 50 DEG C of atmospheric pressure environments and stand 26h, then followed the steps below:
Step 1: be first 3.1V with the voltage of 2.3mA electric current constant-current charge to capacitor batteries under normal temperature and pressure conditions,
It is again 3.5V with the voltage of 6.4mA electric current constant-current charge to capacitor batteries；
Step 2: being 3.8V with the voltage of 4.2mA electric current constant-current charge to capacitor batteries, then powers off and stand 33min；
Step 3: being 4V with the voltage of 10.3mA electric current constant-current charge to capacitor batteries, then with 4V voltage constant-voltage charge
40min, finally power-off stands 27h.
<embodiment 4>
Capacitor batteries are first placed under 45 DEG C of atmospheric pressure environments and are stood for 24 hours, then followed the steps below:
Step 1: being first 3V with the voltage of 2mA electric current constant-current charge to capacitor batteries, simultaneously under normal temperature and pressure conditions
It is aided with ultrasound-magnetic field-electric field Combined Treatment, the frequency of ultrasonic wave is 43KHz, and magnetic direction is parallel with battery axis direction, magnetic
Field intensity is pressedVariation, H unit are T, t1Unit is min, and direction of an electric field is vertical with battery axis direction,
Electric field strength presses E=0.03t2+ 0.12 variation, E unit are V/m, t2Unit is min, then with 6mA electric current constant-current charge to capacitor
The voltage of battery is 3.4V；
Step 2: being 3.7V with the voltage of 4mA electric current constant-current charge to capacitor batteries, while being aided with ultrasound-magnetic field-electric field
The frequency of Combined Treatment, ultrasonic wave is 28~33KHz, and magnetic direction is parallel with battery axis direction, and magnetic field strength is pressedVariation, H unit are T, t3Unit is min, and direction of an electric field is vertical with battery axis direction, electric field strength
By E=0.05t4+ 0.07 variation, E unit are V/m, t4Unit is min, then powers off and stand 30min；
Step 3: being 4V with the voltage of 10mA electric current constant-current charge to capacitor batteries, then with 4V voltage constant-voltage charge
30min, finally power-off is stood for 24 hours.
<comparative example>
This comparative example is melted into capacitor batteries with conventional formation of Li-ion batteries technique, and detailed process is as follows:
First to being 3V with the voltage of 2mA constant-current charge to battery, power-off stands 30min, then extremely using 10mA constant-current charge
The voltage of battery is 4V, and finally power-off is stood for 24 hours.
<electric leakage current test>
The capacitor batteries that embodiment of learning from else's experience 2, embodiment 4, comparative example are handled respectively carry out electric leakage current test, specifically test
Journey is as follows:
Step 1: battery cell is charged to 3.67V, and in 3.67V constant current constant voltage 30min；
Step 2: under room temperature, battery cell is placed on NGI leakage current tester fixture by regulation；
Step 3: voltage sets 3.675V, and charging precision resistance chooses 100 Ω grades in leakage current tester, sampling before testing
Time 30min, sampling interval 1min in test test total duration 48h；
Step 4: current value is final leakage current value when taking 48h.
Test result is as shown in Figure 1 and Figure 2, and Fig. 1 is leakage current value time history plot, and abscissa therein is
Testing time, ordinate are leakage current value, and a is the electric leakage flow curve of comparative example, and b is from the electric leakage flow curve for embodiment 2, c
The electric leakage flow curve of embodiment 4, when Fig. 2 is test end time point, the respective final leakage of embodiment 2, embodiment 4, comparative example
Electric current is said as can be seen that the leakage current of embodiment 2, embodiment 4 is from first to last all significantly less than comparative example from Fig. 1 and Fig. 2
The chemical synthesizing method of bright multisection type capacitor batteries provided by the invention can be substantially reduced the leakage current of capacitor batteries.
<self discharge test>
The capacitor batteries that embodiment of learning from else's experience 2, embodiment 4, comparative example are handled respectively carry out self discharge test, specifically test
Journey is as follows:
Step 1: under room temperature, battery cell is placed on test fixture by regulation；
Step 2: by battery cell with 50mA electric current constant-current charge to 3.67V, and in 3.67V constant-voltage charge, cut-off current
2.5mA；
Step 3: battery cell being opened a way and is stood, and the voltage value for recording battery cell at this time after a certain period of time is placed in storage.
Test results are shown in figure 3, and Fig. 3 is the voltage time history plot of battery, and abscissa therein is quiet
It sets the time, ordinate is voltage value, and a is the voltage curve of embodiment 4, and for b from the voltage curve for embodiment 2, c is comparative example
The voltage data of part-time point in Fig. 3 is now listed in table 1 by voltage curve, beneficial effect in order to further illustrate the present invention
In.
Table 1
| Shelve the time (h) | Embodiment 2 | Embodiment 4 | Comparative example |
| 0 | 3.6680 | 3.6696 | 3.6684 |
| 100 | 3.6600 | 3.6608 | 3.6532 |
| 200 | 3.6588 | 3.6602 | 3.6514 |
| 400 | 3.6561 | 3.6594 | 3.6495 |
| 600 | 3.6555 | 3.6603 | 3.6483 |
| 800 | 3.6543 | 3.6593 | 3.6473 |
| 900 | 3.6540 | 3.6590 | 3.6464 |
Voltage decline 10mV when can be seen that (37 days) capacitor batteries 900h handled through embodiment 4 from Fig. 3 and table 1,
Voltage declines 14mV, absolute value of voltage when absolute value of voltage 3.6590V, the capacitor batteries 900h handled through embodiment 2 (37 days)
3.6540V, voltage declines 22mV, absolute value of voltage 3.6464V when (37 days) capacitor batteries 900h of example processing by contrast, implements
Example 2, embodiment 4 voltage value be significantly greater than comparative example, this illustrates the chemical synthesizing method of multisection type capacitor batteries provided by the invention
It can significantly reduce the self discharge of capacitor batteries.
<battery life test>
The capacitor batteries that embodiment of learning from else's experience 2, embodiment 4, comparative example are handled respectively carry out battery life test, specific to test
Process is as follows
Step 1: under room temperature, monomer being placed in tester grips by regulation, and monomer is charged to 50mA electric current
3.67V, and in 3.67V constant pressure 30min；
Step 2: by monomer with 50mA current discharge to 2.5V, taking this step discharge capacity is C0；
Step 3: it repeats step 1~step 2 1000 times, successively recording discharge capacity is C1、C2、……、C1000。
Step 4: after the completion of the 1000th charge and discharge, C is calculated1000/C0I.e. discharge capacitance (is put compared to first circle
Electricity).
The capacitor batteries discharge capacitance that embodiment 2, embodiment 4, comparative example are handled respectively is respectively 95%, 97%
With 81%, i.e., after multiple charge and discharge cycles, the capacitor batteries through embodiment 2, the processing of embodiment 4 there remains higher
Discharge capacity, this illustrates that the chemical synthesizing method of multisection type capacitor batteries provided by the invention can significantly extend the use longevity of capacitor batteries
Life.
Although the embodiments of the present invention have been disclosed as above, but its is not only in the description and the implementation listed
With it can be fully applied to various fields suitable for the present invention, for those skilled in the art, can be easily
Realize other modification, therefore without departing from the general concept defined in the claims and the equivalent scope, the present invention is simultaneously unlimited
In specific details and legend shown and described herein.
Claims (10)
1. the chemical synthesizing method of multisection type capacitor batteries, which comprises the following steps:
Step 1: under normal temperature and pressure conditions, first with I1The voltage of electric current constant-current charge to capacitor batteries is V1, then with I2Electric current
The voltage of constant-current charge to capacitor batteries is V2, wherein I1<I2, V1<V2；
Step 2: with I3The voltage of electric current constant-current charge to capacitor batteries is V3, then power off standing, wherein I1<I3<I2, V2<V3；
Step 3: with I4The voltage of electric current constant-current charge to capacitor batteries is V4, then with V4Voltage constant-voltage charge finally powers off quiet
It sets, wherein I2<I4, V3<V4, V4For capacitor batteries limiting voltage.
2. the chemical synthesizing method of multisection type capacitor batteries as described in claim 1, which is characterized in that the capacity of the capacitor batteries
For C, I1Range in 0.016~0.023C, V1Range in 72.5%~77.5%V4。
3. the chemical synthesizing method of multisection type capacitor batteries as claimed in claim 2, which is characterized in that I2Range 0.056~
0.064C, V2Range in 80%~87.5%V4。
4. the chemical synthesizing method of multisection type capacitor batteries as claimed in claim 2, which is characterized in that I3Range 0.034~
0.042C, V3Range in 90%~95%V4。
5. the chemical synthesizing method of multisection type capacitor batteries as claimed in claim 2, which is characterized in that I4Range 0.096~
0.103C。
6. the chemical synthesizing method of multisection type capacitor batteries as described in claim 1, which is characterized in that power-off is stood in step 2
28~33min of Shi Changwei.
7. the chemical synthesizing method of multisection type capacitor batteries as described in claim 1, which is characterized in that constant-voltage charge in step 3
26~40min of Shi Changwei.
8. the chemical synthesizing method of multisection type capacitor batteries as described in claim 1, which is characterized in that power-off is stood in step 3
23~27h of Shi Changwei.
9. the chemical synthesizing method of multisection type capacitor batteries as described in claim 1, which is characterized in that the capacitor batteries are carrying out
Before step 1, it is first placed in 22~26h of standing under 40~50 DEG C of atmospheric pressure environments.
10. the chemical synthesizing method of multisection type capacitor batteries as claimed in claim 2, which comprises the following steps:
Step 1: being first 75%V with the voltage of 0.02C electric current constant-current charge to capacitor batteries under normal temperature and pressure conditions4, simultaneously
It is aided with ultrasound-magnetic field-electric field Combined Treatment, the frequency of ultrasonic wave is 40~45KHz, and magnetic direction and battery axis direction are flat
Row, magnetic field strength are pressedVariation, H unit are T, t1Unit is min, direction of an electric field and battery axis direction
Vertically, electric field strength presses E=0.03t2+ 0.12 variation, E unit are V/m, t2Unit is min, then with 0.06C electric current constant-current charge
Voltage to capacitor batteries is 85%V4；
Step 2: being 92.5%V with the voltage of 0.04C electric current constant-current charge to capacitor batteries4, while being aided with ultrasound-magnetic field-electricity
The frequency of field Combined Treatment, ultrasonic wave is 28~33KHz, and magnetic direction is parallel with battery axis direction, and magnetic field strength is pressedVariation, H unit are T, t3Unit is min, and direction of an electric field is vertical with battery axis direction, electric field strength
By E=0.05t4+ 0.07 variation, E unit are V/m, t4Unit is min, then powers off and stand 30min；
Step 3: being V with the voltage of 0.1C electric current constant-current charge to capacitor batteries4, then with V4Voltage constant-voltage charge 30min duration,
Finally power-off is stood for 24 hours.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111477967A (en) * | 2020-04-10 | 2020-07-31 | 浙江工业大学 | Method for preparing SEI film through magnetization |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2358622Y (en) * | 1999-02-04 | 2000-01-12 | 北京有色金属研究总院 | Constant current constant-voltage charging device for secondary battery |
| CN102324570A (en) * | 2011-09-07 | 2012-01-18 | 惠州Tcl金能电池有限公司 | Lithium ion battery, its formation method and preparation method |
| CN103390770A (en) * | 2013-07-25 | 2013-11-13 | 天津力神电池股份有限公司 | Lithium ion battery formation sectional charging method |
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2019
- 2019-01-24 CN CN201910068482.7A patent/CN109921155B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2358622Y (en) * | 1999-02-04 | 2000-01-12 | 北京有色金属研究总院 | Constant current constant-voltage charging device for secondary battery |
| CN102324570A (en) * | 2011-09-07 | 2012-01-18 | 惠州Tcl金能电池有限公司 | Lithium ion battery, its formation method and preparation method |
| CN103390770A (en) * | 2013-07-25 | 2013-11-13 | 天津力神电池股份有限公司 | Lithium ion battery formation sectional charging method |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111477967A (en) * | 2020-04-10 | 2020-07-31 | 浙江工业大学 | Method for preparing SEI film through magnetization |
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Effective date of registration: 20240326 Address after: 430000 No. 37, Tianyuan street, Dongxihu District, Wuhan City, Hubei Province Patentee after: Wuhan Haocheng lithium Technology Co.,Ltd. Country or region after: China Address before: No.18 Xiaguang Road, Mashan street, Binhu District, Wuxi City, Jiangsu Province Patentee before: WUXI CAPATTERY TECHNOLOGY Co.,Ltd. Country or region before: China |