CN108106880A - The sampling and testing method and sampler of a kind of lithium battery moisture measurement - Google Patents
The sampling and testing method and sampler of a kind of lithium battery moisture measurement Download PDFInfo
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- CN108106880A CN108106880A CN201711332069.4A CN201711332069A CN108106880A CN 108106880 A CN108106880 A CN 108106880A CN 201711332069 A CN201711332069 A CN 201711332069A CN 108106880 A CN108106880 A CN 108106880A
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- lithium battery
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- 238000012360 testing method Methods 0.000 title claims abstract description 83
- 238000005070 sampling Methods 0.000 title claims abstract description 55
- 238000005259 measurement Methods 0.000 title claims abstract description 31
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 28
- 238000012546 transfer Methods 0.000 claims abstract description 24
- 230000001681 protective effect Effects 0.000 claims abstract description 8
- 239000000523 sample Substances 0.000 claims description 20
- 239000007789 gas Substances 0.000 claims description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000013100 final test Methods 0.000 claims description 4
- 239000011888 foil Substances 0.000 claims description 4
- 230000000873 masking effect Effects 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 230000001351 cycling effect Effects 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 15
- 230000001788 irregular Effects 0.000 abstract description 3
- 238000002360 preparation method Methods 0.000 abstract description 3
- 239000003792 electrolyte Substances 0.000 description 6
- 238000010586 diagram Methods 0.000 description 4
- 238000005520 cutting process Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 206010028347 Muscle twitching Diseases 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000036461 convulsion Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 150000003839 salts Chemical group 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/04—Devices for withdrawing samples in the solid state, e.g. by cutting
- G01N1/08—Devices for withdrawing samples in the solid state, e.g. by cutting involving an extracting tool, e.g. core bit
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
-
- G01N33/0077—
Abstract
The present invention relates to lithium battery moisture measurement technical fields, particularly a kind of lithium battery moisture measurement sampler, and including glove box, the glove box includes test chamber and transfer chamber, and moveable transfer chamber Inner hatch doors are equipped between the test chamber and transfer chamber；The edge of a knife and print rewinding box under sampling mould upper punch, sampling mould are disposed with from top to bottom in the middle part of the test chamber；Divide at left and right sides of the test chamber upper end and be connected with dry wind air inlet and dry wind air outlet；Test chamber lower end one side is connected with protective gas input port.After the above method and device, the present invention can rationally quickly finish entire pole piece moisture measurement using the preparation method of standardization:Include the overall process that pole piece to be measured prepares, pole piece samples, pole piece is tested.And it is no longer put into during sampling using the pole piece of the irregular area of clip polylith of conventional scissors in drift bottle；It avoids and was originally sampled in nonstandard overall situation.
Description
Technical field
The present invention relates to lithium battery moisture measurement technical fields, particularly a kind of sampling and testing side of lithium battery moisture measurement
Method and sampler.
Background technology
Moisture is one of major factor for influencing lithium battery performance and security：Moisture is out of control, not only causes electrolyte lithium
The decomposition of salt, and ill effect is generated to film forming and stability.Water is unfavorable to the formation of lithium ion battery SEI films, and
It has a certain impact to battery performance.With the increase of moisture, the discharge capacity for the first time of battery reduces, and internal resistance increases, cyclicity
It can decline, battery bulging etc..Moisture control is one of most important control condition in Production Process of Lithium Battery.
During the moisture measurement of battery, sample rate and sampling amount have test result large effect, routinely take
Sample amount is generally smaller than 3g, traditional sampling method be using the pole piece of the scissors irregular area of clip polylith by rule of thumb, it is such
Sampling method sample rate is slow, and sampling amount is unstable, can influence the result of battery moisture content test.The present invention is battery moisture measurement
Provide a kind of sampling specification, the sampling preparation method that sampling amount is stable, sampling region is relatively uniform.
104568510 A of Chinese invention patent application CN disclose a kind of sampling side for testing lithium battery electrolytes moisture
Method and sampler, the sampling method include：Crossover sub is set on electrolyte bucket；By the manual switch valve of crossover sub
Door is opened；The syringe needle of syringe is extend into the conduit of crossover sub, twitches syringe sucking electrolyte；Close crossover sub
Manual switch valve.The sampler includes electrolyte bucket, crossover sub, and the electrolyte bucket can with the crossover sub
Tear formula connection open, the crossover sub is equipped with manual switch valve, conduit.
The content of the invention
The technical problem to be solved in the invention is to provide pole piece moisture in a kind of accurate evaluation battery.
In order to solve the above technical problems, a kind of sampler of lithium battery moisture measurement of the present invention, including glove box, institute
Stating glove box includes test chamber and transfer chamber, and moveable transfer chamber Inner hatch doors are equipped between the test chamber and transfer chamber；Institute
It states and is disposed with the edge of a knife and print rewinding box under sampling mould upper punch, sampling mould from top to bottom in the middle part of test chamber；It is described
Divide at left and right sides of test chamber upper end and be connected with dry wind air inlet and dry wind air outlet；Test chamber lower end one side is connected with
Protective gas input port.
Further, the test chamber side wall is provided with hanging temperature and humidity measuring instrument, the transfer chamber test hatch door top
It is provided with dew point control probe.
Further, battery core is provided in the test chamber and disassembles box, the test chamber middle and upper part is provided with rotating hanging article
Rack.
Further, electronic balance is provided in the test chamber, drift bottle is placed in the electronic balance.
Further, the print rewinding box includes print feeding box main body, if being provided on the print feeding box main body
Dry sample piece feeding box rewinding mouth, the print feeding box rewinding mouth is tilted to be provided with print feeding box cant timber.
Further, the print feeding box cant timber angle of inclination is 60 °.
Present invention additionally comprises a kind of sampling and testing methods of lithium battery moisture measurement, which is characterized in that comprise the following steps,
(1) battery is disassembled；Battery enters from the transfer chamber of glove box, and enters in glove box test chamber, by transition
It is locked after hatch door is rotated down in cabin, dry battery is disassembled in battery core disassembles box to obtain battery core pole piece；
(2) sample；It is put into battery core pole piece is smooth in the detent mechanism of sampling mould, exists by sampling mould upper punch
It moves up and down under sampling mould in the edge of a knife, is smoothly punched out the disk of φ 12mm, the disk of the φ 12mm to fall down smoothly enters
Into print rewinding box；
(3) print is weighed；The print sampled is put into clean drift bottle, and is weighed with electronic balance；
(4) print encapsulates；, it is necessary to the lid of drift bottle reliably be sealed with masking foil, from mistake after the completion of weighing
It crosses in cabin and passes out, carry out the test of next step moisture tester；
(5) print moisture measurement；The drift bottle sealed is put on the test turntable of moisture tester, according to this rotational latency
The test of moisture tester stylus；The heating furnace 16 that pipeline connection is also needed to during test carries out assisted evaporative moisture, warp
It crosses in the test period of 10-15min, completes the test of single drift bottle, final test result is shown in moisture tester master
On the screen of instrument 15.
Further, the dew point environment in probe monitors glove box is controlled by dew point in the step (1), by dry
Dry wind air inlet and dry wind air outlet lead to dry wind, ensure the cycling of dry wind.
Further, nitrogen or argon gas are inputted by protective gas input port in the step (1).
Further, the battery core pole piece chosen in the step (2) is located at the middle part of battery core.
After the above method and device, the present invention can be quickly finished rationally whole using the preparation method of standardization
A pole piece moisture measurement:Include the overall process that pole piece to be measured prepares, pole piece samples, pole piece is tested.And in the process of sampling
In be no longer put into using the pole piece of the irregular area of clip polylith of conventional scissors in drift bottle.It avoids originally nonstandard
It is sampled in overall situation.Although in the range of overall situation dew point T >=-50 DEG C, the space of test room is bigger, and pole piece takes
It cannot be guaranteed at sample position in ambient dew point T >=-50 DEG C temperature range at this time, casual can so cause the moisture of pole piece
Pollution.The later stage deviation of test also can be bigger.Special sampling mould in glove box is operated by the way of pneumatic control
Flexibly and easily, to avoid heavy and inefficiency manual control.And the position sampled is completed by experimental demonstration.
Rewinding box is provided with below sampling, the material that sampling mould is removed is avoided to receive pollution and fold.Sample circle in rewinding box
Piece can facilitate taking-up using tweezers, in the range of the 2-2.5g for meeting sampling craft requirement, the final completion water that can standardize
Divide the whole process of test.
Description of the drawings
The present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments.
Fig. 1 is a kind of structure diagram of the sampler of lithium battery moisture measurement of the present invention.
Fig. 2 is a kind of moisture tester schematic diagram of the sampling method of lithium battery moisture measurement of the present invention.
Fig. 3 is the sample position schematic diagram of pole piece in a kind of sampling method of lithium battery moisture measurement of the present invention.
Fig. 4 is the structure diagram of pole piece rewinding box in a kind of sampling method of lithium battery moisture measurement of the present invention.
In figure：1 is hanging temperature and humidity measuring instrument, and 2 disassemble box for battery core, and 3 be protective gas input port, 4 for dry wind into
Air port, 5 be rotating hanging article holder, and 6 be dry wind return air inlet, and 7 be dew point control probe, and 8 be hatch door in transfer chamber, and 9 be electricity
Sub- balance, 10 be drift bottle, and 11 be sampling mould upper punch, and 12 be battery core pole piece, and 13 be the edge of a knife under sampling mould, and 14 be print
Rewinding box, 15 be the main instrument of moisture tester, and 16 be heating furnace, and 17 be test turntable, and 18 be moisture tester stylus, and 19 be to apply
Jiao Qu, 20 be a cutting wires, and 14-1 is print feeding box main body, and 14-2 is print sampling box rewinding mouth, and 14-3 takes for print
Sample box cant timber
Specific embodiment
As shown in Figure 1, the present invention includes a kind of sampler of lithium battery moisture measurement, including glove box, the gloves
Case includes test chamber and transfer chamber, and moveable transfer chamber Inner hatch doors 8 are equipped between the test chamber and transfer chamber；The test
The edge of a knife 13 and print rewinding box 14 under sampling mould upper punch 11, sampling mould are disposed with from top to bottom in the middle part of cabin；It is described
Divide at left and right sides of test chamber upper end and be connected with dry wind air inlet 4 and dry wind air outlet 6；Test chamber lower end one side connects
There is protective gas input port 3.
Further, the test chamber side wall is provided with hanging temperature and humidity measuring instrument 1, the transfer chamber test hatch door top
It is provided with dew point control probe 7.Battery core is provided in the test chamber and disassembles box 2, the test chamber middle and upper part is provided with rotating hanging
Article holder 5.Electronic balance 9 is provided in the test chamber, drift bottle 10 is placed in the electronic balance 9.
Further, as shown in figure 4, the print rewinding box 14 includes print feeding box main body 14-1, the print takes
Several print feeding box rewinding mouth 14-2, the tilted settings of the print feeding box rewinding mouth 14-2 are provided on magazine body 14-1
There is print feeding box cant timber 14-3, the print feeding box cant timber 14-3 preferred angles are 60 °.
Present invention additionally comprises a kind of sampling and testing methods of lithium battery moisture measurement, which is characterized in that comprise the following steps,
(1) battery is disassembled；Battery enters from the transfer chamber of glove box, and enters in glove box test chamber, by transition
It is locked after hatch door is rotated down in cabin, dry battery is disassembled in battery core disassembles box to obtain battery core pole piece；
(2) sample；It is put into battery core pole piece is smooth in the detent mechanism of sampling mould, exists by sampling mould upper punch
It moves up and down under sampling mould in the edge of a knife, is smoothly punched out the disk of φ 12mm, the disk of the φ 12mm to fall down smoothly enters
Into print rewinding box；
(3) print is weighed；The print sampled is put into clean drift bottle, and is weighed with electronic balance；
(4) print encapsulates；, it is necessary to the lid of drift bottle reliably be sealed with masking foil, from mistake after the completion of weighing
It crosses in cabin and passes out, carry out the test of next step moisture tester；
(5) print moisture measurement；The drift bottle sealed is put on the test turntable of moisture tester, according to this rotational latency
The test of moisture tester stylus；The heating furnace 16 that pipeline connection is also needed to during test carries out assisted evaporative moisture, warp
It crosses in the test period of 10-15min, completes the test of single drift bottle, final test result is shown in moisture tester master
On the screen of instrument 15.
Specific sampling and test process are as follows：
(1) battery is disassembled；As shown in Figure 1, testing staff either operates employee from offline dried of large-scale drying oven
Battery.Battery enters from the transfer chamber of glove box, and enters in glove box test chamber, it is necessary to by hatch door in transfer chamber 8
It is locked after being rotated down.Dry battery is disassembled using nipper plier, this operation needs what is specially prepared in glove box
Battery core is disassembled to be operated in box 2.In order to ensure dew point environmental Kuznets Curves therein in entire glove box, upper left is provided with drying
Wind air inlet 4, upper right are then provided with dry wind return air inlet 6, to ensure the cycling of dry wind.Dew point is disposed in glove box
Control probe 7, monitors the dew point environment in glove box in real time.It also provided hanging humiture instrument 1 in glove box, monitor hand in real time
Temperature and humidity in casing.These monitoring are provided to the real-time of environmental Kuznets Curves during print sampling, and to testing staff
There is the time of reaction.In order to more stablize moisture and oxygen content in entire glove box, therefore also need to by protecting gas
Body input port 3 is passed through protective gas (nitrogen or argon gas) into glove box.
(2) sample；As shown in figure 3, battery core all uses the form of winding now, 22 lugs are distributed on the pole piece of whole,
For the accuracy of sampling, whole monolithic pole piece of selection is located at the middle part of battery core, and middle part is also to be most difficult to dry
Into.The disk of sampling is evenly distributed on monolithic pole piece, and diameter range is controlled in φ 12 (+0.03, -0.03), obtained weight
Scope is measured between 2.15-2.20g.It is needed when operation by the abnormal partially thick position in coating area 19 along a cutting wires 20 1
It is secondary to crop.As shown in Figure 1：It is put into battery core pole piece 12 is smooth in the detent mechanism of sampling mould, by sampling mould
Punch 11 moves up and down under sampling mould in the edge of a knife 13, is smoothly punched out the disk of φ 12mm.The circle of the φ 12mm to fall down
Piece is smoothly entered in print rewinding box 14, and unordered tune is avoided to fall on the tables of glove box, causes the pollution of pole piece.Such as Fig. 4
It is shown：The print rewinding box 14 that disk is fallen into is by print feeding box main body 14-1, print feeding box rewinding mouth 14-2, and print takes
Magazine cant timber 14-3 is constituted jointly.The placement position of wherein print rewinding box main body 14-1 corresponds to dropping off for sampling mould
Mouthful；Print feeding box rewinding mouth 14-2 is designed as φ 15mm, rewinding mouth diameter less times greater than the diameter of print, be for print more
Good drops to corresponding drop off in mouth；Print feeding box cant timber 14-3 is designed as 60 °, after exactly print being avoided to fall down,
The bottom of print feeding box rewinding mouth 14-2 is directly fallen to, so as to cause relatively difficult to pick up print with instrument.
(3) print is weighed；As shown in Figure 1：The print sampled is put into clean drift bottle 10, and uses ME203E
Type electronic balance 9 is weighed.The resolution ratio of this electronic balance reaches 0.1mg, can accurately identify the error of print.
(4) print encapsulates；, it is necessary to which the lid of drift bottle 10 is reliably sealed with masking foil after the completion of weighing, from
It is passed out in transfer chamber, carries out the test of next step moisture tester.
(5) print moisture measurement；As shown in Figure 2：The drift bottle 10 sealed is put into the test turntable 17 of moisture tester
On, the test of rotational latency moisture tester stylus 18 according to this.Also needed to during test pipeline connection heating furnace 16 into
Row assisted evaporative moisture.By in the test period of 10-15min, completing the test of single drift bottle 10, final test result
It is shown on the screen of the main instrument 15 of plum Teller moisture tester, testing staff to be facilitated to record data, completes entire survey
Examination process.
Although specific embodiments of the present invention have been described above, those skilled in the art should be appreciated that this
It is merely illustrative of, various changes or modifications can be made to present embodiment, without departing from the principle and substance of the present invention,
Protection scope of the present invention is only limited by the claims that follow.
Claims (10)
1. a kind of sampler of lithium battery moisture measurement, including glove box, it is characterised in that：The glove box includes test chamber
And transfer chamber, moveable transfer chamber Inner hatch doors are equipped between the test chamber and transfer chamber；In the middle part of the test chamber from up to
Under be disposed with the edge of a knife and print rewinding box under sampling mould upper punch, sampling mould；At left and right sides of the test chamber upper end
Divide and be connected with dry wind air inlet and dry wind air outlet；Test chamber lower end one side is connected with protective gas input port.
2. a kind of sampler of lithium battery moisture measurement described in accordance with the claim 1, it is characterised in that：The test chamber side
Wall is provided with hanging temperature and humidity measuring instrument, and dew point control probe is provided with above the transfer chamber test hatch door.
3. a kind of sampler of lithium battery moisture measurement described in accordance with the claim 1, it is characterised in that：In the test chamber
It is provided with battery core and disassembles box, the test chamber middle and upper part is provided with rotating hanging article holder.
4. a kind of sampler of lithium battery moisture measurement described in accordance with the claim 1, it is characterised in that：In the test chamber
Electronic balance is provided with, drift bottle is placed in the electronic balance.
5. a kind of sampler of lithium battery moisture measurement described in accordance with the claim 1, it is characterised in that：The print rewinding
Box includes print feeding box main body, is provided with several print feeding box rewinding mouths on the print feeding box main body, the print takes
Magazine rewinding mouth is tilted to be provided with print feeding box cant timber.
6. according to a kind of sampler of lithium battery moisture measurement described in claim 5, it is characterised in that：The print feeding
Box cant timber angle of inclination is 60 °.
A kind of 7. sampling and testing method of lithium battery moisture measurement, which is characterized in that comprise the following steps,
(1) battery is disassembled；Battery enters from the transfer chamber of glove box, and enters in glove box test chamber, will be in transfer chamber
Hatch door is locked after being rotated down, and dry battery is disassembled in battery core disassembles box to obtain battery core pole piece；
(2) sample；It is put into battery core pole piece is smooth in the detent mechanism of sampling mould, is being sampled by sampling mould upper punch
It moves up and down under mold in the edge of a knife, is smoothly punched out the disk of φ 12mm, the disk of the φ 12mm to fall down smoothly enters sample
In piece rewinding box；
(3) print is weighed；The print sampled is put into clean drift bottle, and is weighed with electronic balance；
(4) print encapsulates；, it is necessary to the lid of drift bottle reliably be sealed with masking foil, from transfer chamber after the completion of weighing
In pass out, carry out next step moisture tester test；
(5) print moisture measurement；The drift bottle sealed is put on the test turntable of moisture tester, according to this rotational latency moisture
The test of tester stylus；The heating furnace 16 that pipeline connection is also needed to during test carries out assisted evaporative moisture, by 10-
In the test period of 15min, the test of single drift bottle is completed, final test result is shown in the main instrument 15 of moisture tester
Screen on.
8. according to a kind of sampling and testing method of lithium battery moisture measurement described in claim 7, it is characterised in that：The step
(1) the dew point environment in probe monitors glove box is controlled by dew point in, by dry wind air inlet and dry wind air outlet
Logical dry wind ensures the cycling of dry wind.
9. according to a kind of sampling and testing method of lithium battery moisture measurement described in claim 7, it is characterised in that：The step
(1) nitrogen or argon gas are inputted by protective gas input port in.
10. according to a kind of sampling and testing method of lithium battery moisture measurement described in claim 7, it is characterised in that：The step
Suddenly the battery core pole piece chosen in (2) is located at the middle part of battery core.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711332069.4A CN108106880A (en) | 2017-12-13 | 2017-12-13 | The sampling and testing method and sampler of a kind of lithium battery moisture measurement |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711332069.4A CN108106880A (en) | 2017-12-13 | 2017-12-13 | The sampling and testing method and sampler of a kind of lithium battery moisture measurement |
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| CN112595754A (en) * | 2020-12-02 | 2021-04-02 | 株洲时代新材料科技股份有限公司 | Water-dispersing rate testing device and method |
| CN115615181A (en) * | 2022-09-30 | 2023-01-17 | 广东利元亨智能装备股份有限公司 | Moisture detection method and baking device |
| WO2023071784A1 (en) * | 2021-10-25 | 2023-05-04 | 宁德时代新能源科技股份有限公司 | Battery sheet water removal system and battery sheet water removal method |
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Address after: 213200 Jiangdong Avenue 1, Jintan District, Jiangsu, Changzhou Applicant after: AVIC lithium Technology Co., Ltd Address before: 213200 Jiangdong Avenue 1, Jintan District, Jiangsu, Changzhou Applicant before: CHINA AVIATION LITHIUM BATTERY Co.,Ltd. |
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