CN103969148B - The lithium ion battery detection method of material with carbon element kind stability - Google Patents
The lithium ion battery detection method of material with carbon element kind stability Download PDFInfo
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- CN103969148B CN103969148B CN201410211136.7A CN201410211136A CN103969148B CN 103969148 B CN103969148 B CN 103969148B CN 201410211136 A CN201410211136 A CN 201410211136A CN 103969148 B CN103969148 B CN 103969148B
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Abstract
This application provides a kind of detection method of lithium ion battery material with carbon element kind stability, comprise the following steps: a. sample pre-treatments: different types of material with carbon element sample is fully dry respectively; B. thermogravimetric test: use thermogravimetric analyzer, carries out the thermogravimetric test of material with carbon element sample, obtains thermal gravimetric analysis curve and the derivative thermogravimetric analysis curve of material with carbon element sample; C. interpretation of result: determine the weightless peak initial temperature of different material with carbon element sample and weightless peak temperature according to the weightless peak of derivative thermogravimetric analysis curve, and with the difference of the kind material with carbon element of weightless peak initial temperature and weightless peak temperature determination material with carbon element sample.The detection method of the lithium ion battery material with carbon element kind stability using the application to provide, sample use amount is few, highly sensitive, accuracy is good, detection speed is fast, is easy to promote.
Description
Technical field
The application relates to material with carbon element field, in particular to a kind of detection method of lithium ion battery material with carbon element kind stability.
Background technology
Graphite and similar material with carbon element thereof are lithium ion battery negative materials most widely used, the most ripe at present.The kind of graphite and similar material with carbon element thereof and lot stability are directly connected to the performance of lithium ion battery.At present, kind and the lot stability detection method of the material with carbon element generally used that is in the news comprise, infrared (IR), Raman (Raman), x-ray photoelectron power spectrum (XPS) etc.Wherein, infrared is utilize the difference of the surface functional group of graphite and similar material with carbon element thereof to distinguish the kind of these material with carbon elements, but due to the surface functional group of material with carbon element different from processing technology is identical substantially identical, just quantitatively have little bit different.In this case, infrared very difficult different types of material with carbon element separately; It is according to the different degree of graphitization of carbon material surface that Raman (Raman) distinguishes different types of material with carbon element, this Comparison between detecting methods be suitable for having clad and without clad graphite between difference, be difficult to the graphite distinguishing different batches; X-ray photoelectron power spectrum (XPS) is although effectively can distinguish the lot stability of different types of material with carbon element and material with carbon element of the same race, and equipment is valuable, testing cost is high, require high to tester's professional knowledge, is not suitable for promoting the use of of method of testing.
Summary of the invention
This application provides a kind of detection method of lithium ion battery material with carbon element kind stability to solve the problem.
The present invention is achieved in that
The application provides a kind of detection method of lithium ion battery material with carbon element kind stability, comprises the following steps:
A. sample pre-treatments: different types of material with carbon element sample is fully dry respectively;
B. thermogravimetric test: use thermogravimetric analyzer, carries out the thermogravimetric test of described material with carbon element sample, obtains thermal gravimetric analysis curve and the derivative thermogravimetric analysis curve of described material with carbon element sample;
C. interpretation of result: determine the weightless peak initial temperature of different described material with carbon element sample and weightless peak temperature according to the weightless peak of derivative thermogravimetric analysis curve, and determine the difference of the kind material with carbon element of described material with carbon element sample with described weightless peak temperature and described weightless peak temperature.
Preferably, described sample is that lithium ion battery commonly uses graphite, comprises the mixing of one or more in Delanium, native graphite, coated natural graphite, carbonaceous mesophase spherules, hard carbon and soft carbon.
Preferably, the step of described sample pre-treatments comprises: get described sample 0.01g ~ 1g and be put in drying box, 60 ~ 90 DEG C of drying 2 ~ 4h, are then cooled to room temperature, obtains the sample after dry process.
Preferably, the step of described sample pre-treatments comprises: get described sample 0.01g ~ 1g and be placed in dry 2 ~ 4h under infrared lamp box, be then cooled to room temperature, obtain the sample after dry process.
Preferably, the amount of described sample is 25mg.
Preferably, be 0.5mg to the weighing precision of sample and weightlessness in the test of described thermogravimetric.
Preferably, the step of described thermogravimetric test also comprises: the alumina crucible of thermogravimetric analyzer put into by the sample got after described drying process, thermogravimetric analysis is carried out after balance is stable, wherein, the flow rate of carrier gas of gas is set as 20 ~ 70ml/min, programming rate controls at 1 DEG C/min ~ 10 DEG C/min, and final temperature is set as 1100 DEG C ~ 1200 DEG C, and described flow rate of carrier gas, described programming rate and described final temperature remain unchanged in testing process.
Preferably, the amount of the sample after described drying process is 5 ~ 50mg, and described flow rate of carrier gas is 30ml/min, and described programming rate is 2 DEG C/min, and described final temperature is 1200 DEG C.
Preferably, described balance is stable refers to that balance numerical value fluctuates and is no more than 0.02mg.
Preferably, described gas is air or oxygen.
The detection method of the lithium ion battery material with carbon element kind stability using the application to provide, following beneficial effect can be brought:
The first, sample pretreatment is simple, and technological requirement difficulty is low; The second, use thermogravimetric analysis, sample use amount is few, highly sensitive, accuracy is good, detection speed is fast; 3rd, checkout equipment is simple to operate, cost is lower, is applicable to large-scale promotion and uses; 4th, obtain TG and DTG curve by thermogravimetric analysis, result is distinct, easily judges.
Accompanying drawing explanation
Fig. 1 shows thermogravimetric curve and the differential thermogravimetric curve of the material with carbon element of the same race that the embodiment of the present application provides;
Fig. 2 shows thermogravimetric curve and the differential thermogravimetric curve of the different material with carbon elements that the embodiment of the present application provides;
Embodiment
Below in conjunction with drawings and Examples, the application is described in further detail.Be understandable that, specific embodiment described herein is only for explaining the application, but not the restriction to the application.
The application provides a kind of detection method of lithium ion battery material with carbon element kind stability, comprises the following steps:
A. sample pre-treatments: different types of material with carbon element sample is fully dry respectively;
B. thermogravimetric test: use thermogravimetric analyzer, carries out the thermogravimetric test of described material with carbon element sample, obtains thermal gravimetric analysis curve and the derivative thermogravimetric analysis curve of described material with carbon element sample;
C. interpretation of result: determine the weightless peak initial temperature of different described material with carbon element sample and weightless peak temperature according to the weightless peak of derivative thermogravimetric analysis curve, and determine the difference of the kind material with carbon element of described material with carbon element sample with described weightless peak initial temperature and described weightless peak temperature.
Preferably, described sample is that lithium ion battery commonly uses graphite, comprises the mixing of one or more in Delanium, native graphite, coated natural graphite, carbonaceous mesophase spherules, hard carbon and soft carbon.
Preferably, the step of described sample pre-treatments comprises: get described sample 0.01g ~ 1g and be put in drying box, 60 ~ 90 DEG C of drying 2 ~ 4h, are then cooled to room temperature, obtains the sample after dry process.
Preferably, the step of described sample pre-treatments comprises: get described sample 0.01g ~ 1g and be placed in dry 2 ~ 4h under infrared lamp box, be then cooled to room temperature, obtain the sample after dry process.
Preferably, the amount of described sample is 25mg.
Preferably, be 0.5mg to the weighing precision of sample and weightlessness in the test of described thermogravimetric.
Preferably, the step of described thermogravimetric test also comprises: the alumina crucible of thermogravimetric analyzer put into by the sample got after described drying process, thermogravimetric analysis is carried out after balance is stable, wherein, the flow rate of carrier gas of gas is set as 20 ~ 70ml/min, programming rate controls at 1 DEG C/min ~ 10 DEG C/min, and final temperature is set as 1100 DEG C ~ 1200 DEG C, and described flow rate of carrier gas, described programming rate and described final temperature remain unchanged in testing process.
Preferably, the amount of the sample after described drying process is 5 ~ 50mg, and described flow rate of carrier gas is 30ml/min, and described programming rate is 2 DEG C/min, and described final temperature is 1200 DEG C.
Preferably, described balance is stable refers to that balance numerical value fluctuates and is no more than 0.02mg.
Preferably, described gas is air or oxygen.
Fig. 1 shows thermogravimetric curve and the differential thermogravimetric curve of the material with carbon element of the same race that the embodiment of the present application provides.
Curve as shown in Figure 1, mainly shows the reappearance of thermogravimetric analysis in material with carbon element context of detection.
Have two groups of totally 4 curves in Fig. 1, left side have first mild after sharply decline the again suite line (left direction arrow) of lofted features be differential thermogravimetric curve, right side have first mild after sharply decline an again suite line of mild feature be thermogravimetric curve.In this curve, by material with carbon element sample called after Gr-1 roughly the same batch of the same race, first time test curve be Gr-1-1st, second time test curve is Gr-1-2nd.First time test and second time are tested respective thermogravimetric curve and are overlapped, and its respective differential thermogravimetric curve also overlaps.
Its preparation method is as described below:
Take 0.5g roughly the same batch material with carbon element (Gr-1) of the same race, put into drying box, 80 DEG C of dry 4h, are then cooled to room temperature, material with carbon element dry after obtaining pre-service.Respectively getting the pretreated material with carbon element of about 25mg (precision controlling is within 0.5mg) loads in the alumina crucible of thermogravimetric analyzer, take dry air as carrier gas, flow velocity is 30ml/min, after thermogravimetric analyzer balance is stable (left and right float 0.02mg), with the programming rate of 2 DEG C/min from room temperature to 1200 DEG C, finally obtain thermogravimetric curve (TG) and differential thermogravimetric curve (DTG).
Twice test result (Gr-1-1st, Gr-1-2nd) weightless peak initial temperature (i.e. material with carbon element temperature of initial combustion) and weightless peak temperature (i.e. material with carbon element maximum combustion temperature) overlap completely, and its thermogravimetric curve overlaps completely, differential thermogravimetric curve also overlaps completely.It can thus be appreciated that thermogravimetric analysis has superior reappearance in material with carbon element context of detection.
Fig. 2 shows thermogravimetric curve and the differential thermogravimetric curve of the different material with carbon elements that the embodiment of the present application provides.
Curve as shown in Figure 2, mainly distinguishes detection to carry out material with carbon element kind.Its preparation method is as described below:
Respectively take 1.0g variety classes material with carbon element, put into drying box, 60 DEG C of dry 3h, are then cooled to room temperature, material with carbon element dry after obtaining pre-service.Respectively getting the pretreated material with carbon element of about 25mg (precision controlling is within 0.5mg) loads in the alumina crucible of thermogravimetric analyzer, take dry air as carrier gas, flow velocity is 20ml/min, after thermogravimetric analyzer balance is stable (fluctuate and be no more than 0.02mg), with the programming rate of 1 DEG C/min from room temperature to 1200 DEG C, finally obtain thermogravimetric curve (TG) and differential thermogravimetric curve (DTG).
Have two groups of totally 6 curves in Fig. 2, have first mild after sharply decline the again suite line (left direction arrow) of lofted features be differential thermogravimetric curve, have first mild after sharply decline an again suite line of mild feature be thermogravimetric curve.
Three kinds of material with carbon element (Gr-1, Gr-2 and Gr-3) weightless peaks initial temperature (i.e. material with carbon element temperature of initial combustion) and weightless peak temperature (i.e. material with carbon element maximum combustion temperature) with detect material with carbon element and have one-to-one relationship, weightless peak temperature (i.e. material with carbon element maximum combustion temperature) respectively, Gr-1:810 DEG C, Gr-2:885 DEG C, Gr-3:905 DEG C.Thus, different types of material with carbon element can be distinguished.
The detection method of the lithium ion battery material with carbon element kind stability using the application to provide, sample use amount is few, highly sensitive, accuracy is good, detection speed is fast, and obtain TG and DTG curve by thermogravimetric analysis, result is distinct, easily judges.
The foregoing is only the preferred embodiment of the application, be not limited to the application, for a person skilled in the art, the application can have various modifications and variations.Within all spirit in the application and principle, any amendment done, equivalent replacement, improvement etc., within the protection domain that all should be included in the application.
Claims (10)
1. a lithium ion battery detection method for material with carbon element kind stability, is characterized in that, comprise the following steps:
A. sample pre-treatments: different types of material with carbon element sample is fully dry respectively;
B. thermogravimetric test: use thermogravimetric analyzer, carries out the thermogravimetric test of described material with carbon element sample, obtains thermal gravimetric analysis curve and the derivative thermogravimetric analysis curve of described material with carbon element sample;
C. interpretation of result: determine the weightless peak initial temperature of different described material with carbon element sample and weightless peak temperature according to the weightless peak of derivative thermogravimetric analysis curve, and determine the difference of the kind material with carbon element of described material with carbon element sample with described weightless peak initial temperature and described weightless peak temperature.
2. detection method according to claim 1, is characterized in that, wherein, described sample is that lithium ion battery commonly uses graphite, comprises the mixing of one or more in Delanium, native graphite, coated natural graphite, carbonaceous mesophase spherules, hard carbon and soft carbon.
3. detection method according to claim 1, is characterized in that, wherein, the step of described sample pre-treatments comprises: get described sample 0.01g ~ 1g and be put in drying box, 60 ~ 90 DEG C of drying 2 ~ 4h, are then cooled to room temperature, obtains the sample after dry process.
4. detection method according to claim 1, is characterized in that, wherein, the step of described sample pre-treatments comprises: get described sample 0.01g ~ 1g and be placed in dry 2 ~ 4h under infrared lamp box, be then cooled to room temperature, obtain the sample after dry process.
5. the detection method according to claim 3 or 4, is characterized in that, wherein, the amount of described sample is 25mg.
6. detection method according to claim 1, is characterized in that, wherein, is 0.5mg to the weighing precision of sample and weightlessness in the test of described thermogravimetric.
7. the detection method according to claim 3 or 4, it is characterized in that, wherein, the step of described thermogravimetric test also comprises: the alumina crucible of thermogravimetric analyzer put into by the sample got after described drying process, thermogravimetric analysis is carried out after balance is stable, wherein, the flow rate of carrier gas of gas is set as 20 ~ 70ml/min, programming rate controls at 1 DEG C/min ~ 10 DEG C/min, final temperature is set as 1100 DEG C ~ 1200 DEG C, and described flow rate of carrier gas, described programming rate and described final temperature remain unchanged in testing process.
8. detection method according to claim 7, is characterized in that, wherein, the amount of the sample after described drying process is 5 ~ 50mg, and described flow rate of carrier gas is 30ml/min, and described programming rate is 2 DEG C/min, and described final temperature is 1200 DEG C.
9. detection method according to claim 7, is characterized in that, wherein, described balance is stable to be referred to that balance numerical value fluctuates and be no more than 0.02mg.
10. detection method according to claim 7, is characterized in that, wherein, described gas is air or oxygen.
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