CN113155887A - Method for testing stability of lithium boron alloy for thermal battery - Google Patents
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- PPTSBERGOGHCHC-UHFFFAOYSA-N boron lithium Chemical compound [Li].[B] PPTSBERGOGHCHC-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 229910000521 B alloy Inorganic materials 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 37
- 238000012360 testing method Methods 0.000 title claims abstract description 20
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 70
- 239000000956 alloy Substances 0.000 claims abstract description 70
- 238000003825 pressing Methods 0.000 claims abstract description 21
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 229910052751 metal Inorganic materials 0.000 claims abstract description 10
- 239000002184 metal Substances 0.000 claims abstract description 10
- 238000005520 cutting process Methods 0.000 claims abstract description 6
- 239000000178 monomer Substances 0.000 claims abstract description 4
- 229910052744 lithium Inorganic materials 0.000 claims description 33
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 32
- 238000013112 stability test Methods 0.000 claims 7
- 229910008290 Li—B Inorganic materials 0.000 description 10
- 239000007773 negative electrode material Substances 0.000 description 7
- 239000007788 liquid Substances 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 4
- 238000011156 evaluation Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 229910000733 Li alloy Inorganic materials 0.000 description 1
- 229910010199 LiAl Inorganic materials 0.000 description 1
- 229910012506 LiSi Inorganic materials 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000010416 ion conductor Substances 0.000 description 1
- 239000001989 lithium alloy Substances 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000012430 stability testing Methods 0.000 description 1
- 230000002277 temperature effect Effects 0.000 description 1
- 238000007725 thermal activation Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/02—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering
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- 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
- G01N33/20—Metals
- G01N33/204—Structure thereof, e.g. crystal structure
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/06—Electrodes for primary cells
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
- G01N2015/0866—Sorption
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Abstract
The invention discloses a method for testing the stability of lithium boron alloy for a thermal battery, which belongs to the technical field of thermal batteries and is characterized by comprising the following steps: s1, cutting the LiB alloy strip into round pieces with the diameter equal to that of the monomer, wherein the diameter range of the round pieces is phi 18 mm-phi 120 mm; s2, placing the LiB alloy sheet between two metal fixing plates, enabling the diameters of the two metal fixing plates and the LiB alloy sheet to be equal, locking the fixing device after applying certain pressure, and pressing the pressure to be 1.5-2.5 t/cm2(ii) a S3, placing a fixing device with LiB alloy sheets in the crucible resistor in a dry environment with the relative humidity not more than 2%Heating to 480-500 ℃ in a furnace at a heating rate of 10-20 ℃/min, and keeping the temperature for 1-2 h; and S4, taking the fixing device out of the crucible furnace, observing the integrity of the edge of the lithium boron alloy, and evaluating the stability of the LiB alloy.
Description
Technical Field
The invention belongs to the technical field of thermal batteries, and particularly relates to a method for testing stability of a lithium boron alloy for a thermal battery.
Background
The thermal battery is a thermal activation reserve battery which uses a heating system to heat and melt non-conductive solid-state salt electrolyte to form an ionic conductor connected to a load and enter a working state. The negative electrode material of the thermal battery is generally selected from metal materials with high specific capacity, negative electrode potential and strong loading capacity, and lithium metal is widely concerned by battery researchers at home and abroad due to the lower electrode potential. The melting point of lithium is 180.6 ℃, if the lithium is directly used as the negative electrode material of the thermal battery, the lithium is in a liquid state at the working temperature of the thermal battery, and the short circuit is easily caused to the positive electrode and the negative electrode of the battery, so that the alloy is generally used as the negative electrode material, the electrode potential and the effective capacity of the negative electrode are reduced to a certain extent, the negative electrode material can still keep a solid state at the working temperature, and the use requirement of the thermal battery can still be met. Lithium alloy negative electrode materials for thermal batteries have undergone a progression from LiAl to LiSi to LiB.
As early as 1978, the united states sea surface weapons center laboratory issued patents for LiB alloys. LiB is used as a negative electrode material of a thermal battery, has about 70 wt% of Li content, generally has silvery white luster and metal flexibility, is easy to roll into a thin strip, and has metal conductivity. After a patent of LiB alloy preparation is published shortly, Satula R A and the like apply for a patent of LiB alloy as a negative electrode material for preparing a thermal battery, and then Szware R performs feasibility research of LiB alloy as a negative electrode of the thermal battery, so that basic parameters required by designing the thermal battery are obtained. The research of the domestic LiB alloy starts late, from 2000 years, professor Liushijian university in China and south China dedicated to the attack research of the LiB alloy for a long time, and the LiB alloy is prepared in 2006 and provided for multiple domestic thermal battery development units.
The lithium boron alloy is a composite material consisting of lithium and lithium boron compounds, and the LiB compound serving as a matrix is of a net-shaped porous structure and can resist heat exceeding 1000 ℃, and lithium melted at high temperature is absorbed in the LiB compound. The internal balance temperature in the working process of the thermal battery is up to 500 ℃ or even higher, lithium in the lithium boron alloy is in a molten liquid state at the moment, the molten liquid lithium is absorbed by virtue of the porous structure of the LiB compound, and if the pressing pressure of the single battery is too large or under severe mechanical working conditions, the problem of overflow of the molten lithium can occur. Once the overflowing lithium is in contact with the anode material, the problem of local short circuit and even the short circuit of the whole battery is directly caused, and the safety and the reliability of the thermal battery are seriously influenced.
With the upgrading and progress of weapon systems, the requirements on the working environment and the mechanical resistance of the thermal battery are more and more strict, for example, the high-temperature working environment is increased from 70 ℃ to 450 ℃, and the impact condition is increased from the conventional 70g to 300 g. In order to improve the safety and reliability of the thermal battery while maintaining compatibility, a stability testing method for lithium boron alloy for the thermal battery is developed. .
Disclosure of Invention
The invention provides a method for testing the stability of a lithium boron alloy for a thermal battery, aiming at overcoming the defects in the prior art and improving the safety and reliability of the thermal battery.
The invention aims to provide a method for testing the stability of a lithium boron alloy for a thermal battery, which comprises the following steps:
s1, cutting the LiB alloy sheet; the method specifically comprises the following steps:
cutting the LiB alloy strip into a wafer with the diameter equal to that of the monomer, wherein the diameter range of the wafer is phi 18 mm-phi 120 mm;
s2, pressing and fixing the LiB alloy sheet; the method specifically comprises the following steps:
placing the LiB alloy sheet between two metal fixing plates, wherein the diameters of the two metal fixing plates and the LiB alloy sheet are equal, and locking the fixing device after applying certain pressure, wherein the pressing pressure is 1.5-2.5 t/cm2；
S3, high-temperature treatment; the method specifically comprises the following steps:
under a dry environment with the relative humidity not more than 2%, placing a fixing device with a LiB alloy sheet in a crucible resistance furnace, heating to 480-500 ℃ at the heating rate of 10-20 ℃/min, and keeping the temperature for 1-2 h;
s4, evaluating the stability of the LiB alloy; the method specifically comprises the following steps:
and taking the fixing device out of the crucible furnace, observing the integrity of the edge of the lithium boron alloy, and evaluating the stability of the LiB alloy.
Preferably, the width of the LiB alloy strip is 140mm, the thickness is 0.2 mm-1.1 mm, and the lithium content is 58 wt% -64 wt%.
Preferably, the diameter of the circular plate is phi 18mm, the lithium content of the LiB alloy strip is 58 wt%, and the pressing pressure is 1.5t/cm2And the temperature rise rate is 10 ℃/min.
Preferably, the diameter of the circular plate is phi 18mm, the lithium content of the LiB alloy strip is 64 wt%, and the pressing pressure is 2.5t/cm2And the temperature rise rate is 20 ℃/min.
Preferably, the diameter of the circular plate is phi 54mm, the lithium content of the LiB alloy strip is 58 wt%, and the pressing pressure is 1.5t/cm2And the temperature rise rate is 10 ℃/min.
Preferably, the diameter of the circular plate is phi 54mm, the lithium content of the LiB alloy strip is 60 wt%, and the pressing pressure is 2.5t/cm2And the temperature rise rate is 20 ℃/min.
Preferably, the diameter of the circular plate is phi 82mm, the lithium content of the LiB alloy strip is 60 wt%, and the pressing pressure is 2.5t/cm2And the temperature rise rate is 20 ℃/min.
Preferably, the diameter of the circular plate is phi 120mm, the lithium content of the LiB alloy strip is 58 wt%, and the pressing pressure is 1.5t/cm2And the temperature rise rate is 10 ℃/min.
The beneficial effect of this application is:
according to the invention, the LiB alloy sheet is placed between two metal fixing plates, after a certain pressure is applied according to the assembly parameters of the battery, the fixing device is locked, the device is placed in a high-temperature furnace for heat preservation, the fixing device is taken out, and the integrity of the edge of the LiB alloy sheet is observed so as to evaluate the stability of the lithium boron alloy.
1) According to the invention, the stability of the lithium boron alloy can be evaluated only by monitoring the overflow amount of the lithium boron alloy under pressurization fixation and high-temperature treatment, and the operation is simple and rapid;
2) the method can develop the safety design of the battery in the material evaluation stage, obviously improve the safety, effectively reduce the debugging cost and have great application value.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present application, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without inventive exercise.
FIG. 1 is a graph showing the test results of the first preferred embodiment of the present invention;
FIG. 2 is a graph showing the test results of a second preferred embodiment of the present invention;
FIG. 3 is a graph showing the test results of the third preferred embodiment of the present invention;
FIG. 4 is a graph showing the test results of the fourth preferred embodiment of the present invention;
FIG. 5 is a graph showing the test results of a fifth preferred embodiment of the present invention;
fig. 6 is a test result graph of the sixth preferred embodiment of the present invention.
Detailed Description
In order to make the technical solutions better understood by those skilled in the art, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are only partial embodiments of the present application, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
It should be noted that the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover non-exclusive inclusions, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present application will be described in detail below with reference to the embodiments with reference to the attached drawings.
Internal balance temperature reaches 500 ℃ or even higher in the thermal battery working process, and lithium in the lithium boron alloy is in a molten liquid state at the moment, and the molten liquid lithium is adsorbed by depending on a porous structure of a LiB compound. The main points of this patent are the overflow volume of control lithium boron alloy under pressure, temperature effect to this evaluation lithium boron alloy's stability:
a method for testing the stability of lithium boron alloy for a thermal battery comprises the following steps:
(1) LiB alloy sheet cutting punch
The LiB alloy strip with the width of 140mm, the thickness of 0.2 mm-1.1 mm and the lithium content of 58 wt% -64 wt% is cut into a wafer with the diameter equal to that of the monomer, and the diameter range is phi 18 mm-phi 120 mm.
(2) LiB alloy sheet is fixed by pressing
Placing a LiB alloy sheet between two metal fixing plates with the same diameter, applying a certain pressure, and locking the fixing device, wherein the pressing pressure is 1.5-2.5 t/cm2。
(3) High temperature treatment
Under the dry environment with the relative humidity less than or equal to 2 percent, the fixing device with the LiB alloy sheet is placed in a crucible resistance furnace, the temperature is raised to 480-500 ℃ at the heating rate of 10-20 ℃/min, and the heat preservation time is 1-2 h.
(4) Evaluation of LiB alloy stability
And taking the fixing device out of the crucible furnace, observing the integrity of the edge of the lithium boron alloy, and evaluating the stability of the LiB alloy.
Referring to FIG. 1, a method for testing the stability of Li-B alloy for thermal batteries is disclosed, in which a phi 18mm die is used to punch a LiB alloy sheet with a width of 140mm, a thickness of 0.2mm and a lithium content of 58 wt% into a phi 18mm Li-B alloy sheet with a thickness of 1.5t/cm2The pressure drop of the lithium boron alloy is fixed on a device, the fixing device is placed in a crucible furnace, the temperature is increased to 480 ℃ at the heating rate of 10 ℃/min, the temperature is kept for 1h, the device is taken out, and the integrity of the edge of the lithium boron alloy is observed.
Referring to FIG. 2, a method for testing the stability of Li-B alloy for thermal batteries is disclosed, in which a phi 18mm die is used to punch a LiB alloy sheet with a width of 140mm, a thickness of 0.2mm and a lithium content of 64 wt% into a phi 18mm Li-B alloy sheet with a thickness of 2.5t/cm2The pressure drop of the lithium boron alloy is fixed on a device, the fixing device is placed in a crucible furnace, the temperature is raised to 500 ℃ at the heating rate of 20 ℃/min, the temperature is kept for 2h, the device is taken out, and the integrity of the edge of the lithium boron alloy is observed.
Referring to FIG. 3, a method for testing the stability of Li-B alloy for thermal batteries is disclosed, in which a phi 54mm stamping die is used to stamp a LiB alloy with a width of 140mm, a thickness of 0.3mm and a lithium content of 58 wt% into a phi 54mm Li-B alloy sheet with a thickness of 1.5t/cm2The pressing pressure drop is fixed on a device, the fixing device is placed in a crucible furnace, the temperature is increased to 480 ℃ at the heating rate of 10 ℃/min, the temperature is kept for 1h, the device is taken out, and the integrity of the edge of the lithium boron alloy is observed.
Referring to FIG. 4, a method for testing the stability of Li-B alloy for thermal batteries is disclosed, in which a phi 54mm stamping die is used to stamp a LiB alloy with a width of 140mm, a thickness of 0.8mm and a lithium content of 60 wt% into a phi 54mm Li-B alloy sheet with a thickness of 2.5t/cm2The pressure drop of the lithium boron alloy is fixed on a device, the fixing device is placed in a crucible furnace, the temperature is raised to 500 ℃ at the heating rate of 20 ℃/min, the temperature is kept for 2h, the device is taken out, and the integrity of the edge of the lithium boron alloy is observed.
Referring to fig. 5, a method for testing the stability of a lithium boron alloy for a thermal battery, which comprises punching a LiB alloy with a width of 140mm, a thickness of 1.1mm and a lithium content of 60 wt% into a lithium boron alloy sheet with a diameter of 82mm by using a punch die with a diameter of 82mm, fixing the lithium boron alloy sheet on a device under a pressure drop of 2.5t/cm2, placing the fixing device in a crucible furnace, heating to 500 ℃ at a heating rate of 20 ℃/min, preserving heat for 2h, taking out the device, and observing the integrity of the edge of the lithium boron alloy.
Referring to FIG. 6, a method for testing the stability of Li-B alloy for thermal batteries is disclosed, in which a phi 120mm punch die is used to punch a LiB alloy sheet with a width of 140mm, a thickness of 0.6mm and a lithium content of 58 wt% into a phi 120mm Li-B alloy sheet with a thickness of 1.5t/cm2The pressure drop of the lithium boron alloy is fixed on a device, the fixing device is placed in a crucible furnace, the temperature is increased to 480 ℃ at the heating rate of 10 ℃/min, the temperature is kept for 1h, the device is taken out, and the integrity of the edge of the lithium boron alloy is observed.
The above description is only a preferred embodiment of the present application and is not intended to limit the present application, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.
Claims (8)
1. A method for testing the stability of lithium boron alloy for a thermal battery is characterized by at least comprising the following steps:
s1, cutting the LiB alloy sheet; the method specifically comprises the following steps:
cutting the LiB alloy strip into a wafer with the diameter equal to that of the monomer, wherein the diameter range of the wafer is phi 18 mm-phi 120 mm;
s2, pressing and fixing the LiB alloy sheet; the method specifically comprises the following steps:
placing the LiB alloy sheet between two metal fixing plates, wherein the diameters of the two metal fixing plates and the LiB alloy sheet are equal, and locking the fixing device after applying certain pressure, wherein the pressing pressure is 1.5-2.5 t/cm2；
S3, high-temperature treatment; the method specifically comprises the following steps:
under a dry environment with the relative humidity not more than 2%, placing a fixing device with a LiB alloy sheet in a crucible resistance furnace, heating to 480-500 ℃ at the heating rate of 10-20 ℃/min, and keeping the temperature for 1-2 h;
s4, evaluating the stability of the LiB alloy; the method specifically comprises the following steps:
and taking the fixing device out of the crucible furnace, observing the integrity of the edge of the lithium boron alloy, and evaluating the stability of the LiB alloy.
2. The lithium boron alloy stability test method for the thermal battery according to claim 1, wherein: the width of the LiB alloy strip is 140mm, the thickness of the LiB alloy strip is 0.2 mm-1.1 mm, and the lithium content of the LiB alloy strip is 58 wt% -64 wt%.
3. The lithium boron alloy stability test method for the thermal battery according to claim 2, wherein: the diameter of the round piece is phi 18mm, the lithium content of the LiB alloy strip is 58 wt%, and the pressing pressure is 1.5t/cm2And the temperature rise rate is 10 ℃/min.
4. The lithium boron alloy stability test method for the thermal battery according to claim 2, wherein: the diameter of the round piece is phi 18mm, the lithium content of the LiB alloy strip is 64 wt%, and the pressing pressure is 2.5t/cm2And the temperature rise rate is 20 ℃/min.
5. The lithium boron alloy stability test method for the thermal battery according to claim 2, wherein: the diameter of the round piece is phi 54mm, the lithium content of the LiB alloy strip is 58 wt%, and the pressing pressure is 1.5t/cm2And the temperature rise rate is 10 ℃/min.
6. The lithium boron alloy stability test method for the thermal battery according to claim 2, wherein: the diameter of the round piece is phi 54mm, the lithium content of the LiB alloy strip is 60 wt%, and the pressing pressure is 2.5t/cm2And the temperature rise rate is 20 ℃/min.
7. The lithium boron alloy stability test method for the thermal battery according to claim 2, wherein: the diameter of the round piece is phi 82mm, the lithium content of the LiB alloy strip is 60 wt%, and the pressing pressure is 2.5t/cm2And the temperature rise rate is 20 ℃/min.
8. The lithium boron alloy stability test method for the thermal battery according to claim 2, wherein: the diameter of the round piece is phi 120mm, the lithium content of the LiB alloy strip is 58 wt%, and the pressing pressure is 1.5t/cm2And the temperature rise rate is 10 ℃/min.
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| CN114023985A (en) * | 2021-10-18 | 2022-02-08 | 中国电子科技集团公司第十八研究所 | Method for detecting pressure of activated thermal battery stack |
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| 北京有色金属研究总院: "《中华人民共和国有色金属行业标准》", 18 September 2018 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114023985A (en) * | 2021-10-18 | 2022-02-08 | 中国电子科技集团公司第十八研究所 | Method for detecting pressure of activated thermal battery stack |
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