CN107633930A - A kind of positive temperature coefficient thermo-sensitive material and preparation method thereof - Google Patents
A kind of positive temperature coefficient thermo-sensitive material and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of positive temperature coefficient thermo-sensitive material and preparation method thereof, belong to thermo-sensitive material technical field.The positive temperature coefficient thermo-sensitive material of the present invention is made up of the raw material including following component：Barium source and one kind, titanium source, manganese source, metal oxide, sintering aid in lead source；The barium source or lead source and the mol ratio of titanium source, manganese source, metal oxide, sintering aid are 99 99.5:100.85‑100.95:0.04‑0.05:0.2‑0.5:0.1‑0.2；The metal oxide is the combination of the oxide or oxide of any one in Nb, Ta, Bi, Sb, Y, La.For the positive temperature coefficient thermo-sensitive material of the present invention when more than certain temperature (Curie temperature), for its resistance value with rise the increasing in step evolution of temperature, the material has small resistor below Curie temperature；The material causes PTC layers to have temperature sensitivity.
Description
Technical field
The present invention relates to a kind of positive temperature coefficient thermo-sensitive material and preparation method thereof, belong to thermo-sensitive material technical field.
Background technology
Lithium ion battery has many advantages as a kind of emerging technology compared with conventional batteries.In the prior art, lithium from
Sub- battery has been widely used in all trades and professions, most prominent to be represented as mobile phone using monolithic lithium ion battery as power
Source, and New-energy electric vehicle uses Li-ion batteries piles as power source substantially.Both at home and abroad based on lithium ion battery itself
Advantage, primary study and constantly broken through in terms of theory is with engineering in recent years, grasped the application characteristic of the battery substantially.Lithium from
Although sub- battery pack can be very good the growth requirement for meeting electric product, but hide unsafe factor always.Existing skill
Lithium ion battery in art is occurring short circuit, burning and then is causing the probability of blast to be far above other conventional batteries.
The reason for lithium ion battery explodes can be summarized as battery external short circuit and the aspect of battery internal short-circuit two.
In battery short circuit, inside battery can release substantial amounts of heat, cause to elevate the temperature, and a variety of side reactions can occur for inside battery, special
When not being the negative pole shorted contacts under aluminum foil current collector and full power state, it is easier to make lithium ion battery that thermal runaway occur anti-
Should, cause the security performance of lithium ion battery to substantially reduce.Therefore how the safeguard procedures inside battery, block from root
The possibility that thermal runaway occurs for battery is highly important.
Positive temperature coefficient thermo-sensitive material (PTC) has in lower temperature coefficient that resistance is relatively low, and temperature rises to necessarily
The characteristic that resistance steeply rises during degree.This materials'use can block inside battery on lithium ion battery under the condition of high temperature
Short-circuit reaction, it is significant to the security of raising lithium ion battery.But the structure of this thermo-sensitive material is mostly similar
With ceramic material, during using in lithium ion battery, the internal resistance of battery can be caused necessarily to influence.Therefore when in use, it is necessary to
The usage amount of this material is limited, and when usage amount is too small, the lifting to battery security is then very limited.
The content of the invention
It is an object of the invention to provide a kind of positive temperature coefficient that can be had a distinct increment to lithium ion battery security
Thermo-sensitive material.
The present invention also aims to provide the preparation method of above-mentioned positive temperature coefficient thermo-sensitive material.
To achieve the above object, the technical scheme of positive temperature coefficient thermo-sensitive material of the invention is：
A kind of positive temperature coefficient thermo-sensitive material, is made up of the raw material including following component：Barium source and one kind in lead source, titanium
Source, manganese source, metal oxide, sintering aid；The barium source or lead source and titanium source, manganese source, metal oxide, the mol ratio of sintering aid
For 0.9915:1.0095:0.0004:0.002:0.001；The metal oxide is any one in Nb, Ta, Bi, Sb, Y, La
Oxide or oxide combination.
The positive temperature coefficient thermo-sensitive material of the present invention is the semiconductor resistor that a kind of typical case has temperature sensitivity, more than one
During fixed temperature (Curie temperature), its resistance value with rise the increasing in step evolution of temperature, the material Curie temperature with
There is down small resistor；The material causes PTC layers to have temperature sensitivity.
Particularly, positive temperature coefficient thermo-sensitive material of the invention is lithium ion battery positive temperature coefficient thermo-sensitive material.
The sintering aid is that aluminum oxide, silica zirconium dioxide according to mol ratio are 0.03：0.03：0.62 composition mixes
Compound.The present invention using many oxide mixture be used as sintering aid, can make made from PTC material structure
More stable homogeneous, material is finer and close, and intensity is bigger.
Titanium source can select titanium salt or titanyl compound, and in order to facilitate sintering reaction, in general, the titanium source is dioxy
Change titanium.
Barium source and lead source are using conventional raw materials for sintering, and the barium source is strontium titanates, and the lead source is lead titanates.
The metal oxide is Nd2O3、Ta2O5、Bi2O3、Sb2O3、Sb2O5、Y2O3、La2O3In any one or group
Close.Preferably, metal oxide uses Nd2O3、Ta2O5、Bi2O3、Sb2O3、Sb2O5、Y2O3、La2O3In any two kinds of group
Close.It is further preferred that using Ta2O5、Bi2O3、Sb2O3、Sb2O5、Y2O3、La2O3In any one and Nd2O3Combination.Two
The mol ratio of person is 3:1.Or using Ta2O5、Bi2O3、Sb2O3、Sb2O5、Y2O3、La2O3In any two kinds of combination.
Mn (NO in step 2)3)2Use mass fraction for 50% Mn (NO3)2Solution.Using manganese nitrate solution, can make
Manganese source is sufficiently mixed uniformly with other raw materials.
The technical scheme of preparation method of the positive temperature coefficient thermo-sensitive material of the present invention is：
A kind of preparation method of positive temperature coefficient thermo-sensitive material, comprises the following steps：
1) barium source or lead source are well mixed with titanium source, metal oxide, 6-8h are calcined at 1200-1250 DEG C, cooled down,
Grinding, obtains pre-sintered powder；The metal oxide is the oxide or oxide of any one in Nb, Ta, Bi, Sb, Y, La
Combination；
2) the pre-sintered powder for obtaining step 1) and sintering aid, Mn (NO3)2It is well mixed, burnt at 1350-1400 DEG C
30-60min is tied, is produced.
Particularly, positive temperature coefficient thermo-sensitive material of the invention is lithium ion battery positive temperature coefficient thermo-sensitive material.
The sintering aid is that aluminum oxide, silica, zirconium dioxide according to mol ratio are 0.03：0.03：0.62 composition
Mixture.The present invention using many oxide mixture be used as sintering aid, can make made from PTC material knot
Structure more stable homogeneous, material is finer and close, and intensity is bigger.
Titanium source can select titanium salt or titanyl compound, and in order to facilitate sintering reaction, in general, the titanium source is dioxy
Change titanium.
Barium source and lead source are using conventional raw materials for sintering, and the barium source is strontium titanates, and the lead source is lead titanates.
The metal oxide is Nd2O3、Ta2O5、Bi2O3、Sb2O3、Sb2O5、Y2O3、La2O3In any one or group
Close.Preferably, metal oxide uses Nd2O3、Ta2O5、Bi2O3、Sb2O3、Sb2O5、Y2O3、La2O3In any two kinds of group
Close.It is further preferred that using Ta2O5、Bi2O3、Sb2O3、Sb2O5、Y2O3、La2O3In any one and Nd2O3Combination.Two
The mol ratio of person is 3:1.Or using Ta2O5、Bi2O3、Sb2O3、Sb2O5、Y2O3、La2O3In any two kinds of combination.
Mn (NO in step 2)3)2Use mass fraction for 50% Mn (NO3)2Solution.Using manganese nitrate solution, can make
Manganese source is sufficiently mixed uniformly with other raw materials.
It is well mixed in step 2) as first by pre-sintered powder, first time ball milling 6h, then addition help burning in ball mill
Agent, Mn (NO3)2Carry out second of ball milling 6h.
Dry temperature and time can be selected depending on drying efficiency and degree, in general, mixed after second of ball milling
Close material 110 DEG C of dry 10h in drying box.It is ground after drying to obtain the powder of appropriate particle size.
First time ball milling in step 1) and step 2) is to add water wet-milling.Material, water, the mass ratio of ball are 1 during ball milling：2：
2。
The beneficial effects of the invention are as follows：
The positive temperature coefficient thermo-sensitive material of the present invention is applied on lithium ion battery, is risen in internal temperature of battery critical
During point, PTC (positive temperature coefficient resistor) layer resistance rapidly becomes big or even insulated, so as to effectively control lithium ion battery big
Battery temperature during rate charge-discharge.When battery can effectively be prevented directly connecing for negative pole and aluminium foil by puncturing etc. during injury
Touch, so as to avoid the possibility of negative pole and aluminium foil short circuit dischange, battery exothermic reaction when slow down short circuit；Further improve lithium ion
The security of battery.The lithium ion battery collector of the present invention can be good at improving the anti-over-charging of lithium ion battery, anti-short
Road, puncture resistance, improve the security of lithium ion battery.
Embodiment
Embodiments of the present invention are described further with reference to specific embodiment.
Embodiment 1
The positive temperature coefficient thermo-sensitive material of the present embodiment is made up of the following raw material：Barium source, titanium source, manganese source, metal oxide,
Sintering aid；Above-mentioned barium source, titanium source, manganese source, metal oxide, the mol ratio of sintering aid are 0.9915:1.0095:0.0004:
0.002:0.001；Wherein barium source is strontium titanates, and titanium source is titanium dioxide, and manganese source is Mn (NO3)2, metal oxide be mol ratio
For 1:3 Nd2O3And La2O3, sintering aid is that aluminum oxide, silica, zirconium dioxide according to mol ratio are 0.03：0.03：0.62
The mixture of composition.
The preparation method of the positive temperature coefficient thermo-sensitive material of the present embodiment comprises the following steps：
1) batch mixing
It is 0.9915 by mol ratio：1.0095：0.0005：0.0015 strontium titanates, titanium dioxide, Nd2O3、La2O3It is put into
In ball mill, add water wet-milling 6 hours, it is uniformly mixed, material, water, the mass ratio of ball are 1 during ball milling：2：2；Ball milling is good
Material is placed on 110 DEG C of dry 6h in drying box, and dried material takes out, and is put into mortar and grinds fully, it is standby to obtain powder；
2) calcine
The powder mixed is calcined into 6h at 1200 DEG C, cools to room temperature with the furnace, is taken out, grinding in mortar is put into and fills
Point, it is standby to obtain pre-sintered powder；
3) double sintering
Finely ground pre-sintered powder is put into ball mill plus water wet-milling 6 hours, material, water, the mass ratio of ball are during grinding
1：2：2；Then sintering aid is added, the Mn (NO that mass fraction is 50%3)2Solution, continuing ball milling 6h makes it uniformly mix；Help burning
The mol ratio of agent and strontium titanates is 0.001:0.9915, sintering aid is that mol ratio is 0.03：0.03：0.62 aluminum oxide, dioxy
SiClx, zirconia mixture；Mn(NO3)2Mn (NO in solution3)2Mol ratio with strontium titanates is 0.0004:0.9915；
The good material of ball milling is placed on 110 DEG C of dry 10h in drying box, dried material takes out, and is put into grinding in mortar and fills
Point；Then 30min is sintered at 1350 DEG C, produced.
Embodiment 2
The positive temperature coefficient thermo-sensitive material of the present embodiment is made up of the following raw material：Barium source, titanium source, manganese source, metal oxide,
Sintering aid；Above-mentioned barium source, titanium source, manganese source, metal oxide, the mol ratio of sintering aid are 0.99:1.0085:0.0005:
0.005:0.002；Wherein barium source is strontium titanates, and titanium source is titanium dioxide, and manganese source is Mn (NO3)2, metal oxide be mol ratio
For 1:3 Nd2O3And Sb2O3, sintering aid is that aluminum oxide, silica, zirconium dioxide according to mol ratio are 0.03：0.03：0.62
The mixture of composition.
The preparation method of the positive temperature coefficient thermo-sensitive material of the present embodiment comprises the following steps：
1) batch mixing
It is 0.99 by mol ratio：1.0085：0.0005：0.0015 strontium titanates, titanium dioxide, Nd2O3、Sb2O3It is put into ball
In grinding machine, add water wet-milling 6 hours, it is uniformly mixed, material, water, the mass ratio of ball are 1 during ball milling：2：2；By the good material of ball milling
110 DEG C of dry 6h in drying box are placed on, dried material takes out, and is put into mortar and grinds fully, it is standby to obtain powder；
2) calcine
The powder mixed is calcined into 8h at 1250 DEG C, cools to room temperature with the furnace, is taken out, grinding in mortar is put into and fills
Point, it is standby to obtain pre-sintered powder；
3) double sintering
Finely ground pre-sintered powder is put into ball mill plus water wet-milling 6 hours, material, water, the mass ratio of ball are during grinding
1：2：2；Then sintering aid is added, the Mn (NO that mass fraction is 50%3)2Solution, continuing ball milling 6h makes it uniformly mix；Help burning
The mol ratio of agent and strontium titanates is 0.002:0.99, sintering aid is that mol ratio is 0.03：0.03：0.62 aluminum oxide, titanium dioxide
Silicon, zirconia mixture；Mn(NO3)2Mn (NO in solution3)2Mol ratio with strontium titanates is 0.0005:0.99；
The good material of ball milling is placed on 110 DEG C of dry 10h in drying box, dried material takes out, and is put into grinding in mortar and fills
Point；Then 50min is sintered at 1400 DEG C, produced.
Embodiment 3
The positive temperature coefficient thermo-sensitive material of the present embodiment is made up of the following raw material：Lead source, titanium source, manganese source, metal oxide,
Sintering aid；Above-mentioned lead source, titanium source, manganese source, metal oxide, the mol ratio of sintering aid are 0.9915:1.0095:0.0004:
0.002:0.001；Wherein lead source is lead titanates, and titanium source is titanium dioxide, and manganese source is Mn (NO3)2, metal oxide be mol ratio
For 1:3 Nd2O3And Y2O3, sintering aid is that aluminum oxide, silica, zirconium dioxide according to mol ratio are 0.03：0.03：0.62
The mixture of composition.
The preparation method of the positive temperature coefficient thermo-sensitive material of the present embodiment comprises the following steps：
1) batch mixing
It is 0.9915 by mol ratio：1.0095：0.0005：0.0015 lead titanates, titanium dioxide, Nd2O3、Y2O3It is put into
In ball mill, add water wet-milling 6 hours, it is uniformly mixed, material, water, the mass ratio of ball are 1 during ball milling：2：2；Ball milling is good
Material is placed on 110 DEG C of dry 6h in drying box, and dried material takes out, and is put into mortar and grinds fully, it is standby to obtain powder；
2) calcine
The powder mixed is calcined into 6h at 1200 DEG C, cools to room temperature with the furnace, is taken out, grinding in mortar is put into and fills
Point, it is standby to obtain pre-sintered powder；
3) double sintering
Finely ground pre-sintered powder is put into ball mill plus water wet-milling 6 hours, material, water, the mass ratio of ball are during grinding
1：2：2；Then sintering aid is added, the Mn (NO that mass fraction is 50%3)2Solution, continuing ball milling 6h makes it uniformly mix；Help burning
The mol ratio of agent and lead titanates is 0.001:0.9915, sintering aid is that mol ratio is 0.03：0.03：0.62 aluminum oxide, dioxy
SiClx, zirconia mixture；Mn(NO3)2Mn (NO in solution3)2Mol ratio with lead titanates is 0.0004:0.9915；
The good material of ball milling is placed on 110 DEG C of dry 10h in drying box, dried material takes out, and is put into grinding in mortar and fills
Point；Then 30min is sintered at 1350 DEG C, produced.
Test example
1) resistance v. temperature is tested
Its resistance data at different temperatures is tested to the PTC material in embodiment 1,3, as shown in table 1：
The resistance data of PTC material at different temperatures in the embodiment 1,3 of table 1
2) safety testing
PTC material in Example 1 prepares lithium ion battery in accordance with the following steps：
1) PVDF binding agents are dissolved in 1-METHYLPYRROLIDONE, then add PTC material powder, positive temperature
The mass ratio of coefficient material powder and binding agent is 98:2, be uniformly dispersed the PTC slurries for being made that solid content is 80%, by gained
PTC slurries are coated uniformly on the two sides of aluminium foil with spraying process, drying, obtain lithium ion battery collector；
2) positive pole is made
The PVDF (polyvinylidene fluoride) of 2 parts by weight is dissolved in NMP (1-METHYLPYRROLIDONE), mixes binding agent
Slurry, the electrically conductive graphite of 1.5 parts by weight is evenly mixed in binding agent, by the LiNi of 100 parts by weight0.5Co0.2Mn0.3
In (positive active material) mixing and electrocondution slurry；By obtained anode sizing agent coated in the i.e. obtained coating of above-mentioned collector
On two surfaces of aluminium foil of positive temperature coefficient heat-sensitive layer, then it is dried, carries out roll-in and cross cutting afterwards, obtains required positive pole pole
Piece；
3) negative pole is made
The CMC (sodium carboxymethylcellulose) of 1.5 parts by weight is molten with ionized water, binding agent slurry being mixed, by 1.5
The electrically conductive graphite of parts by weight is evenly mixed in binding agent, negative electrode active material mixing and conductive paste by 100 parts by weight
In material, in the well mixed obtained electrocondution slurries of SBR (butadiene-styrene rubber) for adding 2 parts by weight；Obtained cathode size is applied
On obtained two surfaces of coating 9um thickness copper foil, then it is dried, carries out roll-in and cross cutting afterwards, obtains required bear
Pole pole piece；
4) battery makes
Battery diaphragm is 32um thickness PP barrier films, and the electrolyte used is LiPF6(1mol/l)EMC：DEC：EC=1:1:1,
Lithium ion battery is made by the form of coating lamination.
According to above-mentioned battery production method, using the normal aluminium foil of the uncoated positive temperature coefficient thermo-sensitive materials of normal 18um,
The lithium ion battery of making is as a comparison case.
Above-mentioned obtained lithium ion battery is tested as follows：
(1) inner walkway
Lithium ion battery obtained above is tested using internal resistance test device, test result is as shown in table 2.
(2) acupuncture experimental evaluation
Above-mentioned gained lithium ion battery is charged, specific charging process is to carry out constant-current charge using 10A electric current, fill
To blanking voltage 4.2V, constant-current charge is changed to after being charged to 4.2V, until electric current ends for 200mA.
Then under conditions of normal temperature, lithium-ion electric is vertically pierced through using Φ 5 high temperature resistant draw point instrument 25mm/s speed
In the middle part of pond, and draw point is stopped in the battery, observed one hour.Result of the test is as shown in table 2.
(3) experiment is overcharged
Above-mentioned gained lithium ion battery is charged, specific charging process is to carry out constant-current charge using 10A electric current, fill
To blanking voltage 6.3V, observe the apparent condition of lithium ion battery and whether burn.Result of the test is as shown in table 2.
Lithium ion battery test result in the embodiment 1 of table 2 and comparative example
| Internal resistance (m Ω) | Cells burst quantity during acupuncture | Overcharge cells burst quantity | |
| Embodiment 1 | 4.26 | 0/5 | 0/5 |
| Comparative example | 2.92 | 3/5 | 2/5 |
When acupuncture is tested, find that coating positive temperature coefficient thermo-sensitive material is not used, made 5 batteries, there are 3 electricity
Core burns, it is thus impossible to ensure the security performance of lithium ion battery acupuncture.But use coating made in the present invention
After positive temperature coefficient thermo-sensitive material aluminium foil, made 5 lithium ion batteries are all without generation combustion phenomena.
When overcharging experiment, find that coating positive temperature coefficient thermo-sensitive material is not used, made 5 batteries, there are 2 electricity
Core burns, it is thus impossible to ensure the security performance of lithium ion battery acupuncture.But use coating made in the present invention
After positive temperature coefficient thermo-sensitive material aluminium foil, made 5 lithium ion batteries are all without generation combustion phenomena.
As can be seen here lithium can be greatly promoted using the aluminium foil of the coating positive temperature coefficient thermo-sensitive material prepared by the present invention
The security performance of ion battery.
Claims (10)
1. a kind of positive temperature coefficient thermo-sensitive material, it is characterised in that be made up of the raw material including following component：In barium source and lead source
One kind, titanium source, manganese source, metal oxide, sintering aid；The barium source or lead source and titanium source, manganese source, metal oxide, help burning
The mol ratio of agent is 99-99.5:100.85-100.95:0.04-0.05:0.2-0.5:0.1-0.2；The metal oxide is
The combination of the oxide or oxide of any one in Nb, Ta, Bi, Sb, Y, La.
2. positive temperature coefficient thermo-sensitive material according to claim 1, it is characterised in that：The sintering aid is aluminum oxide, two
Silica, zirconium dioxide are 0.03 according to mol ratio：0.03：The mixture of 0.62 composition.
3. a kind of preparation method of positive temperature coefficient thermo-sensitive material, it is characterised in that comprise the following steps：
1) barium source or lead source are well mixed with titanium source, metal oxide, 6-8h is calcined at 1200-1250 DEG C, cooled down, grind
Mill, obtains pre-sintered powder；The metal oxide is the oxide or oxide of any one in Nb, Ta, Bi, Sb, Y, La
Combination；
2) the pre-sintered powder for obtaining step 1) and sintering aid, Mn (NO3)2It is well mixed, sinter 30- at 1350-1400 DEG C
60min, produce.
4. the preparation method of positive temperature coefficient thermo-sensitive material according to claim 3, it is characterised in that the sintering aid is
Aluminum oxide, silica, zirconium dioxide are 0.03 according to mol ratio：0.03：The mixture of 0.62 composition.
5. the preparation method of positive temperature coefficient thermo-sensitive material according to claim 3, it is characterised in that the titanium source is two
Titanium oxide.
6. the preparation method of positive temperature coefficient thermo-sensitive material according to claim 3, it is characterised in that the barium source is titanium
Sour strontium, the lead source are lead titanates.
7. the preparation method of positive temperature coefficient thermo-sensitive material according to claim 3, it is characterised in that the metal oxidation
Thing is Nd2O3、Ta2O5、Bi2O3、Sb2O3、Sb2O5、Y2O3、La2O3In any one or combination.
8. the preparation method of positive temperature coefficient thermo-sensitive material according to claim 3, it is characterised in that Mn in step 2)
(NO3)2Use mass fraction for 50% Mn (NO3)2Solution.
9. the preparation method of positive temperature coefficient thermo-sensitive material according to claim 3, it is characterised in that mixed in step 2)
Uniformly for first by pre-sintered powder in ball mill first time ball milling 6h, then add sintering aid, Mn (NO3)2Carry out second of ball
Grind 6h.
10. the preparation method of positive temperature coefficient thermo-sensitive material according to claim 9, it is characterised in that second of ball milling
The 110 DEG C of dry 10h in drying box of compound afterwards.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113644276A (en) * | 2021-08-13 | 2021-11-12 | 湖州南木纳米科技有限公司 | Current collector and application thereof |
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| JP2010254536A (en) * | 2009-04-28 | 2010-11-11 | Nichicon Corp | Positive characteristic thermistor ceramic composition |
| CN103904294A (en) * | 2012-12-24 | 2014-07-02 | 财团法人工业技术研究院 | Lithium ion battery and electrode structure thereof |
| CN107010944A (en) * | 2017-05-08 | 2017-08-04 | 句容市博远电子有限公司 | A kind of PTC thermistor and preparation method thereof |
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| CN101127265A (en) * | 2007-07-30 | 2008-02-20 | 韩城市华龙电子有限责任公司 | Below curie point positive temperature coefficient PTCR heat-sensitive resistance element |
| JP2010254536A (en) * | 2009-04-28 | 2010-11-11 | Nichicon Corp | Positive characteristic thermistor ceramic composition |
| CN103904294A (en) * | 2012-12-24 | 2014-07-02 | 财团法人工业技术研究院 | Lithium ion battery and electrode structure thereof |
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