CN109411171A - A kind of preparation method of negative temperature coefficient bead thermistor - Google Patents
A kind of preparation method of negative temperature coefficient bead thermistor Download PDFInfo
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- CN109411171A CN109411171A CN201811242010.0A CN201811242010A CN109411171A CN 109411171 A CN109411171 A CN 109411171A CN 201811242010 A CN201811242010 A CN 201811242010A CN 109411171 A CN109411171 A CN 109411171A
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- H—ELECTRICITY
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- H01—ELECTRIC ELEMENTS
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- H01C17/28—Apparatus or processes specially adapted for manufacturing resistors adapted for applying terminals
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- H01—ELECTRIC ELEMENTS
- H01C—RESISTORS
- H01C17/00—Apparatus or processes specially adapted for manufacturing resistors
- H01C17/30—Apparatus or processes specially adapted for manufacturing resistors adapted for baking
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01C—RESISTORS
- H01C7/00—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material
- H01C7/04—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material having negative temperature coefficient
- H01C7/042—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material having negative temperature coefficient mainly consisting of inorganic non-metallic substances
- H01C7/043—Oxides or oxidic compounds
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
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- C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
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Abstract
The invention discloses a kind of preparation methods of negative temperature coefficient bead thermistor.It uses cobalt sesquioxide, mangano-manganic oxide, nickel oxide, di-iron trioxide and magnesia for raw material, prepares five elements oxide thermosensitive resistor powder body material by ball-milling method；Thermistor is prepared using organic solvent；Pearl shaping is quantitatively controlled using dispenser；After high temperature sintering, welding outer lead, using obtained bead thermistor after the encapsulation of inorganic high-temp glue, welding p-wire.Thermistor prepared by the present invention is suitable for high temperature, material constant B25℃/50℃For 3500K ± 5%, resistance value is 45k Ω ± 10% at 0 DEG C of temperature, 900 DEG C of temperature, R after high temperature ageing 200h0℃Resistance varying-ratio is less than ± 4%.High-temperature thermistor prepared by the present invention has stable high-temperature performance, and consistency is good, and ageing properties are stablized, and is suitable for aerospace, automotive field therm-param method.
Description
Technical field
The present invention relates to a kind of preparation method of negative temperature coefficient bead thermistor, which passes through high temperature 900
DEG C aged properties is stablized, and consistency is good, is suitable for aerospace, automotive field therm-param method.
Background technique
High temperature negative temperature coefficient (NTC) thermistor material can be prepared to be led for automotive electronics, military project, aerospace etc.
The temperature-sensitive element of domain ultra-wide warm area thermometric.It can be used for measuring the temperature of turbogenerator high-temperature fuel gas in aviation field；
It can be used for carrying out real-time monitoring to the temperature of thruster heating period and working stage in space industry；It is available in automotive field
It measures and controls in the temperature to engine engine.
NTC thermistor is most commonly that Mn-Co-Ni-O base ternary system and the multicomponent system to its element doping.Mesh
The preceding research to high-temperature NTC heat-sensitive resistance is less, and the resistance value of thermistor material is easily drifted about after high temperature ageing,
Influence the test accuracy of thermal resistor.
Thermistor packing forms are usually glass-encapsulated, but simple glass encapsulation can occur at high temperature softening or
Fusing, using high temp glass encapsulation, there are difficult formings again, and high temp glass needs to encapsulate at high temperature, and package temperature is close
The sintering temperature of thermistor will affect the performance of thermistor.
Sheet, rod-shaped thermistor usually use silver electrode as the transition zone between porcelain body and lead, make in long term high temperature
Under, silver electrode can generate aging, increase contact resistance.And bead thermistor directly forms on platinum filament, it can be to avoid
The preparation of silver electrode and the welding of electrode and lead, improve the reliability used.
Summary of the invention
Technology of the invention solves the problems, such as: overcoming the deficiencies of the prior art and provide a kind of negative temperature coefficient pearl temperature-sensitive
The preparation method of resistance solves the problems, such as that thermistor material resistance value after high temperature ageing is easily drifted about.
The technical solution of the invention is as follows: a kind of preparation method of negative temperature coefficient bead thermistor, this method packet
Include following steps:
(1), it uses cobalt sesquioxide, mangano-manganic oxide, nickel oxide, di-iron trioxide and magnesia for raw material, prepares
Thermistor powder body material；
(2), it is mixed using organic solvent with thermistor powder body material, prepares Thermistor；
(3), Thermistor is molded on the platinum filament lead that two are parallel to each other, it is raw forms bead thermistor
Base, later, by bead thermistor green compact curing molding；
(4), the bead thermistor green compact after curing molding are sintered；
(5), outer lead is welded for sintered bead thermistor；
(6), the bead thermistor after welding outer lead is encapsulated, bead thermistor is made.
The molar percentage of cobalt, manganese, nickel, iron, magnesium each component in the thermistor powder body material are as follows: cobalt: manganese: nickel:
Iron: magnesium=30~35:35~40:6~10:15~20:1~5.
The mass ratio of thermistor powder body material and organic solvent in Thermistor are as follows: 50~70:30~50.
The organic solvent be terpinol, diglycol and dibutyl phthalate mixture, terpinol,
The quality proportioning of diglycol and dibutyl phthalate are as follows: 60~80:10~30:5~15.
The step (3) quantitatively controls pearl shaping using dispenser.
The diameter of the platinum filament is 80~100 μm, and the distance between two platinum filaments are 260~300 μm.
Step (4) sintering range is 1150 DEG C~1250 DEG C.
Bead thermistor is packaged using the inorganic high-temp glue of model OMEGABOND 600.
Thermistor powder in the step (1) the preparation method is as follows:
(1.1), according to preset thermistor material cobalt, manganese, nickel, iron, magnesium each component molar percentage, calculate three
Aoxidize the mass ratio of two cobalts, mangano-manganic oxide, nickel oxide, di-iron trioxide and magnesia raw material；
(1.2), according to the matter of cobalt sesquioxide, mangano-manganic oxide, nickel oxide, di-iron trioxide and magnesia raw material
Ratio is measured, cobalt sesquioxide, mangano-manganic oxide, nickel oxide, di-iron trioxide and magnesia are mixed, thermistor powder is obtained
Raw material；
(1.3), thermistor powder raw material are used into wet-mixing ball milling, it is former obtains uniformly mixed thermistor
Material paste；
(1.4), the thermistor raw material slurry after wet-milling is dried, obtains thermistor raw material block；
(1.5), thermistor powder body material is obtained after being ground up, sieved to the thermistor raw material block after drying.
The granularity of thermistor powder body material is 300 or 400 mesh in the step (1.5).
The advantages of the present invention over the prior art are that:
(1), the present invention in Mn-Co-Ni-Fe base quaternary system using Mg element is adulterated, preferably to adjust Mn-Co-
The resistivity and material constant B value of Ni-Fe base quaternary system material, the resistance after high temperature ageing can be reduced by addition Mg element
Value drift has good resistance stability after Co-Mn-Ni-Fe-Mg-O five elements thermistor high temperature ageing.
(2), present invention employs terpinol (CP), diglycol (AR) and dibutyl phthalate (AR)
Mixture is uniformly mixed to obtain Thermistor as organic solvent with heat-sensitive powder material, carries out pearl using the slurry
Molding thermistor surface is smooth, and compactness is good.
(3), the present invention carries out thermistor pearl shaping using dispenser, has played the pressure controllable of dispenser, has got
The controllable advantage of amount of slurry ensure that requirement of the thermistor to pearl shaping size identical property, with existing point pearl phase by hand
Than having significant progress.
(4), the present invention selects bead thermistor form, and Thermistor directly forms on platinum filament, can be to avoid
The preparation of electrode and the welding of electrode and lead, improve the reliability used.
(5), the present invention selects the inorganic height with the model OMEGABOND 600 of corrosion-and high-temp-resistant of insulation performance
Warm glue carries out thermistor encapsulation, thermistor and solder joint can be protected and be fixed.
(6), using material constant of thermistor B prepared by the present invention25℃/50℃For 3500K ± 5%, resistance at 0 DEG C of temperature
Value is 45k Ω ± 10%, 900 DEG C of temperature, R after high temperature ageing 200h0℃Resistance varying-ratio is less than ± 4%.
Detailed description of the invention
Fig. 1 is bead thermistor of embodiment of the present invention preparation technology flow chart；
Fig. 2 is thermistor structure of embodiment of the present invention schematic diagram.
Specific embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
The present invention provides a kind of preparation methods of negative temperature coefficient bead thermistor, mainly include powder preparation, pearl
Shape molding, high temperature sintering, high-temp glue encapsulation and etc..Using cobalt sesquioxide, mangano-manganic oxide, nickel oxide, di-iron trioxide
It is raw material with magnesia, prepares five elements oxide thermosensitive resistor powder body material by ball-milling method；It is prepared using organic solvent
Thermistor；Pearl shaping is quantitatively controlled using dispenser；After high temperature sintering, welding outer lead, using inorganic height
Bead thermistor is made after warm glue encapsulation, welding p-wire.Specific step is as follows:
(1), it uses cobalt sesquioxide, mangano-manganic oxide, nickel oxide, di-iron trioxide and magnesia for raw material, prepares
Thermistor powder body material；
(1.1), according to thermistor material cobalt, manganese, nickel, iron, magnesium each component molar percentage, calculate three oxidation two
Cobalt, mangano-manganic oxide, nickel oxide, di-iron trioxide and magnesia raw material mass ratio；In the thermistor powder body material
Cobalt, manganese, nickel, iron, magnesium each component molar percentage are as follows: cobalt: manganese: nickel: iron: magnesium=30~35:35~40:6~10:15~
20:1~5.
(1.2), according to the matter of cobalt sesquioxide, mangano-manganic oxide, nickel oxide, di-iron trioxide and magnesia raw material
Ratio is measured, cobalt sesquioxide, mangano-manganic oxide, nickel oxide, di-iron trioxide and magnesia are mixed, thermistor powder is obtained
Raw material；
(1.3), thermistor powder raw material are used into wet-mixing ball milling, it is former obtains uniformly mixed thermistor
Material paste；
(1.4), the thermistor raw material slurry after wet-milling is dried, obtains thermistor raw material block；
(1.5), thermistor powder body material is obtained after being ground up, sieved to the thermistor raw material block after drying.Institute
The granularity for stating thermistor powder body material in step (1.5) is 300~400 mesh.
(2), using with certain cohesiveness and volatile alcohols and based organic solvent and thermistor powder body material
Thermistor is prepared in mixing；The mass ratio of thermistor powder and organic solvent in the Thermistor are as follows:
50~70:30~50, as a preferred solution of the present invention, the organic solvent are terpinol (CP), diglycol (AR)
With the mixture of dibutyl phthalate (AR), terpinol (CP), diglycol (AR) and dibutyl phthalate
(AR) quality proportioning are as follows: 60~80:10~30:5~15.The thermistor surface light of pearl shaping is carried out using the slurry
It is sliding, and compactness is good.
(3), Thermistor is molded on the platinum filament lead that two are parallel to each other, it is raw forms bead thermistor
Base, later, by bead thermistor green compact curing molding；Pearl shaping can quantitatively be controlled using dispenser.The platinum filament
Diameter is 80~100 μm, and the distance between two platinum filaments are 260~300 μm.Pressure size and the time of dispenser are adjusted, it is right
Quasi- platinum filament dispensing is allowed into the spherical shape that diameter is 1~2mm and hangs on two platinum filaments.The forming method has played the pressure of dispenser
Power is controllable, gets the controllable advantage of amount of slurry, ensure that requirement of the thermistor to pearl shaping size identical property, and existing
Manual point pearl compare, there is significant progress.
(4), the bead thermistor green compact after curing molding are sintered, sintering range be 1150 DEG C~
1250℃.Thermistor is sintered after forming directly on platinum filament, can be to avoid the preparation of electrode and the weldering of electrode and lead
It connects, improves the reliability used.
(5), outer lead is welded for sintered bead thermistor, the electric signal of thermistor can be drawn.
(6), the bead thermistor after welding outer lead is encapsulated, bead thermistor is made.Using model
The inorganic high-temp glue of OMEGABOND 600 is packaged bead thermistor.The inorganic glue good insulation preformance, and can be right
Thermistor and solder joint are protected and are fixed.
Embodiment 1
Steps are as follows for the realization of the present embodiment:
The preparation of (1-1), thermistor powder:
(1-1.1) weigh ingredient: according to thermistor material cobalt, manganese, nickel, iron, magnesium each component molar percentage are as follows:
Cobalt: manganese: nickel: iron: magnesium=35:40:9:15:1 calculates and successively weighs cobalt sesquioxide, mangano-manganic oxide, nickel oxide, three oxygen
Change two iron and magnesia raw material.
(1-1.2) ball milling: raw material are carried out wet-mixing ball milling 4 hours using ball mill.
(1-1.3) drying: the slurry after wet-milling carries out 100 DEG C of drying.
(1-1.4) is ground up, sieved: to obtaining thermistor powder body material after ground 300 mesh of powder after drying.
(1-2), Thermistor are prepared:
Thermistor is configured to using organic solvent and the stirring of thermistor vacuum powder.Thermistor powder with
The mass ratio of organic solvent are as follows: 70:30.Organic solvent is terpinol (CP), diglycol (AR) and phthalic acid
The mixture of dibutyl ester (AR), quality proportioning are as follows: 60:30:10.
(1-3), pearl shaping:
Thermistor is molded on the platinum filament that two are parallel to each other using dispenser, forms bead thermistor
Green compact；Make green compact curing molding through overbaking.The platinum filament that two diameters are 80 μm is specially fixed, keeps two platinum filaments parallel, and
Spacing is 260 μm.The pressure size for adjusting dispenser is 20KPa, time 10s, is directed at platinum filament dispensing, and being allowed into diameter is 1
The spherical shape of~2mm is hung on two platinum filaments.
(1-4), high temperature sintering:
Thermistor high temperature sintering is carried out using high temperature sintering furnace, sintering temperature is 1200 DEG C.
(1-5), welding outer lead:
By diameter be 80 μm platinum filament lead and diameter be that 300 μm of platinum filament leads pass through accurate reserve energy spot welding machine and weld
Come.
The endpoint for being located at the same root platinum filament lead at bead thermistor both ends is welded together, and then common weldering
It connects on another platinum filament outer lead, forms two point two-wire bead thermistor.The diameter of the platinum filament outer lead is 300 μm.
The encapsulation of (1-6), high-temp glue:
High-temp glue encapsulation is carried out to bead thermistor.Using the inorganic high-temp glue of model OMEGABOND 600 to pearl
Shape thermistor is packaged.Add water to be mixed into slurry form in inorganic high-temp glue, slurry is wrapped around bead thermistor
Material, is then placed in Muffle furnace and solidifies, program curing are as follows: DEG C 4h → 105 DEG C 4h → Slow cooling of room temperature 18~for 24 hours → 82.
Embodiment 2
Steps are as follows for the realization of the present embodiment:
The preparation of (2-1), thermistor powder:
(2-1.1) weigh ingredient: according to thermistor material cobalt, manganese, nickel, iron, magnesium each component molar percentage are as follows:
Cobalt: manganese: nickel: iron: magnesium=30:35:10:20:5 calculates and successively weighs cobalt sesquioxide, mangano-manganic oxide, nickel oxide, three
Aoxidize two iron and magnesia raw material.
(2-1.2) ball milling: raw material are carried out wet-mixing ball milling 5 hours using ball mill.
(2-1.3) drying: the slurry after wet-milling carries out 100 DEG C of drying.
(2-1.4) is ground up, sieved: to obtaining thermistor powder body material after ground 400 mesh of powder after drying.
(2-2), Thermistor are prepared:
Thermistor is configured to using organic solvent and the stirring of thermistor vacuum powder.Thermistor powder with
The mass ratio of organic solvent are as follows: 50:50.Organic solvent is terpinol (CP), diglycol (AR) and phthalic acid
The mixture of dibutyl ester (AR), quality proportioning are as follows: 80:15:5.
(2-3), pearl shaping:
Thermistor is molded on the platinum filament that two are parallel to each other using dispenser, forms bead thermistor
Green compact；Make green compact curing molding through overbaking.The platinum filament that two diameters are 100 μm is specially fixed, keeps two platinum filaments parallel,
And spacing is 300 μm.The pressure size for adjusting dispenser is 25KPa, time 6s, is directed at platinum filament dispensing, being allowed into diameter is
The spherical shape of 2mm is hung on two platinum filaments.
(2-4), high temperature sintering:
Thermistor high temperature sintering is carried out using high temperature sintering furnace, sintering temperature is 1250 DEG C.
(2-5), welding outer lead:
By diameter be 100 μm platinum filament lead and diameter be that 300 μm of platinum filament leads pass through accurate reserve energy spot welding machine and weld
Come.
The encapsulation of (2-6), high-temp glue:
High-temp glue encapsulation is carried out to bead thermistor.Using the inorganic high-temp glue of model OMEGABOND 600 to pearl
Shape thermistor is packaged.
Embodiment 3
Steps are as follows for the realization of the present embodiment:
The preparation of (3-1), thermistor powder:
(3-1.1) weigh ingredient: according to thermistor material cobalt, manganese, nickel, iron, magnesium each component molar percentage are as follows:
Cobalt: manganese: nickel: iron: magnesium=34:38:6:18:4 calculates and successively weighs cobalt sesquioxide, mangano-manganic oxide, nickel oxide, three oxygen
Change two iron and magnesia raw material.
(3-1.2) ball milling: raw material are carried out wet-mixing ball milling 5.5 hours using ball mill.
(3-1.3) drying: the slurry after wet-milling carries out 100 DEG C of drying.
(3-1.4) is ground up, sieved: to obtaining thermistor powder body material after ground 400 mesh of powder after drying.
(3-2), Thermistor are prepared:
Thermistor is configured to using organic solvent and the stirring of thermistor vacuum powder.Thermistor powder with
The mass ratio of organic solvent are as follows: 60:40.Organic solvent is generally chosen with certain cohesiveness and volatile alcohols and ester
The mixture of class together by thermistor powder adhesion convenient for molding, is easy to vapor away by sintering process after molding.Have
Solvent is terpinol (CP), the mixture of diglycol (AR) and dibutyl phthalate (AR), quality proportioning
Are as follows: 75:10:15.
(3-3), pearl shaping:
Thermistor is molded on the platinum filament that two are parallel to each other using dispenser, forms bead thermistor
Green compact make green compact curing molding through overbaking, form sensitive body.As shown in Figure 2.In the present embodiment, two are specially fixed directly
The platinum filament that diameter is 90 μm, keeps two platinum filaments parallel, and spacing is 280 μm.The pressure size for adjusting dispenser is 25KPa, time
For 6s, it is directed at platinum filament dispensing, the spherical sensitive body that diameter is 1.5mm is allowed into and hangs on two platinum filaments.
(3-4), high temperature sintering:
Thermistor high temperature sintering is carried out using high temperature sintering furnace.The sintering temperature is 1150 DEG C.
(3-5), welding outer lead:
By diameter be 90 μm platinum filament lead and diameter be that 300 μm of platinum filament leads pass through accurate reserve energy spot welding machine and weld
Come.
The encapsulation of (3-6), high-temp glue:
High-temp glue encapsulation is carried out to bead thermistor.Using the inorganic high-temp glue of model OMEGABOND 600 to pearl
Shape thermistor is packaged.
It using accurate reserve energy spot welding machine welding test lead and is carried out for thermistor prepared by above-described embodiment
Performance test after thermistor performance test, thermistor degradation, degradation.Test case is as follows:
(1a) thermistor performance test:
The measurement of resistance value is carried out to the thermal resistor after encapsulation, is tested in the desk-top thermostatical oil of FLUKE7341 type deep-well
It is carried out in slot.The material constant of thermistor B measured25℃/50℃For 3500K ± 5%, at 0 DEG C of temperature resistance value be 45k Ω ±
10%.
(1b), thermistor degradation:
The test of constant-pressure and high-temperature bin aging is carried out using Muffle furnace, 900 DEG C of storage temperature, period of storage accumulative 200 is small
When.
Performance test after (1c), degradation:
Resistance value test is carried out using the desk-top thermostatic oil bath of FLUKE7341 type deep-well.Material constant of thermistor B25℃/50℃For
3500K ± 5%, resistance value is 45k Ω ± 10% at 0 DEG C of temperature, after 900 DEG C of aging 200h of high temperature, R0℃Resistance varying-ratio is small
In ± 4%.
It can be seen that using cobalt sesquioxide, mangano-manganic oxide, nickel oxide, di-iron trioxide and magnesia for former material
Material prepares five elements oxide thermosensitive resistor powder body material by ball-milling method；Using pearl shaping, high temperature sintering, high-temp glue
Encapsulation and etc. be made bead thermistor, after 900 DEG C of aging 200h of high temperature, resistance varying-ratio is less than the thermistor
± 4%, ageing properties are stablized.
High-temperature thermistor prepared by the present invention has stable high-temperature performance, and consistency is good, and ageing properties are stablized, and is suitable for boat
Empty space flight, automotive field therm-param method.
It is not described in detail in this specification and partly belongs to common sense well known to those skilled in the art.
Claims (10)
1. a kind of preparation method of negative temperature coefficient bead thermistor, it is characterised in that include the following steps:
(1), it uses cobalt sesquioxide, mangano-manganic oxide, nickel oxide, di-iron trioxide and magnesia for raw material, prepares temperature-sensitive
Resistance powder body material；
(2), it is mixed using organic solvent with thermistor powder body material, prepares Thermistor；
(3), Thermistor is molded on the platinum filament lead that two are parallel to each other, forms bead thermistor green compact, it
Afterwards, by bead thermistor green compact curing molding；
(4), the bead thermistor green compact after curing molding are sintered；
(5), outer lead is welded for sintered bead thermistor；
(6), the bead thermistor after welding outer lead is encapsulated, bead thermistor is made.
2. a kind of preparation method of negative temperature coefficient bead thermistor according to claim 1, it is characterised in that described
The molar percentage of cobalt, manganese, nickel, iron, magnesium each component in thermistor powder body material are as follows: cobalt: manganese: nickel: iron: magnesium=30~35:
35~40:6~10:15~20:1~5.
3. a kind of preparation method of negative temperature coefficient bead thermistor according to claim 1, it is characterised in that temperature-sensitive
The mass ratio of thermistor powder body material and organic solvent in resistance slurry are as follows: 50~70:30~50.
4. a kind of preparation method of negative temperature coefficient bead thermistor according to claim 1, it is characterised in that described
Organic solvent be terpinol, diglycol and dibutyl phthalate mixture, terpinol, diglycol and
The quality proportioning of dibutyl phthalate are as follows: 60~80:10~30:5~15.
5. a kind of preparation method of negative temperature coefficient bead thermistor according to claim 1, it is characterised in that described
Step (3) quantitatively controls pearl shaping using dispenser.
6. a kind of preparation method of negative temperature coefficient bead thermistor according to claim 1, it is characterised in that described
The diameter of platinum filament is 80~100 μm, and the distance between two platinum filaments are 260~300 μm.
7. a kind of preparation method of negative temperature coefficient bead thermistor according to claim 1, it is characterised in that described
Step (4) sintering range is 1150 DEG C~1250 DEG C.
8. a kind of preparation method of negative temperature coefficient bead thermistor according to claim 1, it is characterised in that use
The inorganic high-temp glue of model OMEGABOND 600 is packaged bead thermistor.
9. a kind of preparation method of negative temperature coefficient bead thermistor according to claim 2, it is characterised in that described
Thermistor powder in step (1) the preparation method is as follows:
(1.1), according to preset thermistor material cobalt, manganese, nickel, iron, magnesium each component molar percentage, calculate three oxidation two
Cobalt, mangano-manganic oxide, nickel oxide, di-iron trioxide and magnesia raw material mass ratio；
(1.2), according to cobalt sesquioxide, mangano-manganic oxide, nickel oxide, di-iron trioxide and magnesia raw material mass ratio,
Cobalt sesquioxide, mangano-manganic oxide, nickel oxide, di-iron trioxide and magnesia are mixed, thermistor powder raw material are obtained；
(1.3), thermistor powder raw material are used into wet-mixing ball milling, obtains uniformly mixed thermistor former material slurry
Material；
(1.4), the thermistor raw material slurry after wet-milling is dried, obtains thermistor raw material block；
(1.5), thermistor powder body material is obtained after being ground up, sieved to the thermistor raw material block after drying.
10. a kind of preparation method of negative temperature coefficient bead thermistor according to claim 9, it is characterised in that described
The granularity of thermistor powder body material is 300 or 400 mesh in step (1.5).
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111872370A (en) * | 2020-07-15 | 2020-11-03 | 深圳市惠拓电子材料有限公司 | Preparation method of NTC thermistor material with ultrafine particle size |
| CN114864204A (en) * | 2022-05-18 | 2022-08-05 | 中国科学院新疆理化技术研究所 | Packaging method for improving thermal shock resistance of bead-shaped high-temperature-resistant thermistor |
| CN116283274A (en) * | 2023-03-06 | 2023-06-23 | 肇庆市金龙宝电子有限公司 | NTC thermistor material based on rare earth element and preparation method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101183578A (en) * | 2007-12-13 | 2008-05-21 | 上海维安热电材料股份有限公司 | Plate type NTC thermosensitive resistor with low resistor and high B value and its making method |
| CN101882490A (en) * | 2010-03-25 | 2010-11-10 | 中国科学院新疆理化技术研究所 | Rare earth oxide doped negative temperature coefficient thermistor material |
| CN102249648A (en) * | 2011-04-01 | 2011-11-23 | 中国科学院新疆理化技术研究所 | Magnesium-containing quaternary system negative temperature coefficient thermistor material |
| CN103617851A (en) * | 2013-12-03 | 2014-03-05 | 中国科学院新疆理化技术研究所 | Method for preparing thermistor powder material by using improved co-precipitation method |
| US20150049788A1 (en) * | 2013-08-12 | 2015-02-19 | Mitsubishi Materials Corporation | Metal nitride material for thermistor, method for producing same, and film type thermistor sensor |
| CN104671746A (en) * | 2015-02-11 | 2015-06-03 | 深圳顺络电子股份有限公司 | Ceramic wafer of thermistor, thermistor and preparation method thereof |
-
2018
- 2018-10-24 CN CN201811242010.0A patent/CN109411171B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101183578A (en) * | 2007-12-13 | 2008-05-21 | 上海维安热电材料股份有限公司 | Plate type NTC thermosensitive resistor with low resistor and high B value and its making method |
| CN101882490A (en) * | 2010-03-25 | 2010-11-10 | 中国科学院新疆理化技术研究所 | Rare earth oxide doped negative temperature coefficient thermistor material |
| CN102249648A (en) * | 2011-04-01 | 2011-11-23 | 中国科学院新疆理化技术研究所 | Magnesium-containing quaternary system negative temperature coefficient thermistor material |
| US20150049788A1 (en) * | 2013-08-12 | 2015-02-19 | Mitsubishi Materials Corporation | Metal nitride material for thermistor, method for producing same, and film type thermistor sensor |
| CN103617851A (en) * | 2013-12-03 | 2014-03-05 | 中国科学院新疆理化技术研究所 | Method for preparing thermistor powder material by using improved co-precipitation method |
| CN104671746A (en) * | 2015-02-11 | 2015-06-03 | 深圳顺络电子股份有限公司 | Ceramic wafer of thermistor, thermistor and preparation method thereof |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111872370A (en) * | 2020-07-15 | 2020-11-03 | 深圳市惠拓电子材料有限公司 | Preparation method of NTC thermistor material with ultrafine particle size |
| CN111872370B (en) * | 2020-07-15 | 2022-04-26 | 深圳市惠拓电子材料有限公司 | Preparation method of NTC thermistor material with ultrafine particle size |
| CN114864204A (en) * | 2022-05-18 | 2022-08-05 | 中国科学院新疆理化技术研究所 | Packaging method for improving thermal shock resistance of bead-shaped high-temperature-resistant thermistor |
| CN114864204B (en) * | 2022-05-18 | 2023-11-14 | 中国科学院新疆理化技术研究所 | Packaging method for improving thermal shock resistance of bead-shaped high-temperature-resistant thermal resistor |
| CN116283274A (en) * | 2023-03-06 | 2023-06-23 | 肇庆市金龙宝电子有限公司 | NTC thermistor material based on rare earth element and preparation method thereof |
| CN116283274B (en) * | 2023-03-06 | 2024-04-16 | 肇庆市金龙宝电子有限公司 | NTC thermistor material based on rare earth element and preparation method thereof |
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