CN104916345B - A kind of thick-film resistor paste and preparation method thereof - Google Patents
A kind of thick-film resistor paste and preparation method thereof Download PDFInfo
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Abstract
The invention provides a kind of thick-film resistor paste and preparation method thereof, belong to technical field of electronic materials.Slurry includes function phase and organic carrier, and the weight ratio of function phase and organic carrier is (60~90)：(40~10), function phase is LSMO ceramic powders, and ceramic powder component molar compares La2O3：SrCO3：MnO2=1：(0.5~2)：(1~4)；Organic carrier each component mass percent is：40%≤terpinol≤80%, 5%≤diethyl phthalate≤20%, 5%≤ATBC≤10%, 5%≤ethyl cellulose≤10%, 0%≤rilanit special≤5%, 0% ＜ polyoxyethylene sorbitan monoleate≤5%, 0%≤lecithin≤5%.Thick-film resistor paste of the present invention is with low cost, and sheet resistance is low, without adding inorganic bond phase, preparation process is simple.
Description
Technical field
The present invention relates to electronic material technology, and in particular to a kind of thick-film resistor paste and preparation method thereof.
Background technology
In electric heating field, heating element heater requirement small volume, power is big, and thermal inertia is small, and surface thermal load is big, and power consumption is low,
The thermal efficiency is high, and thermal starting is fast, power stability, and stationary field is uniform, good manufacturability, body temp auto-controlled, safe and reliable to operation, life-span
It is long, it is applied widely, it is therefore desirable to use thick-film heating element, rather than electrothermal tube or ptc heater.Current thick film heating electricity
Resistance is added as the glass phase of inorganic binder typically with the noble metal powders such as Au Ag Pt Pd or its oxide as matrix,
And be mixed to form heating resistor slurry with organic carrier, then silk screen process is on ceramic substrate, air atmosphere, 300~
Sintering is prepared from 1200 DEG C of temperature ranges.
It is resistance slurry (Chinese invention patent, the patent No. of conductive filler that the National University of Defense Technology is proposed with silver, palladium
ZL 02139894.1)；The thick-film resistor paste for stainless steel substrate that Hunan Leed Thick Film Paste Co., Ltd. releases
DZ430XXXX, conductor paste DT4306, DT4306A are with noble metal as conductive filler.Although using noble metal as conduction
Filler has the advantages that heating-up temperature is high, not oxidizable, technical maturity；But noble metal is with high costs, and addition is used as inorganic viscous
The glass of knot agent is met and electrical property is affected greatly so that the extensive use of noble metal thick-film resistor paste and its conductor is received
To considerable restraint.
For the defect for overcoming noble metal thick-film resistor paste with high costs, Shaanxi Tech Univ proposes one kind with graphite
Be conductive filler, unorganic glass powder as Binder Phase environment-friendly graphite resistance paste (Chinese invention patent application number
201010204512.1)；XiAn Hongxing Electronic Paste Co., Ltd. is then proposed with nano-sized carbon system as conductive filler
Electrothermal organic power resistance slurry for heater (Chinese invention patent application number 200810232431.5).Although with stone
Ink, organic resistance slurry that carbon fiber is representative can effectively reduce the production cost of slurry, but have that operating temperature is low, easy quilt
The defects such as oxidation, complex process, limit application of this kind of resistance slurry under compared with elevated operating temperature, cannot still replace noble metal
Resistance slurry is used for resistance heating element.
Guilin Electronic Science and Technology Univ. proposes a kind of base metal thick-film resistor paste (Chinese invention with barium titanate as function phase
Patent, application number 201010137147.7)；The sharp bright grade (Chinese invention patent application number 200810143397.4) of silver develops one
Plant the thick-film resistor paste with yttrium barium copper oxide (YBCO) based material as conductive filler mixing inorganic binder；University of Electronic Science and Technology carries
Go out the YBCO thick-film resistor pastes based on stainless steel substrate and preparation method thereof (Chinese invention patent, application number
201010158934.X), average sheet resistance reaches 10~15M Ω/；Tang of University of Electronic Science and Technology peak etc. exists《LSCO thick-film resistors
The research of slurry》The thick-film resistor paste with LSCO based materials as function phase composite inorganic Binder Phase is proposed in Master's thesis,
Its optimal average sheet resistance reaches 37K Ω/.It is above-mentioned using base metal oxide as the thick-film resistor paste of conductive filler in all add
Inorganic bond phase is added, electrical property decline can be caused, the defects such as sheet resistance, technology difficulty increase, cost increases are difficult to control to；And on
State larger as the sheet resistance of the thick-film resistor paste of conductive filler using base metal oxide, it is impossible to substitute noble metal thick-film resistor slurry
Material.Therefore, urgent need searching is a kind of need not add inorganic bond phase and the relatively low base metal thick-film resistor paste of sheet resistance value.
The content of the invention
A kind of defect that the present invention exists for background technology, it is proposed that thick-film resistor paste and preparation method thereof.This hair
Bright thick-film resistor paste is with low cost, sheet resistance is low, need not add inorganic bond phase, preparation process is simple, is a kind of function admirable
Thick-film resistor paste.
Technical scheme is as follows：
A kind of weight ratio of thick-film resistor paste, including function phase and organic carrier, function phase and organic carrier for (60~
90)：(40~10), wherein function phase are LSMO ceramic powders or LSCO ceramic powders, and the component of the LSMO ceramic powders includes La2O3、
SrCO3And MnO2, in molar ratio, La2O3：SrCO3：MnO2=1：(0.5~2)：(1~4), the component bag of the LSCO ceramic powders
Include La2O3、SrCO3And Co2O3, in molar ratio, La2O3：SrCO3：Co2O3=1：(0.5~3)：(1~4)；The organic carrier is each
Constituent mass percentage is：40wt%≤terpinol≤80wt%, 5wt%≤diethyl phthalate≤20wt%, 5wt%
≤ ATBC≤10wt%, 5wt%≤ethyl cellulose≤10wt%, 0wt%≤rilanit special≤5wt%,
0wt% ＜ Tween-80s≤5wt%, 0wt%≤lecithin≤5wt%.
Further, the weight ratio of function phase and organic carrier is 70：30.
Further, LSMO ceramic powders function phase each component mol ratio is La2O3：SrCO3：MnO2=1：(1~2)：(1~
3)；LSCO ceramic powder function phase each components mol ratio is La2O3：SrCO3：Co2O3=1：(1~3)：(1~3).
Further, LSMO ceramic powders function phase each component mol ratio is La2O3：SrCO3：MnO2=1：0.85：2.85；
LSCO ceramic powder function phase each components mol ratio is La2O3：SrCO3：Co2O3=1：2.66：1.66
Further, glass phase can also be added in the thick-film resistor paste, the glass each component weight ratio is
NaNO3：10~15%, H3BO3：10~25%, SiO2：15~35%, CaCO3：15~30%, Al2O3：10~25%, Bi2O3：
10~15%.
Present invention also offers a kind of preparation method of thick-film resistor paste, comprise the following steps：
1) prepared by ceramic powder：With La2O3、SrCO3And MnO2It is raw material, material molar ratio is La2O3：SrCO3：MnO2=1：
(0.5~2)：(1~4), or with La2O3、SrCO3And Co2O3It is raw material, material molar ratio is La2O3：SrCO3：Co2O3=1：
(0.5~3)：(1~4)；Raw material is inserted into ball milling 6~30 hours in ball mill, is dried, insert pre-burning in sintering furnace, pre-burning temperature
It is 650~850 DEG C to spend, and is incubated 2~4 hours；Powder after pre-burning is inserted into ball milling 6~30 hours in ball mill, is dried, obtained
LSMO ceramic powders or LSCO ceramic powders；
2) prepared by organic carrier：Proportioning weighs following raw materials according by mass percentage：40wt%≤terpinol≤80wt%,
5wt%≤diethyl phthalate≤20wt%, 5wt%≤ATBC≤10wt%, 5wt%≤ethyl cellulose
≤ 10wt%, 0wt%≤rilanit special≤5wt%, 0wt% ＜ Tween-80≤5wt%, 0wt%≤lecithin≤
5wt%, in 60~90 DEG C of water-bath dissolving a few hours, adjusts the content of ethyl cellulose, the viscosity of organic carrier is controlled 100
~200PaS；
3) ceramic powder and organic carrier are pressed into (60~90)：The weight of (40~10) is inserted in batch mixer and mixed than mixing,
Obtain the thick-film resistor paste.
Further, step 1) in La2O3、SrCO3And MnO2During for raw material, each material molar ratio is La2O3：SrCO3：
MnO2=1：(1~2)：(1~3)；With La2O3、SrCO3And Co2O3During for raw material, each material molar ratio is La2O3：SrCO3：
Co2O3=1：(1~3)：(1~3).
Further, step 1) in La2O3、SrCO3And MnO2During for raw material, each material molar ratio is La2O3：SrCO3：
MnO2=1：0.85：2.85；With La2O3、SrCO3And Co2O3During for raw material, each material molar ratio is La2O3：SrCO3：Co2O3=
1：2.66：1.66.
Further, step 3) in ceramic powder and organic carrier weight ratio be 70：30.
Further, by step 3) thick-film resistor paste for preparing bitten onto substrate by silk-screen printing, dried,
Insert in sintering furnace and sinter, sintering temperature is 750~1200 DEG C, is incubated 2~4h, you can obtain resistance thick film.
Beneficial effects of the present invention are：
1st, the thick-film resistor paste that the present invention is provided is with low cost compared with conventional precious metal thick-film resistor paste；And phase
For thick-film resistor pastes such as graphite, carbon fibers, its operating temperature is higher, is difficult to be oxidized, and stability more preferably, and can be
Sintered in air atmosphere and obtain thick-film resistor.
2nd, the thick-film resistor paste that the present invention is provided need not add inorganic bond and just can mutually realize sintering, preparation technology letter
Single, sheet resistance value is substantially reduced, with more excellent electrical property.
3rd, the resistance of thick-film resistor that resistance slurry of the present invention is prepared can reach 50~400 (Ω/), electrical conductivity and silver
Similar, alternative conventional precious metal thick film heating resistance slurry greatly reduces industrial cost.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of the LSMO thick-film resistors that the embodiment of the present invention 2 is obtained.
Specific embodiment
Embodiment 1
The weight ratio of a kind of LSMO thick-film resistor pastes, including function phase and organic carrier, function phase and organic carrier is
70：30, wherein function phase is LSMO ceramic powders, and the component of LSMO ceramic powders includes La2O3、SrCO3And MnO2, in molar ratio,
La2O3：SrCO3：MnO2=1：1.7：2.85；The organic carrier each component mass percent is：Terpinol 60wt%, adjacent benzene two
Formic acid diethylester 10wt%, ATBC 10wt%, ethyl cellulose 10wt%, rilanit special 4wt%, poly- sorb
The 4wt% of ester -80, lecithin 2wt%.
The preparation method of above-mentioned LSMO thick-film resistor pastes, comprises the following steps：
1) prepared by LSMO ceramic powders：Proportioning weighs following raw materials according in molar ratio：La2O3：SrCO3：MnO2=1：1.7：2.85,
By La2O3、SrCO3And MnO2Well mixed, wet ball grinding 24h is dried；Pre-burning in sintering furnace is placed in, calcined temperature is 800 DEG C,
Insulation 2 hours；Powder after pre-burning wet ball grinding 24h again, dries；Crushing, the levigate, eye mesh screen of ultrasonic mistake 300；
2) prepared by organic carrier：Proportioning weighs following raw materials according by mass percentage：Terpinol 60wt%, phthalic acid two
Ethyl ester 10wt%, ATBC 10wt%, ethyl cellulose 10wt%, rilanit special 4wt%, Tween-80
4wt%, lecithin 2wt%；12h is mixed under 80 DEG C of water bath conditions, is cooled down；
3) LSMO ceramic powders and organic carrier are pressed 70：30 weight inserts ball milling 24h in ball mill than mixing, obtains
The LSMO thick-film resistor pastes.
4) by step 3) the LSMO thick-film resistor pastes that obtain are bitten onto substrate by silk-screen printing, inserted in sintering furnace
Sintering, sintering temperature is 1200 DEG C, and soaking time 2h obtains LSMO thick-film resistors.
To LSMO thick-film resistors sample test obtained above, performance is as follows：
Sheet resistance：≥200Ω/□
Viscosity：125~200PaS
Linear resolution：200μm
Sintering thickness：10~16 μm
Initial adhesion：≥20.3N.
Embodiment 2
The weight ratio of a kind of LSMO thick-film resistor pastes, including function phase and organic carrier, function phase and organic carrier is
70：30, wherein function phase is LSMO ceramic powders, and the component of LSMO ceramic powders includes La2O3、SrCO3And MnO2, in molar ratio,
La2O3：SrCO3：MnO2=1：0.85：2.85；The organic carrier each component mass percent is：Terpinol 55wt%, adjacent benzene
Dicarboxylate 10wt%, ATBC 10wt%, ethyl cellulose 10wt%, rilanit special 5wt%, poly- sorb
The 5wt% of ester -80, lecithin 5wt%.
The preparation method of above-mentioned LSMO thick-film resistor pastes, comprises the following steps：
1) prepared by LSMO ceramic powders：Proportioning weighs following raw materials according in molar ratio：La2O3：SrCO3：MnO2=1：0.85：
2.85, by La2O3、SrCO3And MnO2Well mixed, wet ball grinding 24h is dried；Pre-burning in sintering furnace is placed in, calcined temperature is
800 DEG C, it is incubated 2 hours；Powder after pre-burning wet ball grinding 24h again, dries；Crushing, the levigate, eye mesh screen of ultrasonic mistake 300；
2) prepared by organic carrier：Proportioning weighs following raw materials according by mass percentage：Terpinol 55wt%, phthalic acid two
Ethyl ester 10wt%, ATBC 10wt%, ethyl cellulose 10wt%, rilanit special 5wt%, Tween-80
5wt%, lecithin 5wt%；12h is mixed under 80 DEG C of water bath conditions, is cooled down；
3) LSMO ceramic powders and organic carrier are pressed 70：30 weight inserts ball milling 24h in ball mill than mixing, obtains
The LSMO thick-film resistor pastes.
4) by step 3) the LSMO thick-film resistor pastes that obtain are bitten onto substrate by silk-screen printing, inserted in sintering furnace
Sintering, sintering temperature is 1100 DEG C, and soaking time 2h obtains LSMO thick-film resistors.
To LSMO thick-film resistors sample test obtained above, performance is as follows：
Sheet resistance：≥50Ω/□
Viscosity：125~200PaS
Linear resolution：200μm
Sintering thickness：10~16 μm
Initial adhesion：≥20.3N.
Fig. 1 is the scanning electron microscope (SEM) photograph of the LSMO thick-film resistors that embodiment 2 is obtained, as shown in Figure 1, the thickness that embodiment 2 is obtained
Film resistance surface is three-dimensional chain structure, and particle size is nanoscale, with good electric conductivity.
Embodiment 3
The weight ratio of a kind of LSCO thick-film resistor pastes, including function phase and organic carrier, function phase and organic carrier is
60：40, wherein function phase is LSCO ceramic powders, and the component of LSCO ceramic powders includes La2O3、SrCO3And Co2O3, in molar ratio,
La2O3：SrCO3：Co2O3=1：2.66：1.66；The organic carrier each component mass percent is：Terpinol 70wt%, adjacent benzene
Dicarboxylate 10wt%, ATBC 5wt%, ethyl cellulose 10wt%, Tween-80 5wt%.
The preparation method of above-mentioned LSCO thick-film resistor pastes, comprises the following steps：
1) prepared by LSCO ceramic powders：Proportioning weighs following raw materials according in molar ratio：La2O3：SrCO3：Co2O3=1：2.66：
1.66, by La2O3、SrCO3And Co2O3Well mixed, wet ball grinding 24h is dried；Pre-burning in sintering furnace is placed in, calcined temperature is
700 DEG C, it is incubated 2 hours；Powder after pre-burning wet ball grinding 24h again, dries；Crushing, the levigate, eye mesh screen of ultrasonic mistake 300；
2) prepared by organic carrier：Proportioning weighs following raw materials according by mass percentage：Terpinol 70wt%, phthalic acid two
Ethyl ester 10wt%, ATBC 5wt%, ethyl cellulose 10wt%, Tween-80 5wt%；In 80 DEG C of water-bath bars
12h is mixed under part, is cooled down；
3) LSCO ceramic powders and organic carrier are pressed 60：40 weight inserts ball milling 24h in ball mill than mixing, obtains
The LSCO thick-film resistor pastes.
4) by step 3) the LSCO thick-film resistor pastes that obtain are bitten onto substrate by silk-screen printing, inserted in sintering furnace
Sintering, sintering temperature is 800 DEG C, and soaking time 2h obtains LSCO thick-film resistors.
Sheet resistance：≥400Ω/□
Viscosity：125~200PaS
Linear resolution：200μm
Sintering thickness：10~16 μm
Initial adhesion：≥20.3N.
Embodiment 4
The weight ratio of a kind of LSCO thick-film resistor pastes, including function phase and organic carrier, function phase and organic carrier is
70：30, wherein function phase is LSCO ceramic powders, and the component of LSCO ceramic powders includes La2O3、SrCO3And Co2O3, in molar ratio,
La2O3：SrCO3：Co2O3=1：1：2；The organic carrier each component mass percent is：Terpinol 70wt%, phthalic acid
Diethylester 5wt%, ATBC 5wt%, ethyl cellulose 10wt%, rilanit special 4wt%, Tween-80
4wt%, lecithin 2wt%.
The preparation method of above-mentioned LSCO thick-film resistor pastes, comprises the following steps：
1) prepared by LSCO ceramic powders：Proportioning weighs following raw materials according in molar ratio：La2O3：SrCO3：Co2O3=1：1：2, will
La2O3、SrCO3And Co2O3Well mixed, wet ball grinding 24h is dried；Pre-burning in sintering furnace is placed in, calcined temperature is 800 DEG C, is protected
Temperature 2 hours；Powder after pre-burning wet ball grinding 24h again, dries；Crushing, the levigate, eye mesh screen of ultrasonic mistake 300；
2) prepared by organic carrier：Components by weight percentage weighs following raw materials according：Terpinol 70wt%, phthalic acid two
Ethyl ester 5wt%, ATBC 5wt%, ethyl cellulose 10wt%, rilanit special 4wt%, Tween-80
4wt%, lecithin 2wt%；12h is mixed under 80 DEG C of water bath conditions, is cooled down；
3) LSCO ceramic powders and organic carrier are pressed 70：30 weight inserts ball milling 24h in ball mill than mixing, obtains
The LSCO thick-film resistor pastes.
4) by step 3) the LSCO thick-film resistor pastes that obtain are bitten onto substrate by silk-screen printing, inserted in sintering furnace
Sintering, sintering temperature is 1100 DEG C, and soaking time 2h obtains LSCO thick-film resistors.
Claims (8)
1. a kind of thick-film resistor paste, is made up of function phase and organic carrier, the weight ratio of function phase and organic carrier for (60~
90)：(40~10), wherein function phase are LSMO ceramic powders or LSCO ceramic powders, and the component of the LSMO ceramic powders includes La2O3、
SrCO3And MnO2, in molar ratio, La2O3：SrCO3：MnO2=1：(0.5~2)：(1~4), the component bag of the LSCO ceramic powders
Include La2O3、SrCO3And Co2O3, in molar ratio, La2O3：SrCO3：Co2O3=1：(0.5~3)：(1~4)；The organic carrier is each
Constituent mass percentage is：40wt%≤terpinol≤80wt%, 5wt%≤diethyl phthalate≤20wt%, 5wt%
≤ ATBC≤10wt%, 5wt%≤ethyl cellulose≤10wt%, 0wt%≤rilanit special≤5wt%,
0wt% ＜ Tween-80s≤5wt%, 0wt%≤lecithin≤5wt%, and organic carrier each component mass percent sum
It is 100%.
2. thick-film resistor paste according to claim 1, it is characterised in that the weight ratio of function phase and organic carrier is
70：30.
3. thick-film resistor paste according to claim 1, it is characterised in that LSMO ceramic powder function phase each component mol ratios
It is La2O3：SrCO3：MnO2=1：(1~2)：(1~3)；LSCO ceramic powder function phase each components mol ratio is La2O3：SrCO3：
Co2O3=1：(1~3)：(1~3).
4. thick-film resistor paste according to claim 1, it is characterised in that LSMO ceramic powder function phase each component mol ratios
It is La2O3：SrCO3：MnO2=1：0.85：2.85；LSCO ceramic powder function phase each components mol ratio is La2O3：SrCO3：Co2O3=
1：2.66：1.66.
5. a kind of preparation method of thick-film resistor paste as claimed in claim 1, comprises the following steps：
1) prepared by ceramic powder：With La2O3、SrCO3And MnO2It is raw material, material molar ratio is La2O3：SrCO3：MnO2=1：(0.5~
2)：(1~4), or with La2O3、SrCO3And Co2O3It is raw material, material molar ratio is La2O3：SrCO3：Co2O3=1：(0.5~
3)：(1~4)；Raw material is inserted into ball milling 6~30 hours in ball mill, is dried, insert pre-burning in sintering furnace, calcined temperature is 650
~850 DEG C, it is incubated 2~4 hours；Powder after pre-burning is inserted into ball milling 6~30 hours in ball mill, is dried, obtain LSMO potteries
Porcelain powder or LSCO ceramic powders；
2) prepared by organic carrier：Proportioning weighs following raw materials according by mass percentage：40wt%≤terpinol≤80wt%, 5wt%
≤ diethyl phthalate≤20wt%, 5wt%≤ATBC≤10wt%, 5wt%≤ethyl cellulose≤
10wt%, 0wt%≤rilanit special≤5wt%, 0wt% ＜ Tween-80≤5wt%, 0wt%≤lecithin≤
5wt%, in 60~90 DEG C of water-bath dissolving a few hours, adjusts the content of ethyl cellulose, the viscosity of organic carrier is controlled 100
~200PaS；
3) ceramic powder and organic carrier are pressed into (60~90)：The weight of (40~10) is inserted in batch mixer and mixed than mixing, is obtained
The thick-film resistor paste.
6. the preparation method of thick-film resistor paste according to claim 5, it is characterised in that step 1) in La2O3、
SrCO3And MnO2During for raw material, each material molar ratio is La2O3：SrCO3：MnO2=1：(1~2)：(1~3)；With La2O3、SrCO3
And Co2O3During for raw material, each material molar ratio is La2O3：SrCO3：Co2O3=1：(1~3)：(1~3).
7. the preparation method of thick-film resistor paste according to claim 5, it is characterised in that step 1) in La2O3、
SrCO3And MnO2During for raw material, each material molar ratio is La2O3：SrCO3：MnO2=1：0.85：2.85；With La2O3、SrCO3With
Co2O3During for raw material, each material molar ratio is La2O3：SrCO3：Co2O3=1：2.66：1.66.
8. the preparation method of thick-film resistor paste according to claim 5, it is characterised in that step 3) in ceramic powder and have
The weight ratio of airborne body is 70：30.
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| CN1937856B (en) * | 2006-07-28 | 2010-12-15 | 王克政 | Rare earth basic-metal resistance size for metal base board based rare earth thick film circuit and its preparing process |
| CN101727997A (en) * | 2008-10-23 | 2010-06-09 | 银锐明 | YBCO thick film resistor slurry |
| CN101826377B (en) * | 2010-03-31 | 2011-05-04 | 桂林电子科技大学 | Thick film thermistor slurry, preparation method thereof and thick film thermistor |
| CN101923911B (en) * | 2010-04-27 | 2011-11-02 | 电子科技大学 | YBCO thick film resistance paste based on stainless steel base board and preparation method thereof |
| CN102005273B (en) * | 2010-09-30 | 2012-08-08 | 桂林电子科技大学 | High-performance lead-free negative temperature coefficient temperature-sensitive thick film and preparation method thereof |
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