CN118039271A - Thermistor slurry and preparation method thereof - Google Patents

Thermistor slurry and preparation method thereof Download PDF

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Publication number
CN118039271A
CN118039271A CN202211369301.2A CN202211369301A CN118039271A CN 118039271 A CN118039271 A CN 118039271A CN 202211369301 A CN202211369301 A CN 202211369301A CN 118039271 A CN118039271 A CN 118039271A
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China
Prior art keywords
thermistor
content
slurry
functional ceramic
ceramic powder
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Pending
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CN202211369301.2A
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Chinese (zh)
Inventor
韩蕊
林聪毅
倪德峰
李琪
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Shanghai Sansi Technology Co Ltd
Shanghai Sansi Electronic Engineering Co Ltd
Jiashan Sansi Photoelectric Technology Co Ltd
Pujiang Sansi Optoelectronics Technology Co Ltd
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Shanghai Sansi Technology Co Ltd
Shanghai Sansi Electronic Engineering Co Ltd
Jiashan Sansi Photoelectric Technology Co Ltd
Pujiang Sansi Optoelectronics Technology Co Ltd
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Application filed by Shanghai Sansi Technology Co Ltd, Shanghai Sansi Electronic Engineering Co Ltd, Jiashan Sansi Photoelectric Technology Co Ltd, Pujiang Sansi Optoelectronics Technology Co Ltd filed Critical Shanghai Sansi Technology Co Ltd
Priority to CN202211369301.2A priority Critical patent/CN118039271A/en
Publication of CN118039271A publication Critical patent/CN118039271A/en
Pending legal-status Critical Current

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Abstract

The invention provides a thermistor slurry and a preparation method thereof, wherein the thermistor slurry comprises functional ceramic powder, glass powder and an organic carrier; the content of the functional ceramic powder is 15-25 wt%, the content of the glass powder is 35-45 wt% and the content of the organic carrier is 30-50 wt% based on the total weight of the thermistor slurry. The thermistor formed by the technology has the advantages of no lead, adjustable resistance, good repeatability, low cost, convenience for large-scale industrial production and the like, and has a wide application prospect.

Description

Thermistor slurry and preparation method thereof
Technical Field
The invention relates to electronic paste, in particular to thermistor paste and a preparation method thereof.
Background
In the prior art, the thermistor is mainly manufactured by a granulation powder compression molding process, the production efficiency of the process is low, the production cost is high, and the target product is related to the size of a die and the tonnage of a press. Because the size of the die is fixed, the size of the obtained thermistor product is also fixed, if the size of the thermistor product needs to be adjusted, the size of the thermistor product can be only adjusted by changing the die, the larger the size of the product is, the larger the tonnage of the required press is, the higher the price is, the production cost is greatly increased due to the factors, and the application of the thermistor product in production is limited to a certain extent.
Disclosure of Invention
In view of the above-mentioned drawbacks of the prior art, an object of the present invention is to provide a thermistor slurry and a preparation method thereof, which are used for solving the problem of high cost caused by the limitation of a die and other factors on a product obtained by a granulation powder compression molding process in the prior art.
To achieve the above and other related objects, the present invention is achieved by the following technical means.
The invention provides a thermistor slurry, which comprises functional ceramic powder, glass powder and an organic carrier; the content of the functional ceramic powder is 15-25 wt%, the content of the glass powder is 35-45 wt% and the content of the organic carrier is 30-50 wt% based on the total weight of the thermistor slurry.
According to the technical scheme, the functional ceramic powder comprises a main material and an additive, wherein the main material comprises BaCO 3 and TiO 2, and the additive is one or more selected from SrCO3、PbO、Y2O3、Nb2O5、Sb2O3、La2O3、Bi2O3、MnCO3 and CuO.
In the technical scheme of the invention, srCO 3 and PbO are used as peak shifting agents in a system, and when the SrCO 3 and the PbO are not added, the Curie temperature Tc of the prepared thermistor is 120 ℃; the Curie temperature Tc of the thermistor can be reduced to be lower than 120 ℃ by adding SrCO 3, and the more the addition amount of SrCO 3 is, the smaller the Tc is; conversely, the greater the amount of PbO added, the higher the Tc. Proper addition of Y 2O3、Nb2O5、Sb2O3、La2O3 and Nb 2O5 can result in good PTC effect for thermistors.
According to the technical scheme of the invention, the total weight of the functional ceramic powder is taken as a reference, the weight percentage of the main material is 85-99 wt%, and the sum of the weight percentages of the additives is 1-15 wt%.
According to the technical scheme of the invention, the grain size of the main material is 1-2 mu m.
According to the technical scheme of the invention, the particle size of the additive is less than 1 mu m.
According to the technical scheme of the invention, the functional ceramic powder is obtained by a method comprising the following steps: and (3) performing curing reaction on the main material at 1100-1300 ℃ to obtain BaTiO 3 powder, and ball-milling and mixing the BaTiO 3 powder and the additive. Preferably, a drying step is also included after ball milling.
According to the technical scheme, the total mass of the glass powder is taken as a reference, the content of bismuth oxide in the glass powder is 35-68 wt%, the content of boron oxide is 8-36 wt%, the content of silicon dioxide is 0.5-6.0 wt%, the content of zinc oxide is 5.0-22.0 wt%, the content of cobaltous oxide is 0.1-3.0 wt%, and the content of titanium dioxide is 0.5-4.0 wt%. According to the technical scheme, the glass powder also contains copper oxide with the weight percent of not more than 5 percent.
According to the technical scheme, the glass powder also contains not more than 3.5 weight percent of aluminum oxide.
According to the technical scheme, the glass powder also contains not more than 0.8 weight percent of magnesium oxide.
The glass powder plays a role in dispersing a conductive phase in slurry, and plays a role in combining a substrate in a thermistor after sintering.
According to the technical scheme of the invention, the raw material components of the organic carrier comprise resin, solvent and organic additive; the resin content is 8-15 wt%, the solvent content is 80-90 wt% and the organic additive content is 1-5 wt% based on the total weight of the raw material components of the organic carrier.
The solvent in the organic carrier is usually a relatively viscous liquid organic matter, and the molecule of the solvent usually contains polar groups, so that the solvent can dissolve resin, and the solvent usually has a relatively high boiling point and is not easy to volatilize at normal temperature.
According to the technical scheme of the invention, the resin enables the electronic paste to have certain viscosity. The resin is one or more selected from modified cellulose and epoxy resin. Preferably, the modified cellulose is selected from polyanionic celluloses. Specifically, the polyanionic cellulose is sodium carboxymethyl cellulose.
According to the technical scheme, the solvent is selected from one or more of terpineol, butyl carbitol, tributyl citrate and butyl carbitol acetate.
According to the technical scheme of the invention, the organic additive comprises a dispersing agent, a lubricating agent, a thixotropic agent and a rheological agent. Preferably, the dispersing agent is lecithin. Preferably, the dispersant is 1.5 to 2.5wt%.
Preferably, the lubricant is lauric acid. Preferably, the lubricant is 1 to 2wt%.
Preferably, the thixotropic agent is a polyethylene wax or hydrogenated castor oil. Preferably, the thixotropic agent is 1 to 2wt%.
Preferably, the rheological agent is 1,4 butyrolactone. Preferably, the rheology agent is 0.1 to 0.5wt%.
According to the technical scheme of the invention, the organic carrier is obtained by uniformly mixing the raw material components. More preferably, the organic carrier is obtained by a method comprising the steps of: and completely dissolving the resin in the solvent, and then adding the organic additive to mix uniformly.
The organic carrier is used for dispersing functional ceramic powder and glass powder, providing basic rheological property of slurry, meeting the technological requirements of slurry printing, drying and the like, and no residue exists in the thermistor after firing.
For PTC thermistor slurry, the square resistance value can be controlled and regulated by regulating the proportion between the functional ceramic powder and the glass powder. But the ratio between the two is not arbitrarily adjustable. Such as: when the content of the functional ceramic powder is lower than a certain content, the prepared thick film thermistor loses the thermosensitive property; the cost can be greatly increased if the functional ceramic powder is higher than a certain content; the glass powder content is larger than a certain range, so that the resistance value of the element is large and the performance is deteriorated; the glass powder content is smaller than a certain range, so that the glass powder cannot be bonded, and the glass powder are mutually restricted and can be regulated only in a certain range.
The invention also discloses a preparation method of the thermistor slurry, which is characterized in that the functional ceramic powder, the glass powder and the organic carrier are uniformly mixed, and the thermistor slurry is obtained through rolling.
The invention also discloses a thermistor, which is obtained by adopting the thermistor slurry through molding, sintering and metallization.
The thermistor formed by the technology has the advantages of no lead, adjustable resistance, good repeatability, low cost, convenience for large-scale industrial production and the like, and has a wide application prospect.
Detailed Description
Further advantages and effects of the present invention will become apparent to those skilled in the art from the disclosure of the present invention, which is described by the following specific examples.
Before the embodiments of the invention are explained in further detail, it is to be understood that the invention is not limited in its scope to the particular embodiments described below; it is also to be understood that the terminology used in the examples of the invention is for the purpose of describing particular embodiments only, and is not intended to limit the scope of the invention. The test methods in the following examples, in which specific conditions are not noted, are generally conducted under conventional conditions or under conditions recommended by the respective manufacturers.
Where numerical ranges are provided in the examples, it is understood that unless otherwise stated herein, both endpoints of each numerical range and any number between the two endpoints are significant both in the numerical range. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In addition to the specific methods, devices, materials used in the embodiments, any methods, devices, and materials of the prior art similar or equivalent to those described in the embodiments of the present invention may be used to practice the present invention according to the knowledge of one skilled in the art and the description of the present invention.
In the thermistor slurries of specific embodiments 1 to 5 of the present application, the functional ceramic powder was 25wt%, 40wt% glass frit, and 35% organic vehicle. The formulations of the functional ceramic powder and the thermistor paste in each example are shown in table 1.
TABLE 1
The thermistor slurry formed in examples 1 to 5 was formed on the surface of the resistor substrate by a screen printing process to a thickness of 10 to 50 μm, and dried and sintered to form a thermistor. Specifically, the sintering temperature is 800-1200 ℃ and the sintering time is 10-120 min.
The results of the performance test of the thermistor are also shown in table 1.
The Tc test method is a Curie temperature experiment:
(1) The thermistor is welded on the PCB in series, and leads are connected at two ends of each thermistor;
(2) The thermistor is placed in the oven, and the leading-out end is placed outside the oven;
(3) Raising the temperature of the box body to the lower limit of the Curie temperature minus 1 ℃ and keeping for 30min, and measuring the thermistor by using a universal meter; resistance value;
(4) Raising the temperature of the box body to the upper limit of the Curie temperature and keeping the temperature for 30min, and measuring the resistance of the thermistor by using a universal meter;
(5) Judging whether the initial resistance value of 2 times is within the range of the resistance value measured at the upper limit temperature and the lower limit temperature;
Note that: the effect of air flow should be minimized during the test.
The testing method or the calculating method of the R25 change rate comprises the following steps: (R25 after sintering-R25 before sintering) ×100%/R25 before sintering.
The resistance value adjusting mode and mechanism are as follows:
1. The PTC area is fixed, and the resistance value can be flexibly adjusted by adjusting the area of the ohmic silver paste;
2. The ohmic silver paste area is fixed, and the resistance value can be adjusted by adjusting the PTC area and shape;
3. Resistance calculation formula: r=ρl/S, where ρ is the resistivity of the conductor, L is the length of the conductor, and S is the cross-sectional area of the conductor (electrode paste area).
The PTC paste printing area or the ohmic electrode area can be adjusted flexibly to adjust the resistance of the thermistor, the precision and the quality stability of the resistance are improved, the yield of preparing the target resistance is improved, the material usage amount (the thickness is reduced, the thickness is generally 10-50 micrometers, and the conventional dry pressing process is about 2 mm) required by producing the resistor is reduced, and the PTC paste is compatible with the new-era environment-friendly production concept.
The above embodiments are merely illustrative of the principles of the present invention and its effectiveness, and are not intended to limit the invention. Modifications and variations may be made to the above-described embodiments by those skilled in the art without departing from the spirit and scope of the invention. Accordingly, it is intended that all equivalent modifications and variations of the invention be covered by the claims, which are within the ordinary skill of the art, be within the spirit and scope of the present disclosure.

Claims (10)

1. The thermistor slurry is characterized by comprising functional ceramic powder, glass powder and an organic carrier; the content of the functional ceramic powder is 15-25 wt%, the content of the glass powder is 35-45 wt% and the content of the organic carrier is 30-50 wt% based on the total weight of the thermistor slurry.
2. The thermistor paste according to claim 1, characterized in that the functional ceramic powder comprises a main material and an additive, the main material comprises BaCO 3 and TiO 2, and the additive is one or more selected from SrCO3、PbO、Y2O3、Nb2O5、Sb2O3、La2O3、Bi2O3、MnCO3 and CuO.
3. The thermistor paste according to claim 2, characterized in that the weight percentage of the main material is 85-99 wt% and the sum of the weight percentages of the additives is 1-15 wt% based on the total weight of the functional ceramic powder.
4. The thermistor paste according to claim 1, characterized in that the content of bismuth oxide in the glass frit is 35 to 68wt%, the content of boron oxide is 8 to 36wt%, the content of silicon dioxide is 0.5 to 6.0wt%, the content of zinc oxide is 5.0 to 22.0wt%, the content of cobalt trioxide is 0.1 to 3.0wt%, and the content of titanium dioxide is 0.5 to 4.0wt%, based on the total mass of the glass frit.
5. The thermistor paste of claim 4, comprising one or more of the following features:
The glass powder also contains copper oxide with the weight percentage of not more than 5 percent;
The glass powder also contains not more than 3.5 weight percent of aluminum oxide;
the glass powder also contains not more than 0.8wt% of magnesium oxide.
6. The thermistor paste according to claim 1, characterized in that the raw material components of the organic carrier contain a resin, a solvent and an organic additive; the resin content is 8-15 wt%, the solvent content is 80-90 wt% and the organic additive content is 1-5 wt% based on the total weight of the raw material components of the organic carrier.
7. The thermistor paste of claim 6, comprising one or more of the following features:
the resin is one or more selected from modified cellulose and epoxy resin;
The solvent is selected from one or more of terpineol, butyl carbitol, tributyl citrate and butyl carbitol acetate;
the organic additives include dispersants, lubricants, thixotropic agents, and rheological agents.
8. The thermistor paste of claim 7, comprising one or more of the following features:
the dispersing agent is lecithin;
The dispersant is 1.5-2.5 wt%;
The lubricant is lauric acid;
the weight of the lubricant is 1-2wt%;
The thixotropic agent is polyethylene wax or hydrogenated castor oil;
the thixotropic agent is 1-2wt%;
the rheological agent is 1, 4-butyrolactone;
the rheological agent is 0.1 to 0.5 weight percent.
9. A method for preparing the thermistor slurry according to any one of claims 1 to 8, wherein the functional ceramic powder, the glass frit and the organic carrier are uniformly mixed, and the thermistor slurry is obtained by rolling.
10. A thermistor, characterized in that the thermistor is obtained by adopting the thermistor slurry according to any one of claims 1 to 8 through molding, sintering and metallization.
CN202211369301.2A 2022-11-03 2022-11-03 Thermistor slurry and preparation method thereof Pending CN118039271A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202211369301.2A CN118039271A (en) 2022-11-03 2022-11-03 Thermistor slurry and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202211369301.2A CN118039271A (en) 2022-11-03 2022-11-03 Thermistor slurry and preparation method thereof

Publications (1)

Publication Number Publication Date
CN118039271A true CN118039271A (en) 2024-05-14

Family

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Family Applications (1)

Application Number Title Priority Date Filing Date
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Country Status (1)

Country Link
CN (1) CN118039271A (en)

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