CN117342797A - Gold electrode glass powder, preparation method, gold electrode slurry and NTC thermistor - Google Patents

Gold electrode glass powder, preparation method, gold electrode slurry and NTC thermistor Download PDF

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Publication number
CN117342797A
CN117342797A CN202311288764.0A CN202311288764A CN117342797A CN 117342797 A CN117342797 A CN 117342797A CN 202311288764 A CN202311288764 A CN 202311288764A CN 117342797 A CN117342797 A CN 117342797A
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gold electrode
glass powder
ntc thermistor
glass
phosphate
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柏小海
谢远富
梁银
练明辉
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Exsense Electronics Technology Co ltd
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Exsense Electronics Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C12/00Powdered glass; Bead compositions
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01CRESISTORS
    • H01C1/00Details
    • H01C1/14Terminals or tapping points or electrodes specially adapted for resistors; Arrangements of terminals or tapping points or electrodes on resistors
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01CRESISTORS
    • H01C7/00Non-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
    • H01C7/04Non-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

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  • Engineering & Computer Science (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Electromagnetism (AREA)
  • Glass Compositions (AREA)

Abstract

The invention belongs to the technical field of NTC thermistors, and relates to gold electrode glass powder, a preparation method, gold electrode slurry and an NTC thermistor. The glass powder consists of the following components in percentage by mass: bi (Bi) 2 O 3 20%‑60%、B 2 O 3 20%‑40%、CuO 15%‑35%、Li 2 2% -10% of O. In the formula of the NTC thermistor gold electrode glass powder, the original Si element is replaced by the B element, the melting point of the B element is lower than that of the Si element, and the melting point of a glass powder system is about 650-670 ℃, so that the melting point of gold electrode paste glass powder is reduced, meanwhile, the gold electrode paste is stable, good in performance and difficult to process, and the gold electrode paste is difficult to be well adapted to NTC ceramic materials.

Description

Gold electrode glass powder, preparation method, gold electrode slurry and NTC thermistor
Technical Field
The invention relates to the technical field of NTC thermistors, in particular to gold electrode glass powder, a preparation method, gold electrode slurry and an NTC thermistor.
Background
The NTC thermistor is a resistor and is made by covering a layer of electrode slurry on a porcelain body. Unlike a general resistor, the resistance value of the NTC thermistor may vary with a change in temperature. It has the following characteristics: the temperature sensitivity coefficient is large, the volume is small, the response time is short, and the like.
The gold electrode paste is one of the NTC thermistor electrode pastes. Glass frit is one of the base materials of gold electrode paste, and the melting point of the common glass frit is too high at present, so that the processing is difficult, and the gold electrode paste is difficult to be well adapted to NTC ceramic materials.
Disclosure of Invention
The invention aims to provide gold electrode glass powder, a preparation method, gold electrode slurry and an NTC thermistor, which can skillfully solve the problems.
The invention discloses NTC thermistor gold electrode glass powder, which comprises the following components in percentage by mass:
optionally, the glass frit is composed of the following components in mass percent:
optionally, the glass frit is composed of the following components in mass percent:
optionally, the glass frit is composed of the following components in mass percent:
the invention also discloses a preparation method of the NTC thermistor gold electrode glass powder, which is used for preparing the gold electrode glass powder according to any one of the above steps, and is characterized in that the preparation method comprises the following steps:
weighing the components of the gold electrode glass powder according to any proportion, and uniformly mixing to obtain a mixed raw material;
smelting the mixed raw materials at a high temperature of 650-670 ℃ to obtain a glass solution;
quenching the glass solution in water to obtain glass particles;
ball milling, drying and sieving the glass particles to obtain the gold electrode glass powder.
Optionally, the smelting temperature of the high temperature smelting mixed feed material is 650 ℃.
The invention also discloses NTC thermistor gold electrode slurry, which consists of the following components in percentage by mass:
wherein the glass powder is any one of the glass powders.
Optionally, the organic carrier is composed of the following components in mass percent:
20-30% of organic resin
1 to 5 percent of dispersing agent
The balance of organic solvent.
Optionally, the organic resin is ethylcellulose; the dispersing agent is one or more of ammonium polymethacrylate, NP phosphate (nonylphenol polyether phosphate), 600 phosphate, TSP phosphate (styryl polyether phosphate) and AEO-9 phosphate (fatty alcohol ether phosphate); the organic solvent is one or more of terpineol, diethylene glycol butyl ether acetate, octanol, benzyl alcohol, dibutyl phthalate and dimethyl diformate.
The invention also discloses an NTC thermistor which comprises a gold electrode, wherein the gold electrode comprises the gold electrode glass powder.
In the formula of the NTC thermistor gold electrode glass powder, the original Si element is replaced by the B element, the melting point of the B element is lower than that of the Si element, and the melting point of a glass powder system is about 650-670 ℃, so that the melting point of gold electrode paste glass powder is reduced, meanwhile, the gold electrode paste is stable, good in performance and difficult to process, and the gold electrode paste is difficult to be well adapted to NTC ceramic materials.
Detailed Description
It is to be understood that the terminology used herein, the specific structural and functional details disclosed are merely representative for the purpose of describing particular embodiments, but that the invention may be embodied in many alternate forms and should not be construed as limited to only the embodiments set forth herein.
The invention is described in detail below with reference to alternative embodiments.
As an embodiment of the present invention, an NTC thermistor gold electrode glass frit is disclosed, which is composed of the following components in mass percent: bi (Bi) 2 O 3 20%-60%、B 2 O 3 20%-40%、CuO 15%-35%、Li 2 O 2%-10%。
In the formula of the NTC thermistor gold electrode glass powder, the original Si element is replaced by the B element, the melting point of the B element is lower than that of the Si element, and the melting point of a glass powder system is about 650-670 ℃, so that the melting point of gold electrode paste glass powder is reduced, meanwhile, the gold electrode paste is stable, good in performance and difficult to process, and the gold electrode paste is difficult to be well adapted to NTC ceramic materials.
Specifically, bi 2 O 3 May be 20%, 25%, 30%, 35%, 40%, 45%, 50%, 55%, 60%. B (B) 2 O 3 The ratio of (2) may be 20%, 25%, 30%, 35%, 40%. The CuO may be 15%, 20%, 25%, 30%, 35%. Li (Li) 2 The O may be 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%.
Specifically, the glass powder comprises the following components in percentage by massThe method comprises the following steps: bi (Bi) 2 O 3 40%-50%、B 2 O 3 25%-35%、CuO 17%-30%、Li 2 O5-8%. More specifically, bi 2 O 3 May be 40%, 42%, 44%, 46%, 48%, 50%. B (B) 2 O 3 The ratio of (2) may be 25%, 27%, 30%, 32%, 35%. The CuO may be 17%, 19%, 20%, 22%, 25%, 27%, 30%. Li (Li) 2 The O may be 5%, 5.5%, 6%, 6.5%, 7%, 7.5%, 8%.
In one embodiment, the glass frit is composed of the following components in percentage by mass: bi (Bi) 2 O 3 20%、B 2 O 3 40%、CuO 30%、Li 2 O10%. In another embodiment, the glass frit is composed of the following components in mass percent: bi (Bi) 2 O 3 60%、B 2 O 3 20%、CuO 15%、Li 2 O5%。
The invention also discloses a preparation method of the NTC thermistor gold electrode glass powder, which is used for preparing the gold electrode glass powder, and specifically comprises the following steps:
weighing the components of the gold electrode glass powder according to any proportion, and uniformly mixing to obtain a mixed raw material;
s100: smelting the mixed raw materials at a high temperature of 650-670 ℃ to obtain a glass solution;
s200: quenching the glass solution in water to obtain glass particles;
s300: ball milling, drying and sieving the glass particles to obtain the gold electrode glass powder.
In the formula of the NTC thermistor gold electrode glass powder prepared by the preparation method, the original Si element is replaced by the B element, the melting point of the B element is lower than that of the Si element, and the melting point of a glass powder system is about 650-670 ℃, so that the melting point of gold electrode paste glass powder is reduced, meanwhile, the gold electrode paste is stable, the performance is good, the processing difficulty is reduced, and the gold electrode paste is difficult to be better adapted to NTC ceramic materials.
Specifically, in step S100, the high-temperature melting of the mixed raw materials may be performed at 650 ℃, 655 ℃, 660 ℃, 665 ℃, 670 ℃ depending on the ratio of the components of the mixed raw materials. Preferably, the smelting temperature of the high-temperature smelting mixed raw material can be 670 ℃, so that the mixed raw material is ensured to be sufficiently melted. In step S100, the step of high-temperature smelting the mixed raw material includes: the mixed raw materials are kept at 700-780 ℃ for 0.6-1.5h. The heat preservation time can be 0.6h, 0.7h, 0.8h, 0.9h, 1h, 1.1h, 1.2h, 1.3h, 1.4h and 1.5h. Preferably, the incubation time is 1h.
In the step S300, the drying temperature is 60-80deg.C, specifically 60 deg.C, 65 deg.C, 70 deg.C, 75 deg.C, 80 deg.C.
The invention also discloses NTC thermistor gold electrode slurry, which consists of the following components in percentage by mass: 70-80% of gold powder, 2-10% of glass powder, 1-3% of glassy carbon and 15-20% of organic carrier. Wherein the glass powder is any one of the glass powder. The NTC thermistor gold electrode slurry adopts the glass powder, the addition amount is 2-10%, and the gold electrode slurry is stable and has good performance.
Specifically, the gold powder may have a ratio of 70%, 71%, 72%, 73%, 74%, 75%, 76%, 77%, 78%, 79%, 80%. The glass frit may be 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%. The ratio of the glassy carbon can be 1%, 1.2%, 1.5%, 1.7%, 2%, 2.2%, 2.5%, 2.7%, 3%. The organic carrier may be 15%, 16%, 17%, 18%, 19%, 20%.
In one embodiment, the gold electrode paste is composed of the following components: 70% of gold powder, 2% of glass powder, 1% of glass carbon and 17% of organic carrier. In another embodiment, the gold electrode paste consists of the following components: 75% of gold powder, 5% of glass powder, 3% of glass carbon and 17% of organic carrier. In another embodiment, the gold electrode paste consists of 70% gold powder, 7% glass powder, 3% glass carbon and 20% organic carrier.
Specifically, the organic carrier consists of the following components in percentage by mass: 20-30% of organic resin, 1-5% of dispersing agent and the balance of organic solvent. The organic resin may be 20%, 21%, 22%, 23%, 24%, 25%, 26%, 27%, 28%, 29%, 30%.
Specifically, the organic resin is ethyl cellulose; the dispersing agent is one or more of ammonium polymethacrylate, NP phosphate (nonylphenol polyether phosphate), 600 phosphate, TSP phosphate (styryl polyether phosphate) and AEO-9 phosphate (fatty alcohol ether phosphate); the organic solvent is one or more of terpineol, diethylene glycol butyl ether acetate, octanol, benzyl alcohol, dibutyl phthalate and dimethyl diformate. When the dispersing agent and the organic solvent are the plurality of the dispersing agents and the organic solvent, the plurality of dispersing agents and the organic solvent are matched according to the needs.
The invention also discloses an NTC thermistor which comprises a gold electrode, wherein the gold electrode comprises the gold electrode glass powder. The gold electrode on the NTC thermistor is formed by paving the gold electrode paste on the NTC ceramic body.
For the NTC thermistor of the present invention, in particular, in an embodiment, the NTC thermistor further includes an NTC ceramic body, a gold dioxide electrode is disposed on one side of the NTC ceramic body, the gold electrode is disposed on the gold dioxide electrode, and the gold electrode is directly disposed on the other side of the NTC ceramic body. In another embodiment, the NTC thermistor further includes an NTC ceramic body, gold dioxide electrodes are disposed on both sides of the NTC ceramic body, and the gold electrodes are disposed on both sides of the NTC ceramic body.
The following is a detailed description of specific examples and comparative examples.
Example 1
Weighing the components of the gold electrode glass powder according to the proportion of the table 1, and uniformly mixing to obtain a mixed raw material;
transferring the mixed raw materials into a corundum crucible or a platinum crucible, gradually heating and smelting in a muffle furnace, gradually heating the muffle furnace, melting the mixed raw materials to obtain a glass solution, and recording the melting temperature;
after the heat preservation time is 1h at the melting temperature, quenching the glass solution in water to obtain glass particles;
ball milling, drying and sieving the glass particles to obtain the gold electrode glass powder.
Example 2
Weighing the components of the gold electrode glass powder according to the proportion of the table 1, and uniformly mixing to obtain a mixed raw material;
transferring the mixed raw materials into a corundum crucible or a platinum crucible, gradually heating and smelting in a muffle furnace, gradually heating the muffle furnace, melting the mixed raw materials to obtain a glass solution, and recording the melting temperature;
after the heat preservation time is 1h at the melting temperature, quenching the glass solution in water to obtain glass particles;
ball milling, drying and sieving the glass particles to obtain the gold electrode glass powder.
Example 3
Weighing the components of the gold electrode glass powder according to the proportion of the table 1, and uniformly mixing to obtain a mixed raw material;
transferring the mixed raw materials into a corundum crucible or a platinum crucible, gradually heating and smelting in a muffle furnace, gradually heating the muffle furnace, melting the mixed raw materials to obtain a glass solution, and recording the melting temperature;
after the heat preservation time is 1h at the melting temperature, quenching the glass solution in water to obtain glass particles;
ball milling, drying and sieving the glass particles to obtain the gold electrode glass powder.
Example 4
Weighing the components of the gold electrode glass powder according to the proportion of the table 1, and uniformly mixing to obtain a mixed raw material;
transferring the mixed raw materials into a corundum crucible or a platinum crucible, gradually heating and smelting in a muffle furnace, gradually heating the muffle furnace, melting the mixed raw materials to obtain a glass solution, and recording the melting temperature;
after the heat preservation time is 1h at the melting temperature, quenching the glass solution in water to obtain glass particles;
ball milling, drying and sieving the glass particles to obtain the gold electrode glass powder.
Comparative example 1
Weighing the components of the gold electrode glass powder according to the proportion of the table 1, and uniformly mixing to obtain a mixed raw material;
transferring the mixed raw materials into a corundum crucible or a platinum crucible, gradually heating and smelting in a muffle furnace, gradually heating the muffle furnace, melting the mixed raw materials to obtain a glass solution, and recording the melting temperature;
after the heat preservation time is 1h at the melting temperature, quenching the glass solution in water to obtain glass particles;
ball milling, drying and sieving the glass particles to obtain the gold electrode glass powder.
TABLE 1
Bi 2 O 3 B 2 O 3 CuO Li 2 O CaO B 2 O 3 ZnO MnO
Example 1 20% 40% 30% 10%
Example 2 60% 20% 15% 5%
Example 3 50% 33% 15% 2%
Example 4 30% 25% 35% 10%
Comparative example 1 1% 25% 5% - 40% 20% 8% 1%
Melting points of examples 1 to 4 and comparative example 1 are shown in Table 2 below.
TABLE 2
Melting point
Example 1 650℃
Example 2 653℃
Implementation of the embodimentsExample 3 661℃
Example 4 670℃
Comparative example 1 1200℃
As is clear from the above table, the melting point of examples 1 to 3 of the present invention is only about 650 to 670℃and the melting point of the glass frit system is low, compared with comparative example 1.
It should be noted that, the limitation of each step in the present solution is not to be considered as limiting the sequence of steps on the premise of not affecting the implementation of the specific solution, and the steps written in the previous step may be executed before, or executed after, or even executed simultaneously, so long as the implementation of the present solution is possible, all the steps should be considered as falling within the protection scope of the present invention.
The above description of the invention in connection with specific alternative embodiments is further detailed and it is not intended that the invention be limited to the specific embodiments disclosed. It will be apparent to those skilled in the art that several simple deductions or substitutions may be made without departing from the spirit of the invention, and these should be considered to be within the scope of the invention.

Claims (10)

1. The NTC thermistor gold electrode glass powder is characterized by comprising the following components in percentage by mass:
2. the NTC thermistor gold electrode glass powder of claim 1, characterized in that the glass powder consists of the following components in mass percent:
3. the NTC thermistor gold electrode glass powder of claim 2, characterized in that the glass powder consists of the following components in mass percent:
4. the NTC thermistor gold electrode glass powder of claim 3, characterized in that the glass powder consists of the following components in mass percent:
5. a method for preparing the gold electrode glass powder of the NTC thermistor, which is used for preparing the gold electrode glass powder according to any one of claims 1 to 4, and is characterized in that the preparation method comprises the following steps:
weighing the components of the gold electrode glass powder according to any proportion of claims 1 to 4, and uniformly mixing to obtain a mixed raw material;
smelting the mixed raw materials at a high temperature of 650-670 ℃ to obtain a glass solution;
quenching the glass solution in water to obtain glass particles;
ball milling, drying and sieving the glass particles to obtain the gold electrode glass powder.
6. The process of claim 5 wherein the high temperature smelting mixed feed material has a smelting temperature of 650 ℃.
7. The NTC thermistor gold electrode slurry is characterized by comprising the following components in percentage by mass:
wherein the glass frit is the glass frit according to any one of claims 1 to 4.
8. The NTC thermistor gold electrode slurry of claim 7, characterized in that the organic carrier consists of the following components in mass percent:
20-30% of organic resin
1 to 5 percent of dispersing agent
The balance of organic solvent.
9. The NTC thermistor gold electrode slurry of claim 8, characterized in that the organic resin is ethylcellulose; the dispersing agent is one or more of ammonium polymethacrylate, NP phosphate (nonylphenol polyether phosphate), 600 phosphate, TSP phosphate (styryl polyether phosphate) and AEO-9 phosphate (fatty alcohol ether phosphate); the organic solvent is one or more of terpineol, diethylene glycol butyl ether acetate, octanol, benzyl alcohol, dibutyl phthalate and dimethyl diformate.
10. An NTC thermistor comprising a gold electrode comprising the gold electrode glass frit according to any one of claims 1 to 4.
CN202311288764.0A 2023-10-07 2023-10-07 Gold electrode glass powder, preparation method, gold electrode slurry and NTC thermistor Pending CN117342797A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202311288764.0A CN117342797A (en) 2023-10-07 2023-10-07 Gold electrode glass powder, preparation method, gold electrode slurry and NTC thermistor

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Application Number Priority Date Filing Date Title
CN202311288764.0A CN117342797A (en) 2023-10-07 2023-10-07 Gold electrode glass powder, preparation method, gold electrode slurry and NTC thermistor

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CN117342797A true CN117342797A (en) 2024-01-05

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