CN102126852B - Method for preparing zinc oxide piezoresistor ceramic - Google Patents

Method for preparing zinc oxide piezoresistor ceramic Download PDF

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CN102126852B
CN102126852B CN 201110068064 CN201110068064A CN102126852B CN 102126852 B CN102126852 B CN 102126852B CN 201110068064 CN201110068064 CN 201110068064 CN 201110068064 A CN201110068064 A CN 201110068064A CN 102126852 B CN102126852 B CN 102126852B
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汪丽
翟毅
姜胜林
黄国贤
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Three or three Electric Applicance Co., Ltd of Xiangyang City
Huazhong University of Science and Technology
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Huazhong University of Science and Technology
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Abstract

The invention discloses a method for preparing zinc oxide high voltage piezoresistor ceramic, comprising the following steps of: adding Bi2O3-Sb2O3 presintering powder and SiO2-ZnO presintering powder into a piezoresistor formula, wherein the mole ratio of the Bi2O3-Sb2O3 presintering powder to the SiO2-ZnO presintering powder to the piezoresistor formula is x: y: (1-x-y), x is between 0.005 and 0.01, and y is between 0.005 and 0.01; baking after ball milling and mixing; then smashing, and adding PVA (poly vinyl alcohol) solution with the concentration of 3-7%, wherein the solution accounts for 8-13% of the powder by mass percent; pelleting, dry pressing and moulding, and then sintering at the temperature of 1150-1250 DEG C for 1.5-3.5 hours to finally obtain the ZnO piezoresistor ceramic. In the invention, by adding pretreated additive into the formula, the low current and heavy current performances of the zinc oxide piezoresistor are effectively improved. The prepared zinc oxide piezoresistor ceramic has excellent low current performance, and the durability under the impact of 8/20Mus pulse current is greatly improved, thus the prepared zinc oxide piezoresistor ceramic meets the requirement for preparing a piezoresistor.

Description

A kind of preparation method of zinc oxide piezoresistor ceramic
Technical field
The invention belongs to the preparation method of varistor ceramics materials, particularly synthetic Bi 2O 3-Sb 2O 3And SiO 2The preparation method of-ZnO powder belongs to materials science field.
Background technology
Zinc oxide piezoresistor ceramic is take zinc oxide as material of main part, by adding multiple other trace element, and the poly semiconductor device made from the conditional electronic ceramic process.Because the electric property of its fast response time, the excellence such as nonlinear factor is large, through-current capability is strong becomes rapidly the leading material of making piezoresistor, be mainly used in current foldback circuit.The U.S., Japan and other countries have obtained rapidly to prepare in batches the technology of Zinc-oxide piezoresistor at 20 century 70s, its electric property is broken through, thereby be widely used in high-voltage power system.Along with the growth of electricity needs, transmitting capacity is more and more large, and the voltage range of transmitting line is more and more high, and therefore high performance voltage dependent resistor is prepared into for key.
For the zinc oxide piezoresistor ceramic of multi-component, pyroreaction complexity, it is particularly important that material prescription seems.Wherein, the processing treatment of additive is the most key, and the method for the processing treatment be a kind of additive commonly used is processed in the preprocessing of portions additive.
Summary of the invention
The invention provides a kind of preparation method of zinc oxide piezoresistor ceramic, for the problem that existing preparation method exists, portions additive is carried out pre-treatment to prepare the varistor ceramics materials of better performances.
The preparation method of a kind of zinc oxide piezoresistor ceramic provided by the invention, the preparation method of a kind of zinc oxide high voltage varistor of its feature pottery is at first with Bi 2O 3-Sb 2O 3Pre-burning powder and SiO 2-ZnO pre-burning powder joins in the voltage dependent resistor formula, wherein, and Bi 2O 3-Sb 2O 3Pre-burning powder, SiO 2The mol ratio of-ZnO pre-burning powder and voltage dependent resistor formula is x: y: (1-x-y), wherein, x=0.005～0.01, y=0.005～0.01; Ball milling mixes post-drying, then pulverizes, and adds the PVA solution of concentration 3%～7%, the mass percent that solution accounts for powder is 8～13%, and then through granulation, dry-pressing formed after, sintering is 1.5～3.5 hours at 1150～1250 ℃ of temperature, makes the ZnO varistor pottery.
Described Bi 2O 3-Sb 2O 3The preparation process of pre-burning powder:
The bismuth of 1: 1 in molar ratio～1: 1.6 and the ratio of antimony, configuration Bi 2O 3, Sb 2O 3Powder after 14～18 hours, oven dry after is being crushed to powder particle diameter 10 μ ms below at 90～120 ℃ of temperature with the deionized water ball milling, then the corundum crucible of mixed powder being packed into, temperature rise rate with 5～7 ℃/min is heated to 600～700 ℃, is incubated 1～2 hour, obtains Bi 2O 3-Sb 2O 3Preburning powder.
Described SiO 2The preparation process of-ZnO pre-burning powder:
The silicon of 1: 1 in molar ratio～1: 2 and the ratio of zinc, the pure SiO of Allocation Analysis 2, the ZnO powder, after 14～18 hours, oven dry after powder be crushed to particle diameter 10 μ ms below at 90～120 ℃ of temperature with the deionized water ball milling, then the corundum crucible of mixed powder being packed into, temperature rise rate with 5～7 ℃/min is heated to 900～1000 ℃, is incubated 2～3 hours, obtains SiO 2-ZnO preburning powder.
In order to form surface state to improve nonlinear exponent, added a small amount of MnCO 3, Co 2O 3In order to suppress abnormal grain growth to increase pressure sensitive voltage, added a small amount of Cr in formula 2O 3In order to improve the large Current Zone nonlinear exponent of resistor disc, added a small amount of Al (NO) in formula 39H 2O。
The based varistor of the present invention's preparation has larger pressure sensitive voltage, less leakage current, and have good large electric current through-current capability, meet the requirement of making voltage dependent resistor.
Embodiment
Below by specific embodiment, further illustrate characteristics of the present invention and effect:
Embodiment 1:
With Bi 2O 3-Sb 2O 3Pre-burning powder and SiO 2-ZnO pre-burning powder joins in the voltage dependent resistor formula, wherein, and Bi 2O 3-Sb 2O 3Pre-burning powder, SiO 2The mol ratio of-ZnO pre-burning powder and voltage dependent resistor formula is 1: 1: 98.Ball milling mixed 14 hours, dry at 100 ℃ of temperature, then powder is crushed to particle diameter below 10 μ m, the mass percent that the PVA solution that adds concentration 7%, solution account for powder is 8%, then through granulation, dry-pressing formed after, sintering is 2 hours at 1200 ℃ of temperature, make the ZnO varistor pottery, burn till rear ceramic plate thickness 1.70mm (± 0.10mm), diameter 13.30mm (± 0.05mm).
Described Bi 2O 3-Sb 2O 3The preparation process of pre-burning powder:
The bismuth of 1: 1 in molar ratio and the ratio of antimony, the pure Bi of Allocation Analysis 2O 3, Sb 2O 3Powder, is dried at 90 ℃ of temperature after 14 hours with the deionized water ball milling, then powder is crushed to particle diameter below 10 μ m, and the corundum crucible of then mixed powder being packed into is heated to 600 ℃ with the temperature rise rate of 5 ℃/min, is incubated 1 hour, obtains Bi 2O 3-Sb 2O 3Preburning powder.
Described SiO 2The preparation process of-ZnO pre-burning powder:
The silicon of 1: 1 in molar ratio and the ratio of zinc, the pure SiO of Allocation Analysis 2, the ZnO powder,, dry at 90 ℃ of temperature after 18 hours with the deionized water ball milling, powder is crushed to particle diameter below 10 μ m, the corundum crucible of then mixed powder being packed into is heated to 900 ℃ with the temperature rise rate of 5 ℃/min, is incubated 2 hours, obtains SiO 2-ZnO preburning powder.
Embodiment 2
With Bi 2O 3-Sb 2O 3Pre-burning powder and SiO 2-ZnO pre-burning powder joins in the voltage dependent resistor formula, wherein, and Bi 2O 3-Sb 2O 3Pre-burning powder, SiO 2The mol ratio of-ZnO pre-burning powder and voltage dependent resistor formula is 1: 1: 98.Ball milling mixed 14 hours, dry at 100 ℃ of temperature, then powder is crushed to particle diameter below 10 μ m, the mass percent that the PVA solution that adds concentration 7%, solution account for powder is 8%, then through granulation, dry-pressing formed after, sintering is 2 hours at 1200 ℃ of temperature, make the ZnO varistor pottery, burn till rear ceramic plate thickness 1.70mm (± 0.10mm), diameter 13.30mm (± 0.05mm).
Described Bi 2O 3-Sb 2O 3The preparation process of pre-burning powder:
The bismuth of 5: 6 in molar ratio and the ratio of antimony, the pure Bi of Allocation Analysis 2O 3, Sb 2O 3Powder, is dried at 100 ℃ of temperature after 16 hours with the deionized water ball milling, then powder is crushed to particle diameter below 10 μ m, and the corundum crucible of then mixed powder being packed into is heated to 650 ℃ with the temperature rise rate of 5 ℃/min, is incubated 1.5 hours, obtains Bi 2O 3-Sb 2O 3Preburning powder.
Described SiO 2The preparation process of-ZnO pre-burning powder:
The silicon of 2: 3 in molar ratio and the ratio of zinc, the pure SiO of Allocation Analysis 2, the ZnO powder,, dry at 100 ℃ of temperature after 16 hours with the deionized water ball milling, powder is crushed to particle diameter below 10 μ m, the corundum crucible of then mixed powder being packed into is heated to 950 ℃ with the temperature rise rate of 5 ℃/min, is incubated 2.5 hours, obtains SiO 2-ZnO preburning powder.
Embodiment 3
With Bi 2O 3-Sb 2O 3Pre-burning powder and SiO 2-ZnO pre-burning powder joins in the voltage dependent resistor formula, wherein, and Bi 2O 3-Sb 2O 3Pre-burning powder, SiO 2The mol ratio of-ZnO pre-burning powder and voltage dependent resistor formula is 1: 1: 98.Ball milling mixed 14 hours, dry at 100 ℃ of temperature, then powder is crushed to particle diameter below 10 μ m, the mass percent that the PVA solution that adds concentration 5%, solution account for powder is 10%, then through granulation, dry-pressing formed after, sintering is 2 hours at 1200 ℃ of temperature, make the ZnO varistor pottery, burn till rear ceramic plate thickness 1.70mm (± 0.10mm), diameter 13.30mm (± 0.05mm).
Described Bi 2O 3-Sb 2O 3The preparation process of pre-burning powder:
The bismuth of 5: 7 in molar ratio and the ratio of antimony, the pure Bi of Allocation Analysis 2O 3, Sb 2O 3Powder, is dried at 120 ℃ of temperature after 18 hours with the deionized water ball milling, then powder is crushed to particle diameter below 10 μ m, and the corundum crucible of then mixed powder being packed into is heated to 700 ℃ with the temperature rise rate of 5 ℃/min, is incubated 2 hours, obtains Bi 2O 3-Sb 2O 3Preburning powder.
Described SiO 2The preparation process of-ZnO pre-burning powder:
The silicon of 1: 1 in molar ratio and the ratio of zinc, the pure SiO of Allocation Analysis 2, the ZnO powder,, dry at 120 ℃ of temperature after 16 hours with the deionized water ball milling, powder is crushed to particle diameter below 10 μ m, the corundum crucible of then mixed powder being packed into is heated to 1000 ℃ with the temperature rise rate of 5 ℃/min, is incubated 3 hours, obtains SiO 2-ZnO preburning powder.
Embodiment 4
With Bi 2O 3-Sb 2O 3Pre-burning powder and SiO 2-ZnO pre-burning powder joins in the voltage dependent resistor formula, wherein, and Bi 2O 3-Sb 2O 3Pre-burning powder, SiO 2The mol ratio of-ZnO pre-burning powder and voltage dependent resistor formula is 1: 1: 98.Ball milling mixed 14 hours, dry at 100 ℃ of temperature, then powder is crushed to particle diameter below 10 μ m, the mass percent that the PVA solution that adds concentration 3%, solution account for powder is 13%, then through granulation, dry-pressing formed after, sintering is 2 hours at 1200 ℃ of temperature, make the ZnO varistor pottery, burn till rear ceramic plate thickness 1.70mm (± 0.10mm), diameter 13.30mm (± 0.05mm).
Described Bi 2O 3-Sb 2O 3The preparation process of pre-burning powder:
The bismuth of 5: 8 in molar ratio and the ratio of antimony, the pure Bi of Allocation Analysis 2O 3, Sb 2O 3Powder, is dried at 100 ℃ of temperature after 16 hours with the deionized water ball milling, then powder is crushed to particle diameter below 10 μ m, and the corundum crucible of then mixed powder being packed into is heated to 600 ℃ with the temperature rise rate of 5 ℃/min, is incubated 1.5 hours, obtains Bi 2O 3-Sb 2O 3Preburning powder.
Described SiO 2The preparation process of-ZnO pre-burning powder:
The silicon of 1: 2 in molar ratio and the ratio of zinc, the pure SiO of Allocation Analysis 2, the ZnO powder,, dry at 100 ℃ of temperature after 14 hours with the deionized water ball milling, powder is crushed to particle diameter below 10 μ m, the corundum crucible of then mixed powder being packed into is heated to 900 ℃ with the temperature rise rate of 5 ℃/min, is incubated 2.5 hours, obtains SiO 2-ZnO preburning powder.
With the ceramic sample abrasive disc of embodiment 1～4 gained, clean, be coated with silver electrode, burn electrode, obtain respectively ceramic plate sample 1～4; Then clean, after coated epoxy resin, make zinc oxide varistor, can use.Sample is carried out power dissipation characteristics in leakage current region test and at 8/20 μ s pulsed current impact experiment, its result is as shown in table 1.
Can find out, in the present invention, zinc oxide pressure-sensitive ceramic main raw bismuth oxide and weisspiessglanz be carried out pre-treatment, silicon-dioxide and partial oxidation zinc carried out joining in basic components after pre-treatment its pressure sensitive voltage V 1mA＞300V/mm, nonlinear factor α＞75, leakage current＜0.2 μ A, 8/20 μ s pulsed current impact lower pressure-sensitive voltage change ratio and can be stabilized in 5%.
Table 1 sample Specifeca tion speeification
Figure BDA0000051329950000051
Figure BDA0000051329950000061
In the present invention, change the part processing parameter as shown in the table, still can reach performance perameter preferably.
Table 2 fabrication process parameters
Bi 2O 3-Sb 2O 3The pre-burning powder 0.005 0.0075 0.01 0.005 0.005
SiO 2-ZnO pre-burning powder 0.005 0.005 0.005 0.0075 0.01
The voltage dependent resistor formula 0.990 0.9875 0.985 0.9875 0.985
Sintering temperature 1150℃ 1175℃ 1200℃ 1225℃ 1250℃
Sintering time 1.5 hour 2 hours 2.5 hour 3 hours 3.5
The present invention not only is confined to above-mentioned embodiment; persons skilled in the art are according to content disclosed by the invention; can adopt other multiple embodiment to implement the present invention; therefore; every employing project organization of the present invention and thinking; do some simple designs that change or change, all fall into the scope of protection of the invention.

Claims (1)

1. the preparation method of a zinc oxide high voltage varistor pottery is at first with Bi 2O 3-Sb 2O 3Pre-burning powder and SiO 2-ZnO pre-burning powder joins in the voltage dependent resistor formula, wherein, and Bi 2O 3-Sb 2O 3Pre-burning powder, SiO 2The mol ratio of-ZnO pre-burning powder and voltage dependent resistor formula is x: y: (1-x-y), and x=0.005 ~ 0.01 wherein, y=0.005 ~ 0.01; Ball milling mixes post-drying, then pulverizes, and adds the PVA solution of concentration 3% ~ 7%, and the mass percent that solution accounts for powder is 8 ~ 13%, and then through granulation, dry-pressing formed after, sintering is 1.5～3.5 hours at 1150～1250 ℃ of temperature, makes the ZnO varistor pottery;
Described Bi 2O 3-Sb 2O 3The preparation process of pre-burning powder:
The ratio of the bismuth of 1:1 ~ 1:1.6 and antimony, configure Bi in molar ratio 2O 3, Sb 2O 3Powder after 14 ~ 18 hours, oven dry after is being crushed to powder particle diameter 10 μ ms below at 90～120 ℃ of temperature with the deionized water ball milling, then the corundum crucible of mixed powder being packed into, temperature rise rate with 5 ~ 7 ℃/min is heated to 600～700 ℃, is incubated 1～2 hour, obtains Bi 2O 3-Sb 2O 3Preburning powder;
Described SiO 2The preparation process of-ZnO pre-burning powder:
The ratio of the silicon of 1:1 ~ 1:2 and zinc in molar ratio, the pure SiO of Allocation Analysis 2, the ZnO powder, after 14 ~ 18 hours, oven dry after powder be crushed to particle diameter 10 μ ms below at 90～120 ℃ of temperature with the deionized water ball milling, then the corundum crucible of mixed powder being packed into, temperature rise rate with 5 ~ 7 ℃/min is heated to 900～1000 ℃, is incubated 2 ~ 3 hours, obtains SiO 2-ZnO preburning powder.
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CN105016721B (en) * 2015-07-01 2020-07-28 清华大学 Method for preparing ZnO varistor ceramic by co-doping aluminum ions, gallium ions and yttrium ions
CN108558389B (en) * 2018-05-04 2021-02-05 南阳中祥电力电子股份有限公司 High-resistance layer slurry for voltage-sensitive resistor chip and preparation method thereof
CN111816398B (en) * 2020-06-23 2022-01-07 上海大学 Resistor disc preparation method capable of improving high-current impact stability
CN112225553A (en) * 2020-10-08 2021-01-15 烟台大学 ZnO-based low-voltage high-nonlinearity pressure-sensitive ceramic co-fired with pure silver inner electrode and preparation method thereof
CN115368129A (en) * 2022-08-23 2022-11-22 如东宝联电子科技有限公司 Laminated zinc oxide composition for reducing residual pressure and preparation method thereof

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