阅读说明：本技术 一种热压烧结工艺制备Zn0电阻片的方法 (Method for preparing Zn0 resistance card by hot-pressing sintering process ) 是由 潘俊乔 张磊 于 2020-08-07 设计创作，主要内容包括：本发明公开了一种热压烧结工艺制备Zn0电阻片的方法,ZnO电阻片由ZnO、Bi-2O-3、Sb-2O-3、Co-3O-4、NiO、MnO-2、Cr-2O-3、Al(NO-3)-3、SiO-2混合组成；混合物中ZnO的摩尔分数为93.8%～97.3%,BiO2的摩尔分数为0.5%～1%,Sb-2O-3、Co-3O-4、NiO、MnO-2、Cr-2O-3、Al(NO-3)-3·-9H-2O、SiO-2的摩尔分数为1.5%～3.35%；向上述混合物中加入粘结剂PVA和超纯水后使用球磨机进行球磨混合得到混合浆料。本发明通过采用铋、锑、钴、镍、锰、铬、铝、硅元素进行掺杂,提高其电学性能,本发明使用热压烧结的工艺制备氧化锌电阻,相比一般使用的烧结工艺,热压烧结在配料过程中不需要加入成型剂,消除了排胶和烧结过程中由于成型剂挥发使得烧结后的成品气孔率高的影响,且烧结过程中压力更高可以降低烧结温度。(The invention discloses a method for preparing a Zn0 resistor disc by a hot-pressing sintering process, wherein the ZnO resistor disc is prepared from ZnO and Bi 2 O 3 、Sb 2 O 3 、Co 3 O 4 、NiO、MnO 2 、Cr 2 O 3 、Al（NO 3 ） 3 、SiO 2 Mixing to form a mixture; the molar fraction of ZnO in the mixture was 93.8 to 97.3 percent of the total weight of the composition, 0.5 to 1 percent of BiO2 in molar fraction and Sb 2 O 3 、Co 3 O 4 、NiO、MnO 2 、Cr 2 O 3 、Al（NO 3 ） 3 · 9 H 2 O、SiO 2 The mole fraction of (A) is 1.5% -3.35%; after the binder PVA and ultrapure water were added to the above mixture, ball milling and mixing were performed using a ball mill to obtain a mixed slurry. The invention improves the electrical property by doping bismuth, antimony, cobalt, nickel, manganese, chromium, aluminum and silicon elements, and prepares the zinc oxide resistor by using the hot-pressing sintering process.)

1. A method for preparing a Zn0 resistor disc by a hot-pressing sintering process is characterized by comprising the following steps: the preparation method comprises the following steps:

the first step is as follows: the ZnO resistance card consists of ZnO and Bi₂O₃、Sb₂O₃、Co₃O₄、NiO、MnO₂、Cr₂O₃、Al（NO₃）₃、SiO₂Mixing to form a mixture; the mol fraction of ZnO in the mixture is 93.8 percent to 97.3 percent, the mol fraction of BiO2 is 0.5 percent to 1 percent, and the mol fraction of Sb is₂O₃、Co₃O₄、NiO、MnO₂、Cr₂O₃、Al（NO₃）₃·₉H₂O、SiO₂The mole fraction of (A) is 1.5% -3.35%;

the second step is that: adding a binder PVA and ultrapure water into the mixture, then carrying out ball milling and mixing by using a ball mill to obtain mixed slurry, drying the obtained slurry at 90 ℃, and carrying out granulation and sieving to obtain mixed powder; wherein PVA accounts for 0.003-0.006 percent of the mass fraction of the powder mixture, and the mass ratio of the ultrapure water to the powder is 2: 1, ball milling rate: 500r/min, ball milling time: 0.5-4 h;

the third step: pouring the dried powder into a die, pressing the mixed powder into a shape under 7.5MPa by using a tablet press to obtain a blank, and drying for 30min at 150 ℃ by using a blast drier;

the fourth step: sintering the formed blank in a hot-pressing sintering furnace at 850-1250 ℃ under 10-30 MPa to obtain a ZnO ceramic wafer;

the fifth step: and printing silver electrode slurry on two surfaces of the chip ZnO ceramic chip by adopting a screen printing process, drying the chip ZnO ceramic chip by using an air-blast drying oven at the temperature of 150 ℃, and processing the chip ZnO ceramic chip in an air atmosphere at the temperature of 550-650 ℃ to obtain the ZnO resistance chip.

2. The method for preparing the Zn0 resistor disc by the hot-pressing sintering process according to claim 1, wherein the hot-pressing sintering process comprises the following steps: the powder materials are weighed according to the molar mass, wherein the molar fraction of ZnO is 95.2 percent, and Bi is₂O₃The mole fraction of (B) is 0.8%, and the mole fractions of the oxides of Sb, Co, Ni, Mn, Cr and Si are 1.1%, 0.5%, 1%, 0.5%, 0.4% and 0.5%, respectively.

3. The method for preparing the Zn0 resistor disc by the hot-pressing sintering process according to claim 1, wherein the hot-pressing sintering process comprises the following steps: wherein PVA is 0.003 percent of the mass fraction of the powder mixture, and the mass ratio of the ultrapure water to the powder is 2: 1, ball milling rate: 500r/min, ball milling time: and (4) 1 h.

4. The method for preparing the Zn0 resistor disc by the hot-pressing sintering process according to claim 1, wherein the hot-pressing sintering process comprises the following steps: and pressing the powder into a sheet blank under the pressure of 7.5MPa by using a tablet press, and keeping the pressure for 30 s.

5. The method for preparing the Zn0 resistor disc by the hot-pressing sintering process according to claim 1, wherein the hot-pressing sintering process comprises the following steps: and sintering the molded blank at 1080 ℃ under the pressure of 21MPa to obtain the ZnO ceramic chip.

6. The method for preparing the Zn0 resistor disc by the hot-pressing sintering process according to claim 1, wherein the hot-pressing sintering process comprises the following steps: and printing silver electrode slurry on two surfaces of the sheet type ZnO ceramic sheet by adopting a screen printing process, drying the sheet type ZnO ceramic sheet at the temperature of 150 ℃ by using an air-blast drying oven, and processing the sheet type ZnO ceramic sheet at the temperature of 600 ℃ in an air atmosphere after the drying is finished to obtain the ZnO resistance sheet.

Technical Field

The invention relates to the technical field of electronic ceramic components, in particular to a method for preparing a Zn0 resistor disc by a hot-pressing sintering process.

Background

Compared with other systems, the ZnO resistor disc has more excellent nonlinear characteristics and higher flow capacity, and is widely applied to protection systems of electrical equipment due to excellent electrical properties.

The hot-pressing sintering is carried out simultaneously because the heating and the pressurizing are carried out, the powder is in a thermoplastic state, the contact diffusion process of powder particles is facilitated, the sintering temperature can be reduced, the contact surface of ceramic grains is effectively increased to promote the densification of the ceramic, the excessive growth of the grains can be stopped under the action of external pressure, a forming agent is required to be added in the traditional ZnO resistance card preparation process, the volatilization speed of the forming agent at high temperature is too high in the preparation process, the sintered compact finished product is not good, and the porosity is high.

Disclosure of Invention

The invention provides a method for preparing a ZnO resistance card by a hot-pressing sintering process, which reduces the influence brought by a forming agent, reduces the sintering temperature and improves the density by adopting the hot-pressing sintering process.

In order to achieve the purpose, the invention provides the following technical scheme: a method for preparing a Zn0 resistor disc by a hot-pressing sintering process comprises the following preparation steps:

the first step is as follows: the ZnO resistance card consists of ZnO and Bi₂O₃、Sb₂O₃、Co₃O₄、NiO、MnO₂、Cr₂O₃、Al（NO₃）₃、SiO₂Mixing to form a mixture; of ZnO in the mixture93.8 to 97.3 percent of mol fraction, 0.5 to 1 percent of BiO2 mol fraction, and Sb₂O₃、Co₃O₄、NiO、MnO₂、Cr₂O₃、Al（NO₃）₃·₉H₂O、SiO₂The mole fraction of (A) is 1.5% -3.35%;

the second step is that: adding a binder PVA and ultrapure water into the mixture, then carrying out ball milling and mixing by using a ball mill to obtain mixed slurry, drying the obtained slurry at 90 ℃, and carrying out granulation and sieving to obtain mixed powder; wherein PVA accounts for 0.003-0.006 percent of the mass fraction of the powder mixture, and the mass ratio of the ultrapure water to the powder is 2: 1, ball milling rate: 500r/min, ball milling time: 0.5-4 h;

the third step: pouring the dried powder into a die, pressing the mixed powder into a shape under 7.5MPa by using a tablet press to obtain a blank, and drying for 30min at 150 ℃ by using a blast drier;

the fourth step: sintering the formed blank in a hot-pressing sintering furnace at 850-1250 ℃ under 10-30 MPa to obtain a ZnO ceramic wafer;

the fifth step: and printing silver electrode slurry on two surfaces of the chip ZnO ceramic chip by adopting a screen printing process, drying the chip ZnO ceramic chip by using an air-blast drying oven at the temperature of 150 ℃, and processing the chip ZnO ceramic chip in an air atmosphere at the temperature of 550-650 ℃ to obtain the ZnO resistance chip.

Preferably, the powder materials are weighed according to molar mass, wherein the molar fraction of ZnO is 95.2 percent, and Bi is₂O₃The mole fraction of (B) is 0.8%, and the mole fractions of the oxides of Sb, Co, Ni, Mn, Cr and Si are 1.1%, 0.5%, 1%, 0.5%, 0.4% and 0.5%, respectively.

Preferably, the PVA is 0.003 percent of the mass fraction of the powder mixture, and the mass ratio of the ultrapure water to the powder is 2: 1, ball milling rate: 500r/min, ball milling time: and (4) 1 h.

Preferably, the powder is pressed into a sheet blank under the pressure of 7.5MPa by using a tablet press, and the pressure is maintained for 30 s.

Preferably, the molded blank is sintered at 1080 ℃ under the pressure of 21MPa to obtain the ZnO ceramic chip.

Preferably, the silver electrode slurry is printed on two sides of the sheet type ZnO ceramic sheet by adopting a screen printing process, the sheet type ZnO ceramic sheet is dried by using an air-blowing drying oven at the temperature of 150 ℃, and after the drying is finished, the sheet type ZnO ceramic sheet is processed at the temperature of 600 ℃ in an air atmosphere to obtain the ZnO resistance sheet.

Compared with the prior art, the invention has the following beneficial effects:

1. the invention improves the electrical property by doping bismuth, antimony, cobalt, nickel, manganese, chromium, aluminum and silicon elements, and prepares the zinc oxide resistor by using the hot-pressing sintering process.

Drawings

FIG. 1 is a flow chart of the preparation method of the ZnO resistance card.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

Referring to fig. 1, the present invention provides the following technical solutions: a method for preparing a Zn0 resistor disc by a hot-pressing sintering process comprises the following preparation steps:

the first step is as follows: the ZnO resistance card consists of ZnO and Bi₂O₃、Sb₂O₃、Co₃O₄、NiO、MnO₂、Cr₂O₃、Al（NO₃）₃、SiO₂Mixing to form a mixture; the mol fraction of ZnO in the mixture is 93.8 percent to 97.3 percent, the mol fraction of BiO2 is 0.5 percent to 1 percent, and the mol fraction of Sb is₂O₃、Co₃O₄、NiO、MnO₂、Cr₂O₃、Al（NO₃）₃·₉H₂O、SiO₂The mole fraction of (A) is 1.5% -3.35%;

the second step is that: adding a binder PVA and ultrapure water into the mixture, then carrying out ball milling and mixing by using a ball mill to obtain mixed slurry, drying the obtained slurry at 90 ℃, and carrying out granulation and sieving to obtain mixed powder; wherein PVA accounts for 0.003-0.006 percent of the mass fraction of the powder mixture, and the mass ratio of the ultrapure water to the powder is 2: 1, ball milling rate: 500r/min, ball milling time: 0.5-4 h;

the third step: pouring the dried powder into a die, pressing the mixed powder into a shape under 7.5MPa by using a tablet press to obtain a blank, and drying for 30min at 150 ℃ by using a blast drier;

the fourth step: sintering the formed blank in a hot-pressing sintering furnace at 850-1250 ℃ under 10-30 MPa to obtain a ZnO ceramic wafer;

the fifth step: and printing silver electrode slurry on two surfaces of the chip ZnO ceramic chip by adopting a screen printing process, drying the chip ZnO ceramic chip by using an air-blast drying oven at the temperature of 150 ℃, and processing the chip ZnO ceramic chip in an air atmosphere at the temperature of 550-650 ℃ to obtain the ZnO resistance chip.

The first embodiment is as follows:

a ZnO resistor chip prepared by hot-pressing sintering process comprises ZnO ceramic and silver electrode, wherein the ceramic chip comprises ZnO and Bi₂O₃And oxides of Sb, Co, Ni, Mn, Cr and Si, and the preparation method comprises the following steps:

the first step is as follows: weighing the powder materials according to molar mass, wherein the molar fraction of ZnO is 95.2 percent, and Bi is₂O₃The mole fraction of Sb, Co, Ni, Mn, Cr and Si is respectively 1.1%, 0.5%, 1%, 0.5%, 0.4% and 0.5%;

the second step is that: adding a forming agent PVA and ultrapure water into the mixture, then carrying out ball milling and mixing by using a ball mill to obtain mixed slurry, drying the obtained slurry at 90 ℃, and carrying out granulation and sieving to obtain mixed powder; wherein PVA is 0.003 percent of the mass fraction of the powder mixture, and the mass ratio of the ultrapure water to the powder is 2: 1, ball milling rate: 500r/min, ball milling time: 1 h;

the third step: pressing the powder into a sheet blank under the pressure of 7.5MPa by using a tablet press, and keeping the pressure for 30 s;

the fourth step: sintering the molded blank at 1080 ℃ under the pressure of 21MPa to obtain a ZnO ceramic wafer;

the fifth step: and printing silver electrode slurry on two surfaces of the chip ZnO ceramic chip by adopting a screen printing process, drying the chip ZnO ceramic chip by using an air-blast drying oven at the temperature of 150 ℃, and processing the chip ZnO ceramic chip in an air atmosphere at the temperature of 600 ℃ to obtain the ZnO resistor chip.

Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.