CN115662718A - High-gradient nonlinear resistance card and preparation method thereof - Google Patents
High-gradient nonlinear resistance card and preparation method thereof Download PDFInfo
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- CN115662718A CN115662718A CN202211438294.7A CN202211438294A CN115662718A CN 115662718 A CN115662718 A CN 115662718A CN 202211438294 A CN202211438294 A CN 202211438294A CN 115662718 A CN115662718 A CN 115662718A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000000463 material Substances 0.000 claims abstract description 51
- 229910020599 Co 3 O 4 Inorganic materials 0.000 claims abstract description 9
- 229910004298 SiO 2 Inorganic materials 0.000 claims abstract description 9
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 claims abstract description 4
- 230000008859 change Effects 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims description 31
- 239000000843 powder Substances 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 16
- 238000005245 sintering Methods 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 11
- 238000000227 grinding Methods 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000000498 ball milling Methods 0.000 claims description 5
- 238000001354 calcination Methods 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 239000002270 dispersing agent Substances 0.000 claims description 4
- 238000010304 firing Methods 0.000 claims description 4
- 239000002671 adjuvant Substances 0.000 claims description 3
- 239000002518 antifoaming agent Substances 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 3
- 239000002002 slurry Substances 0.000 claims description 3
- 238000001694 spray drying Methods 0.000 claims description 3
- 238000005507 spraying Methods 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 239000000853 adhesive Substances 0.000 claims description 2
- 230000001070 adhesive effect Effects 0.000 claims description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 38
- 239000011787 zinc oxide Substances 0.000 description 19
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 description 10
- 238000012360 testing method Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000032683 aging Effects 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 229920000058 polyacrylate Polymers 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000013530 defoamer Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention provides a high-gradient nonlinear resistance card which comprises the following components in percentage by mole: main material ZnO:65-90%, and Sb 2 O 3 ：2‑8％，Bi 2 O 3 ：2‑6％，Co 2 O 3 ：0.2‑3％，Co 3 O 4 ：0.5‑1.2％，SiO 2 ：1‑4％，MnO 2 ：1‑3％，Cr 2 O 3 ：2‑4％，NiO：1‑3％，B 2 O 3 ：0.2‑1.2％，Al(NO 3 ) 3 ：0.3‑0.5％，Y 2 O 3 :0.03-0.8% of auxiliary materials. The invention also provides a preparation method of the alternating-current high-gradient nonlinear resistance card. The gradient of the resistance card obtained by the invention is more than 500V/mm, and the energy density is more than 250J/cm 3 And the impact change rate is less than 5%.
Description
Technical Field
The invention relates to the field of preparation of nonlinear resistance cards, in particular to a high-gradient nonlinear resistance card and a preparation method thereof.
Background
The ZnO nonlinear resistor has the characteristics of excellent protection performance, large through-current capacity, no follow current and the like, and is widely applied to internal and external overvoltage protection of electric power and electronic systems, and the lightning arrester is a main product form applied to the electric power systems. When the zinc oxide resistor disc has high potential gradient, large through-current capacity, low residual voltage ratio and excellent aging performance, the volume and the quality of the lightning arrester can be reduced, the insulation level and the manufacturing cost of protected equipment are reduced, and safer and more reliable protection can be provided for power equipment.
The quality of the nonlinear resistance performance of ZnO mainly depends on the design of the formula components and the optimization of the preparation process, so that the ceramic body with uniform and compact microstructure and small dispersion of characteristic performance is obtained, and finally, the ceramic body shows excellent volt-ampere characteristics, direct-current aging characteristics, large energy absorption capacity, large-current impact stability and the like.
Patent literature (CN 101698597A) discloses a high-gradient nonlinear resistor disc, the gradient of the disclosed resistor disc can be increased from 220V/mm to 416V/mm, but the high-gradient nonlinear resistor disc cannot meet some application scenarios requiring higher performance, such as the gradient being greater than 500V/mm, good flow effect, and the like.
Disclosure of Invention
Aiming at the technical problem, the technical scheme adopted by the invention is as follows:
the embodiment of the invention provides a high-gradient nonlinear resistance card which comprises the following components in percentage by mole: main material ZnO:65-90%, and Sb 2 O 3 ：2-8％，Bi2O3：2-6％，Co 2 O 3 ：0.2-3％，Co 3 O 4 ：0.5-1.2％，SiO 2 ： 1-4％，MnO 2 ：1-3％，Cr 2 O 3 ：2-4％，NiO：1-3％，B 2 O 3 ：0.2-1.2％，Al(NO 3 ) 3 ：0.3-0.5％，Y 2 O 3 :0.03-0.8% of auxiliary materials.
Another embodiment of the invention provides a method for preparing a high-gradient nonlinear resistance chip, which comprises the following steps:
weighing the following components in percentage by mole: main material ZnO:65-90%, and Sb 2 O 3 ：2-8％，Bi2O3：2-6％， Co 2 O 3 ：0.2-3％，Co 3 O 4 ：0.5-1.2％，SiO 2 ：1-4％，MnO 2 ：1-3％，Cr 2 O 3 ：2-4％，NiO：1-3％， B 2 O 3 ：0.2-1.2％，Al(NO 3 ) 3 ：0.3-0.5％，Y 2 O 3 :0.03-0.8% of auxiliary materials;
ball-milling and mixing the weighed components of the auxiliary materials, calcining, cooling and crushing the components, and then finely grinding and drying the components to obtain auxiliary material powder;
adding the auxiliary material powder, the main material ZnO, the organic adhesive, the dispersing agent, the defoaming agent, deionized water, water and 0.003 mol percent of Al (NO) based on the total amount of the auxiliary materials (all the auxiliary material powder except the main material ZnO) and the main material ZnO into a mixing tank 3 ) 3 9H 2 O, mixing to form uniform slurry, and drying and granulating by a spray drying method to obtain granulated powder;
pressing the obtained granulated powder into a green body of the resistance card, and pre-sintering the green body of the resistance card to obtain a green material of the resistance card;
firing the resistance card blank at a high temperature to obtain a coarse resistance card;
and grinding the coarse resistance chip, and performing heat treatment, electrode spraying and glazing after grinding to obtain the high-gradient nonlinear resistance chip.
The invention has at least the following beneficial effects:
the high-gradient nonlinear resistance card obtained by the embodiment of the invention has the gradient of more than 500V/mm and the energy density of more than 250J/cm 3 The impact change rate is less than 5%, the miniaturization of GIS lightning arresters and the lightening of lightning arresters such as lines and offshore wind power can be promoted, the requirement of the development of the modern extra-high voltage power industry is met, the resource advantage configuration on a large scale is realized, land resources are effectively saved, the length of the lightning arrester is shortened, the construction investment cost and the operation cost are saved, and the saving and high-efficiency application of natural resources is realized.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all 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.
Example 1
The high-gradient nonlinear resistance chip provided by the embodiment comprises the following components in percentage by mole: main material ZnO:65-90%, and Sb 2 O 3 ：2-8％，Bi2O3：2-6％，Co 2 O 3 ：0.2-3％，Co 3 O 4 ：0.5-1.2％，SiO 2 ：1-4％，MnO 2 ： 1-3％，Cr 2 O 3 ：2-4％，NiO：1-3％，B 2 O 3 ：0.2-1.2％，Al(NO 3 ) 3 ：0.3-0.5％，Y 2 O 3 :0.03-0.8% of auxiliary materials.
The preparation method of the nonlinear resistance card provided by the embodiment can comprise the following steps:
s100, weighing the following components in percentage by mole: main material ZnO:65-90%, and Sb 2 O 3 ：2-8％，Bi 2 O 3 ：2-6％， Co 2 O 3 ：0.2-3％，Co 3 O 4 ：0.5-1.2％，SiO 2 ：1-4％，MnO 2 ：1-3％，Cr 2 O 3 ：2-4％，NiO：1-3％， B 2 O 3 ：0.2-1.2％，Al(NO 3 ) 3 ：0.3-0.5％，Y 2 O 3 :0.03-0.8% of auxiliary materials.
In the present embodiment, the particle size of ZnO may be 0.2um to 0.3um.
And S110, ball-milling and mixing the weighed components of the auxiliary materials, calcining, cooling and crushing, and then finely grinding and drying to obtain auxiliary material powder.
Specifically, the auxiliary materials are firstly mixed and ball-milled by a roller ball milling rotating speed of 30-60R/min, the ball milling time is 4-7 hours, then the mixture is calcined by a calcining furnace at 700-900 ℃, then the mixture is cooled and crushed, and then the fine grinding is carried out by a high-grade sand mill, for example, a planetary ball mill at the rotating speed of 600-1000R/min. Drying at 90-150 deg.C for 8-12 hr to obtain adjuvant powder. In an exemplary embodiment, the resulting adjuvant powder may have an average particle size of 0.3 to 0.5um.
S120, adding the auxiliary material powder, the main material ZnO, the organic binder, the dispersing agent, the defoaming agent, the deionized water, the water and the Al (NO) with the molar content of 0.003 percent based on the total amount of the auxiliary materials (all the auxiliary material powder except the main material ZnO) and the main material ZnO into a mixing tank 3 ) 3 9H 2 And O, mixing to form uniform slurry, and drying and granulating by a spray drying method to obtain granulated powder.
In this embodiment, the organic binder may be polyacrylate alcohol, the dispersant may be ammonium polyacrylate, the defoamer may be tributyl phosphate, and the deionized water may be ddH 2 o. The grain size of the obtained granulating powder is 7um-9um.
S130, pressing the obtained granulated powder into a green body of the resistor disc, and pre-sintering the green body of the resistor disc to obtain a blank of the resistor disc.
The obtained granulated powder can be pressed into green blanks of the resistance cards by a tablet press. The density of the green body of the resistance card is more than 3.3g/cm 3 。
In this example, the temperature raising procedure for the pre-sintering was: heating from room temperature to 150 ℃, and controlling the heating rate at 40-90 ℃/h; heating from 150 ℃ to 400 ℃, and controlling the heating rate at 50-80 ℃/h; raising the temperature from 400 ℃ to 700 ℃, and controlling the temperature raising rate at 80-90 ℃/h; keeping the temperature at 700 ℃ for 0.5-3 hours.
And S140, sintering the resistance card blank at a high temperature to obtain the coarse resistance card.
In this example, the temperature raising procedure for high-temperature firing was: heating from room temperature to 500 ℃, and controlling the heating rate at 100-120 ℃/h; heating to a sintering temperature from 500 ℃, wherein the heating rate is controlled to be 60-80 ℃/h, and the sintering temperature is 900-1150 ℃; and keeping the temperature at the sintering temperature for 3-7 hours.
And S150, grinding the coarse resistance card, and performing heat treatment, electrode spraying and glazing after grinding to obtain the high-gradient nonlinear resistance card.
In this embodiment, the temperature-raising procedure of the heat treatment may be: heating from room temperature to a heat treatment temperature, wherein the heating rate is controlled to be 80-110 ℃/h, and the heat treatment temperature is 350-500 ℃; and keeping the temperature for 2-4 hours at the heat treatment temperature.
Example 2
The high-gradient nonlinear resistance chip provided by the embodiment comprises the following components in percentage by mole: main material ZnO:65-90%, and Sb 2 O 3 ：2-8％，Bi2O3：2-6％，Co 2 O 3 ：0.2-3％，Co 3 O 4 ：0.5-1.2％，SiO 2 ：1-4％，MnO 2 ： 1-3％，Cr 2 O 3 ：2-4％，NiO：1-3％，B 2 O 3 ：0.2-1.2％，Al(NO 3 ) 3 ：0.3-0.5％，Y 2 O 3 :0.03-0.8% of auxiliary materials.
The present embodiment has the same preparation steps as the high-gradient nonlinear resistance chip provided in embodiment 1, except that the particle size of ZnO is 0.3um, and the average particle size of the auxiliary material is 0.3um to 0.5um.
Comparative example
The high-gradient nonlinear resistance chip provided by the comparative example comprises the following components in percentage by mole: main material ZnO:65-90%, and Sb 2 O 3 ：2-8％，Bi2O3：2-6％，Co 2 O 3 ：0.2-3％，Co 3 O 4 ：0.5-1.2％，SiO 2 ：1-4％，MnO 2 ： 1-3％，Cr 2 O 3 ：2-4％，NiO：1-3％，B 2 O 3 ：0.2-1.2％，Al(NO 3 ) 3 ：0.3-0.5％，Y 2 O 3 :0.03-0.8% of auxiliary materials.
The preparation steps of the high-gradient nonlinear resistor chip provided in this embodiment are the same as those of the high-gradient nonlinear resistor chip provided in embodiment 1, except that the particle size of ZnO is 0.5um, and the average particle size of the auxiliary material is 10um to 20um.
The non-linear characteristics of the resistive sheets prepared in example 2 and comparative example were measured by measuring the voltage across the sheet when a direct current of 1mA was applied (U1 mA) and the voltage across the sheet when a lightning wave of 8/20s was applied (U5 kA), and the ratio thereof was the residual voltage ratio (K), i.e., the non-linear characteristics. The ratio of the 1mA voltage to the thickness of the resistive sheet is called the potential gradient (E1 mA) of the resistive sheet, the high-gradient resistive sheet refers to the E1mA more than 300V/mm, and the measurement results are shown in the tables 1 and 2.
TABLE 1
TABLE 2
As can be seen from tables 1 and 2, although the main material and the auxiliary material have the same components and the same preparation process, the obtained resistance card has different potential gradients, residual pressure ratios and energy densities due to different particle sizes of the main material and the auxiliary material. The potential gradient of the resistance chip obtained in the embodiment 3 is obviously larger than that of the resistance chip obtained in other proportions, the residual voltage ratio is lower, and the energy density is larger.
A group of formulations of the zinc oxide resistance chip serial number 3 obtained in example 2 were subjected to 5 tests in total, including a residual voltage test, a repeated transfer charge tolerance test, a long-term stability test, a large current impact tolerance test, and an action load test, and the test items and results are as follows:
the apparatus used in the examples of the present invention are shown in the following table:
although some specific embodiments of the present invention have been described in detail by way of example, it should be understood by those skilled in the art that the above examples are for illustration only and are not intended to limit the scope of the invention. It will also be appreciated by those skilled in the art that various modifications may be made to the embodiments without departing from the scope and spirit of the invention. The scope of the present disclosure is defined by the appended claims.
Claims (10)
1. A high-gradient nonlinear resistance chip is characterized by comprising the following components in percentage by mole: main material ZnO:65-90%, and Sb 2 O 3 ：2-8％，Bi 2 O 3 ：2-6％，Co 2 O 3 ：0.2-3％，Co 3 O 4 ：0.5-1.2％，SiO 2 ：1-4％，MnO 2 ：1-3％，Cr 2 O 3 ：2-4％，NiO：1-3％，B 2 O 3 ：0.2-1.2％，Al(NO 3 ) 3 ：0.3-0.5％，Y 2 O 3 :0.03-0.8% of auxiliary materials.
2. The high-gradient nonlinear resistor sheet in claim 1, wherein the grain size of ZnO is 0.2um-0.3um; the average particle diameter of the auxiliary materials is 0.3-0.5um.
3. The high-gradient nonlinear resistive sheet according to claim 1, wherein the gradient of the resistive sheet is more than 500V/mm, and the energy density of the resistive sheet is more than 250J/cm 3 And the impact change rate is less than 5 percent.
4. A preparation method of a high-gradient nonlinear resistance chip is characterized by comprising the following steps:
weighing the following components in percentage by mole: main material ZnO:65-90%, and Sb 2 O 3 ：2-8％，Bi 2 O 3 ：2-6％，Co 2 O 3 ：0.2-3％，Co 3 O 4 ：0.5-1.2％，SiO 2 ：1-4％，MnO 2 ：1-3％，Cr 2 O 3 ：2-4％，NiO：1-3％，B 2 O 3 ：0.2-1.2％，Al(NO 3 ) 3 ：0.3-0.5％，Y 2 O 3 :0.03-0.8% of auxiliary materials;
ball-milling and mixing the weighed components of the auxiliary materials, calcining, cooling and crushing the components, and then finely grinding and drying the components to obtain auxiliary material powder;
adding auxiliary material powder, znO as main material, organic adhesive, dispersant, defoaming agent, deionized water, water and 0.003 mol% Al (NO) based on the total amount of the auxiliary material powder and the ZnO as main material into a mixing tank 3 ) 3 9H 2 Mixing O to form uniform slurry, and drying and granulating by a spray drying method to obtain granulated powder;
pressing the obtained granulated powder into a green body of the resistance card, and pre-sintering the green body of the resistance card to obtain a green material of the resistance card;
firing the resistance card blank at a high temperature to obtain a coarse resistance card;
and grinding the coarse resistance chip, and performing heat treatment, electrode spraying and glazing after the chip to obtain the high-gradient nonlinear resistance chip.
5. The method according to claim 4, wherein the particle size of the main material ZnO is 0.2um-0.3um; the average particle diameter of the adjuvant powder is 0.3-0.5um.
6. The method of claim 4, wherein the particle size of the granulated powder is 7um to 9um.
7. The method of claim 4, wherein the green resistor disc has a density greater than 3.3g/cm 3 。
8. The method according to claim 4, wherein the pre-sintering is carried out by a temperature-raising procedure comprising: heating from room temperature to 150 ℃, and controlling the heating rate at 40-90 ℃/h; heating from 150 ℃ to 400 ℃, and controlling the heating rate at 50-80 ℃ per hour; the temperature is increased from 400 ℃ to 700 ℃, and the temperature increase rate is controlled to be
Keeping the temperature at 700 ℃ for 0.5-3 hours.
9. The method according to claim 4, wherein the temperature raising procedure for the high-temperature firing is: heating from room temperature to 500 ℃, and controlling the heating rate at 100-120 ℃/h; heating to a sintering temperature from 500 ℃, wherein the heating rate is controlled to be 60-80 ℃ per hour, and the sintering temperature is 900-1150 ℃; and keeping the temperature at the sintering temperature for 3-7 hours.
10. The method according to claim 4, wherein the temperature-raising procedure of the heat treatment is: heating from room temperature to a heat treatment temperature, wherein the heating rate is controlled to be 80-110 ℃/h, and the heat treatment temperature is 350-500 ℃; and keeping the temperature for 2-4 hours at the heat treatment temperature.
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