CN114907098A - High-strength electroceramic blank with uniform microstructure and preparation method thereof - Google Patents

High-strength electroceramic blank with uniform microstructure and preparation method thereof Download PDF

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CN114907098A
CN114907098A CN202110179517.1A CN202110179517A CN114907098A CN 114907098 A CN114907098 A CN 114907098A CN 202110179517 A CN202110179517 A CN 202110179517A CN 114907098 A CN114907098 A CN 114907098A
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strength
electroceramic
blank
uniform microstructure
soil
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袁志勇
栾艺娜
杨海
徐炎
罗志强
陈章彪
韩佑民
陈震
林建远
刘强
刘淑兰
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SINOMA JIANGXI ELECTRICAL PORCELAIN ELECTRIC CO LTD
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SINOMA JIANGXI ELECTRICAL PORCELAIN ELECTRIC CO LTD
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Abstract

The invention discloses a high-strength electroceramic blank with a uniform microstructure and a preparation method thereof, solves the problems of nonuniform microstructure, low strength and high strength dispersity of the conventional electroceramic material, and relates to the technical field of ceramics. The invention controls Al in the electroceramic material 2 O 3 Content of Al 2 O 3 Crystal form, K 2 O+Na 2 The amount of O + CaO + MgO and the fineness of ball-milling particles are less than or equal to 5 mu m, and the high-strength electroceramic blank with a uniform microstructure is prepared, and the three-dimensional interweaved acicular secondary mullite phase and the enhanced high-alumina glass phase are uniformly distributed in the high-strength electroceramic blank.

Description

High-strength electric porcelain body with uniform microstructure and preparation method thereof
Technical Field
The invention relates to the technical field of ceramics, in particular to a high-strength electroceramic blank body with a uniform microstructure and a preparation method thereof.
Background
With the rise of the voltage grade of a power system and the increase of the transmission capacity of the system, increasingly high requirements are put forward on the mechanical properties of strength, electromechanical breaking load and the like of the electroceramic.
The mechanical property of the electric porcelain material is closely related to the microstructure of the electric porcelain material, and if the microstructure of the electric porcelain material is not uniform, the internal stress distribution of the electric porcelain material is not uniform, so that the strength of the electric porcelain is reduced. The existing high-strength electric porcelain takes a corundum phase as a framework, the grain size of the corundum phase is much larger than that of a mullite crystal phase in an electric porcelain material, the thick corundum phase destroys the uniformity of a microstructure in the electric porcelain, so that the strength of the electric porcelain material is poor, and the more the corundum phase in the electric porcelain material is, the poorer the uniformity of the microstructure in the electric porcelain material is, and the lower the strength of the electric porcelain is. In addition, because cracks are more easily generated around larger corundum phase particles in the electric ceramic material, the more corundum phase particles are contained in the electric ceramic material, the higher the probability of large-size along-crystal cracks generated in the electric ceramic material is, the smaller the surface energy required by large-size crack propagation is, the smaller the yield force along the crystal is, the higher the probability of fracture is, and the electric ceramic material has low strength and high strength dispersity.
Disclosure of Invention
Aiming at the problems of nonuniform microstructure, low strength and high strength dispersity of the existing electric porcelain material, the application provides a high-strength electric porcelain blank body which does not have corundum and other large-particle crystal grains and is completely composed of a three-dimensional interweaving needle-shaped secondary mullite reinforced high-alumina glass phase and has uniform microstructure and a preparation method thereof.
The technical scheme adopted by the application for solving the technical problems is as follows:
a preparation method for preparing a high-strength electroceramic blank with a uniform microstructure comprises the following steps:
1) calcining an alumina raw material to obtain calcined alumina;
2) mixing a clay raw material, potassium feldspar and the calcined alumina obtained in the step 1) to obtain a mixed material, adding water into the mixed material, ball-milling, and sieving to remove iron to obtain required slurry;
3) carrying out filter pressing dewatering, rough refining, ageing and vacuum pugging on the mud obtained in the step 2) to obtain the required pug;
4) the pug prepared in the step 3) is subjected to fettling, drying, glazing and sanding to prepare a required blank body;
5) sintering the blank prepared in the step 4) to prepare the required electrotechnical porcelain blank.
Preferably, the calcination temperature in the step 1) is 1350-1500 ℃, and the calcination heat preservation time is 30-60 min.
Preferably, the proportion of the raw materials in the step 2) is calcined alumina: 15-25 wt%, potassium feldspar: 18-22 wt% of clay raw material: 54 to 76 wt%.
Preferably, the clay raw material in the step 2) comprises Chaozhou soil, first-grade Jilin ball soil and elutriation method soil.
Preferably, the ratio of the clay raw material is Chaozhou soil: 18 to 25 wt%; first-grade Jilin ball clay: 5-10 wt%; elutriation method reservoir soil: 25 to 35 wt%.
Preferably, the chemical components of the mixed material in the step 2) include: al (aluminum) 2 O 3 ：38～50wt％、SiO 2 ：40～50wt％、K 2 O: 3.0 to 4.0 wt% and Na 2 O + CaO + MgO, wherein K 2 O+Na 2 The proportion of O + CaO + MgO in the total mixed material is as follows: 3.5 to 5 wt%.
Preferably, the slurry particles with the fineness less than or equal to 5 mu m after ball milling in the step 2) account for more than 75 percent of the total amount of the slurry.
Preferably, the sintering temperature of the blank in the step 4) is 1230-1260 ℃, and the sintering time is controlled to be 30-60 min.
The application also discloses a high-strength electric porcelain body with a uniform microstructure, which is prepared by the preparation method of the high-strength electric porcelain body with a uniform microstructure.
Preferably, the high-strength electroceramic body with a uniform microstructure is internally provided with a three-dimensional interwoven acicular secondary mullite phase and a glass phase, and the three-dimensional interwoven acicular secondary mullite phase and the reinforced glass phase are uniformly distributed.
The beneficial effects of the invention are:
a) the alumina raw material is calcined to make the gamma-Al in the alumina raw material 2 O 3 And alpha-Al having a poor degree of crystallization 2 O 3 Completely converted into alpha-Al with good crystallization 2 O 3 The sintering temperature in the subsequent sintering process can be reduced, the sintering range is expanded, and the material densification sintering is realized.
b) By controlling Al in the electroceramic material 2 O 3 On the one hand, the strength of the glass phase is enhanced; on the other hand, Al 2 O 3 With SiO 2 The secondary mullite whiskers are precipitated to further enhance the strength of a glass phase and the strength of the electric porcelain material as a whole.
c) By controlling K 2 O+Na 2 The content of the glass phase in the electric porcelain body is controlled by the amount of O + CaO + MgO, so that the problems that the inter-crystal porosity of the material is large and the porosity of the material is large due to the too low content of the glass phase, and the strength of the material is further low are avoided; and the phenomenon that the strength of the corresponding electric porcelain material is lower because the glass phase is mainly used as the glass phase due to overhigh content of the glass phase is avoided, and finally the high-strength electric porcelain blank body with a uniform microstructure and enhanced by the secondary mullite whiskers is obtained.
d) By controlling K in the electroceramic material 2 The content of O improves the viscosity of the high-temperature liquid phase, can effectively avoid the excessive growth of secondary mullite, and is beneficial to preparing the high-strength electroceramic blank with uniform microstructure.
e) By controlling the particle fineness of the slurry particle which is less than or equal to 5 mu m after ball milling in the preparation method of the electric ceramic body to account for more than 75 percent of the total slurry amount, the problem that coarse corundum or quartz particles possibly appear in a final product due to the fact that the particle size of the slurry after ball milling is too coarse and the coarse corundum and quartz particles cannot be completely dissolved in the sintering process, and influence on the uniformity of the microstructure in the electric ceramic body and the mechanical property of the electric ceramic body is avoided.
f) By controlling the sintering temperature and time of the electric porcelain green body, the sintering compactness of the electric porcelain green body is ensured, meanwhile, the mullite is prevented from growing too fast and too large, and the high-strength electric porcelain green body with a uniform microstructure can be further ensured to be prepared.
Compared with the common electric porcelain, the high-strength electric porcelain blank with the uniform microstructure disclosed by the application has the advantages that as the large-particle corundum phase does not exist, and the three-dimensional interwoven acicular secondary mullite phase and the enhanced high-alumina glass phase are uniformly distributed, the internal microstructure of the aluminum porcelain is uniformly distributed, cracks are not easy to generate, and the high strength is maintained under the toughening effect of the three-dimensional interwoven acicular secondary mullite phase.
Drawings
FIG. 1 is a schematic scanning electron microscope diagram of a high-strength electroceramic blank with a uniform microstructure after the glass phase has been etched away in example 1 of the present invention.
FIG. 2 is a spectrum diagram of a high-strength electroceramic body with a uniform microstructure according to example 1 of the present invention.
FIG. 3 is a schematic scanning electron microscope diagram of the high-strength electroceramic blank with a uniform microstructure after the glass phase has been etched away in example 2 of the present invention.
FIG. 4 is a schematic scanning electron microscope diagram of the high-strength electroceramic blank with a uniform microstructure after the glass phase has been etched away in example 3 of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the following examples, but the present invention is not limited to the following examples.
Example 1
1) Calcining the alumina at 1420 ℃ for 40min to obtain calcined alumina;
2) subjecting the calcined alumina obtained in step 1): 22 wt% and potassium feldspar: 21 wt%, Chaozhou soil: 20 wt%, first grade Jilin ball soil: 8% of elutriation method reservoir soil: 29 percent of the raw materials are mixed to obtain a mixed material, the mixed material is added with water and ball-milled, the slurry particles with the fineness of less than or equal to 5 mu m after ball milling account for more than 75 percent of the total amount of the slurry, and the required slurry is obtained after sieving and iron removal;
3) carrying out filter pressing dewatering, rough refining, ageing and vacuum pugging on the mud obtained in the step 2) to obtain the required pug;
4) the mud material prepared in the step 3) is subjected to fettling, drying, glazing and sanding to prepare a required blank body;
5) sintering the green body prepared in the step 4) at 1250 ℃, and preserving heat for 0.5h to prepare the required electric porcelain green body.
Wherein, the raw materials of Chaozhou soil, first-grade Jilin ball soil and elutriation method reservoir soil used in the step 2 are all sold in the market.
The chemical components of the mixed material in the step 2) comprise Al 2 O 3 ：43.5wt％、SiO 2 ：47.5wt％、K 2 O+Na 2 O + CaO + MgO: 4.1 wt%, wherein, K 2 O：3.1wt％。
The scanning photograph of the electroceramic body obtained in this example after the glass phase is etched away is shown in fig. 1, and it can be seen from fig. 1 that the inside of the electroceramic body is mainly three-dimensionally interlaced needle-shaped, and is secondary mullite whiskers, and the secondary mullite whiskers are uniformly distributed. The energy spectrum analysis result of the prepared electric porcelain body is shown in figure 2, the molar ratio of Al, Si and O is 4.1:1:7.8, and the molar ratio is very close to mullite 2Al 2 O 3 .SiO 2 The theoretical molar ratio of Al, Si and O is 4:1:8, so the three-dimensional interweaving needle-shaped substance in the microscopic picture is mullite. The strength of the electroceramic blank test strip with the diameter of about 20mm and the length of about 130mm is 202.67 +/-4.98 MPa when the electroceramic blank test strip is measured by a three-point bending method.
Example 2
1) Calcining alumina at 1420 deg.C for 40min to obtain calcined alumina;
2) calcining the alumina obtained in step 1: 22 wt% and potassium feldspar: 21 wt%, Chaozhou soil: 20 percent, first-grade Jilin ball soil: 8% of elutriation method reservoir soil: 29 percent of the raw materials are mixed to obtain a mixed material, the mixed material is added with water and ball-milled, the slurry particles with the fineness of less than or equal to 5 mu m after ball milling account for more than 75 percent of the total amount of the slurry, and the required slurry is obtained after sieving and iron removal;
3) carrying out filter pressing dewatering, rough refining, ageing and vacuum pugging on the slurry obtained in the step 2 to obtain required pug;
4) the pug prepared in the step 3 is subjected to fettling, drying, glazing and sanding to prepare a required blank body;
5) and (4) sintering the blank prepared in the step (4) at 1250 ℃, and preserving heat for 1h to prepare the required electroceramic blank.
Wherein, the raw materials of Chaozhou soil, first-grade Jilin ball soil and elutriation method reservoir soil used in the step 2 are all sold in the market.
The chemical components of the mixed material in the step 2) comprise Al 2 O 3 ：43.5wt％、SiO 2 ：47.5wt％、K 2 O+Na 2 O + CaO + MgO: 4.1 wt% of K 2 O：3.1wt％。
A scanning photograph of the electroceramic body obtained in this example after the glass phase is etched away is shown in fig. 3, and it can be seen from fig. 3 that the inside of the electroceramic body is mainly three-dimensionally interlaced acicular, and is secondary mullite whiskers, and the secondary mullite whiskers are uniformly distributed. The strength of the electroceramic blank test strip with the diameter of about 20mm and the length of about 130mm is 200.59 +/-8.40 MPa when measured by a three-point bending method.
Example 3
1) Calcining the alumina at 1420 ℃ for 40min to obtain calcined alumina;
2) calcining the alumina obtained in step 1: 22 wt% and potassium feldspar: 21 wt%, Chaozhou soil: 20 wt%, first grade Jilin ball soil: 8 wt%, elutriation method reservoir soil: 29 wt%, mixing to obtain a mixed material, adding water into the mixed material, ball-milling, controlling slurry particles with the fineness of less than or equal to 5 mu m of the ball-milled slurry particles to account for more than 75% of the total amount of the slurry, and sieving to remove iron to obtain the required slurry;
3) the mud obtained in the step 2 is subjected to filter pressing, dewatering, rough smelting, ageing and vacuum pugging to prepare the required pug;
4) the pug prepared in the step 3 is subjected to fettling, drying, glazing and sanding to prepare a required blank body;
5) and (5) sintering the blank prepared in the step (4) at 1250 ℃, and preserving heat for 2 hours to prepare the required electric porcelain blank.
Wherein, the raw materials of Chaozhou soil, first-grade Jilin ball soil and elutriation method reservoir soil used in the step 2 are all sold in the market.
The chemical components of the mixed material in the step 2) comprise Al 2 O 3 ：43.5wt％、SiO 2 ：47.5wt％、K 2 O+Na 2 O + CaO + MgO: 4.1 wt% of K 2 O：3.1wt％。
Fig. 4 shows a scanning photograph of the electroceramic body obtained in this example after the glass phase has been etched away, and as can be seen from fig. 4, the inside of the electroceramic body is mainly in the form of three-dimensional interlaced needle, and is made of secondary mullite whiskers. The strength of the electroceramic blank test strip with the diameter of about 20mm and the length of about 130mm measured by a three-point bending method is 195.83 +/-13.97 MPa.
Example 4
1) Calcining the alumina at 1350 ℃ for 30min to obtain calcined alumina;
2) subjecting the calcined alumina obtained in step 1): 15 wt% and potassium feldspar: 18 wt%, Chaozhou soil: 25 wt%, first grade Jilin ball clay: 7% and elutriation method reservoir soil: 35 percent of the raw materials are mixed to obtain a mixed material, the mixed material is added with water and ball-milled, the slurry particles with the fineness less than or equal to 5 mu m after ball milling account for more than 75 percent of the total amount of the slurry, and the required slurry is obtained after sieving and iron removal;
3) carrying out filter pressing dewatering, rough refining, ageing and vacuum pugging on the mud obtained in the step 2) to obtain the required pug;
4) the pug prepared in the step 3) is subjected to fettling, drying, glazing and sanding to prepare a required blank body;
5) sintering the blank prepared in the step 4) at 1230 ℃, and preserving the heat for 45min to prepare the required electric porcelain blank.
Wherein, the raw materials of Chaozhou soil, first-grade Jilin ball soil and elutriation method reservoir soil used in the step 2 are all sold in the market.
Example 5
1) Calcining the alumina at 1500 ℃ for 30min to obtain calcined alumina;
2) subjecting the calcined alumina obtained in step 1): 25 wt% and potassium feldspar: 22 wt%, Chaozhou soil: 23 wt%, first-grade Jilin ball clay: 5%, elutriation method reservoir soil: 25 percent of the raw materials are mixed to obtain a mixed material, the mixed material is added with water and ball-milled, the slurry particles with the fineness less than or equal to 5 mu m after ball milling account for more than 75 percent of the total amount of the slurry, and the required slurry is obtained after sieving and iron removal;
3) carrying out filter pressing dewatering, rough refining, ageing and vacuum pugging on the mud obtained in the step 2) to obtain the required pug;
4) the pug prepared in the step 3) is subjected to fettling, drying, glazing and sanding to prepare a required blank body;
5) sintering the blank prepared in the step 4) at 1260 ℃, and preserving heat for 30min to prepare the required electric porcelain blank.
Wherein, the raw materials of Chaozhou soil, first-grade Jilin ball soil and elutriation method reservoir soil used in the step 2 are all sold in the market.
Example 6
1) Calcining the alumina at 1500 ℃ for 30min to obtain calcined alumina;
2) subjecting the calcined alumina obtained in step 1): 25 wt% and potassium feldspar: 22 wt%, Chaozhou soil: 18 wt%, first grade Jilin ball soil: 10%, elutriation method reservoir soil: 25 percent of the raw materials are mixed to obtain a mixed material, water is added into the mixed material for ball milling, the slurry particles with the fineness of less than or equal to 5 mu m after ball milling account for more than 75 percent of the total amount of the slurry, and the required slurry is obtained after sieving and iron removal;
3) carrying out filter pressing dewatering, rough refining, ageing and vacuum pugging on the slurry obtained in the step 2) to obtain the required pug;
4) the mud material prepared in the step 3) is subjected to fettling, drying, glazing and sanding to prepare a required blank body;
5) sintering the blank prepared in the step 4) at 1260 ℃, and preserving heat for 45min to prepare the required electrotechnical porcelain blank.
Wherein, the raw materials used in the step 2 are all commercial Chaozhou soil, first-grade Jilin ball soil and elutriation method reservoir soil
The above are merely exemplary embodiments of the features of the present invention, and do not limit the scope of the present invention in any way. All technical solutions formed by adopting the equivalent exchange or the equivalent substitution fall within the protection scope of the present invention.

Claims (10)

1. A preparation method of a high-strength electroceramic blank with a uniform microstructure is characterized by comprising the following steps:
1) calcining an alumina raw material to obtain calcined alumina;
2) mixing a clay raw material, potassium feldspar and the calcined alumina obtained in the step 1) to obtain a mixed material, adding water into the mixed material, ball-milling, and sieving to remove iron to obtain required slurry;
3) carrying out filter pressing dewatering, rough refining, ageing and vacuum pugging on the slurry obtained in the step 2) to obtain the required pug;
4) the pug prepared in the step 3) is subjected to fettling, drying, glazing and sanding to prepare a required blank body;
5) sintering the blank prepared in the step 4) to prepare the required electrotechnical porcelain blank.
2. The method for preparing a high-strength electroceramic blank with a uniform microstructure according to claim 1, wherein the method comprises the following steps: the calcination temperature in the step 1) is 1350-1500 ℃, and the calcination time is 30-60 min.
3. The method for preparing the high-strength electroceramic body with uniform microstructure according to claim 1, characterized in that: the raw materials in the step 2) are clay raw materials in percentage by weight: 53-77 wt%, potash feldspar: 18-22 wt%, calcined alumina: 15 to 25 wt%.
4. The method for preparing a high-strength electroceramic blank with a uniform microstructure according to claim 1, wherein the method comprises the following steps: the clay raw materials in the step 2) comprise Chaozhou soil, first-grade Jilin ball soil and elutriation method reservoir soil.
5. The method for preparing the high-strength electroceramic body with uniform microstructure according to claim 4, wherein the method comprises the following steps: the proportion of the clay raw materials is Chaozhou soil: 18 to 25 wt%; first-grade Jilin ball clay: 5-10 wt%; elutriation method reservoir soil: 25 to 35 wt%.
6. The method for preparing a high-strength electroceramic blank with a uniform microstructure according to claim 1, wherein the method comprises the following steps: the chemical components of the mixed material in the step 2) comprise: al (aluminum) 2 O 3 ：38～50wt％、SiO 2 ：40～50wt％、K 2 O: 3.0 to 4.0 wt% and Na 2 O + CaO + MgO, wherein K 2 O+Na 2 The proportion of O + CaO + MgO in the total mixed material is 3.5-5 wt%.
7. The method for preparing a high-strength electroceramic blank with a uniform microstructure according to claim 1, wherein the method comprises the following steps: the slurry particles with the fineness less than or equal to 5 mu m after ball milling in the step 2) account for more than 75 percent of the total amount of the slurry.
8. The method for preparing a high-strength electroceramic blank with a uniform microstructure according to claim 1, wherein the method comprises the following steps: the sintering temperature of the blank in the step 4) is 1230-1260 ℃, and the sintering time is controlled to be 30-60 min.
9. The utility model provides a high strength electroceramics body that microstructure is even which characterized in that: the high-strength electric porcelain body with a uniform microstructure is prepared by the preparation method of the high-strength electric porcelain body with a uniform microstructure according to any one of claims 1 to 8.
10. The microstructurally homogeneous high-strength electroceramic body according to claim 9, characterized in that: the interior of the high-strength electroceramic body with uniform microstructure is a three-dimensional interwoven acicular secondary mullite phase and a glass phase, and the three-dimensional interwoven acicular secondary mullite phase and the reinforced glass phase are uniformly distributed.
CN202110179517.1A 2021-02-09 2021-02-09 High-strength electroceramic blank with uniform microstructure and preparation method thereof Pending CN114907098A (en)

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JPH03141181A (en) * 1989-10-24 1991-06-17 Saga Pref Gov Production of alumina ceramic having improved surface
US20020155943A1 (en) * 1999-09-03 2002-10-24 Johannes Liebermann Method for producing porcelain, porcelain and ceramic isolator formed from porcelain
CN101514099A (en) * 2009-03-26 2009-08-26 中国科学院地球化学研究所 Method for selection and proportioning of raw materials of 160,210kN grades suspension porcelain insulator blank
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Application publication date: 20220816