CN104844175A - Electroceramic added with CaB2O4 seed crystal and CaB2O4 seed non-crystal and preparation method of electroceramic - Google Patents
Electroceramic added with CaB2O4 seed crystal and CaB2O4 seed non-crystal and preparation method of electroceramic Download PDFInfo
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- CN104844175A CN104844175A CN201510219978.1A CN201510219978A CN104844175A CN 104844175 A CN104844175 A CN 104844175A CN 201510219978 A CN201510219978 A CN 201510219978A CN 104844175 A CN104844175 A CN 104844175A
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Abstract
The invention discloses an electroceramic added with CaB2O4 seed crystal and CaB2O4 seed non-crystal and a preparation method of the electroceramic. The electroceramic is prepared from such raw materials in percentage by weight as 10-20% of SiO2, 10-25% of Al2O3, 10-20% of Fe2O3, 1-5% of TiO2, 2-10% of CaO, 0-3% of MgO, 5-15% of K2O, 3-8% of Na2O, 1.0-7.5% of CaB2O4 seed crystal and 1.0-7.5% of CaB2O4 seed non-crystal. As the CaB2O4 seed crystal and the CaB2O4 seed non-crystal are added, the sintering process of the electroceramic can be accelerated, the density of the electroceramic can be increased and the breaking strength of the electroceramic can be remarkably enhanced; besides, due to the addition of the CaB2O4 seed crystal and the CaB2O4 seed non-crystal, the crystallization of the mullite phase also can be effectively promoted, and therefore, the mechanical strength of the electroceramic can be remarkably improved. The preparation raw materials of the electroceramic are simple and easily available, and the process is stable and mature, and satisfies the practical and industrial conditions.
Description
Technical field
The invention belongs to high tension insulator field, be specifically related to a kind of interpolation CaB
2o
4seed crystal and CaB
2o
4electroceramics of seed amorphous and preparation method thereof.
Background technology
High tension insulator refers to that voltage rating is at the electrotechnical porcelain product higher than 1kV.Main finger is used for the insulating ceramic of ultra-high-tension power transmission line and power station and various electrical appliance, and also claiming insulator, is the important component part of power industry.High tension insulator difference of chemical composition contained by it is divided into siliceous electroceramics and aluminous lightning rob, aluminous lightning rob is divided into aluminium matter porcelain and high-strength aluminum porcelain, also different according to the different application field of electroceramics kind, the electroceramics that the present invention relates to belongs to high-strength aluminum porcelain, is mainly used in the insulator of extra-high tension insulator or high mechanical strength.Compare with external type of industry, domestic most enterprises state of the art is poor, causes quality product uneven.At present, intensity that is domestic, general porcelain is at 60-80kN/cm
2, the intensity of high-strength ceramic is at 100-180kN/cm
2, 15%-25% lower than the intensity of external homotype porcelain body.Therefore, electroceramics undercapacity is the most distinct issues of the domestic high tension insulator of restriction.Relevant research shows, in electroceramics, the content of mullite phase is the key (silicate circulate a notice of, 2010,29 (6): 1472-1477) determining its mechanical property especially breaking tenacity.
In recent years, domestic electric ceramic industry adjusts production technique one after another, all drops into a large amount of human and material resources and undergo technological transformation and upgrading in the formula, ball-milling technology, forming method, calcining system etc. of raw material.Wherein, by adjusting chemical constitution and the processing parameter of powder raw material, be the main path improving porcelain body performance at present.Such as West China Electric power Co, Fushun high-tech Electric Manufacture company limited, leaf victory equality patent applicant improve the electroceramics performance (patent No. 201310719303.4 respectively by composition of raw materials such as adjustment such as interpolation kaolin and illite clay, modified alta-mud, commercial alumina etc., 200610134907.2,200510134951.9).
Summary of the invention
In order to solve the difficult problem that above-mentioned domestic electroceramics faces, the invention provides a kind of interpolation CaB
2o
4seed crystal and CaB
2o
4electroceramics of seed amorphous and preparation method thereof.By adding appropriate CaB
2o
4seed crystal and CaB
2o
4seed amorphous, can not only improve the mobility of electroceramics in sintering process, effectively reduces the sintering temperature of electroceramics, reduces energy consumption, can improve the density of electroceramics simultaneously, significantly strengthens the breaking tenacity of electroceramics; And, CaB
2o
4seed crystal and CaB
2o
4seed amorphous add the crystallization that effectively can also promote mullite phase, thus significantly improve the physical strength of electroceramics.
The present invention implements by following technical solution:
A kind of interpolation CaB
2o
4seed crystal and CaB
2o
4the electroceramics of seed amorphous, raw material composition percentage: SiO
210 ~ 20%, Al
2o
310 ~ 25%, Fe
2o
310 ~ 20%, TiO
21 ~ 5%, CaO 2 ~ 10%, MgO 0 ~ 3%, K
2o 5 ~ 15%, Na
2o 3 ~ 8%, CaB
2o
4seed crystal 1.0-7.5% and CaB
2o
4seed amorphous 1.0-7.5%.
Preferably, raw material composition percentage: SiO
210 ~ 20%, Al
2o
310 ~ 25%, Fe
2o
310 ~ 20%, TiO
21 ~ 3%, CaO 4 ~ 10%, MgO 0 ~ 2%, K
2o 8 ~ 15%, Na
2o 3 ~ 8%, CaB
2o
4seed crystal 2.5-5.0% and CaB
2o
4seed amorphous 2.5-5.0%.
Preparation method comprises the following steps:
(1) prepare burden; Raw material dries 12h respectively at 90 ~ 100 DEG C, weighs, compounding ingredient by formula;
(2) ball milling; Adopt zirconium ball, the volume ratio of ball and material is 2:1, crosses 270 mesh sieves;
(3) deironing, press filt, old, pugging: to sieve deironing with the equipment for removing ferric ion of solenoid and permanent magnet, after the press filt that adds water, water ratio is 22%, and the old time is 72h, and vacuum tightness is pugging under 0.05 ~ 0.09MPa;
(4) shaping; Vacuum tightness is carry out extrusion molding under 0.01MPa, and molded samples is the column of diameter 2.3cm, long 13.6cm;
(5) dry; First dry in the shade 12h, then dry 48h at 90 ~ 100 DEG C;
(6) kiln sintering; Temperature rise rate is 5 DEG C/min, and sintering temperature is 1150 ~ 1260 DEG C, insulation 30min.
Remarkable advantage of the present invention is:
(1) during kiln in-furnace temperature <1100 DEG C, CaB
2o
4seed amorphous occurs softening, improves the mobility of electroceramics, fills electroceramics hole, improves the density of electroceramics;
(2) during kiln in-furnace temperature >1100 DEG C, CaB
2o
4seed crystal starts to melt (CaB
2o
4fusing point be 1122 ± 10 DEG C, J POWER SOURCES, 2011,196, P1321 – 1323), for the sintering process of electroceramics provides liquid phase, improve further the density of electroceramics;
(3) CaB
2o
4the nucleus that seed amorphous is formed in sintering process and CaB
2o
4the core of heterogeneous nucleation process in seed crystal shared electroceramics, the precipitation for mullite crystalline phase provides a large amount of forming core places, significantly promotes the precipitation of mullite phase;
(4) Si mostly is in electroceramics component
4+and Al
3+etc. small size ion, large-size ion Ca
2+introducing, the elastic strain energy of system can be increased, for the sintering of electroceramics and crystallization provide motivating force;
(5) Ca is passed through
2+replace Si
4+and Al
3+plasma, forms a large amount of oxygen vacancies in electroceramics, significantly improves the rate of diffusion of oxonium ion in electroceramics, also further promotes the sintering of electroceramics and the Crystallization Process of mullite phase;
(6) raw materials of the present invention is simple, is easy to get, and process stabilizing is ripe, reaches practical and industrialized condition.
Accompanying drawing explanation
Fig. 1 is the XRD figure of electroceramics after 1230 DEG C of sintering of adding different content compound seed crystal.
Embodiment
A kind of interpolation CaB
2o
4seed crystal and CaB
2o
4the electroceramics of seed amorphous, raw material composition percentage: SiO
210 ~ 20%, Al
2o
310 ~ 25%, Fe
2o
310 ~ 20%, TiO
21 ~ 5%, CaO 2 ~ 10%, MgO 0 ~ 3%, K
2o 5 ~ 15%, Na
2o 3 ~ 8%, CaB
2o
4seed crystal 1.0-7.5% and CaB
2o
4seed amorphous 1.0-7.5%.
Preparation method comprises the following steps:
(1) prepare burden; Raw material dries 12h respectively at 90 ~ 100 DEG C, weighs, compounding ingredient by formula;
(2) ball milling; Adopt zirconium ball, the volume ratio of ball and material is 2:1, crosses 270 mesh sieves;
(3) deironing, press filt, old, pugging: to sieve deironing with the equipment for removing ferric ion of solenoid and permanent magnet, after the press filt that adds water, water ratio is 22%, and the old time is 72h, and vacuum tightness is pugging under 0.05 ~ 0.09MPa;
(4) shaping; Vacuum tightness is carry out extrusion molding under 0.01MPa, and molded samples is the column of diameter 2.3cm, long 13.6cm;
(5) dry; First dry in the shade 12h, then dry 48h at 90 ~ 100 DEG C;
(6) kiln sintering; Temperature rise rate is 5 DEG C/min, and sintering temperature is 1150 ~ 1260 DEG C, insulation 30min.
Table 1 is the electroceramics component table (mass percent) in embodiment 1-6
Embodiment 1: the preparation of electroceramics and sintering
According to the proportioning of each component of table 1, take a certain amount of raw material (Samantabhadra soil, Xia Xitu, elutriation soil, lithium feldspar, ZhangZhou soil, flint clay, Feldspar Powder, bauxitic clay, compound seed crystal), then carry out ball milling, deironing, press filt, old, pugging, the operation such as shaping and dry successively according to aforesaid ceramic preparation step.Dried sample is placed in program control stove and sinters.Add 2% compound seed crystal (CaB
2o
4seed crystal and CaB
2o
4seed amorphous is respectively 1%) sample 1230 DEG C sintering after thing phase composite as shown in Figure 1.Known by quantitative analysis, in this sample, the mass percent of contained mullite phase (ICCD79-1458) is 15.2%.The breaking tenacity of sample is lower, is only 1366 ± 10MPa.
Embodiment 2: the preparation of electroceramics and sintering
According to the proportioning of each component of table 1, take a certain amount of raw material (Samantabhadra soil, Xia Xitu, elutriation soil, lithium feldspar, ZhangZhou soil, flint clay, Feldspar Powder, bauxitic clay, compound seed crystal), then prepare electroceramics according to the technique of example 1.As shown in Figure 1,5% compound seed crystal (CaB is added
2o
4seed crystal and CaB
2o
4seed amorphous is respectively 2.5%) sample 1230 DEG C sintering after can improve mullite phase content further.Wherein, mullite phase mass percent is 17.6%.Now the breaking tenacity of sample is 1421 ± 10MPa, and breaking tenacity improves compared with original formulation.
Embodiment 3: the preparation of electroceramics and sintering
According to the proportioning of each component of table 1, take a certain amount of raw material (Samantabhadra soil, Xia Xitu, elutriation soil, lithium feldspar, ZhangZhou soil, flint clay, Feldspar Powder, bauxitic clay, compound seed crystal), then prepare electroceramics according to the technique of example 1.As shown in Figure 1,7.5% compound seed crystal (CaB is added
2o
4seed crystal and CaB
2o
4seed amorphous is respectively 2.5% and 5.0%) sample 1230 DEG C sintering after can improve mullite phase content further.Wherein, mullite phase mass percent is 25.3%.Now the breaking tenacity of sample is 1612 ± 14MPa, and breaking tenacity improves compared with original formulation.
Embodiment 4: the preparation of electroceramics and sintering
According to the proportioning of each component of table 1, take a certain amount of raw material (Samantabhadra soil, Xia Xitu, elutriation soil, lithium feldspar, ZhangZhou soil, flint clay, Feldspar Powder, bauxitic clay, compound seed crystal), then prepare electroceramics according to the technique of example 1.As shown in Figure 1,7.5% compound seed crystal (CaB is added
2o
4seed crystal and CaB
2o
4seed amorphous is respectively 5.0% and 2.5%) sample 1230 DEG C sintering after can improve mullite phase content further.Wherein, mullite phase mass percent is 26.1%.The breaking tenacity of sample is 1661 ± 16MPa, and breaking tenacity improves compared with original formulation.
Embodiment 5: the preparation of electroceramics and sintering
According to the proportioning of each component of table 1, take a certain amount of raw material (Samantabhadra soil, Xia Xitu, elutriation soil, lithium feldspar, ZhangZhou soil, flint clay, Feldspar Powder, bauxitic clay, compound seed crystal), then prepare electroceramics according to the technique of example 1.As shown in Figure 1,10% compound seed crystal (CaB is added
2o
4seed crystal and CaB
2o
4seed amorphous is respectively 5.0% and 5.0%) sample 1230 DEG C sintering after can improve mullite phase content further.Wherein, the mass percent of mullite phase is 43.7%.The breaking tenacity of sample is 1961 ± 17MPa.This embodiment is preference.
Embodiment 6: the preparation of electroceramics and sintering
According to the proportioning of each component of table 1, take a certain amount of raw material (Samantabhadra soil, Xia Xitu, elutriation soil, lithium feldspar, ZhangZhou soil, flint clay, Feldspar Powder, bauxitic clay, compound seed crystal), then prepare electroceramics according to the technique of example 1.As shown in Figure 1,15% compound seed crystal (CaB is added
2o
4seed crystal and CaB
2o
4seed amorphous is respectively 7.5% and 7.5%) sample 1230 DEG C sintering after can improve mullite phase content further.Wherein, the mass percent of mullite phase is 49.6%.The breaking tenacity of sample is 2383 ± 16MPa, and breaking tenacity improves greatly compared with original formulation.This embodiment is preference.
The present invention obtains the electroceramics with high breaking tenacity by above-described embodiment.Its significant effect embodies a concentrated reflection of in the lifting of electroceramics breaking tenacity.From the XRD figure of above embodiment, work as CaB
2o
4seed crystal and CaB
2o
4the best results when ratio of seed amorphous is 1:1, significantly can promote the formation of mullite phase when compound seed crystal content is 10-15%, thus effectively improves the intensity of electroceramics.
The present invention relates generally to high tension insulator field, can make different shape as required for use.
The foregoing is only preferred embodiment of the present invention, all equalizations done according to the present patent application the scope of the claims change and modify, and all should belong to covering scope of the present invention.
Claims (3)
1. one kind is added CaB
2o
4seed crystal and CaB
2o
4the electroceramics of seed amorphous, is characterized in that: raw material composition percentage: SiO
210 ~ 20%, Al
2o
310 ~ 25%, Fe
2o
310 ~ 20%, TiO
21 ~ 5%, CaO 2 ~ 10%, MgO 0 ~ 3%, K
2o 5 ~ 15%, Na
2o 3 ~ 8%, CaB
2o
4seed crystal 1.0-7.5% and CaB
2o
4seed amorphous 1.0-7.5%.
2. interpolation CaB according to claim 1
2o
4seed crystal and CaB
2o
4the electroceramics of seed amorphous, is characterized in that: raw material composition percentage: SiO
210 ~ 20%, Al
2o
310 ~ 25%, Fe
2o
310 ~ 20%, TiO
21 ~ 3%, CaO 4 ~ 10%, MgO 0 ~ 2%, K
2o 8 ~ 15%, Na
2o 3 ~ 8%, CaB
2o
4seed crystal 2.5-5.0% and CaB
2o
4seed amorphous 2.5-5.0%.
3. prepare and add CaB as claimed in claim 1 for one kind
2o
4seed crystal and CaB
2o
4the method of the electroceramics of seed amorphous, is characterized in that: comprise the following steps:
(1) prepare burden; Raw material dries 12h respectively at 90 ~ 100 DEG C, weighs, compounding ingredient by formula;
(2) ball milling; Adopt zirconium ball, the volume ratio of ball and material is 2:1, crosses 270 mesh sieves;
(3) deironing, press filt, old, pugging: to sieve deironing with the equipment for removing ferric ion of solenoid and permanent magnet, after the press filt that adds water, water ratio is 22%, and the old time is 72h, and vacuum tightness is pugging under 0.05 ~ 0.09MPa;
(4) shaping; Vacuum tightness is carry out extrusion molding under 0.01MPa;
(5) dry; First dry in the shade 12h, then dry 48h at 90 ~ 100 DEG C;
(6) kiln sintering; Temperature rise rate is 5 DEG C/min, and sintering temperature is 1150 ~ 1260 DEG C, insulation 30min.
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CN112898003A (en) * | 2021-03-18 | 2021-06-04 | 湖南省醴陵市华电电瓷制造有限公司 | High-strength siliceous brown glaze electric porcelain and preparation method thereof |
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CN112898003A (en) * | 2021-03-18 | 2021-06-04 | 湖南省醴陵市华电电瓷制造有限公司 | High-strength siliceous brown glaze electric porcelain and preparation method thereof |
CN112898003B (en) * | 2021-03-18 | 2021-09-21 | 湖南省醴陵市华电电瓷制造有限公司 | High-strength siliceous brown glaze electric porcelain and preparation method thereof |
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