CN115304275B - Composite insulating glaze suitable for supercritical water application and processing method thereof - Google Patents

Composite insulating glaze suitable for supercritical water application and processing method thereof Download PDF

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CN115304275B
CN115304275B CN202210503514.3A CN202210503514A CN115304275B CN 115304275 B CN115304275 B CN 115304275B CN 202210503514 A CN202210503514 A CN 202210503514A CN 115304275 B CN115304275 B CN 115304275B
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composite insulating
temperature
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firing
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CN115304275A (en
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赵晓强
冯文慧
娄宗勇
贺晓
高轶德
吴靖宇
王博
张茉
胡旭
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Chengde Petroleum College
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Chengde Petroleum College
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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C8/00Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/50Improvements relating to the production of bulk chemicals
    • Y02P20/54Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids

Abstract

A composite insulating glaze suitable for supercritical water application comprises SiO 2 、BaO、CaO、ZnO and the like are used as processing raw materials and are prepared by the raw materials; grinding and crushing; fully mixing; filtering raw materials; coating; firing; detecting to finish the preparation of the product; the composite insulating glaze can not fall off after continuous 10 times of temperature shock impact in water at 450-20 ℃; the insulating resistance in the air is measured by placing the insulating material in the air at 15-450 ℃, and the insulating resistance is over 700MΩ after 120h test, so that the insulating performance is good; the insulating resistance of the alloy is measured every 180min after the alloy is placed in tap water at 20+/-5 ℃, the insulating resistance of the alloy is reduced to 0.8MΩ from initial 100MΩ after 72 h soaking, the alloy is placed in tap water and heated and pressurized for 72 h, and the insulating performance of the alloy is still better when the alloy is kept at 350 ℃ and 16.5MPa for 48 h, so that the requirement is completely met.

Description

Composite insulating glaze suitable for supercritical water application and processing method thereof
Technical Field
The invention relates to the technical field of composite materials, in particular to a glaze with insulation property suitable for supercritical water and a processing method thereof.
Background
With the continuous development of thickened oil thermal recovery technology, water retention measurement is extremely important in technical development; the technology for measuring the underground water retention rate by a capacitance method is mature, but the insulating material which can be stably used for a long time in the underground variable-temperature variable-pressure water environment becomes one of the difficult problems puzzled in the development of the technology.
The method is applied to detection, wherein the material matrix is a good conductor, and a thin-wall insulating layer is tightly laid on the outer side of the conductor; when the substrate with the insulating layer is immersed in water, the capacitance generated between the substrate and the water changes along with the change of the wetting area of the substrate, and the water retention rate is further reflected by the size of the capacitance; this requires that the insulating material outside the matrix must have good insulation, high temperature resistance, high voltage resistance in water, while requiring that the material is less affected by the surface tension of the water after it is immersed in water.
The main direction of the current research is focused on the research of the insulating property of the material in the air or the research of the insulating property of the material in the low-temperature normal-pressure water, and the research of the insulating property of the material in the water through temperature and pressure changing belongs to the technical blank; the traditional glaze is easy to fall off in a high-temperature state, the glaze does not have insulating property, and the insulating enamel is difficult to ensure long-term insulation under high pressure.
The technical scheme is that the basic ground glaze of the existing special glass is improved and modified, and the related processing technology is optimized, and the existing special glass ground glaze comprises raw materials such as silicon dioxide, barium oxide, calcium oxide, zinc oxide and the like.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a composite insulating glaze suitable for supercritical water application in a relatively harsh environment and a processing method thereof.
The invention is realized by the following technical scheme: a composite insulating glaze suitable for supercritical water application comprises SiO 2 、BaO、CaO、ZnO、B 2 O 3 、TiO 2 、Fe 2 O 3 、SO 3 、Cr 2 O 3 Clay, caSO 4 、MgSO 4 、Ca(OH) 2 、SiO 2 As a processing raw material.
Preferably, the specific components of the processing raw materials are as follows: 25.025% SiO2, 17.016% BaO, 4.600% CaO, 1.829% ZnO, 2.537% B2O3, 1.248% TiO2, 0.007% Fe2O3, 0.009% SO3, 17.491% Cr2O3, 2.966% clay, 6.818% CaSO4, 6.818% MgSO4, and 13.636% Ca (OH) 2.
A composite insulating glaze processing method suitable for supercritical water application comprises the following steps:
step one, raw material preparation: the above-mentioned raw materials were prepared by mixing 25.025% of SiO2, 17.016% of BaO, 4.600% of CaO, 1.829% of ZnO, 2.537% of B2O3, 1.248% of TiO2, 0.007% of Fe2O3, 0.009% of SO3, 17.491% of Cr2O3, 2.966% of clay, 6.818% of CaSO4, 6.818% of MgSO4 and 13.636% of Ca (OH) 2. Mixing the materials according to the proportion to obtain a mixture;
grinding and crushing: fully grinding the mixture obtained in the first step for 1-1.5 hours, and screening by using a screen to obtain a carefully selected raw material;
step three, fully mixing: mixing the carefully selected raw materials in the second step with distilled water according to the proportion of 7:5 to obtain a mixed raw material;
step four, filtering raw materials: filtering the mixed raw material obtained in the step three by using a 600-mesh screen to obtain a filtered mixture, standing the filtered mixture to obtain a material in a solid-liquid separation state, and discharging clear water at the upper part to obtain a precipitate at the bottom;
step five, coating: uniformly coating the precipitate obtained in the fourth step on an object to be processed to obtain a fired blank;
step six, firing: placing the fired blank obtained in the fifth step into a firing kiln, and fully firing to obtain a finished product material;
step seven, detecting: and D, detecting the finished material obtained in the step six.
Preferably, the screen in the second step is a 420-mesh stainless steel screen.
Preferably, the mixing method in the third step is as follows: then mixing the water with distilled water according to the mass ratio of 7:5, mixing and uniformly stirring, filtering the prepared liquid slurry by a 600-mesh sieve before use, standing for 2.5-3 hours after filtering, pumping clear water, and continuously stirring for 2 minutes at a stirring speed of 150 r/min.
Preferably, the water content of the precipitate in the fourth step is 16%.
Preferably, the coating method in the fifth step comprises the following steps: the object to be processed is quickly and vertically inserted into the sediment in the fourth step, dipped for 10 seconds and then vertically taken out and kept still for 2-3 minutes.
Preferably, the firing process in the sixth step is as follows: placing the fired blank into a firing kiln, wherein the kiln is a muffle furnace, the furnace temperature is respectively controlled to be fired for 40 minutes at 160 ℃, the furnace temperature is gradually controlled to be uniformly increased to 1200 ℃ after 60 minutes, the furnace temperature is kept at 1200 ℃ for 10 minutes, the furnace temperature is gradually controlled to be uniformly increased to 1280 ℃ after 20 minutes, the furnace temperature is kept at 1280 ℃ for 10 minutes, natural cooling is carried out to room temperature, and the muffle furnace is taken out and cleaned by acetone, thus the process is completed.
Preferably, the detection method in the step seven is as follows: filling tap water into a self-made stainless steel container for high-pressure test, mounting the blank sintered with the composite insulating glaze and the stainless steel container for high-pressure test in a muffle furnace, arranging a pressure release hole at the container and connecting a pressure gauge, and controlling the pressure to be not more than 12MPa by using a pressure regulating valve; in the experimental process, the temperature of the muffle furnace is regulated, data is recorded once after the temperature is increased by 30 ℃ and is constant, the continuous three-time temperature transformation rate is required to be not more than 1.0 ℃/10min during recording, the comprehensive temperature transformation rate is required to be not more than 2 ℃/30min, and meanwhile, the difference between the constant temperature and the set temperature is required to be not more than +/-5 ℃ until the temperature reaches 350 ℃.
Further, the detection standard of the step seven is as follows: the insulation resistance is not lower than 0.1MΩ at 350+ -10deg.C and 12+ -1 MPa.
The invention has the beneficial effects that: the composite insulating glaze can not fall off after continuous 10 times of impact of abrupt temperature change in water at 450-20 ℃.
The insulating resistance in the air is measured by placing the insulating material in the air at 15-450 ℃, and the insulating property is good when the insulating resistance is more than 700MΩ after 120h test.
The resistance of the alloy is measured every 180min after the alloy is placed in tap water with the temperature of 20+/-5 ℃ and the insulation resistance of the alloy is reduced from the initial 100MΩ to 0.8MΩ after 72 hours of soaking,
the insulating material is placed in tap water for 72 hours, heated and pressurized, and the insulating performance is still better when the insulating material is kept at 350 ℃ and 16.5MPa for 48 hours, so that the requirement is completely met.
Drawings
FIG. 1 is an overall process flow diagram of a composite insulating glaze processing method suitable for supercritical water applications.
Fig. 2 is a firing process flow diagram of step six of a composite insulating glaze processing method suitable for supercritical water application.
Detailed Description
In the description of the present invention, it is also to be noted that, unless explicitly stated and defined otherwise; the specific meaning of the above terms in the present invention will be understood in specific cases by those of ordinary skill in the art.
The technical solutions in the embodiments of the present invention will be clearly and completely described in the following in conjunction with the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments; all other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
A composite insulating glaze suitable for supercritical water application comprises SiO 2 、BaO、CaO、ZnO、B 2 O 3 、TiO 2 、Fe 2 O 3 、SO 3 、Cr 2 O 3 Clay, caSO 4 、MgSO 4 、Ca(OH) 2 、SiO 2 As a processing raw material.
Preferably, the specific components of the processing raw materials are as follows: 25.025% SiO2, 17.016% BaO, 4.600% CaO, 1.829% ZnO, 2.537% B2O3, 1.248% TiO2, 0.007% Fe2O3, 0.009% SO3, 17.491% Cr2O3, 2.966% clay, 6.818% CaSO4, 6.818% MgSO4, and 13.636% Ca (OH) 2.
A composite insulating glaze processing method suitable for supercritical water application comprises the following steps:
step one, raw material preparation: the above-mentioned raw materials were prepared by mixing 25.025% of SiO2, 17.016% of BaO, 4.600% of CaO, 1.829% of ZnO, 2.537% of B2O3, 1.248% of TiO2, 0.007% of Fe2O3, 0.009% of SO3, 17.491% of Cr2O3, 2.966% of clay, 6.818% of CaSO4, 6.818% of MgSO4 and 13.636% of Ca (OH) 2. Mixing the materials according to the proportion to obtain a mixture;
grinding and crushing: fully grinding the mixture obtained in the first step for 1-1.5 hours, and screening by using a screen to obtain a carefully selected raw material;
step three, fully mixing: mixing the carefully selected raw materials in the second step with distilled water according to the proportion of 7:5 to obtain a mixed raw material;
step four, filtering raw materials: filtering the mixed raw material obtained in the step three by using a 600-mesh screen to obtain a filtered mixture, standing the filtered mixture to obtain a material in a solid-liquid separation state, and discharging clear water at the upper part to obtain a precipitate at the bottom;
step five, coating: uniformly coating the precipitate obtained in the fourth step on an object to be processed to obtain a fired blank;
step six, firing: placing the fired blank obtained in the fifth step into a firing kiln, and fully firing to obtain a finished product material;
step seven, detecting: and D, detecting the finished material obtained in the step six.
Preferably, the screen in the second step is a 420-mesh stainless steel screen.
Preferably, the mixing method in the third step is as follows: then mixing the water with distilled water according to the mass ratio of 7:5, mixing and uniformly stirring, filtering the prepared liquid slurry by a 600-mesh sieve before use, standing for 2.5-3 hours after filtering, pumping clear water, and continuously stirring for 2 minutes at a stirring speed of 150 r/min.
Preferably, the water content of the precipitate in the fourth step is 16%.
Preferably, the coating method in the fifth step comprises the following steps: the object to be processed is quickly and vertically inserted into the sediment in the fourth step, dipped for 10 seconds and then vertically taken out and kept still for 2-3 minutes.
Preferably, the firing process in the sixth step is as follows: placing the fired blank into a firing kiln, wherein the kiln is a muffle furnace, the furnace temperature is respectively controlled to be fired for 40 minutes at 160 ℃, the furnace temperature is gradually controlled to be uniformly increased to 1200 ℃ after 60 minutes, the furnace temperature is kept at 1200 ℃ for 10 minutes, the furnace temperature is gradually controlled to be uniformly increased to 1280 ℃ after 20 minutes, the furnace temperature is kept at 1280 ℃ for 10 minutes, natural cooling is carried out to room temperature, and the muffle furnace is taken out and cleaned by acetone, thus the process is completed.
Preferably, the detection method in the step seven is as follows: filling tap water into a self-made stainless steel container for high-pressure test, mounting the blank sintered with the composite insulating glaze and the stainless steel container for high-pressure test in a muffle furnace, arranging a pressure release hole at the container and connecting a pressure gauge, and controlling the pressure to be not more than 12MPa by using a pressure regulating valve; in the experimental process, the temperature of the muffle furnace is regulated, data is recorded once after the temperature is increased by 30 ℃ and is constant, the continuous three-time temperature transformation rate is required to be not more than 1.0 ℃/10min during recording, the comprehensive temperature transformation rate is required to be not more than 2 ℃/30min, and meanwhile, the difference between the constant temperature and the set temperature is required to be not more than +/-5 ℃ until the temperature reaches 350 ℃.
Further, the detection standard of the step seven is as follows: the insulation resistance is not lower than 0.1MΩ at 350+ -10deg.C and 12+ -1 MPa.
CaSO is carried out 4 、Mg(OH) 2 And CaCO (CaCO) 3 The relevant performance data in air after adding color uranium are shown in table 1 below. As the temperature increases, the resistance decreases. When the temperature is 449.5 ℃, the resistance is 702.3MΩ, and the insulating performance is basically achieved; the material has good insulating property in air and under the condition of high temperature.
Table 1 relationship between test temperature and resistance in air:
CaSO is carried out 4 、Mg(OH) 2 And CaCO (CaCO) 3 After uranium is added, the mixture is added into the water for different timeThe relevant performance data are as follows in table 2:
table 2 relationship between temperature and resistance measured at different times in water:
table 3 relationship between temperature and resistance measured at different times in water:
finally, it should be noted that: the foregoing description is only illustrative of the preferred embodiments of the present invention, and although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments described, or equivalents may be substituted for elements thereof, and any modifications, equivalents, improvements or changes may be made without departing from the spirit and principles of the present invention.

Claims (8)

1. The composite insulating glaze suitable for supercritical water application is characterized in that: the composite insulating glaze comprises the following raw materials in percentage by weight: siO (SiO) 2 25.025%、BaO 17.016%、CaO 4.600%、ZnO 1.829%、B 2 O 3 2.537%、TiO 2 1.248% of Fe 2 O 3 0.007%、SO 3 0.009%、Cr 2 O 3 17.491% clay 2.966% CaSO 4 6.818%、MgSO 4 6.818%、Ca(OH) 2 13.636%。
2. A composite insulating glaze processing method suitable for supercritical water application is characterized by comprising the following steps: the method comprises the following steps:
step one, raw material preparation: the composite insulating glaze comprises the following raw materials in percentage by weight 2 25.025%、BaO 17.016%、CaO 4.600%、ZnO 1.829%、B 2 O 3 2.537%、TiO 2 1.248% of Fe 2 O 3 0.007%、SO 3 0.009%、Cr 2 O 3 17.491% clay 2.966% CaSO 4 6.818%、MgSO 4 6.818%、Ca(OH) 2 13.636% of the prescription amount is mixed to obtain a mixture;
grinding and crushing: fully grinding the mixture obtained in the step one for 1-1.5 hours, and screening by using a screen to obtain a carefully selected raw material;
step three, fully mixing: mixing the carefully selected raw materials in the second step with distilled water according to the mass ratio of 7:5 to obtain a mixed raw material;
step four, filtering raw materials: filtering the mixed raw material obtained in the step three by using a 600-mesh screen to obtain a filtered mixture, standing the filtered mixture to obtain a material in a solid-liquid separation state, and discharging clear water at the upper part to obtain a precipitate at the bottom;
step five, coating: uniformly coating the precipitate obtained in the fourth step on an object to be processed to obtain a fired blank;
step six, firing: placing the fired blank obtained in the fifth step into a firing kiln, and fully firing to obtain a finished product material;
step seven, detecting: and D, detecting the finished material obtained in the step six.
3. The method for processing the composite insulating glaze suitable for supercritical water application according to claim 2, wherein the method comprises the following steps: in the second step, the screen is a 420-mesh stainless steel screen.
4. The method for processing the composite insulating glaze suitable for supercritical water application according to claim 2, wherein the method comprises the following steps: in step four, the water content of the precipitate was 16%.
5. The method for processing the composite insulating glaze suitable for supercritical water application according to claim 2, wherein the method comprises the following steps: in the fifth step, the coating method comprises the following steps: and (3) rapidly and vertically inserting the object to be processed into the precipitate in the fourth step, dipping for 10 seconds, and vertically taking out and standing for 2-3 minutes.
6. The method for processing the composite insulating glaze suitable for supercritical water application according to claim 2, wherein the method comprises the following steps: the firing process in the step six is as follows: placing the fired blank into a firing kiln which is a muffle furnace, firing at 160 ℃ for 40 minutes, gradually controlling the furnace temperature to be uniformly increased to 1200 ℃ after 60 minutes, firing at 1200 ℃ for 10 minutes, gradually controlling the furnace temperature to be uniformly increased to 1280 ℃ after 20 minutes, firing at 1280 ℃ for 10 minutes, naturally cooling to room temperature, taking out the muffle furnace, and cleaning by using acetone.
7. The method for processing the composite insulating glaze suitable for supercritical water application according to claim 2, wherein the method comprises the following steps: in the seventh step, the detection method comprises the following steps: filling tap water into a self-made high-pressure-resistant test stainless steel container, mounting the finished product material prepared in the step six and the high-pressure-resistant test stainless steel container, and then placing the finished product material and the high-pressure-resistant test stainless steel container into a muffle furnace, wherein a pressure release hole is formed in the container and is connected with a pressure gauge, and controlling the pressure to be not more than 12MPa by using a pressure regulating valve; in the experimental process, the temperature of the muffle furnace is regulated, data is recorded once after the temperature is increased by 30 ℃ and is constant, the continuous three-time temperature transformation rate is required to be not more than 1.0 ℃/10min during recording, the comprehensive temperature transformation rate is required to be not more than 2 ℃/30min, and meanwhile, the difference between the constant temperature and the set temperature is required to be not more than +/-5 ℃ until the temperature reaches 350 ℃.
8. The method for processing the composite insulating glaze suitable for supercritical water application according to claim 7, wherein the method comprises the following steps: in step seven, the detection criteria are: the insulation resistance is not lower than 0.1MΩ at 350+ -10deg.C and 12+ -1 MPa.
CN202210503514.3A 2022-05-09 2022-05-09 Composite insulating glaze suitable for supercritical water application and processing method thereof Active CN115304275B (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101786904A (en) * 2009-12-22 2010-07-28 咸阳陶瓷研究设计院 Color-changing glaze for metallic luster ceramics and preparation method thereof
CN102515733A (en) * 2011-12-14 2012-06-27 李学武 Production process for famille-rose peony porcelain
WO2018167268A1 (en) * 2017-03-17 2018-09-20 Merck Patent Gmbh Effect pigments
CN109715297A (en) * 2016-11-14 2019-05-03 美敦力先进能量有限公司 Colored glaze ceramic composite for electrosurgical tool
CN113200740A (en) * 2021-05-25 2021-08-03 德化县韵丽陶瓷有限公司 Manufacturing process for enabling color development on glaze to be uniform and rich in layering sense

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101786904A (en) * 2009-12-22 2010-07-28 咸阳陶瓷研究设计院 Color-changing glaze for metallic luster ceramics and preparation method thereof
CN102515733A (en) * 2011-12-14 2012-06-27 李学武 Production process for famille-rose peony porcelain
CN109715297A (en) * 2016-11-14 2019-05-03 美敦力先进能量有限公司 Colored glaze ceramic composite for electrosurgical tool
WO2018167268A1 (en) * 2017-03-17 2018-09-20 Merck Patent Gmbh Effect pigments
CN113200740A (en) * 2021-05-25 2021-08-03 德化县韵丽陶瓷有限公司 Manufacturing process for enabling color development on glaze to be uniform and rich in layering sense

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