This standard specifies the method for determining the sintering temperature range of ceramic materials using a high-temperature dilatometer or a high-temperature microscope. This standard is applicable to the determination of the sintering temperature range of ceramic materials with sintering properties such as daily-use ceramic raw materials and blanks. QB/T 1547-1992 Method for determining the sintering temperature range of ceramic materials QB/T1547-1992 Standard download decompression password: www.bzxz.net

Light Industry Standard of the People's Republic of China
Method for Determining the Sintering Temperature Range of Ceramic Materials 1 Subject Content and Scope of Application
QB/T 1547---1992
This standard specifies the method for determining the sintering temperature range of ceramic materials using a high-temperature dilatometer or a high-temperature microscope. This standard is applicable to the determination of the sintering temperature range of ceramic materials with sintering properties such as daily-use ceramic raw materials and bad materials. Part I High-temperature Dilatometer Method (Arbitration Method) 2 Principlewww.bzxz.net
The expansion and contraction curve of the sample during heating is recorded by a thermal dilatometer, and its sintering temperature range is determined according to the upper and lower temperature points of the curve
1. Limit temperature point: At this point, the sample sintering shrinkage has stopped, the density is the highest, and over-sintering expansion or softening shrinkage has not occurred. Lower limit temperature point: At this point, the sample sintering line shrinkage is 1.0%, and the water absorption rate is not more than 0.5%. 3 Night instrument equipment
a High automatic recording dilatometer
The maximum operating temperature is not less than 1400C. The dilatometer has the ability to measure the change in sample length of 2×10-1 (i.e. the sample changes 2um for 100mm).
The temperature measuring device should have the ability to measure the temperature change of ±2C. The dilatometer furnace has a reasonable structure, good thermal insulation performance, convenient sample loading and unloading, and uniform heating during the entire heating process. The sample temperature gradient is not greater than 4C. The temperature control system of the dilatometer can make the furnace body heat up at a uniform speed at the specified speed, and ensure that the heating rate has good linearity: Sample preparation tools: crushing equipment, sieves and forming molds, etc.: h
Platinum gasket: The platinum gasket should be flat, smooth and suitable for the dilatometer support; c
. Length measurement tool: The accuracy is 0.1%. 4 Sample preparation
4.1 The processed bad block mud section can be directly connected to the sample. 4.2 For processed powders, the same process conditions as those in actual production should be used as far as possible to prepare the samples. 4.3 For samples not treated with .T, crush them until they all pass through a 0.063mm aperture sieve, and prepare them into samples by grouting, extrusion or other molding methods:
4.4 When preparing samples with poor plasticity or no plastic raw materials and recyclables, organic plasticizers and binders may be appropriately added. 4.5 When conducting comparative tests, the samples should be prepared under the same conditions. 4.6 The samples should be dried to a moisture content of no more than 3%. 4.? The shape and size of the sample should be combined with the neck and support of the dilatometer. The cross-sectional area should not be less than 10mm, and the diameter or edge length should not be more than 12mm. The length of the sample should be suitable for the dilatometer. 4.8 The sample should be straight, with both ends flat, parallel and perpendicular to the long axis. There should be no defects such as holes, cracks, and incompleteness that affect the test results. Approved by the Ministry of Light Industry of the People's Republic of China on July 6, 1992 188
Implementation on March 1, 1993
QB/T 1547---1992
4.9 The sample and the dilatometer should not react chemically during the test. 5 Test steps
5.1 Measure the length Lo of the sample at room temperature.
5.2 The sample is loaded into the dilatometer, and the sample is completely separated from the top rod and support of the dilatometer by a platinum gasket, and the sample is kept stable and solid. During the entire test process, the compression force is less than 10*Pa (0.01N/mm*). The compression force for parallel tests should be constant. 5.3 After the sample has been left in the dilatometer for 5 minutes, start the instrument according to the dilatometer operating procedures. Select an appropriate range and determine the starting recording point. 54 Increase the temperature at a predetermined heating rate. For samples with a diameter or edge length not greater than 61, the heating rate can be selected within the range of 3~5C/min; for samples greater than 6mm, the heating rate should not exceed 3C/min. 5.5 The test endpoint is when the sample shows obvious secondary expansion or begins to soften and shrink. 5.6 When the furnace temperature cools to room temperature, remove the sample and clean the platinum gasket. 6.1 Upper limit temperature T: On the expansion-contraction curve, when the sintering shrinkage stops and the over-burning expansion or softening shrinkage just begins, the corresponding temperature is Tha
6.2 Lower limit temperature T: On the expansion-contraction curve, push the shrinkage rate back to 1.0% at the upper limit temperature T, and the corresponding temperature foot is T.6.3 The sintering shrinkage rates of the upper and lower limits of the sample are calculated according to the following formula: S(%)=
Where: S Sample sintering shrinkage rate
AL-sample sintering shrinkage, mm;
L Original length of the sample at room temperature, mm
6.4 The sintering temperature range is expressed as T~T.
7 Precision
For parallel tests, the upper and lower limit temperature tolerances shall not be greater than 5°C, otherwise, the test should be retested. 8 Report
The test report includes the following contents:
Product name, shape and size of the sample;
Sample preparation method (processing process: molding method, molding pressure, type and quantity of additives),
Instrument model + firing gas:
Test room temperature, heating rate;
9 Principle
Sample expansion-shrinkage curve:
Sintering temperature range, maximum sintering line shrinkage rate; other situations that need to be explained.
Part II High-temperature microscope method
The sintering temperature range is determined according to the change of the sample projection size during the heating process. The temperature when the sample projection shrinkage reaches the maximum value to the temperature before the sample expands or softens due to overburning is defined as the sintering temperature range. 189
10 Instruments and equipment
Paste: High-temperature microscope
QB/T 1547-1992
The maximum use temperature is not less than 1400℃. The optical system of the high-temperature microscope should have a clear and stable imaging function. The furnace body has a reasonable structure and good thermal insulation performance. During the entire test process, the temperature gradient of the sample is not greater than 4. The temperature control device of the high-temperature microscope can make the furnace body heat up at a given heating speed, and ensure that the heating speed is linear. The temperature control device has the ability to control the temperature change to ±2°C;
Sample press: constant pressure (about 3MPa) and good match with the mold: h.
Sample support plate and platinum gasket: should be flat and smooth. No deformation that affects the test occurs at high temperature; d. Agate mortar:
The sieve aperture is 0.063mm.
11 Sample preparation
11.1 Processed powders are directly sampled; processed bad blocks and mud segments are sampled after being evenly dispersed into powders; unprocessed samples are crushed in an agate mortar until all pass through a 0.063mm aperture sieve and then sampled. 11.2 Take 5 samples by the quartering method, place them in an agate mortar, and spray a small amount of water or organic bonding (to facilitate sample molding). 11.3 Use a sample press to press the powder into a cylinder with equal diameter and height. Its size should be suitable for the instrument used. The sample projection is required to be a square with regular corners.
12 Test steps
12.1 Turn on the power, turn on the lighting, place the prepared sample on the alumina plate with a platinum gasket, and place the support plate steadily on the sample holder so that the sample and the thermocouple end are in the same position. 12.2 Slowly push the sample holder into the center of the furnace and close the furnace. 12.3 Adjust the eyepiece and the displacement bolt so that the sample projection is a complete and clear square and is in the center of the field of view. 12.4 Turn on the electric furnace heating switch and increase the temperature at a uniform rate of 5 to 7C/min. 12.5 Take a photo of the sample projection at room temperature, and then take photos every 20°C or so starting from the temperature close to the end of sintering, until obvious overburning expansion or softening shrinkage occurs. During this process, carefully observe the changes in the shape of the projection, and record the initial temperature when the sample shrinks to the maximum and the temperature at which overburning expansion or softening shrinkage begins. 13 Expression of results
13.1 Upper limit temperature T: The temperature at which overburning expansion (or softening shrinkage) begins is Th. 13.2 Lower limit temperature T: The temperature at which the maximum sintering shrinkage is initially reached is T. 13.3 The sintering temperature range is expressed as TL~T. 14 Precision
For parallel tests, the upper and lower limit temperature tolerances shall not be greater than 10°C, otherwise the test should be retested. 15 Report
The test report shall include the following contents:
Sample name, sample size:
Instrument model, firing gas, heating rate: b.
Photographs of sample shape changes at various temperatures: a.
Sintering temperature range;
Other situations that need to be explained.
Additional explanation:
This standard is proposed by the Quality Standards Department of the Ministry of Light Industry. This standard is under the jurisdiction of the National Ceramic Standardization Center. QB/T 15471992
This standard was drafted by the Ceramics Research Institute of the Ministry of Light Industry. The main drafters of this standard are Wang Xiaoping and Jiang Weihui. From the date of implementation of this standard, the former Ministry of Light Industry standard QB897-1983 "Determination Method for Sintering Temperature Range of Daily Ceramic Materials" shall be used as the standard of 191
Tip: This standard content only shows part of the intercepted content of the complete standard. If you need the complete standard, please go to the top to download the complete standard document for free.