CN111781086A - Method for rapidly detecting high-temperature oxidation resistance of silicon carbide refractory material - Google Patents
Method for rapidly detecting high-temperature oxidation resistance of silicon carbide refractory material Download PDFInfo
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Abstract
The invention provides a method for rapidly detecting the high-temperature oxidation resistance of a silicon carbide refractory material, which is used for judging the high-temperature oxidation resistance of the material through the mass change rate and the volume change rate before and after a test sample is tested, wherein the smaller the change rate is, the better the oxidation resistance of the material is, and which index of the mass change rate and the volume change rate is used as a main variable of a judgment standard is determined according to the specific application environment of the material. The method realizes the rapid detection of the high-temperature oxidation resistance of the silicon carbide refractory material by using the atmosphere with the strongest oxidation effect on the silicon carbide material, namely water vapor, and overlapping, sealing and pressurizing modes, and greatly improves the detection efficiency compared with the existing detection method. The detection method has the advantages of high reproduction rate, stability, accuracy and strong practicability.
Description
Technical Field
The invention belongs to the technical field of refractory material performance detection, and particularly relates to a method for rapidly detecting high-temperature oxidation resistance of a silicon carbide refractory material.
Background
The silicon carbide refractory material has high thermal conductivity, small linear expansion coefficient, high strength at normal temperature and high temperature, good thermal shock stability, chemical corrosion resistance and high-temperature wear resistance, and is widely applied to the fields of steel, nonferrous metallurgy, chemistry, electric power, ceramics, waste incineration power generation and the like.
The silicon carbide material belongs to a non-oxidation refractory material and is easy to oxidize, and high-temperature oxidation is a main cause for damage of the silicon carbide refractory material in a use environment containing an oxidation atmosphere; for example, in the ceramic industry, the main cause of damage to silicon carbide kiln furniture is the high-temperature oxidation of water vapor generated after oxygen and fuel gas are combusted; for example, in a household garbage incinerator, the water content of the household garbage is higher, so that the water vapor content of the atmosphere in the incinerator is higher, and the high-temperature oxidation of oxidizing gases such as water vapor, oxygen and the like in the incinerator is just the main cause of the damage of a silicon carbide lining; therefore, the high-temperature oxidation resistance of the silicon carbide material is an important index for judging the service life of the silicon carbide refractory material in an oxidizing atmosphere working environment; how to detect and judge the high-temperature oxidation resistance of the silicon carbide refractory material, namely, the silicon carbide material has the strongest oxidation effect of water vapor in common oxidizing gases such as water vapor, oxygen, carbon monoxide, carbon dioxide and the like; the ASTM C863 standard in the United states proposes the use of steam to speed up the test process at 32kg/m per hour depending on the volume of the chamber3Introducing steam into the heating chamber at the speed of (1), preserving heat for 500 hours at a certain standard test temperature (800 ℃, 900 ℃, 1000 ℃, 1100 ℃, 1200 ℃), and taking the volume change rate of the sample before and after the test as the judgment standard of the high-temperature oxidation resistance of the silicon carbide material; at present, no clear method is provided for detecting the high-temperature oxidation resistance of the silicon carbide refractory material at home; the ASTM C863 standard detection time is 500 hours, the time is very long, a large amount of manpower and material resources are consumed, and the method for detecting the performance of the refractory material with a strong application type needs to have two characteristics of rapidness and accuracy at the same time, so that the method can play a more timely and accurate guiding role in the actual application of the material.
Disclosure of Invention
The invention aims to provide a method for rapidly detecting the high-temperature oxidation resistance of a silicon carbide refractory material, so that the detection efficiency can be improved.
The technical scheme is as follows:
a method for rapidly detecting high-temperature oxidation resistance of a silicon carbide refractory material comprises the following steps:
step one, measuring the mass and volume of a sample:
sample size: cutting three samples along the standard brick, wherein the weight of each sample is at least 300g and more, and each sample at least retains 2 original brick surfaces; the mass and volume of each specimen were measured to the nearest 0.1g and 0.1cm, respectively, as specified in ASTM C20, ASTM C830 or ASTM C9143；
Step two, carrying out high-temperature oxidation test:
the sample was placed in a heating chamber and sealed, the heating chamber was heated to a predetermined experimental temperature (any one of 800 ℃, 900 ℃, 1000 ℃, 1100 ℃ and 1200 ℃), and then 32 kg/m/h was measured according to the volume of the heating chamber3Introducing water vapor into the heating chamber at a speed of 50-100 mm water column, and simultaneously keeping positive pressure of the heating chamber; after the temperature is kept for 100-200 hours at the specified temperature, the air source is turned off, and the heat source is turned off;
step three, measuring the mass and volume of the test sample:
after the sample is cooled, measuring the mass and the volume of the sample by adopting the same method as the step one, and calculating the volume density;
step four, calculating the mass change rate and the volume change rate of the sample, and taking an average value;
in the formula (I), the compound is shown in the specification,m n-a new weight of the piece of paper,m 0-the weight of the original weight,
V n-a new volume of the sample,V 0-an original volume;
the high-temperature oxidation resistance of the material is judged through the mass change rate and the volume change rate before and after the test of the sample, the smaller the change rate is, the better the oxidation resistance of the material is, and which index of the mass change rate and the volume change rate is used as a main variable of the judgment standard is determined according to the specific application environment of the material.
In the second step, the positive pressure is 100 mm water column, and the heat preservation time is 100 hours.
According to the method for rapidly detecting the high-temperature oxidation resistance of the silicon carbide refractory material, the high-temperature oxidation resistance of the silicon carbide refractory material is rapidly detected by using the atmosphere steam with the strongest oxidation effect on the silicon carbide material and overlapping, sealing and pressurizing modes, the detection time is shortened, the detection efficiency is greatly improved, and the detection method is high in repeatability, stable, accurate and strong in practicability.
Detailed Description
The present invention will be described in detail with reference to specific embodiments;
the instrument and equipment used in the invention are as follows:
electrically heating the drying box, and controlling the precision to be +/-5 ℃; an electronic balance with the precision of 0.01 g; a vacuum pumping device; a dryer; a vessel with an overflow tube; liquid immersion: tap water or an industrially pure organic liquid; a liquid immersion tank; a pressurizable high temperature furnace, a steam generator.
Example 1:
the oxidation resistance of the silicon carbide refractory material is detected at 1000 ℃, and the detected silicon carbide refractory material comprises the following 6 types: silicon dioxide bonded SiC, silicon nitride bonded SiC, silicon oxynitride bonded SiC, sialon bonded SiC, self-bonded SiC, SiC casting material (SiC content 70%).
The method comprises the following steps: three samples were cut for each material, each sample size: 114X 65X 50 mm;
the mass and volume of each specimen were measured according to ASTM C20.
Step two: the sample was placed in a heating chamber and sealed, and after heating the heating chamber to 1000 ℃ at a rate of 32kg/m per hour3The water vapor is introduced into the heating chamber at a rate of 100 mm water column, and simultaneously the positive pressure of the heating chamber is kept, the heat preservation is 100 hoursWhen the current is over;
step three: after the samples are cooled, measuring the mass and the volume of each sample by adopting the same method as the step one, and calculating the volume density;
step four: calculating the mass change rate and the volume change rate of each sample according to the following calculation formula, and taking an average value;
in the formula (I), the compound is shown in the specification,m n-a new weight of the piece of paper,m 0-original weight
V n-a new volume of the sample,V 0original volume
The results of the high temperature oxidation tests calculated for 6 silicon carbide refractories are shown in table 1 below.
The test was repeated 2 times according to the above procedure, and the results are shown in tables 2 and 3, respectively.
As can be seen from the data of the detection results in tables 1, 2 and 3, the stability and the reproducibility of the test method are high.
Example 2:
the same 6 silicon carbide refractories as in example 1 were tested for oxidation resistance at 1000 ℃ as follows:
the method comprises the following steps: three samples were cut for each material, each sample size: 114X 65X 50 mm.
The mass and volume of each specimen were measured according to ASTM C20;
step two: placing the sample in a heating chamber and sealing the sampleSealing, heating the heating chamber to 1000 deg.C, and sealing at 32kg/m per hour3Introducing water vapor into the heating chamber at a speed of (1), simultaneously keeping the positive pressure of the heating chamber, wherein the positive pressure is 50mm water column, and keeping the temperature for 200 hours;
step three: after the samples are cooled, measuring the mass and the volume of each sample by adopting the same method as the step one, and calculating the volume density;
step four: calculating the mass change rate and the volume change rate of each sample according to the following calculation formula, and taking an average value;
in the formula (I), the compound is shown in the specification,m n-a new weight of the piece of paper,m 0-original weight
V n-a new volume of the sample,V 0original volume
The results of the calculated high temperature oxidation tests for 6 silicon carbide refractories are shown in table 4 below.
The test was repeated 2 times according to the above procedure, and the results are shown in tables 5 and 6, respectively.
As can be seen from the data of the detection results in tables 4, 5 and 6, the stability and the reproducibility of the test method are high.
Example 3: comparative experiment
The same 6 kinds of silicon carbide refractories as those of examples 1 and 2 were examined for oxidation resistance at 1000 ℃ according to ASTM C863.
3 specimens of each material were cutThe sample size is 114 × 65 × 50mm, the volume and the mass of the sample are tested, and then the sample is put into a test furnace and heated to 1000 ℃ according to the ASTM-C863 standard, so as to be 32 kg/m/hour3Introducing water vapor at the speed of (1) and keeping the temperature for 500 hours. And after the furnace is stopped and the temperature is reduced, taking out the sample to test the volume and the mass of the sample after oxidation, calculating the volume change rate and the mass change rate, and taking an average value. The results are shown in Table 7.
Comparing examples 1, 2 and 3, it can be seen that the test result of the test method of the present invention is equivalent to the test result of the existing ASTM C863 method, which indicates that the test method of the present invention is effective and accurate.
In conclusion, the detection method provided by the invention has the advantages of high reproduction rate, stability, accuracy, short detection time, high efficiency and strong practicability.
Claims (3)
1. A method for rapidly detecting high-temperature oxidation resistance of a silicon carbide refractory material is characterized by comprising the following steps: the detection method comprises the following steps:
step one, measuring the mass and volume of a sample:
sample size: cutting three samples along the standard brick, wherein the weight of each sample is at least 300g and more, and each sample at least retains 2 original brick surfaces; the mass and volume of each specimen were measured to the nearest 0.1g and 0.1cm, respectively, as specified in ASTM C20, ASTM C830 or ASTM C9143；
Step two, carrying out high-temperature oxidation test:
the sample was placed in a heating chamber and sealed, and after the heating chamber was heated to a predetermined test temperature, the volume of the heating chamber was changed to 32 kg/m/hour3Introducing water vapor into the heating chamber at a speed of 50-100 mm water column, and simultaneously keeping positive pressure of the heating chamber; after the temperature is kept for 100-200 hours at the specified temperature, the air source is turned off, and the heat source is turned off;
step three, measuring the mass and volume of the test sample:
after the sample is cooled, measuring the mass and the volume of the sample by adopting the same method as the step one, and calculating the volume density;
step four, calculating the mass change rate and the volume change rate of the sample, and taking an average value;
in the formula (I), the compound is shown in the specification,m n-a new weight of the piece of paper,m 0-the weight of the original weight,
V n-a new volume of the sample,V 0-an original volume;
the high-temperature oxidation resistance of the material is judged through the mass change rate and the volume change rate before and after the test of the sample, the smaller the change rate is, the better the oxidation resistance of the material is, and which index of the mass change rate and the volume change rate is used as a main variable of the judgment standard is determined according to the specific application environment of the material.
2. The method for rapidly detecting the high-temperature oxidation resistance of the silicon carbide refractory material as claimed in claim 1, wherein the method comprises the following steps: in the second step, the positive pressure is 100 mm water column, and the heat preservation time is 100 hours.
3. The method for rapidly detecting the high-temperature oxidation resistance of the silicon carbide refractory material as claimed in claim 1, wherein the method comprises the following steps: the experiment temperature in the second step is one of 800 ℃, 900 ℃, 1000 ℃, 1100 ℃ and 1200 ℃.
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Application publication date: 20201016 |