CN112098452A - Method for calibrating content of cristobalite in ceramic core - Google Patents
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Abstract
The invention discloses a method for calibrating the content of cristobalite in a ceramic core, and belongs to the technical field of high-temperature alloys. Firstly, preparing a plurality of ceramic core calibration samples, wherein the cristobalite in each calibration sample has different content; measuring the temperature rise and temperature drop process of each calibration sample by using a DSC method, observing the endothermic peak value in the temperature range of 180-270 ℃ on a temperature rise or temperature drop curve, and counting the peak area of the temperature range; establishing a relation curve of the DSC curve peak area and the cristobalite content; and finally, detecting the endothermic peak value of the ceramic core sample to be calibrated in the temperature range of 180-270 ℃ under different sintering regimes by using a DSC method, counting the peak area of the temperature range, and substituting the peak area into the relation curve to obtain the content of the cristobalite in the ceramic core to be calibrated. The calibration method can accurately control the content of cristobalite of the ceramic cores with different formulas after sintering, thereby selecting the optimal ceramic core.
Description
Technical Field
The invention relates to the technical field of high-temperature alloys, in particular to a method for calibrating the content of cristobalite in a ceramic core.
Background
The engine blade is the most key hot-end component of an aircraft engine and a gas turbine. With the development of aero-engines and gas turbines, the power and the heat efficiency are continuously improved, and the requirement on the temperature bearing capacity of the blade is higher and higher. In order to improve the temperature bearing capacity, the cooling structure of the blade is increasingly complex, and the preparation difficulty is obviously increased and decreased.
Engine blade cooling cavity structures are typically formed using ceramic cores. At present, the most common ceramic core base material is silicon base, quartz glass is used as a base material, and mineralizers such as alumina, zirconia, zirconium silicate and the like are added. The precipitation amount of the cristobalite must be controlled during sintering of the silicon-based ceramic core to ensure that the ceramic core has good comprehensive performance, a certain amount of cristobalite can be formed after the silicon-based ceramic core is sintered, and the cristobalite can improve the high-temperature creep resistance of the ceramic core and prevent the ceramic core from being broken. Before the blade is poured, the ceramic core is subjected to cold and heat shock for 2-3 times due to process limitation, and in the process, the cubic high-temperature type cristobalite and the tetragonal low-temperature type cristobalite have high and low temperature crystal form transformation at the temperature of 180-270 ℃, namely the transformation of the cubic high-temperature type cristobalite and the tetragonal low-temperature type cristobalite can cause volume change so as to cause the ceramic core to generate cracks. In the process of blade casting, the ceramic core cracks can reduce the strength of the ceramic core at high temperature, and the blade can have the defects of core deviation or core leakage and the like under the strong impact of alloy liquid, so that the blade is scrapped. At present, the relative content of the cristobalite in the ceramic core can be calculated only by analyzing the X-ray spectrum form, the calculated content is not particularly accurate, and how to accurately control the content of the cristobalite so as to ensure the optimal comprehensive performance of the ceramic core is one of the problems to be solved at present.
Disclosure of Invention
The invention aims to provide a method for calibrating the content of cristobalite in a ceramic core so as to quickly obtain the ceramic core with optimal comprehensive performance.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for calibrating the content of cristobalite in a ceramic core comprises the following steps:
(1) preparing a plurality of ceramic core calibration samples, wherein the quartz in each calibration sample has different contents;
(2) measuring the temperature rise and temperature reduction process of each ceramic core calibration sample with different cristobalite contents by utilizing Differential Scanning Calorimetry (DSC), observing the heat absorption peak value of a temperature rise or temperature reduction curve in a temperature range of 180-plus-270 ℃, and counting the peak area of the temperature range; then, drawing data points by taking the content of the cristobalite as an abscissa and the corresponding area of the endothermic peak as an ordinate, and performing straight line fitting on each data point to establish a relation curve between the area of the peak of the DSC curve and the content of the cristobalite;
(3) and (3) detecting the endothermic peak value of the ceramic core sample (unknown content of the cristobalite) to be calibrated under different sintering regimes in a temperature range of 180-270 ℃ by using Differential Scanning Calorimetry (DSC), counting the peak area of the temperature range, and substituting the peak area into the fitting curve obtained in the step (2), thereby obtaining the content of the cristobalite in the ceramic core to be calibrated.
In the step (1), the ceramic core calibration sample is composed of 1-100 wt% of cristobalite and quartz glass, and the balance is quartz glass.
In the step (1), in the ceramic core calibration sample, the purity of quartz glass is more than 99.9%, and the purity of cristobalite is more than 99.9%; the granularity of the quartz glass is less than 400 meshes, and the granularity of the cristobalite is less than 5000 meshes.
The preparation process of the ceramic core calibration sample comprises the following steps: putting quartz glass and cristobalite into a tank mill according to a ratio, performing tank milling for 24 hours at a speed of 80r/min, putting the powder which is uniformly mixed after the tank milling into a vacuum drying oven, and performing heat preservation and drying for 12 hours at a temperature of between 100 and 110 ℃ to obtain the ceramic core calibration sample.
In the step (2), the process of measuring the temperature rise and the temperature fall of the ceramic core calibration sample by using Differential Scanning Calorimetry (DSC) comprises the following steps: weighing 30-35mg of ceramic core calibration sample powder by using an analytical balance with the precision of 0.0001g, and heating to 300-350 ℃ by using DSC equipment at the heating and cooling rate of 15 ℃/min.
The invention has the following advantages and positive effects:
1. according to the method, the relationship between the content of the cristobalite in the core and the phase change peak area is obtained by utilizing the phase change peak area in the DSC cooling curve at the temperature range of 180-270 ℃ measured by the quartz glass and the cristobalite ceramic core powder with determined contents, so that the ceramic core with unknown content of the cristobalite is subjected to contrast calibration.
2. The calibration method can accurately control the content of cristobalite of the ceramic cores with different formulas after sintering, thereby selecting the optimal ceramic core.
3. The calibration method can quickly predict the cristobalite of the ceramic cores prepared by different formulas after sintering, and shorten the development period.
Drawings
FIG. 1 is a typical temperature rise and decrease curve of a DSC experiment for calibrating a ceramic core;
FIG. 2 is a plot of peak area of DSC curves versus cristobalite content using calibrated samples of ceramic cores having different amounts of cristobalite.
Detailed Description
The invention is described in detail below with reference to the figures and examples. All percentages and ratios in the present invention are by weight (percent) unless otherwise specified.
The invention provides a method for calibrating the content of cristobalite in a ceramic core, which comprises the steps of firstly establishing a relation curve between the peak area of a DSC curve and the content of the cristobalite by utilizing a ceramic core calibration sample, then detecting the endothermic peak value of a sample (the content of the unknown cristobalite) of the ceramic core to be calibrated under different sintering regimes in a temperature range of 180-plus-one (270 ℃) by applying Differential Scanning Calorimetry (DSC), counting the peak area of the temperature range, and obtaining the content of the cristobalite in the ceramic core to be calibrated in the obtained relation curve.
The ceramic core calibration sample is composed of cristobalite and quartz glass, five ceramic core calibration samples are manufactured, and the cristobalite in the ceramic core calibration samples accounts for 5%, 10%, 30%, 50%, 70%, 90% and 100% by weight; the purity of the selected quartz glass is more than 99.9 percent, the purity of the cristobalite is more than 99.9 percent, the granularity of the quartz glass is less than 400 meshes, and the granularity of the cristobalite is less than 5000 meshes. The preparation process of the ceramic core calibration sample comprises the following steps: putting quartz glass and cristobalite into a tank mill according to a ratio, performing tank milling at a speed of 80r/min for 24 hours, putting the uniformly mixed powder after the tank milling into a vacuum drying oven, and preserving heat for 12 hours at a temperature of 106 ℃ to obtain the calibration sample of each ceramic core.
Measuring the temperature rise and temperature drop process of each ceramic core calibration sample with different cristobalite contents by utilizing Differential Scanning Calorimetry (DSC): respectively weighing 30-35mg of each ceramic core calibration sample powder by using an analytical balance with the precision of 0.0001g, and heating up to 300-350 ℃ by using DSC equipment at the heating up or cooling down rate of 15 ℃/min. Observing the heat absorption peak value in the temperature range of 180-270 ℃ on the temperature rising or reducing curve, and counting the peak area of the temperature range by utilizing the self-contained protein Analysis software of the equipment (figure 1); and then, drawing data points by taking the content of the cristobalite as an abscissa and the corresponding area of the endothermic peak as an ordinate, and performing straight line fitting on each data point to establish a relation curve between the area of the peak of the DSC curve and the content of the cristobalite, as shown in FIG. 2.
The following example is to calibrate the cristobalite content of the sintered ceramic core using the obtained DSC curve peak area versus cristobalite content.
Example 1
The ceramic core of this example had the following composition (wt.%): quartz glass: 80%, alumina: 20 percent, sintering the ceramic core at 1250 ℃ and keeping the temperature for 2 hours. And (3) weighing 30mg of sintered sample by using an analytical balance, carrying out DSC experiment at a temperature rise and temperature reduction rate of 15 ℃/min, measuring that the peak area of the temperature reduction section at 180-270 ℃ is 3.35J/g, and substituting the area into the relation curve in figure 2 to obtain the cristobalite content of the ceramic core in the current state (the state after sintering at 1250 ℃ and heat preservation for 2 hours) of about 22 wt.%.
Example 2
The ceramic core of the present example had the following composition (wt.%): quartz glass: 80%, alumina: 20 percent; the ceramic core is sintered at 1200 ℃ and kept warm for 2 h. And (3) weighing 30mg of sintered sample by using an analytical balance, carrying out DSC experiment at a temperature rise and temperature reduction rate of 15 ℃/min, measuring that the peak area of the temperature reduction section at 180-270 ℃ is 0.79J/g, and substituting the area into the relation curve in figure 2 to obtain that the content of cristobalite in the current state (after sintering at 1200 ℃ and heat preservation for 2 hours) of the ceramic core is about 5 wt.%.
Example 3
The ceramic core of the present example had the following composition (wt.%): quartz glass: 80%, alumina: 20 percent; the ceramic core is sintered at 1300 ℃ and is kept warm for 3 hours. And (3) weighing 30mg of sintered sample by using an analytical balance, carrying out DSC experiment at the temperature rising and reducing rate of 15 ℃/min, measuring that the peak area of the temperature reducing section at 180-270 ℃ is 7.61J/g, and substituting the area into the relation curve in figure 2 to obtain the cristobalite content of the ceramic core in the current state (the state after sintering at 1300 ℃ and heat preservation for 3 hours) of the ceramic core is about 50 wt.%.
Claims (5)
1. A method for calibrating the content of cristobalite in a ceramic core is characterized by comprising the following steps: the method comprises the following steps:
(1) preparing a plurality of ceramic core calibration samples, wherein the quartz in each calibration sample has different contents;
(2) measuring the temperature rise and temperature reduction process of each ceramic core calibration sample with different cristobalite contents by utilizing Differential Scanning Calorimetry (DSC), observing the heat absorption peak value of a temperature rise or temperature reduction curve in a temperature range of 180-plus-270 ℃, and counting the peak area of the temperature range; then, drawing data points by taking the content of the cristobalite as an abscissa and the corresponding area of the endothermic peak as an ordinate, and performing straight line fitting on each data point to establish a relation curve between the area of the peak of the DSC curve and the content of the cristobalite;
(3) and (3) detecting the endothermic peak value of the ceramic core sample to be calibrated in the temperature range of 180-270 ℃ under different sintering regimes by using Differential Scanning Calorimetry (DSC), counting the peak area of the temperature range, and substituting the peak area into the relation curve obtained in the step (2), thereby obtaining the content of the cristobalite in the ceramic core to be calibrated.
2. The method of calibrating cristobalite content in a ceramic core according to claim 1, wherein: in the step (1), the ceramic core calibration sample consists of 1-100 wt% of cristobalite and quartz glass, and the balance is quartz glass.
3. The method of calibrating cristobalite content in a ceramic core according to claim 2, wherein: in the step (1), in the ceramic core calibration sample, the purity of quartz glass is more than 99.9%, and the purity of cristobalite is more than 99.9%; the granularity of the quartz glass is less than 400 meshes, and the granularity of the cristobalite is less than 5000 meshes.
4. The method of calibrating cristobalite content in a ceramic core according to claim 3, wherein: the preparation process of the ceramic core calibration sample comprises the following steps: putting quartz glass and cristobalite into a tank mill according to a ratio, performing tank milling for 24 hours at a speed of 80r/min, putting the powder which is uniformly mixed after the tank milling into a vacuum drying oven, and performing heat preservation and drying for 12 hours at a temperature of between 100 and 110 ℃ to obtain the ceramic core calibration sample.
5. The method of calibrating cristobalite content in a ceramic core according to claim 1, wherein: in the step (2), the process of measuring the temperature rise and the temperature fall of the ceramic core calibration sample by using Differential Scanning Calorimetry (DSC) comprises the following steps: weighing 30-35mg of ceramic core calibration sample powder by using an analytical balance with the precision of 0.0001g, and heating to 300-350 ℃ by using DSC equipment at the heating and cooling rate of 15 ℃/min.
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| WO2023189590A1 (en) * | 2022-03-28 | 2023-10-05 | デンカ株式会社 | Crystalline silica powder and resin composition |
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Application publication date: 20201218 |