CN110333258B - Method for testing sintering temperature of ceramic product and method for testing precipitation amount of metal element of ceramic product - Google Patents
Method for testing sintering temperature of ceramic product and method for testing precipitation amount of metal element of ceramic product Download PDFInfo
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- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/3103—Atomic absorption analysis
- G01N2021/3114—Multi-element AAS arrangements
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- G01N2223/07—Investigating materials by wave or particle radiation secondary emission
- G01N2223/076—X-ray fluorescence
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- G01N2223/10—Different kinds of radiation or particles
- G01N2223/101—Different kinds of radiation or particles electromagnetic radiation
- G01N2223/1016—X-ray
Abstract
The invention relates to a method for testing sintering temperature of a ceramic product and a method for testing precipitation amount of metal elements of the ceramic product. The method for testing the sintering temperature of the ceramic product comprises the following steps: providing a plurality of standard products with the same preparation raw materials and different sintering temperatures; testing the standard substance by adopting an energy dispersion X-ray fluorescence spectrometry to obtain the percentage content of the characteristic elements; obtaining a functional relation between the percentage content of the characteristic elements and the sintering temperature according to the percentage content of the characteristic elements and the sintering temperature; testing a sample to be tested to obtain the percentage content of the characteristic elements of the sample to be tested; and calculating the sintering temperature of the sample to be detected according to the functional relation and the percentage content of the characteristic elements of the sample to be detected. The method for testing the sintering temperature of the ceramic product can detect the sintering temperature of each ceramic product, and further monitor the precipitation amount of metal elements of the ceramic product by monitoring the sintering temperature so as to ensure the use safety of the ceramic product.
Description
Technical Field
The invention relates to the field of ceramic products, in particular to a method for testing sintering temperature of a ceramic product and a method for testing precipitation amount of metal elements of the ceramic product.
Background
The ceramic product usually contains various natural and artificially added harmful heavy metal elements, which are released excessively in use and absorbed by human bodies, and can cause certain influence and harm to the health of the human bodies after long-term accumulation, such as elements of lead, cadmium, mercury, arsenic, barium, hexavalent chromium, bromide and the like. Particularly, the purple sand ware is widely used as a tool for drinking tea and tasting tea, and the tea water has weak acidity, so that heavy metal ions are easy to be separated out from the tea water. The research shows that the precipitation amount of heavy metal elements of the purple sand device is related to the sintering temperature. Therefore, the precipitation amount of the heavy metal elements can be controlled by monitoring the sintering temperature. However, the conventional sintering temperature testing method is complicated, and the ceramic product is damaged in the testing process, so that the sintering temperature of each produced ceramic product cannot be detected.
Disclosure of Invention
In view of the above, it is necessary to provide a method for testing the sintering temperature of a ceramic product, which is simple and can be performed without damage.
In addition, a method for testing the precipitation amount of the metal elements of the ceramic product is also provided.
A method for testing the sintering temperature of a ceramic product comprises the following steps:
providing a plurality of standard products, wherein the plurality of standard products are prepared from the same raw materials and have different sintering temperatures;
testing the percentage content of the characteristic elements of each standard product by adopting an energy dispersion X-ray fluorescence spectrometry to obtain the percentage content of the characteristic elements of each standard product;
obtaining the functional relation between the percentage content of the characteristic elements and the sintering temperature according to the percentage content of the characteristic elements of the plurality of standard products and the sintering temperatures of the plurality of standard products;
testing a sample to be tested by adopting the energy dispersion X-ray fluorescence spectrometry to obtain the percentage content of the characteristic elements of the sample to be tested, wherein the preparation raw material of the sample to be tested is the same as that of the standard product; and
and calculating the sintering temperature of the sample to be detected according to the functional relation between the percentage content of the characteristic elements and the sintering temperature and the percentage content of the characteristic elements of the sample to be detected.
In one embodiment, the characteristic element includes at least one of iron, titanium, potassium, lead, aluminum, zirconium, yttrium, rubidium, strontium, and manganese.
In one embodiment, the step of obtaining the percentage of the characteristic elements as a function of the sintering temperature according to the percentage of the characteristic elements of the plurality of the standards and the sintering temperatures of the plurality of the standards comprises:
establishing a relation curve of the percentage content of the characteristic elements and the sintering temperature according to the percentage content of the characteristic elements of the plurality of standard products and the sintering temperatures of the plurality of standard products;
and performing linear fitting on the relation curve to obtain a functional relation between the percentage content of the characteristic elements and the sintering temperature.
In one embodiment, the method includes the steps of calculating the sintering temperature of the sample to be tested according to a functional relationship between the percentage of the characteristic elements and the sintering temperature and the percentage of the characteristic elements in the sample to be tested, where the step of calculating the sintering temperature of the sample to be tested includes:
obtaining the sintering temperature calculated by the percentage of each characteristic element according to the functional relation between the percentage of each characteristic element and the sintering temperature and the percentage of each characteristic element of the sample to be tested;
and calculating the average value of the sintering temperatures calculated according to the percentage content of each characteristic element to obtain the sintering temperature of the sample to be detected.
In one embodiment, the standards are at least five.
In one embodiment, the step of testing the percentage content of the characteristic element of each standard by using energy dispersive X-ray fluorescence spectrometry to obtain the percentage content of the characteristic element of each standard includes:
providing a plurality of test articles containing the characteristic elements, wherein the percentage content of the characteristic elements of the test articles is different;
testing each test article by using an energy dispersion X-ray fluorescence spectrometer to obtain the fluorescence intensity of the characteristic elements of each test article;
obtaining a functional relation between the fluorescence intensity of the characteristic elements and the percentage content of the characteristic elements according to the fluorescence intensity of the characteristic elements of the plurality of test articles and the percentage content of the characteristic elements of the plurality of test articles;
testing each standard product by using the energy dispersion X-ray fluorescence spectrometer to obtain the fluorescence intensity of the characteristic elements of each standard product;
and obtaining the percentage content of the characteristic elements of each standard product according to the functional relation between the fluorescence intensity of the characteristic elements and the percentage content of the characteristic elements and the fluorescence intensity of the characteristic elements of each standard product.
In one embodiment, the step of testing a sample to be tested by using the energy dispersive X-ray fluorescence spectrometry to obtain the percentage content of the characteristic elements of the sample to be tested includes:
testing the sample to be tested by using the energy dispersion X-ray fluorescence spectrometer to obtain the fluorescence intensity of the characteristic elements of the sample to be tested;
and obtaining the percentage content of the characteristic elements of the sample to be detected according to the functional relation between the fluorescence intensity of the characteristic elements and the percentage content of the characteristic elements and the fluorescence intensity of the characteristic elements of the sample to be detected.
A method for testing the precipitation amount of metal elements in a ceramic product comprises the following steps:
providing a plurality of standard samples, wherein the plurality of standard samples are prepared from the same raw materials and have different sintering temperatures;
testing the precipitation amount of the metal elements of a plurality of standard samples;
obtaining a functional relation between the precipitation amount of the metal elements and the sintering temperature according to the precipitation amount of the metal elements of the plurality of standard samples and the sintering temperatures of the plurality of standard samples;
obtaining the sintering temperature of the sample to be tested by adopting the method for testing the sintering temperature of the ceramic product; and
and calculating to obtain the precipitation amount of the metal element of the sample to be detected according to the sintering temperature of the sample to be detected and the functional relation between the precipitation amount of the metal element and the sintering temperature.
In one embodiment, the method for testing the precipitation amount of the metal element of the plurality of the standards is flame atomic absorption spectrometry, inductively coupled plasma atomic emission spectrometry or graphite furnace atomic absorption spectrometry.
In one embodiment, the metal element includes at least one of barium, iron, lead, cadmium, manganese, chromium, and cobalt.
According to the method for testing the sintering temperature of the ceramic product, a plurality of standard products with different sintering temperatures are tested by adopting the energy dispersion X-ray fluorescence spectrometry to obtain the percentage content of the characteristic elements of the standard products, then the functional relation between the percentage content of the characteristic elements and the sintering temperature is established, then the energy dispersion X-ray fluorescence spectrometry is adopted to test the characteristic elements of the sample to be tested to obtain the percentage content of the characteristic elements of the sample to be tested, and the sintering temperature of the sample to be tested is obtained according to the functional relation. The method for testing the sintering temperature of the ceramic product is simple, and the percentage content of the characteristic elements is tested by adopting the energy dispersion X-ray fluorescence spectrometry, so that the samples to be tested cannot be damaged, and each sample to be tested can be detected. And the sintering temperature of each sample to be tested can be calculated according to the functional relation between the percentage content of the characteristic elements and the sintering temperature by the different ignition loss of the characteristic elements when the sintering temperatures are different.
Drawings
FIG. 1 is a process flow diagram of a method for testing a sintering temperature of a ceramic article according to one embodiment;
fig. 2 is a process flow chart of a method for testing the precipitation amount of metal elements in a ceramic product according to an embodiment.
Detailed Description
In order that the invention may be more fully understood, reference will now be made to the following description taken in conjunction with the accompanying drawings. The detailed description sets forth the preferred embodiments of the invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
Referring to fig. 1, a method for testing a sintering temperature of a ceramic product according to an embodiment includes the following steps:
step S110: providing a plurality of standard products, wherein the plurality of standard products are prepared from the same raw materials and have different sintering temperatures.
Step S120: and testing the percentage content of the characteristic elements of each standard product by adopting an energy dispersion X-ray fluorescence spectrometry to obtain the percentage content of the characteristic elements of each standard product.
Specifically, step S120 includes:
providing a plurality of test articles containing characteristic elements, wherein the percentage content of the characteristic elements of the test articles is different;
testing each test article by using an energy dispersion X-ray fluorescence spectrometer to obtain the fluorescence intensity of the characteristic elements of each test article;
obtaining a functional relation between the fluorescence intensity of the characteristic elements and the percentage content of the characteristic elements according to the fluorescence intensity of the characteristic elements of the plurality of test articles and the percentage content of the characteristic elements of the plurality of test articles;
testing each standard product by using an energy dispersion X-ray fluorescence spectrometer to obtain the fluorescence intensity of the characteristic elements of each standard product;
and obtaining the percentage content of the characteristic elements of each standard product according to the functional relation between the fluorescence intensity of the characteristic elements and the percentage content of the characteristic elements and the fluorescence intensity of the characteristic elements of each standard product.
The principle of energy dispersive X-ray fluorescence spectroscopy (EDXRF) is to excite electrons in the outer layer of an element through X-rays, capture the energy of the transferred electrons by a detector and analyze the element, and is a systematic, low-cost, high-efficiency, fast, nondestructive and high-accuracy detection method, which forms quantifiable semi-quantitative data and can perform comparative analysis according to a large database.
In the process of testing a plurality of standard products by adopting the energy dispersion X-ray fluorescence spectrometry, the same test conditions are controlled, namely the detection is carried out by using the same tube pressure, the same tube flow, the same energy, the same optical filter and the same time, so as to obtain the percentage content of the characteristic elements of the standard products and the samples to be tested.
Although the raw materials for preparing the standard product are the same, the standard product is sintered at different sintering temperatures, the percentage content of part of elements is reduced due to the ignition effect in the high-temperature sintering process, and the ignition loss is larger along with the higher sintering temperature, so that the percentage content of characteristic elements in the obtained standard product is different.
Based on the shrinkage effect of high-temperature sintering, the sintering shrinkage rate is higher as the sintering temperature is higher because the volume of the ceramic product is reduced (taking a purple sand device as an example, the sintering shrinkage rate is about 3% -10%). Therefore, under the same energy dispersive X-ray fluorescence spectrometry test conditions, the measured characteristic elements of the ceramic products manufactured at different sintering temperatures have obvious differences and distinguishable quantitative data, which is taken as the test basis for detecting the sintering temperature of the ceramic products in the embodiment.
Step S130: and obtaining the functional relation between the percentage content of the characteristic elements and the sintering temperature according to the percentage content of the characteristic elements of the plurality of standard products and the sintering temperatures of the plurality of standard products.
Specifically, step S130 includes:
establishing a relation curve of the percentage content of the characteristic elements and the sintering temperature according to the percentage content of the characteristic elements in the plurality of standard products and the sintering temperatures of the plurality of standard products;
and performing linear fitting on the relation curve to obtain the functional relation between the percentage content of the characteristic elements and the sintering temperature.
Specifically, the characteristic element includes at least one of iron, titanium, potassium, zirconium, lead, aluminum, yttrium, rubidium, strontium, and manganese. In one embodiment, the number of feature elements is 1 to 3.
The percentage content of the characteristic elements is higher, and the sintering shrinkage is more obvious. The raw ores with the same preparation raw materials are sintered at different sintering temperatures, and the percentage content of the characteristic elements of the obtained standard product is greatly changed, so that the functional relation between the sintering temperature and the percentage content of the characteristic elements can be obtained by testing the percentage content of the characteristic elements.
Step S140: and testing the sample to be tested by adopting an energy dispersion X-ray fluorescence spectrometry to obtain the percentage content of the characteristic elements of the sample to be tested, wherein the preparation raw material of the sample to be tested is the same as that of the standard product.
Specifically, the test conditions in step S140 are the same as those in step S120, so as to eliminate errors caused by the test. The preparation raw materials of the sample to be detected are the same as those of the standard product, namely the raw ore for preparing the sample to be detected is the same as that for preparing the standard product, so that the percentage content of the characteristic elements of the sample to be detected obtained after sintering is related to the sintering temperature.
Specifically, step S140 includes:
testing a sample to be tested by using an energy dispersion X-ray fluorescence spectrometer to obtain the fluorescence intensity of characteristic elements in the sample to be tested;
and obtaining the percentage content of the characteristic elements of the sample to be detected according to the functional relation between the fluorescence intensity of the characteristic elements and the percentage content of the characteristic elements and the fluorescence intensity of the characteristic elements of the sample to be detected.
Although the percentage content of the elements tested by the energy dispersion X-ray fluorescence spectrometry has the characteristic of semi-quantification, the standard substance and the sample to be tested are tested under the same condition, and the raw materials in the standard substance and the sample to be tested are the same, so that the tested data has comparability.
Step S150: and calculating the sintering temperature of the sample to be detected according to the functional relation between the percentage content of the characteristic elements and the sintering temperature and the percentage content of the characteristic elements of the sample to be detected.
When the number of the characteristic elements is multiple, the sintering temperature corresponding to each characteristic element is obtained according to the functional relation between the percentage content of each characteristic element and the sintering temperature, and the sintering temperature of the standard product is the average value of the sintering temperatures corresponding to each characteristic element. Specifically, when the feature element is plural, the step S150 includes:
obtaining the sintering temperature calculated by the percentage of each characteristic element according to the functional relation between the percentage of each characteristic element and the sintering temperature and the percentage of each characteristic element of the sample to be tested;
and calculating the average value of the sintering temperature calculated by the percentage content of each characteristic element to obtain the sintering temperature of the sample to be detected.
The raw ore of the purple sand device is mainly divided into three series of red mud, purple mud, green mud and the like, and has different sintering temperatures according to the characteristics of different purple sand raw ore pug materials, generally between 1100 ℃ and 1250 ℃, and the sintering shrinkage rate is about 3-10%.
The method for testing the sintering temperature of the ceramic product at least has the following advantages:
(1) the method for testing the sintering temperature of the ceramic product adopts an energy dispersion X-ray fluorescence spectrometry to test the percentage content of the characteristic elements in the ceramic product, utilizes the characteristics of different element ignition loss and ignition shrinkage rate generated by the ceramic product in different high-temperature sintering temperature sections, uses the characteristic elements with higher percentage content of iron (Fe) and obvious reaction on ignition loss and ignition shrinkage rate to establish enough number of standard products with different sintering temperatures, and obtains the function relation between the sintering temperature in the standard product and the percentage content of the characteristic elements after statistical data such as statistical average value and the like are added, thereby measuring spectral data of a sample to be tested with unknown sintering temperature and obtaining the sintering temperature of the product according to the function relation.
(2) The method for testing the sintering temperature of the ceramic product is simple, and the sample is not required to be damaged, so that each produced sample to be tested can be tested.
Referring to fig. 2, a method for testing the precipitation amount of metal elements in a ceramic product according to an embodiment includes the following steps:
step S210: providing a plurality of standard samples, wherein the plurality of standard samples are prepared from the same raw materials and have different sintering temperatures.
Step S220: the precipitation amount of the metal element was measured for a plurality of standards.
Specifically, the metal element includes at least one of barium, iron, lead, cadmium, manganese, chromium, and cobalt. In step S220, the amount of precipitated metal elements is measured by flame atomic absorption spectrophotometry, inductively coupled plasma atomic emission spectrometry, or graphite furnace atomic absorption spectrophotometry.
Step S230: and obtaining a functional relation between the precipitation amount of the metal elements and the sintering temperature according to the precipitation amount of the characteristic elements of the plurality of standard samples and the sintering temperatures of the plurality of standard samples.
Specifically, step S230 includes:
establishing a relation curve chart of the precipitation amount of the metal elements and the sintering temperature according to the precipitation amount of the characteristic elements of the plurality of standard samples and the sintering temperature of the plurality of standard samples;
and fitting the relation curve graph to obtain a functional relation between the precipitation amount of the metal elements and the sintering temperature.
Step S240: and obtaining the sintering temperature of the sample to be detected.
Specifically, the sintering temperature of the sample to be tested can be calculated by the method for testing the sintering temperature of the ceramic product.
Step S250: and calculating to obtain the precipitation amount of the metal elements of the sample to be detected according to the sintering temperature of the sample to be detected and the functional relationship between the precipitation amount of the metal elements and the sintering temperature.
Research shows that the precipitation amount of metal elements of the ceramic product is in direct proportion to the content and the addition amount of heavy metals except for being related to the pH value of contained liquid, soaking time and porosity of the surface of the ceramic product, namely the precipitation amount is larger as the content and the addition amount are higher; inversely proportional to the sintering temperature, i.e., the higher the sintering temperature, the lower the amount of precipitates. The traditional technology can detect the content and the addition of heavy metals through a wet chemical method and a spectrum semi-quantitative analysis method, but does not have an effective, nondestructive, accurate and data-based method for measuring the sintering temperature of a ceramic product so as to ensure the precipitation of harmful heavy metals, and check and ensure the safety and the reliability of the ceramic product in use.
The method can test the precipitation amount of the metal element of the ceramic product, so that whether the precipitation amount of the metal element after the sample to be tested is contained in the liquid is in a specified range can be judged before the sample to be tested is used, and the safety and the reliability of the ceramic product in use are ensured.
In the actual production, the addition amount of the chemical raw materials is generally below the upper limit value of the addition amount, so that the precipitation amount of the metal elements in the ceramic product in use can be controlled within a safe use range by controlling the sintering temperature.
The method for testing the precipitation amount of the metal elements of the ceramic product at least has the following advantages:
(1) according to the method for testing the precipitation amount of the metal element of the ceramic product, the precipitation amount of the metal element is controlled from the perspective of controlling the sintering temperature by establishing a relation curve between the precipitation amount of the metal element and the sintering temperature, so that a sample to be tested can judge whether the precipitation amount of the metal element after containing liquid is in a specified range before use, and the safety and reliability of the ceramic product in use are ensured.
(2) The method for testing the precipitation amount of the metal elements of the ceramic product is simple, and the precipitation amount of the metal elements of each ceramic product is easy to monitor.
The following are specific examples:
it should be noted that the energy dispersive X-ray fluorescence spectrometer used in the examples is model number EDX 1800B (trade mark: Skyray).
Example 1
The specific process of the method for testing the sintering temperature of the sample to be tested in the embodiment 1 is as follows:
taking purple mud bottom groove green (tender mud) as an example, dividing the purple mud bottom groove green by 10 ℃, making five groups of samples between 1180 ℃ and 1220 ℃, wherein each group of samples comprises 10 purple sand test pieces, the five groups of samples are formed by respectively firing the samples at 1180 ℃, 1190 ℃, 1200 ℃, 1210 ℃ and 1220 ℃ for the same time, and then testing the percentage content of the characteristic elements of the purple sand test pieces by using an energy dispersion X-ray fluorescence spectrometry to obtain the average value of the percentage content of the characteristic elements of each group of samples, and the results are shown in the following table 1. And then according to the percentage content of the characteristic element and the sintering temperature, obtaining a functional relation between the percentage content of the characteristic element Fe and the sintering temperature as follows: y 103.05x-25316, where x denotes sintering temperature in degrees c and y denotes the percentage of Fe in ppm.
And testing the sample to be tested with unknown sintering temperature, which is prepared by taking purple mud bottom green as a raw material, by adopting an energy dispersion X-ray fluorescence spectrometry, wherein the percentage content of the characteristic element Fe of the sample to be tested is 97430 ppm.
And calculating to obtain the sintering temperature of the sample to be detected of about 1190 ℃ according to the percentage content of the characteristic elements of the sample to be detected and the functional relationship between the percentage content of the characteristic elements and the sintering temperature.
Table 1 data table of percent characteristic elements and sintering temperature for each set of samples from example 1
Example 2
The specific process of the method for testing the sintering temperature of the sample to be tested in the embodiment 2 is as follows:
taking the green mud of the Qinglongshan squama Manis as an example, the sintering temperature is generally about 1200-1230 ℃, 8 groups of samples with different sintering temperatures are sintered at 1170-1240 ℃, and the sintering temperature of each group of samples is shown in the following table 2. The number of the samples in each group is 10, the percentage content of the characteristic elements of each sample in each group is obtained by adopting an energy dispersive X-ray fluorescence spectrometry, the average value of the percentage content of the characteristic elements of each group is calculated, and a data table of the sintering temperature and the percentage content of the characteristic elements shown in the following table 2 is obtained.
According to the data of the percentage content of the characteristic element and the sintering temperature shown in the table 2, the functional relationship between the percentage content of the characteristic element Fe and the sintering temperature is obtained as follows: y is1＝5.10x1-3863.6, where x1Denotes the sintering temperature, in degrees Celsius, y1Represents the percentage content of characteristic element Fe, unit ppm; percentage content and sintering of characteristic element PbThe functional relationship of temperature is: y is2＝1.05x21126, wherein x2Denotes the sintering temperature, in degrees Celsius, y2Represents the percentage content of the characteristic element Pb in ppm; the functional relationship between the percentage content of the characteristic element Zr and the sintering temperature is as follows: y is3＝1.01x3-953.11, where x3Denotes the sintering temperature, in degrees Celsius, y3The percentage of Zr as a characteristic element is expressed in ppm.
And then, performing spectrum test on the green mud finished product device (marked as a sample to be tested) of the Qinglongshan armored mud ore with uncertain sintering temperature under the same condition to obtain the sample to be tested, wherein the percentage content of the iron element is 2210ppm, the percentage content of the lead element is 123ppm, and the percentage content of the zirconium element is 245 ppm.
Obtaining the sintering temperature of the sample to be detected to be 1191 ℃ according to the functional relation between the percentage content of the iron element and the sintering temperature and the percentage content of the iron element in the sample to be detected; obtaining the sintering temperature of the sample to be detected to be 1190 ℃ according to the functional relation between the percentage content of the lead element and the sintering temperature and the percentage content of the lead element in the sample to be detected; and obtaining the sintering temperature of the sample to be detected as 1186 ℃ according to the functional relation between the percentage content of the zirconium element and the sintering temperature and the percentage content of the zirconium element in the sample to be detected. And calculating the obtained sintering temperature according to different characteristic elements, and averaging to obtain the sintering temperature of the sample to be measured, which is 1189 ℃.
Table 2 data table of percentage of characteristic elements and sintering temperature for each set of samples in example 2
Example 3
The specific process of the test method for the precipitation amount of the metal element of the sample to be tested in example 3 is as follows:
after each group of samples in example 1 was cleaned, the samples were soaked in a 4% acetic acid solution for 24 hours, and then the amount of precipitated metal element in the acetic acid solution was measured to obtain the amount of precipitated metal element in each sample of each group of samples, and the amounts of precipitated metal element in 10 samples of each group of samples were averaged to obtain the data shown in table 3 below. Wherein, the precipitation amount of the metal elements is tested by adopting an inductively coupled plasma atomic emission spectrometry.
According to the sintering temperature of the sample to be tested which is 1190 ℃ and the precipitation amount of the metal elements and the sintering temperature of the sample which are measured in the embodiment 1, the test values of the precipitation amounts of the different metal elements after the sample to be tested is loaded are respectively shown in table 4.
Cleaning a sample to be tested, containing a 4% acetic acid solution, soaking for 24 hours, and then testing the precipitation amount of the heavy metal elements in the acetic acid solution by using an inductively coupled plasma atomic emission spectrometry to obtain the actual value of the precipitation amount of the metal elements in the sample to be tested, which is shown in the following table 4.
TABLE 3 data of the amount of metallic elements precipitated and sintering temperature for each set of samples in example 3
TABLE 4 table of values of measured values and actual values of the amount of precipitated metal elements in the sample to be measured
As can be seen from table 4, the difference between the test method for the amount of precipitated metal element in example 3 and the metal element precipitation amount obtained by the conventional test method is not large, which indicates that the test method for the amount of precipitated metal element in example 3 can be used for testing the amount of precipitated metal element, and the amount of precipitated metal element can be obtained before the ceramic product is used compared with the conventional method, thereby avoiding unsafe use of the ceramic product.
In examples 1 to 3, the sintering temperature and the amount of metal element precipitation of the purple sand product were measured, and the sintering temperature and the amount of metal element precipitation of other ceramic products were also obtained by the above-mentioned methods.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. A method for testing the sintering temperature of a ceramic product is characterized by comprising the following steps:
step S110, providing a plurality of standard products, wherein the plurality of standard products are prepared from the same raw materials and have different sintering temperatures;
step S120, testing the percentage content of the characteristic elements of each standard product by adopting an energy dispersion X-ray fluorescence spectrometry to obtain the percentage content of the characteristic elements of each standard product;
step S130, obtaining a functional relation between the percentage content of the characteristic elements and the sintering temperature according to the percentage content of the characteristic elements of the plurality of standard products and the sintering temperatures of the plurality of standard products;
step S140, testing a sample to be tested by adopting the energy dispersion X-ray fluorescence spectrometry to obtain the percentage content of the characteristic elements of the sample to be tested, wherein the preparation raw material of the sample to be tested is the same as that of the standard product; and
s150, calculating the sintering temperature of the sample to be detected according to the functional relation between the percentage content of the characteristic elements and the sintering temperature and the percentage content of the characteristic elements of the sample to be detected;
the characteristic elements comprise at least one of iron, titanium, potassium, lead, aluminum, zirconium, yttrium, rubidium, strontium and manganese.
2. The test method according to claim 1, wherein the number of the characteristic elements is 1 to 3.
3. The testing method of claim 1, wherein step S130 comprises:
establishing a relation curve of the percentage content of the characteristic elements and the sintering temperature according to the percentage content of the characteristic elements of the plurality of standard products and the sintering temperatures of the plurality of standard products;
and performing linear fitting on the relation curve to obtain a functional relation between the percentage content of the characteristic elements and the sintering temperature.
4. The testing method according to claim 1, wherein the feature element is a plurality of, and step S150 includes:
obtaining the sintering temperature calculated by the percentage of each characteristic element according to the functional relation between the percentage of each characteristic element and the sintering temperature and the percentage of each characteristic element of the sample to be tested;
and calculating the average value of the sintering temperatures calculated according to the percentage content of each characteristic element to obtain the sintering temperature of the sample to be detected.
5. The test method of claim 1, wherein the standards are at least five.
6. The testing method of claim 1, wherein step S120 comprises:
providing a plurality of test articles containing the characteristic elements, wherein the percentage content of the characteristic elements of the test articles is different;
testing each test article by using an energy dispersion X-ray fluorescence spectrometer to obtain the fluorescence intensity of the characteristic elements of each test article;
obtaining a functional relation between the fluorescence intensity of the characteristic elements and the percentage content of the characteristic elements according to the fluorescence intensity of the characteristic elements of the plurality of test articles and the percentage content of the characteristic elements of the plurality of test articles;
testing each standard product by using the energy dispersion X-ray fluorescence spectrometer to obtain the fluorescence intensity of the characteristic elements of each standard product;
and obtaining the percentage content of the characteristic elements of each standard product according to the functional relation between the fluorescence intensity of the characteristic elements and the percentage content of the characteristic elements and the fluorescence intensity of the characteristic elements of each standard product.
7. The test method of claim 6, wherein step S140 comprises:
testing the sample to be tested by using the energy dispersion X-ray fluorescence spectrometer to obtain the fluorescence intensity of the characteristic elements of the sample to be tested;
and obtaining the percentage content of the characteristic elements of the sample to be detected according to the functional relation between the fluorescence intensity of the characteristic elements and the percentage content of the characteristic elements and the fluorescence intensity of the characteristic elements of the sample to be detected.
8. A method for testing the precipitation amount of metal elements in a ceramic product is characterized by comprising the following steps:
step S210, providing a plurality of standard samples, wherein the plurality of standard samples are prepared from the same raw material and have different sintering temperatures;
step S220, testing the precipitation amount of the metal elements of the plurality of standard samples;
step S230, obtaining a functional relation between the precipitation amount of the metal elements and the sintering temperature according to the precipitation amount of the metal elements of the plurality of standard samples and the sintering temperatures of the plurality of standard samples;
s240, obtaining the sintering temperature of the sample to be tested by adopting the testing method of any one of claims 1-7; and
step S250, calculating the precipitation amount of the metal element of the sample to be detected according to the sintering temperature of the sample to be detected and the functional relationship between the precipitation amount of the metal element and the sintering temperature;
the metal element comprises at least one of barium, iron, lead, cadmium, manganese, chromium and cobalt.
9. The method for testing the precipitation amount of a metal element according to claim 8, wherein the method for testing the precipitation amount of a metal element of a plurality of the standards is flame atomic absorption spectrometry, inductively coupled plasma atomic emission spectrometry, or graphite furnace atomic absorption spectrometry.
10. The testing method of claim 8, wherein step S230 comprises:
establishing a relation curve chart of the precipitation amount of the metal elements and the sintering temperature according to the precipitation amount of the metal elements of the plurality of standard samples and the sintering temperature of the plurality of standard samples;
and fitting the relation curve graph to obtain a functional relation between the precipitation amount of the metal elements and the sintering temperature.
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