CN107462449B - Sample preparation method based on hot wire method - Google Patents
Sample preparation method based on hot wire method Download PDFInfo
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- CN107462449B CN107462449B CN201710652422.0A CN201710652422A CN107462449B CN 107462449 B CN107462449 B CN 107462449B CN 201710652422 A CN201710652422 A CN 201710652422A CN 107462449 B CN107462449 B CN 107462449B
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- hot wire
- water quenching
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/42—Low-temperature sample treatment, e.g. cryofixation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2866—Grinding or homogeneising
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
- G01N2001/386—Other diluting or mixing processes
Abstract
The invention belongs to the technical field of hot wire method detection, and discloses a novel hot wire method sample preparation method, which comprises the following steps: mechanically grinding and homogenizing the sample; placing the mechanically ground and homogenized sample into a beaker, adding analytically pure alcohol, and stirring; putting the sample after the alcohol stirring into a muffle furnace at 825 ℃ for calcining; placing the calcined sample in a dry normal-temperature environment and cooling to room temperature; and finally, grinding the cooled calcined sample and sieving the ground calcined sample by a 200-mesh sieve to obtain a hot wire method sample. According to the invention, the sample preparation is carried out in a two-step mechanical homogenization and calcination mode, so that the sample achieves a good homogenization effect and good repeatability, and the complicated sample preparation steps in the traditional melting water quenching sample preparation process are further simplified; the sample preparation method by the hot wire method can eliminate segregation caused by crystallization of a high-crystallinity sample in the traditional melting water quenching sample preparation process, eliminate component change caused by ion exchange in the traditional melting water quenching sample preparation process, and is simpler and more convenient compared with the traditional melting water quenching sample preparation process.
Description
Technical Field
The invention belongs to a sample preparation method related to a hot wire method detection technology, and particularly relates to a sample preparation method based on a hot wire method.
Technical Field
SHTT (Single Hot thermo technique) is a high-temperature in-situ analyzer, is applied to the aspects of heating and melting state of metallurgical slag, crystallization in continuous cooling process, crystallization in fixed temperature and heat preservation process and the like, and is particularly widely applied to the analysis of crystallization behavior of continuous casting mold powder. The traditional melting water quenching sample preparation method is that 50g of samples are mechanically mixed and then homogenized in a high-temperature silicon-molybdenum furnace at 1400 ℃; then water quenching the homogenized molten covering slag to keep the vitrification structure state of the sample in a high temperature state; and finally, drying and grinding the water quenching slag, and sieving the water quenching slag by a 200-mesh sieve to obtain an experimental slag sample.
When the traditional melting water quenching sample preparation method is used for preparing the continuous casting mold flux with the crystal precipitation temperature higher than 1400 ℃, because the component is over-cooled at 1400 ℃, a small amount of crystals are precipitated in the processes of high-temperature melting and heat preservation homogenization for 15min, so that the slag sample after water quenching has a crystalline phase, the components of the prepared sample are uneven, and the likeThe result of the hot wire method test is sounded; in the traditional water quenching process of a molten water quenching sample, certain ion exchange occurs when high-temperature molten slag is contacted with water, so that the components of the protective slag are changed, such as Na+、K+、F-And the crystallization capacity of the covering slag is weakened due to the diffusion of the covering slag into water, so that the test result of a hot wire method is greatly influenced.
Disclosure of Invention
The invention provides a hot wire method for preparing a sample, aiming at solving the problems of non-uniform components and component change in the sample preparation process of the traditional melt water quenching method.
In order to solve the technical problem, the invention provides a hot wire method based sample preparation method, which comprises the following steps:
s1, grinding and homogenizing the prepared sample;
s2, placing the grinded and homogenized sample into a container, adding analytically pure alcohol, and stirring;
s3, placing the sample after the analytically pure alcohol is stirred and mixed into a muffle furnace for high-temperature calcination;
and S4, cooling the slag sample (sample) after calcination, grinding and sieving to obtain the hot wire method sample.
The invention uses a two-step mechanical homogenization and calcination mode to prepare the sample, so that the sample achieves a good homogenization effect, has good repeatability, solves the problems of component nonuniformity caused by crystal precipitation, component change caused by ion exchange and the like in the traditional melt water quenching sample preparation process, and further simplifies the complicated sample preparation steps in the traditional melt water quenching sample preparation process.
Further, in step S1, the sample is homogenized using a pulverization and homogenization device (e.g., an electromagnetic ore pulverizer).
Further, in step S1, the milling homogenization time should be greater than 40S.
Further, in step S2, the sample is stirred using a stirring device (e.g., a table top stirrer).
Furthermore, 3-8ml of analytically pure alcohol is required to be added into each 10g of sample to promote homogenization, and the stirring time is more than 20 min.
Further, in step S3, a ceramic crucible is used to hold the sample.
Further, in step S3, a muffle furnace is used for calcination.
Furthermore, the calcination temperature is 700-900 ℃, and the calcination time is more than 15 min.
Further, in step S4, the calcined sample is air-cooled to room temperature.
Further, in step S4, the cooled sample was ground using a mortar and passed through a 200-mesh sieve.
The technical scheme provided by the invention can realize accurate analysis of the sample by hot wire method equipment. Specifically, compared with the prior art, the invention has the following technical characteristics:
1. the invention uses a two-step mechanical homogenization and calcination mode to prepare the sample, so that the sample achieves a good homogenization effect, has good repeatability, solves the problems of component nonuniformity caused by crystal precipitation, component change caused by ion exchange and the like in the traditional melt water quenching sample preparation process, and further simplifies the complicated sample preparation steps in the traditional melt water quenching sample preparation process.
2. The method can eliminate segregation caused by crystallization of a high-crystallization-performance sample in the traditional melting water quenching sample process, eliminate component change caused by ion exchange in the traditional melting water quenching sample process, and is simpler and more convenient than the traditional melting water quenching sample process.
Drawings
FIG. 1 is a schematic flow diagram of the present invention;
FIGS. 2(a), 2(b), 2(c) and 2(d) are XRD analysis of sample No. 1 in the novel sample preparation method, XRD analysis of sample No. 1 in the conventional molten water quenching method, XRD analysis of sample No. 2 in the novel sample preparation method and XRD analysis of sample No. 2 in the conventional molten water quenching method, respectively;
FIG. 3 is a temperature control curve of a hot-wire method;
fig. 4(a), 4(b), 4(c), and 4(d) are a sample repeatability experiment of the novel sample preparation method 1# sample, a sample repeatability experiment of the conventional melt water quenching sample preparation method 1# sample, a sample repeatability experiment of the novel sample preparation method 2# sample, and a sample repeatability experiment of the conventional melt water quenching sample preparation method 2# sample, respectively.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In order to solve the problems of component nonuniformity caused by crystal precipitation in the homogenization process of the traditional molten water quenching sample preparation method and component change caused by ion exchange in the water quenching process, the general idea of the scheme provided by the application is as follows, and the method comprises the following steps:
(1) preparing a sample according to the process requirements, and putting the prepared sample (50 g of slag sample) into a grinder to grind and homogenize for more than 40 s;
(2) putting the ground and homogenized sample into a beaker, adding 15-40ml of alcohol (analytically pure), and then stirring and mixing by using a desktop stirrer for more than 20 min;
(3) putting the stirred sample into a ceramic crucible, then putting the ceramic crucible into a muffle furnace, and calcining at the temperature of 700-900 ℃, preferably at the temperature of 800-850 ℃, wherein the calcining time is 15-40 min;
(4) and grinding the calcined and air-cooled sample (slag sample), and sieving with a 200-mesh sieve to obtain the sample of the invention.
Wherein, an electromagnetic ore crusher is used for homogenizing a sample;
in step S1, the grinding homogenization time is greater than 40S, determined in particular according to the sample size;
in step S2, the sample is stirred and mixed by a stirrer, and the fine sample powder 9 (powder) after being ground and homogenized is mixed with alcohol uniformly;
analysis of the amount of pure alcohol added: 3-8ml of analytically pure alcohol is added into each 10g of sample to promote homogenization, and the stirring time is more than 20 min. Specifically, 3ml, 4ml, 5ml, 6ml, 7ml and 8ml of pure analytical alcohol may be added to 10g of the sample, and the requirements of the present invention can be satisfied.
In step S3, a ceramic crucible is used to hold the sample.
In step S3, calcination is performed using a muffle furnace.
The calcining temperature of the muffle furnace is 700-900 ℃, and the calcining time is more than 15min and less than 60 min. The specific calcination temperature can be selected from 700 deg.C, 710 deg.C, 720 deg.C, 730 deg.C, 740 deg.C, 750 deg.C, 760 deg.C, 770 deg.C, 780 deg.C, 790 deg.C, 800 deg.C, 810 deg.C, 820 deg.C, 830 deg.C, 840 deg.C, 850 deg.C, 860 deg.C, 870 deg.C, 880 deg.C, 890 deg.C, 900.
In step S4, after the muffle furnace calcination, the calcined sample was air-cooled to room temperature.
In step S4, the cooled sample is ground and sieved through a 200 mesh sieve.
The performance test is carried out on the sample treated by the method:
TABLE 1 Experimental slag system composition (m%)
The results of X-ray diffraction measurements are shown in FIG. 2.
Fig. 2(a) and 2(c) show the results of X-ray diffraction detection of samples # 1 and # 2 obtained by the novel sample preparation method of the present invention, and it can be seen from the images that the samples obtained by the novel sample preparation method maintain the raw material state.
Fig. 2(b) and 2(d) are X-ray diffraction detection results of # 1 and # 2 samples prepared by a traditional molten water quenching sample preparation method, and it can be seen from the images that the # 1 slag sample with weak crystallization performance achieves disordered glass phase homogenization effect, while the # 2 slag sample with strong crystallization performance has obvious crystallization peak and can not achieve disordered glass phase homogenization effect.
And (3) performing repeated experiment tests, namely selecting 1# and 2# samples prepared by a traditional melting water quenching sample preparation method and a novel sample preparation method to perform thermal insulation crystallization performance tests by a hot wire method, wherein the temperature control curve of the hot wire method is shown in figure 3.
The sample was subjected to the crystallization ability test at the same holding temperature, and repeated 5 times, to obtain the crystallization initiation and crystallization completion times, and the results are shown in FIG. 4.
Comparing fig. 4(a) and 4(b), it can be seen that, for the 1# mold flux with weak crystallization property, the conventional melt water quenching sample preparation method and the novel sample preparation method can both achieve better reproduction requirements, and the fluctuation range is ± 5 ℃.
Comparing fig. 4(c) and 4(d), it can be seen that, for the 2# mold powder with strong crystallization property, the reproducibility of the conventional melt water quenching sample preparation method is poor, the fluctuation range is ± 13 ℃, while the novel sample preparation method of the present invention still achieves good reproducibility requirements, and the fluctuation range is ± 5 ℃.
Therefore, the method can eliminate segregation caused by crystallization of the high-crystallinity sample in the traditional melting water quenching sample process, eliminate component change caused by ion exchange in the traditional melting water quenching sample process, and is simpler and more convenient compared with the traditional melting water quenching sample process.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the technical solutions, and although the present invention has been described in detail by referring to the preferred embodiments, those skilled in the art should understand that modifications or equivalent substitutions to the technical solutions of the present invention can be made without departing from the spirit and scope of the technical solutions, and all the modifications and equivalent substitutions should be covered by the claims of the present invention.
Claims (2)
1. A sample preparation method based on a hot wire method is characterized by comprising the following steps:
s1, putting the prepared sample into a crushing and homogenizing device for grinding and homogenizing; grinding homogenization time is more than 40 s;
s2, putting the grinded and homogenized sample into a container, adding alcohol, and stirring uniformly; adding 3-8ml of alcohol into each 10g of sample to promote homogenization, and stirring for more than 20 min; stirring and mixing the sample by using a stirrer to be uniformly mixed;
s3, putting the alcohol stirred sample into a muffle furnace for high-temperature calcination; a ceramic crucible is used for containing a sample, the calcining temperature in a muffle furnace is 700-850 ℃, and the calcining time is more than 15 min;
and S4, cooling the calcined slag sample in air to room temperature, grinding and sieving the slag sample with a 200-mesh sieve to obtain a hot wire method sample.
2. The sample preparation method according to claim 1, wherein the sample is homogenized by using an electromagnetic ore mill in step S1.
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Effective date of registration: 20230918 Address after: No. 1 Intelligent Equipment Industrial Park, Yichuan County, Luoyang City, Henan Province, 471311 Patentee after: Luoyang Kefeng Metallurgical New Materials Co.,Ltd. Address before: 400044 No. 174 Sha Jie street, Shapingba District, Chongqing Patentee before: Chongqing University |