CN112461635A - Stemming sample and preparation method thereof - Google Patents
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- CN112461635A CN112461635A CN202011444976.XA CN202011444976A CN112461635A CN 112461635 A CN112461635 A CN 112461635A CN 202011444976 A CN202011444976 A CN 202011444976A CN 112461635 A CN112461635 A CN 112461635A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 238000010438 heat treatment Methods 0.000 claims abstract description 59
- 230000008014 freezing Effects 0.000 claims abstract description 36
- 238000007710 freezing Methods 0.000 claims abstract description 36
- 238000000034 method Methods 0.000 claims abstract description 32
- 238000012360 testing method Methods 0.000 claims description 16
- 238000000465 moulding Methods 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 230000008859 change Effects 0.000 abstract description 9
- 239000011819 refractory material Substances 0.000 abstract description 3
- 238000005057 refrigeration Methods 0.000 description 12
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 10
- 238000011056 performance test Methods 0.000 description 9
- 239000002994 raw material Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 6
- 239000004519 grease Substances 0.000 description 6
- 230000001050 lubricating effect Effects 0.000 description 6
- 239000003755 preservative agent Substances 0.000 description 6
- 230000002335 preservative effect Effects 0.000 description 6
- 229910052742 iron Inorganic materials 0.000 description 5
- 238000012986 modification Methods 0.000 description 5
- 230000004048 modification Effects 0.000 description 5
- 239000011230 binding agent Substances 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 230000006835 compression Effects 0.000 description 3
- 238000007906 compression Methods 0.000 description 3
- 230000008961 swelling Effects 0.000 description 3
- 230000032798 delamination Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000003628 erosive effect Effects 0.000 description 2
- 238000010079 rubber tapping Methods 0.000 description 2
- 238000005464 sample preparation method Methods 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 239000010426 asphalt Substances 0.000 description 1
- 238000010009 beating Methods 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000007767 bonding agent Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000009991 scouring Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 239000011269 tar Substances 0.000 description 1
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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
- G01N1/36—Embedding or analogous mounting of samples
-
- 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
-
- 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
-
- 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
- G01N1/36—Embedding or analogous mounting of samples
- G01N2001/366—Moulds; Demoulding
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
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- Sampling And Sample Adjustment (AREA)
Abstract
The invention belongs to the technical field of unshaped refractory materials, and particularly relates to a stemming sample and a preparation method thereof, wherein the method comprises the steps of heating and forming stemming to obtain a sample blank with a mold; and (3) performing first freezing on the sample blank with the mold at the temperature of less than or equal to-5 ℃ for more than or equal to 1h, and then demolding to obtain the stemming sample. The stemming sample prepared by the method provided by the invention has stable appearance size and no bulging problem, and can be used for accurately measuring the performances such as density, strength and linear change related to the stemming sample size.
Description
Technical Field
The invention belongs to the technical field of unshaped refractory materials, and particularly relates to a stemming sample and a preparation method thereof.
Background
The stemming is a refractory material for blocking the tap hole of a blast furnace, which is prepared by materials such as aluminum silicate, SiC, coke particles and the like, a binding agent and an additive. The stemming has the functions of not only filling a blast furnace taphole channel, but also forming a mud bag in a blast furnace hearth and maintaining enough taphole depth; at the same time, the opening is easy, the mud beating operation is easy, and the slag and iron are resistant to physical and chemical erosion. The stemming quality is poor, and problems of a wet iron notch, a shallow iron notch, an iron notch breakage, large flow running, pressure reduction, air release, burnout of equipment in front of a furnace and the like can occur during use, so that the production is influenced.
In order to meet the requirement of safe production of the blast furnace, the taphole stemming is required to have the following properties: 1) the plasticity and the cohesiveness are good, and the iron notch channel is easy to extrude and fill; 2) the porosity is proper, and moisture and gas are conveniently discharged during drying; 3) the high-temperature volume shrinkage is small, and cracks can be avoided; 4) the sintering performance is good, the strength is high, and the scouring resistance and the erosion resistance are realized; 5) the tapping performance is good, and the tapping machine is easy to drill; 6) the environmental pollution is small; 7) has high fire resistance. In order to evaluate the quality of the stemming performance for the blast furnace, a testing of the physical and chemical performance of the stemming is required, a standard stemming sample block must be provided, and the preparation method of the sample has a decisive influence on the test result.
At present, the preparation of the stemming sample is generally to place the weighed stemming into a mold, manually stamp or mechanically press the stemming until the stemming is tamped or mechanically pressed to be compact, then demould the stemming after low-temperature heat treatment at 200-400 ℃ to prepare the stemming sample, and then perform performance tests at different temperatures. The stemming sample prepared by the traditional method has bulging deformation, and meanwhile, the demolding is difficult, so that the accuracy of the detection result of the density, the strength and the linear change performance of the stemming can be influenced.
Disclosure of Invention
In order to solve the technical problems, the invention provides a stemming sample and a preparation method thereof, and the sample prepared by the method has a stable shape and can be used for accurately testing the performance of stemming, such as density, strength and linear change, related to the size of the sample.
In one aspect, the present invention provides a method for preparing a stemming sample, the method comprising,
heating and molding the stemming to obtain a sample blank with a mold;
and (3) performing first freezing on the sample blank with the mold at the temperature of less than or equal to-5 ℃ for more than or equal to 1h, and then demolding to obtain the stemming sample.
Further, the freezing temperature is-5 to-20 ℃, and the freezing time is 1 to 4 hours.
Further, the heating temperature is 40-110 ℃, and the heating time is 0.5-5 h.
Further, the heating device is any one of the following devices: an oven and a heating furnace.
Further, the Marshall value of the sample blank with the die is 0.85-1 MPa.
Further, the pressure of the forming process is 2-5 KN.
Further, the method also comprises the step of carrying out heat treatment on the stemming sample to carry out performance test.
Further, the heat treatment of the stemming sample comprises the following steps,
carrying out second freezing treatment on the stemming sample;
and carrying out heat treatment on the stemming sample subjected to the second freezing treatment.
Further, the time interval between the end of the demolding and the start of the second freezing is less than 0.5h, and the time interval between the end of the second freezing treatment and the start of the heat treatment is less than 0.5 h.
On the other hand, the embodiment of the invention provides a stemming sample which is prepared by the preparation method of the stemming sample.
One or more technical solutions in the embodiments of the present invention have at least the following technical effects or advantages:
the invention provides a stemming sample and a preparation method thereof, which at least have the following advantages:
(1) the formed sample blank with the die is subjected to first freezing, so that the formed shape can be kept without collapsing; the stemming sample after demoulding is taken out from the refrigeration equipment quickly for carbon-embedded heat treatment, and the problem that the upper surface of the sample bulges and deforms due to the fact that the solidification reaction such as resin, tar and the like generates gas and the raw materials volatilize when the stemming sample is prepared in the traditional method for low-temperature heat treatment can be solved due to the fact that the stemming sample passes through the low-temperature section quickly, and the problem that demoulding is difficult due to the adhesion of a binding agent and a mould in the traditional sample preparation low-temperature heat treatment can be solved.
(2) The stemming is softened at a certain temperature and time, and is molded under a certain pressure when reaching a specific Marshall value, so that the prepared sample has small performance test error after molding, and the stemming has comparability when being applied to stemming of different types and stemming prepared at different times.
(3) The surface of the mould is coated with low-temperature lubricating grease and is paved with preservative film or newspaper, so that the sample is easy to demould.
(4) After the sample is frozen for a certain time, the sample is hardened, has initial strength but no icing phenomenon on the surface, and does not influence the performance of the sample. And the sample after hardening and demoulding does not swell and deform.
(5) The freezing time and the taking and placing time are strictly controlled, so that the flatness of the sample is ensured, and the performance tests such as density, strength, linear change and the like are not influenced.
(6) The method can solve the problems of no hardening of stemming sample preparation at normal temperature, bulging deformation, delamination, difficult demoulding and the like of sample preparation at high temperature, and the prepared stemming sample is not deformed, does not delaminate and is easy to demould, and can well meet various physical and chemical property tests.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on the drawings without creative efforts.
Fig. 1 is a process diagram of a preparation method of a stemming sample according to an embodiment of the present invention.
Detailed Description
The present invention will be described in detail below with reference to specific embodiments and examples, and the advantages and various effects of the present invention will be more clearly apparent therefrom. It will be understood by those skilled in the art that these specific embodiments and examples are for the purpose of illustrating the invention and are not to be construed as limiting the invention.
Throughout the specification, unless otherwise specifically noted, terms used herein should be understood as having meanings as commonly used in the art. Accordingly, 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. If there is a conflict, the present specification will control.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
In order to solve the technical problems, the embodiment of the invention provides the following general ideas:
in one aspect, an embodiment of the present invention provides a method for preparing a stemming sample, which, with reference to fig. 1, includes,
s1, heating and molding the stemming to obtain a sample blank with a mold;
s2, demolding the sample blank with the mold after the first freezing for more than or equal to 1h at the temperature of less than or equal to-5 ℃ to obtain the stemming sample.
According to the traditional processing method of the stemming sample, the stemming is tamped or compacted by a machine, and then is subjected to low-temperature heat treatment at the temperature of 200-400 ℃ and then is demoulded, and binding agents such as tar, asphalt, resin and the like in the stemming raw materials can generate curing reaction to produce gas volatilization during the low-temperature heat treatment, so that the upper surface of the stemming sample can be expanded easily. The formed sample blank with the mold is subjected to first freezing, so that the formed shape of the sample blank can be kept and the sample blank does not collapse, the problems that gas is generated by curing reaction of resin, tar and the like and raw materials are volatilized to cause bulging deformation on the upper surface of the sample when the traditional stemming sample is prepared for low-temperature heat treatment can be solved, and the problem that demolding is difficult due to adhesion of a bonding agent and the mold when the traditional sample preparation low-temperature heat treatment is carried out can be solved. And the temperature rising speed of the stemming sample is high in the process of carbon-embedded heat treatment for performance test, and the problem of bulging cannot occur. The first freezing temperature is too high, the first freezing time is too short, and the sample blank is difficult to ensure that the demoulded sample blank keeps the formed shape, so that the preparation of the stemming sample fails.
As an implementation mode of the embodiment of the invention, the freezing temperature is-5 to-20 ℃, and the freezing time is 1 to 4 hours. In order to save energy and prevent the surface from icing, the freezing temperature should not be too low.
As an implementation manner of the embodiment of the invention, the heating temperature is 40-110 ℃, and the heating time is 0.5-5 h.
The stemming can be softened by controlling the heating temperature and the heating time, so that the stemming reaches a specific Marshall value, and is formed by certain pressure, the testing error of the performance of the stemming sample is small, and the stemming sample is applicable to stemming of different types and stemming made in different time and has comparability.
As an implementation manner of the embodiment of the present invention, the heating device is any one of the following devices: an oven and a heating furnace.
As an implementation mode of the embodiment of the invention, the Marshall value of the sample blank with the die is 0.85-1 MPa.
The Marshall value of the stemming is an index for representing the plasticity of the stemming, and the Marshall value of the stemming is controlled in sample preparation mainly for controlling the molding pressure. If the Marshall value is too high, the stemming is hard, the molding pressure is increased, and the performance test is easily influenced by layering during molding; if the Marshall value is low excessively, the stemming is too soft, the contact surface of the pressure head and the stemming is not easy to separate during molding, low-temperature lubricating grease is coated on the surface of the external mold, and a preservative film or newspaper is laid, so that molding is affected by easy compaction.
As an implementation manner of the embodiment of the invention, the pressure in the forming process is 2-5 KN. The stemming sample can be compacted by controlling the pressure.
As an implementation of the embodiment of the invention, the method further comprises heat-treating the stemming sample for performance testing. The heat treatment is generally a buried carbon heat treatment, and the temperature of the heat treatment is selected according to the performance test requirements of the stemming sample, such as 800 ℃, 1000 ℃ and 1200 ℃, and is not particularly limited herein.
As an implementation of the embodiment of the present invention, the heat treatment of the stemming sample includes,
carrying out second freezing treatment on the stemming sample;
and carrying out heat treatment on the stemming sample subjected to the second freezing treatment.
And the sample is subjected to second freezing treatment to serve as a stemming sample for preservation, and can be flexibly taken according to the testing requirement of the stemming sample performance.
In one embodiment of the present invention, the time interval between the end of the mold release and the start of the second freezing is less than 0.5 hour, and the time interval between the end of the second freezing and the start of the heat treatment is less than 0.5 hour. Too long time intervals can cause the temperature rise of the stemming sample, the stemming sample is softened, and the shape of the stemming sample cannot be kept.
On the other hand, the embodiment of the invention provides a stemming sample which is prepared by the preparation method of the stemming sample.
A stemming sample and a preparation method thereof according to the present invention will be described in detail below with reference to examples, comparative examples and experimental data.
Example 1
Embodiment 1 provides a method for preparing a stemming sample, which includes the steps of:
(1) coating low-temperature lubricating grease on the surface of a 25-140 mm special triple die and paving a preservative film to prevent adhesion;
(2) putting the stemming raw material into an oven at 80 ℃, and heating for softening; after heating and softening for 1h, determining the Marshall value of the stemming to be 0.9 MPa; extracting a 500g sample, and forming the sample into a 25 × 140mm triple die by using a pressure tester with the pressure of 2 KN;
(3) putting the molded sample and the mold into a refrigeration device at the temperature of-10 ℃, and quickly demolding after freezing for 2 hours to obtain a stemming sample;
taking out the formed stemming sample from the refrigeration equipment before heat treatment, carrying out carbon-burying heat treatment, and testing the density, strength and linear change of the stemming sample; the time from the freezing equipment to the start of the heat treatment was 14 min.
Example 2
Embodiment 2 provides a stemming sample preparation method, which includes the steps:
(1) coating low-temperature lubricating grease on the surface of a triple die with the thickness of 40-160 mm, and laying newspaper to prevent adhesion;
(2) putting the stemming raw material into a drying oven at 60 ℃, and heating for softening; after heating and softening for 2h, determining the Marshall value of the stemming to be 0.87 MPa; a 1460g sample is extracted and is molded into a 40 × 160mm triple die by a compression testing machine by using 3KN pressure;
(3) putting the molded sample and the mold into a refrigeration device at the temperature of-15 ℃, and quickly demolding after freezing for 1.5h to obtain a stemming sample; the demoulded sample is wrapped by a preservative film and placed into a flat tray, and then placed into refrigeration equipment at the temperature of-10 ℃ again, and the demoulded sample is placed into the refrigeration equipment again for 22 min;
and (3) quickly taking out the molded sample from the refrigeration equipment before heat treatment, carrying out carbon-embedding heat treatment, and testing the density, strength and linear change of the stemming sample.
Example 3
Embodiment 3 provides a stemming sample preparation method, which includes the steps:
(1) coating low-temperature lubricating grease on the surface of a triple die with the thickness of 40-160 mm, and laying newspaper to prevent adhesion;
(2) putting the stemming raw material into an oven at 80 ℃, and heating for softening; after heating and softening for 3h, determining the Marshall value of the stemming to be 0.87 MPa; a 1460g sample is extracted and is molded into a 40 × 160mm triple die by a compression testing machine by using 3KN pressure;
(3) putting the molded sample and the mold into a refrigeration device at the temperature of-18 ℃, and quickly demolding after freezing for 1h to obtain a stemming sample; the demoulded sample is wrapped by a preservative film and placed into a flat tray, and then placed into refrigeration equipment at the temperature of-18 ℃ again, and the demoulded sample is placed into the refrigeration equipment again for 22 min;
and (3) quickly taking out the molded sample from the refrigeration equipment before heat treatment, carrying out carbon-embedding heat treatment, and testing the density, strength and linear change of the stemming sample.
Comparative example 1
Comparative example 1 provides a method for preparing a stemming specimen, comprising the steps of:
(1) putting the same stemming raw material as the embodiment 3 into an oven at 80 ℃, and heating for softening; after heating and softening for 3h, determining the Marshall value of the stemming to be 0.87 MPa; a 1460g sample is extracted and is molded into a 40 × 160mm triple die by a compression testing machine by using 3KN pressure;
(2) and heating the molded sample and the mold to 300 ℃ for 3.5 hours, and demolding to obtain the stemming sample.
And (3) carrying out carbon-embedding heat treatment on the molded sample to test the density, strength and linear change of the stemming sample.
The stemming samples formed in examples 1-3 have no swelling problem, and have good dimensional and appearance, and the dimensions are shown in Table 1. The stemming sample prepared in comparative example 1 had a swelling problem on the upper surface.
TABLE 1
| Numbering | Stemming sample size |
| Example 1 | 25*25*140mm |
| Example 2 | 40*40*160mm |
| Example 3 | 40*40*160mm |
| Comparative example 1 | 40*42*160mm |
The stemming specimens prepared using examples 1 to 3 were identical in size to the mold, and the stemming specimen prepared in comparative example 1 was 42mm in height, 2mm higher than the mold by 40mm in height, indicating that swelling of the upper surface occurred during the preparation process.
The stemming sample and the preparation method thereof provided by the invention at least have the following advantages:
(1) the formed sample blank with the die is subjected to first freezing, so that the formed shape can be kept without collapsing; the stemming sample after demoulding is taken out from the refrigeration equipment quickly for carbon-embedded heat treatment, and the problem that the upper surface of the sample bulges and deforms due to the fact that the solidification reaction such as resin, tar and the like generates gas and the raw materials volatilize when the stemming sample is prepared in the traditional method for low-temperature heat treatment can be solved due to the fact that the stemming sample passes through the low-temperature section quickly, and the problem that demoulding is difficult due to the adhesion of a binding agent and a mould in the traditional sample preparation low-temperature heat treatment can be solved.
(2) The stemming is softened at a certain temperature and time, and is molded under a certain pressure when reaching a specific Marshall value, so that the prepared sample has small performance test error after molding, and the stemming has comparability when being applied to stemming of different types and stemming prepared at different times.
(3) The surface of the mould is coated with low-temperature lubricating grease and is paved with preservative film or newspaper, so that the sample is easy to demould.
(4) After freezing for a certain time, the sample blank is hardened and has initial strength but no icing phenomenon on the surface, and the performance of the sample is not influenced. And the sample after hardening and demoulding does not swell and deform.
(5) The freezing time and the taking and placing time are strictly controlled, so that the flatness of the sample is ensured, and the performance tests such as density, strength, linear change and the like are not influenced.
(6) The method can solve the problems of no hardening of stemming sample preparation at normal temperature, bulging deformation, delamination, difficult demoulding and the like of sample preparation at high temperature, and the prepared stemming sample is not deformed, does not delaminate and is easy to demould, and can well meet various physical and chemical property tests.
Finally, it should also be noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (10)
1. A preparation method of a stemming sample is characterized by comprising the following steps,
heating and molding the stemming to obtain a sample blank with a mold;
and (3) performing first freezing on the sample blank with the mold at the temperature of less than or equal to-5 ℃ for more than or equal to 1h, and then demolding to obtain the stemming sample.
2. The preparation method of the stemming sample according to claim 1, wherein the freezing temperature is-5 to-20 ℃, and the freezing time is 1 to 4 hours.
3. The method for preparing the stemming sample according to claim 1, wherein the heating temperature is 40-110 ℃, and the heating time is 0.5-5 h.
4. The method for preparing a stemming sample according to claim 1, wherein the heating device is any one of the following: an oven and a heating furnace.
5. The method for preparing the stemming sample according to claim 1, wherein the Marshall value of the sample blank with the mold is 0.85-1 MPa.
6. The method for preparing the stemming sample according to claim 1, wherein the pressure of the forming process is 2-5 KN.
7. The method for preparing a stemming sample according to claim 1, further comprising heat-treating the stemming sample for performance testing.
8. The method for preparing a stemming sample according to claim 7, wherein the heat-treating the stemming sample comprises,
carrying out second freezing treatment on the stemming sample;
and carrying out heat treatment on the stemming sample subjected to the second freezing treatment.
9. The method for preparing a stemming specimen according to claim 8, wherein a time interval between the end of the demolding and the start of the second freezing is < 0.5h, and a time interval between the end of the second freezing treatment and the start of the heat treatment is < 0.5 h.
10. A stemming specimen characterized by being produced by the method for producing a stemming specimen according to any one of claims 1 to 9.
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