CN108680412A - A kind of sample preparation methods and test method for calcined coke coefficient of thermal expansion - Google Patents
A kind of sample preparation methods and test method for calcined coke coefficient of thermal expansion Download PDFInfo
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- CN108680412A CN108680412A CN201810562186.8A CN201810562186A CN108680412A CN 108680412 A CN108680412 A CN 108680412A CN 201810562186 A CN201810562186 A CN 201810562186A CN 108680412 A CN108680412 A CN 108680412A
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- thermal expansion
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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
- G01N1/286—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
Abstract
The present invention provides a kind of sample preparation methods and test method for calcined coke coefficient of thermal expansion, it includes sampling, it is broken, kneading, die mould, roast pre-treatment, roasting, graphitization, processed sample and thermal expansion measurement, it carries out being mixed with out graphited sample according to the ratio by using calcined coke and pitch, and sample is processed into rodlike graphite sample, polishing processing is carried out to the surface depth of parallelism and roughness of graphite sample, when graphite sample being made to carry out MEASURING THE THERMAL EXPANSION COEFFICIENT in thermal dilatometer, the thermal expansion amount measurement of graphite sample becomes more precisely, improve the repeatability and precision for measuring coefficient of thermal expansion, solves the problems, such as graphite calcined coke coefficient of thermal expansion preparation method of sample backward technology.
Description
Technical field
The present invention relates to the determination techniques fields of calcined coke coefficient of thermal expansion, specially a kind of to thermally expand system for calcined coke
Several sample preparation methods and test method.
Background technology
The phenomenon that thermal expansion, i.e., condensed state matter volume is varied with temperature and changed, be the basic ermal physics of substance
One of property, and in producing usually degree is varied with temperature to characterize scantling with coefficient of thermal expansion.Coefficient of thermal expansion is usual
It is divided into the coefficient of volume expansion and linear expansion coefficient.Since the measurement of body expansion expands difficulty than line in practice, so general
Measure the linear expansion coefficient of solid material.
Test calcined coke coefficient of thermal expansion at present is mainly mixed with pitch by coke and generates stone by graphitizing process
Ink, the coefficient of thermal expansion of the coefficient of thermal expansion indirect reaction coke powder of re-test graphite.
The existing preparation method (GB/T3074.5-1982) for measuring graphite electrode petroleum coke coefficient of thermal expansion sample has been made
It is useless, temporarily without alternate standard, mainly comprise the following steps：1. 4. die mould 5. of broken 3. kneading of calcining 2. roasting, 6. graphitization.Thermally expand system
Number test Main Basiss graphite electrode coefficient of thermal expansion (CTE) assay method (GB/T 3074.4-2016).
But existing method has the following problems：
1. mainly for the preparation method that graphite electrode petroleum coke coefficient of thermal expansion carries out, application field is narrow, cannot be satisfied
The demand of more graphite fields STRENGTH ON COKE；
2. preparing and the corresponding parameter of testing procedure needing to be optimized and revised.
Invention content
In view of the above problems, the present invention provides a kind of sample preparation methods for calcined coke coefficient of thermal expansion, lead to
It crosses and carries out being mixed with out graphited sample according to the ratio using calcined coke and pitch, and sample is processed into rodlike graphite sample
Product carry out polishing processing to the surface depth of parallelism and roughness of graphite sample, so that graphite sample is carried out heat in thermal dilatometer swollen
When swollen coefficient determination, the repeatability and precision for measuring coefficient of thermal expansion are improved, solves graphite calcined coke coefficient of thermal expansion sample
Preparation method backward technology problem expands the range tested graphite calcined coke coefficient of thermal expansion.
To achieve the above object, the present invention provides the following technical solutions：
A kind of sample preparation methods for calcined coke coefficient of thermal expansion include the following steps：
Step 1, sampling respectively sample point sampling from calcined coke, and repetition extraction sample reaches 0.5kg up to sample quality,
And half is used for sample preparation in the sample extracted, half is for sealing up for safekeeping；
Step 2 is crushed, and by 6.35mm sieves after being dried and be crushed for the sample of sample preparation, passes through sieve
Sample grind into powder sample；
Step 3, kneading stir after mixing in proportion powder sample and coal tar asphalt after being heated to 150 DEG C
Thickener is uniformly pinched into again, and the kneading time is 1.5h；
Paste extruded after kneading is gone out at least three a diameter of 12mm~20mm by step 4, die mould, and a length of 100mm~
The column type sample of 150mm；
Step 5 roasts pre-treatment, in the sand of one thickness 50mm of graphite crucible middle berth, is put after column type sample is marked
Enter in crucible, each sample interval is consistent from, sample at a distance from graphite crucible wall, populated with sand；
Step 6, roasting, graphite crucible is put into 100 DEG C of heating furnace, is heated to 850~900 DEG C, heat preservation 1~3 is small
When, furnace body cooling is less than 300 DEG C, can open wide fire door and be cooled to room temperature, and takes out sample, with sand paper polishing clean surface；
Step 7, graphitization, sample is put into atmosphere furnace and is heated, and is passed through argon gas as protection gas, heating speed to 2700
DEG C, and keep the temperature 30 minutes rear furnace bodies and be cooled to 300 DEG C hereinafter, can blow-on cooling taking-up sample；And
Sample after graphitization is processed into a diameter of 6 ± 0.05mm by step 8, processed sample, and length is 25.5 ±
Through machine-shaping of polishing for test sample after the rodlike graphite sample of 0.05mm.
In the step 1, the quantity of sample point is 3~5 on calcined coke, and repeats to extract 6~10 times.
In the step 2, the drying temperature of sample preparation sample is 110 DEG C, and 2 hours dry, the powder sample after grinding can lead to
That crosses 40 mesh screens reaches at least 95%, passes through at least the 40%~60% of 200 mesh screens.
In the step 3, the mixed proportion of powder sample and coal tar asphalt is 6.5~7.5:3.5~2.5.
In the step 4, the molding pressure of paste extruded after kneading is 60kg/cm2, and its squeeze out first
Column type sample abandons.
In the step 5, column type sample is put into crucible, each sample interval from, sample and graphite crucible wall away from
From both preferably 15mm, and when column type sample is placed in multilayer, the layer of sand of 15mm is set between adjacent two layers column type sample
Interval.
In the step 6, the heating rate that heating furnace is warming up to 850~900 DEG C from 100 DEG C is 90~120 DEG C/h.
In the step 7, the rate for being passed through argon gas is 10L/min, and the heating rate that heating furnace is warming up to 2700 DEG C is 15
℃/min。
In the step 8, the surface depth of parallelism of test sample is 0.015 after polishing, roughness 0.8.
The present invention is compared to the preparation method GB/T3074.5-1982 for measuring graphite electrode petroleum coke coefficient of thermal expansion sample
Has following advantages：
1) in sampling, by the way of multiple spot repeatedly sample, sampling more science, average is suitable for all the present invention
The calcined coke of graphite being produced, and the sample half extracted is used for sample preparation, half is sealed up for safekeeping, and the sample sealed up for safekeeping can be used as and stay shelves,
More rationally, above not recorded in GB3074.5-1982, and GB3074.5-1982 is mainly for graphite electrode
Prepared by the sample of petroleum coke, field is narrow, is not also sampled；
2) on broken, after the present invention is using being crushed, after being sieved with 6.35mm sieves, milling ensures that sample is sieved by 40 mesh
The throughput of net at least 95% is remembered by the sample throughput at least 40%~60% of 200 mesh screens with GB3074.5-1982
What is carried less than 0.075mm be 40 ± 2%, 0.15-0.5mm is 25 ± 5%, and comparing, it is more uniform to be sieved, and granularity is thinner；
3) on die mould, the present invention abandons first column type sample squeezing out, make to avoid the sample of pollution into
It has gone subsequent MEASURING THE THERMAL EXPANSION COEFFICIENT, interference, this point that measurement result generates has not been remembered in GB/T3074.5-1982
It carries；
4) in roasting, the present invention has thickeied the thickness of sand, keeps heat insulation effect more excellent, and calcination temperature is 850-900
DEG C, roasting time is 1-3 hours, and calcination temperature and time, the roasting time for comparing GB3074.5-1982 records are shorter；
5) in graphitization, the present invention is warming up to 2700 DEG C with the rate of 15 DEG C/min, is recorded compared with GB/T3074.5-1982
Interim heating be graphitized, constant heating, sample is heated evenly, and graphitization effect is more preferable；
6) present invention increases processing to test sample outer shape, ensure that the depth of parallelism outside test sample with it is coarse
Degree, when test sample being made to carry out coefficient of thermal expansion test in thermal dilatometer, the more conducively change of instrument detection test sample shape
Change amount, improves the repeatability and precision for measuring coefficient of thermal expansion, which does not record in GB/T3074.5-1982.
In view of the above problems, the present invention provides a kind of test method for calcined coke coefficient of thermal expansion, it is more existing
MEASURING THE THERMAL EXPANSION COEFFICIENT method GB/T 3074.4-2016, the present invention improve the range of test temperature, solve tradition and thermally expand
The small technical problem of coefficient determination method temperature range.
Test sample is put into thermal dilatometer and thermally expands by a kind of test method for calcined coke coefficient of thermal expansion
Coefficient is tested, which is adjusted to 120~150ml/min, and heating rate is adjusted to 2K/min~3K/min,
In room temperature section at least constant temperature 2 hours or more, start heating test.
The present invention has following excellent compared to graphite electrode coefficient of thermal expansion (CTE) assay method (GB/T 3074.4-2016)
Point：
The test temperature of coefficient of thermal expansion of the present invention can reach 1500 DEG C, and the test temperature of GB/T 3074.4-2016 is only
600 DEG C can be reached, be far below 1500 DEG C, far away from the precision for the coefficient of thermal expansion that the present invention tests out.
On the whole, the method for the present invention clear thinking has been eliminated as much as having an impact test result many external
Factor improves the precision of test result, is particularly suitable for the measurement of calcined coke coefficient of thermal expansion.
Description of the drawings
Fig. 1 is that the present invention is a kind of for the sample preparation methods of calcined coke coefficient of thermal expansion and the technological process of test method
Schematic diagram；
Fig. 2 is the sample drawing of calcined coke coefficient of thermal expansion of the present invention；
Fig. 3 is MEASURING THE THERMAL EXPANSION COEFFICIENT schematic diagram of the present invention；
Fig. 4 is typical coefficient of thermal expansion test curve figure.
Specific implementation mode
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation describes, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
In the description of the present invention, it is to be understood that, term "center", " longitudinal direction ", " transverse direction ", " length ", " width ",
" thickness ", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outside", " up time
The orientation or positional relationship of the instructions such as needle ", " counterclockwise " is to be based on the orientation or positional relationship shown in the drawings, and is merely for convenience of
The description present invention and simplified description, do not indicate or imply the indicated equipment or element must have a particular orientation, with spy
Fixed azimuth configuration and operation, therefore be not considered as limiting the invention.
In addition, term " first ", " second " are used for description purposes only, it is not understood to indicate or imply relative importance
Or implicitly indicate the quantity of indicated technical characteristic.Define " first " as a result, the feature of " second " can be expressed or
Implicitly include one or more this feature.In the description of the present invention, the meaning of " plurality " is two or more,
Unless otherwise specifically defined.
Embodiment 1：
As shown in Figure 1, a kind of sample preparation methods for calcined coke coefficient of thermal expansion, include the following steps：
Step 1, sampling respectively sample point sampling from calcined coke, and repetition extraction sample reaches 0.5kg up to sample quality,
And half is used for sample preparation in the sample extracted, half is for sealing up for safekeeping；
Step 2 is crushed, and by 6.35mm sieves after being dried and be crushed for the sample of sample preparation, is ground into later
Powder sample；
After mixing in proportion powder sample and coal tar asphalt, binder kneading is added into paste in step 3, kneading
Material；
Paste extruded after kneading is gone out at least three a diameter of 12mm~20mm by step 4, die mould, and a length of 100mm~
The column type sample of 150mm；
Step 5 roasts pre-treatment, in the sand of one thickness 50mm of graphite crucible middle berth, is put after column type sample is marked
Enter in crucible, each sample interval is consistent from, sample at a distance from graphite crucible wall, populated with sand；
Step 6, roasting, graphite crucible is put into 100 DEG C of heating furnace, is heated to 850~900 DEG C, heat preservation 1~3 is small
When, furnace body cooling is less than 300 DEG C, can open wide fire door and be cooled to room temperature, and takes out sample, with sand paper polishing clean surface；
Step 7, graphitization, sample is put into atmosphere furnace and is heated, and is passed through argon gas as protection gas, heating speed to 2700
DEG C, and keep the temperature warm 30 minutes rear furnace bodies and be cooled to 300 DEG C hereinafter, can blow-on cooling taking-up sample；And
Sample after graphitization is processed into a diameter of 6 ± 0.05mm by step 8, processed sample, and length is 25.5 ±
The test sample of 0.05mm.
Wherein, in the step 1, the quantity of sample point is 3~5 on calcined coke, and repeats to extract 6~10 times, is repeated
Extraction can make the calcined coke of extraction more uniform, in this way, when carrying out the measurement of coefficient of thermal expansion to calcined coke, make measurement
As a result more precisely, reliably.
In the step 2, the drying temperature of sample preparation sample is 110 DEG C, and 2 hours dry, the powder sample after milling passes through
At least the 95% of 40 mesh screens passes through at least the 40%~60% of 200 mesh screens.
After screening, the granularity of powder sample is more uniform, is graphitized to form final test sample in powder sample
When, due to epigranular, when carrying out coefficient of thermal expansion test, dilatancy can show more uniform test sample, Bu Huifa
The case where raw unilateral excessively expansion, it is conducive to the detection of coefficient of thermal expansion.
In the step 3, the mixed proportion of powder sample and coal tar asphalt is 6.5~7.5:3.5~2.5, wherein coal
Tar asphalt plays the role of binder.
The softening point of coal tar asphalt is 110 DEG C, is screened by 10 mesh screens, after screening and coal tar pitch cokes
Powder is uniformly mixed by proper proportion, while forming thickener being heated in 150 DEG C of pots be stirred 1.5 hours with blender, is worth
It is only to be higher than 110 DEG C, coal tar asphalt because the softening point of coal tar asphalt is 110 DEG C it is to be noted that being heated to 150 DEG C
It can be just in the state flowed freely, could be uniformly mixed with powder sample, and in the present embodiment be preferably 150 DEG C of stirring temperature
Degree is to reduce the loss of the energy to the greatest extent in the case where ensureing coal tar asphalt mobility status, while ensureing the effect of stirring kneading again.
In the step 4, the molding pressure of paste extruded after kneading is 60kg/cm2, and its squeeze out first
Column type sample abandons.
In forming process using extruder carry out extrusion forming, abandon first column type sample squeezed out, be because
Column type sample may mix with last residual thickener in extrusion process, lead to first cylinder style squeezed out
Product are polluted by residue, and for contaminated column type sample using thermal expansion measurement, the coefficient of thermal expansion measured can have deviation,
Cause the result measured inaccurate.
In the step 5, column type sample is put into crucible, each sample interval from, sample and graphite crucible wall away from
From both preferably 15mm, and when column type sample is placed in multilayer, the layer of sand of 15mm is set between adjacent two layers column type sample
Interval.
Be laid with sand one be in order to give sample be arranged insulating layer, make sample when being roasted, can effectively be kept the temperature,
Second is that due to being added to coal tar asphalt in column type sample as adhesive, directly by column type sample place in crucible,
Column type sample can be made to generate with crucible to be adhered.
In the step 6, the heating rate that heating furnace is warming up to 850~900 DEG C from 100 DEG C is 90~120 DEG C/h, by
In roasting sample used for MEASURING THE THERMAL EXPANSION COEFFICIENT, there is no need to the preparations of image-stone ink to consider shrinkage rates like that, need to only protect
In the case of demonstrate,proving roasting effect, the time of roasting is shortened as far as possible, to improve efficiency.
In the step 7, the rate for being passed through argon gas is 10L/min, and the heating rate that heating furnace is warming up to 2700 DEG C is 15
DEG C/min, it uses and is uniformly heated with the constant rate heating sample of 15 DEG C/min, graphitization effect can be more preferable.
Such as Fig. 2, in the step 8, the surface depth of parallelism of test sample is 0.015, roughness 0.8.
The depth of parallelism and the roughness for limiting test sample surface be in order to ensure sample when carrying out MEASURING THE THERMAL EXPANSION COEFFICIENT,
The volume energy of sample uniformly expands, the swell increment for facilitating thermal dilatometer detection outlet to occur, while swell increment is quick
Detection, the present embodiment allow meet the needs of more graphite field STRENGTH ON COKE MEASURING THE THERMAL EXPANSION COEFFICIENTs.
Embodiment 2：
The test sample prepared according to embodiment 1 is put into heat by a kind of test method for calcined coke coefficient of thermal expansion
Coefficient of thermal expansion test is carried out in dilatometer, which is adjusted to 120~150ml/min, heating rate
It is adjusted to 2K/min~3K/min, in room temperature section at least constant temperature 2 hours or more, starts heating test.
Thermal dilatometer heating furnace is opened, test sample is put into the quartz ampoule in stove, sample both ends quartz spacer pad
Good (operating procedure of unrelated gasket if equipment does not have quartz spacer), sample, quartz dilatometer, quartz spacer will be in one
On axis, temperature measuring equipment thermometric end is then close to side surface at sample 1/2 and is placed, bell is closed, records displacement measurement
Device initial reading or by device back to zero.
As shown in figure 3,1 indicates displacement measuring device, 2 indicate furnace wall, and 3 indicate calandria, and 4 representing samples, 5 indicate quartz
Reference substance, 6 indicate quartz mandril, and 7 indicate pedestals, and the principle of MEASURING THE THERMAL EXPANSION COEFFICIENT is that sample and quartzy object of reference are mounted on together
On one pedestal, the other end of sample is in contact with mandril, and when stove heats, sample, mandril, object of reference are heated swollen simultaneously
It is swollen, since mandril and object of reference are all the quartzy standard substances of same material, although they out of stove to outside stove, residing warm area
Difference, but they are identical in the temperature of the same horizontal position, and the swell increment of the two is cancelled out each other, and with sample with length
Region, since material difference cannot be offset, the reading of displacement device is sample and the relative expansion with length object of reference
Amount, so the true swell increment of sample is swell increment of the reading on displacement measuring device plus object of reference.
The calculating formula of coefficient of thermal expansion is：
A=△ L/ △ TL0+ a quartz
a：Sample room temperature~1500 DEG C coefficient of thermal expansion (DEG C-1)；
L0：Length (mm) of the sample in room temperature；
△L：Sample is in 1500 DEG C of swell incremenies for being (mm)；
△T：The temperature difference (DEG C) of room temperature~1500 DEG C；
A quartz：Quartz in the temperature of room temperature~1500 DEG C mean thermal expansion coefficients (DEG C-1)。
The Accurate Determining of thermal expansion amount is vital to graphite material MEASURING THE THERMAL EXPANSION COEFFICIENT known to as a result, therefore,
So that test sample is formed the shape of ad hoc rules by processing of polishing, and require the depth of parallelism and roughness on its surface, and then comes
The uniformity of swell increment of test sample during thermal expansion measurement is promoted, and conscientiously necessary.
As shown in figure 4, for the typical coefficient of thermal expansion test curve figure that the present embodiment is tested out in room temperature~1500 DEG C, by
The figure is it is found that the second trial temperature of the present embodiment, which reaches 1500 DEG C, can be reached really and in the thermal expansion of real material
It is used in coefficient determination.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement etc., should all be included in the protection scope of the present invention made by within refreshing and principle.
Claims (10)
1. a kind of sample preparation methods for calcined coke coefficient of thermal expansion, which is characterized in that include the following steps：
Step 1, sampling respectively sample point sampling from calcined coke, repeat to extract sample until sample quality reaches 0.5kg, and takes out
Half is used for sample preparation in the sample taken, and half is for sealing up for safekeeping；
Step 2 is crushed, and by 6.35mm sieves after being dried and be crushed for the sample of sample preparation, passes through the sample of sieve
Grind into powder sample；
Step 3, kneading stir evenly after mixing in proportion powder sample and coal tar asphalt after being heated to 150 DEG C
Thickener is pinched into again, and the kneading time is 1.5h；
Paste extruded after kneading is gone out at least three a diameter of 12mm~20mm, a length of 100mm~150mm by step 4, die mould
Column type sample；
Step 5 roasts pre-treatment, and in the sand of one thickness 50mm of graphite crucible middle berth, earthenware is put into after column type sample is marked
In crucible, each sample interval is consistent from, sample at a distance from graphite crucible wall, populated with sand；
Step 6, roasting, graphite crucible is put into 100 DEG C of heating furnace, is heated to 850~900 DEG C, keeps the temperature 1~3 hour,
Furnace body cooling is less than 300 DEG C, can open wide fire door and be cooled to room temperature, and takes out sample, with sand paper polishing clean surface；
Step 7, graphitization, sample is put into atmosphere furnace and is heated, and is passed through argon gas as protection gas, and heating is fast to 2700 DEG C, and
30 minutes rear furnace bodies of heat preservation are cooled to 300 DEG C hereinafter, can blow-on cooling taking-up sample；And
Sample after graphitization is processed into a diameter of 6 ± 0.05mm by step 8, processed sample, and length is 25.5 ± 0.05mm
Rodlike graphite sample after through polish machine-shaping be test sample.
2. a kind of sample preparation methods for calcined coke coefficient of thermal expansion according to claim 1, which is characterized in that institute
It states in step 1, the quantity of sample point is 3~5 on calcined coke, and repeats to extract 6~10 times.
3. a kind of sample preparation methods for calcined coke coefficient of thermal expansion according to claim 1, which is characterized in that institute
It states in step 2, the drying temperature of sample preparation sample is 110 DEG C, and 2 hours dry, the powder sample after grinding can pass through 40 mesh screens
Reach at least 95%, pass through at least the 40%~60% of 200 mesh screens.
4. a kind of sample preparation methods for calcined coke coefficient of thermal expansion according to claim 1, which is characterized in that institute
It states in step 3, the mixed proportion of powder sample and coal tar asphalt is 6.5~7.5：3.5~2.5.
5. a kind of sample preparation methods for calcined coke coefficient of thermal expansion according to claim 1, which is characterized in that institute
It states in step 4, the molding pressure of the paste extruded after kneading is 60kg/cm2, and its first column type sample squeezing out
It abandons.
6. a kind of sample preparation methods for calcined coke coefficient of thermal expansion according to claim 1, which is characterized in that institute
It states in step 5, column type sample is put into crucible, and each sample interval is at a distance from graphite crucible wall from, sample
15mm, and when column type sample is placed in multilayer, the layer of sand interval of 15mm is set between adjacent two layers column type sample.
7. a kind of sample preparation methods for calcined coke coefficient of thermal expansion according to claim 1, which is characterized in that institute
It states in step 6, the heating rate that heating furnace is warming up to 850~900 DEG C from 100 DEG C is 90~120 DEG C/h.
8. a kind of sample preparation methods for calcined coke coefficient of thermal expansion according to claim 1, which is characterized in that institute
It states in step 7, the rate for being passed through argon gas is 10L/min, and the heating rate that heating furnace is warming up to 2700 DEG C is 15 DEG C/min.
9. a kind of sample preparation methods for calcined coke coefficient of thermal expansion according to claim 1, which is characterized in that institute
It states in step 8, the surface depth of parallelism of the test sample after polishing is 0.015, roughness 0.8.
10. a kind of test method for calcined coke coefficient of thermal expansion, which is characterized in that by what is prepared according to claim 1-9
Test sample is put into thermal dilatometer progress coefficient of thermal expansion test, and which is adjusted to 120~
150ml/min, heating rate are adjusted to 2K/min~3K/min, in room temperature section at least constant temperature 2 hours or more, start heating test.
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| CN114112602A (en) * | 2021-12-20 | 2022-03-01 | 昆明理工大学 | Pretreatment method for detecting small amount of fragile sample for ELEMENT GD glow discharge mass spectrum detection |
| CN114112602B (en) * | 2021-12-20 | 2023-12-22 | 昆明理工大学 | Pre-detection treatment method for small amount of fragile sample for ELEMENT GD glow discharge mass spectrum detection |
| CN114460128A (en) * | 2022-01-26 | 2022-05-10 | 鞍山中特新材料科技有限公司 | Method for rapidly testing thermal expansion coefficient of needle coke |
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