CN106006622B - The preparation method and graphite powder of high temperature gas cooled reactor nuclear fuel element natural graphite powder - Google Patents
The preparation method and graphite powder of high temperature gas cooled reactor nuclear fuel element natural graphite powder Download PDFInfo
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- CN106006622B CN106006622B CN201610420471.7A CN201610420471A CN106006622B CN 106006622 B CN106006622 B CN 106006622B CN 201610420471 A CN201610420471 A CN 201610420471A CN 106006622 B CN106006622 B CN 106006622B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 76
- 239000003758 nuclear fuel Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 229910021382 natural graphite Inorganic materials 0.000 title claims abstract description 23
- 238000000746 purification Methods 0.000 claims abstract description 41
- 239000002245 particle Substances 0.000 claims abstract description 24
- 238000007493 shaping process Methods 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 15
- 238000012545 processing Methods 0.000 claims abstract description 15
- 238000003801 milling Methods 0.000 claims abstract description 12
- 239000000843 powder Substances 0.000 claims description 69
- 229910002804 graphite Inorganic materials 0.000 claims description 23
- 239000010439 graphite Substances 0.000 claims description 23
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 15
- 239000000460 chlorine Substances 0.000 claims description 15
- 229910052801 chlorine Inorganic materials 0.000 claims description 15
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 14
- 229910052796 boron Inorganic materials 0.000 claims description 14
- 238000009826 distribution Methods 0.000 claims description 8
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000000446 fuel Substances 0.000 abstract description 7
- 238000012360 testing method Methods 0.000 abstract description 5
- 239000008187 granular material Substances 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 19
- 239000002956 ash Substances 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 13
- 235000003283 Pachira macrocarpa Nutrition 0.000 description 5
- 241001083492 Trapa Species 0.000 description 5
- 235000014364 Trapa natans Nutrition 0.000 description 5
- 239000011162 core material Substances 0.000 description 5
- 235000009165 saligot Nutrition 0.000 description 5
- 235000002918 Fraxinus excelsior Nutrition 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 2
- 229910052770 Uranium Inorganic materials 0.000 description 2
- 230000005856 abnormality Effects 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 239000005011 phenolic resin Substances 0.000 description 2
- 229920001568 phenolic resin Polymers 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 230000003044 adaptive effect Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000005087 graphitization Methods 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- -1 phenolic aldehyde Chemical class 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21C—NUCLEAR REACTORS
- G21C3/00—Reactor fuel elements and their assemblies; Selection of substances for use as reactor fuel elements
- G21C3/42—Selection of substances for use as reactor fuel
-
- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21C—NUCLEAR REACTORS
- G21C3/00—Reactor fuel elements and their assemblies; Selection of substances for use as reactor fuel elements
- G21C3/42—Selection of substances for use as reactor fuel
- G21C3/58—Solid reactor fuel Pellets made of fissile material
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
Landscapes
- Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- Plasma & Fusion (AREA)
- General Engineering & Computer Science (AREA)
- High Energy & Nuclear Physics (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses the preparation methods and graphite powder of high temperature gas cooled reactor nuclear fuel element natural graphite powder, wherein, preparation method is specially milling, shaping and classification processing and high temperature purification step, when the graphite powder being prepared by this method carries out nuclear fuel element engineer testing, since graphite powder is all circular or ellipse shape, and granule size is reasonably distributed, suppress the nuclear fuel element formed, inside will not form hole because of bridging phenomenon, the density of fuel particle is big, intensity is high, and stability is good, and the service life in reactor is long.
Description
Technical field
The present invention discloses the technical field for being related to graphite preparation more particularly to a kind of high temperature gas cooled reactor nuclear fuel element day
The preparation method and graphite powder of right graphite powder.
Background technology
High temperature gas cooled reactor is the forth generation nuclear reactor that Tsinghua University is built by independent research and success, is had completely certainly
Main intellectual property.High temperature gas cooled reactor is the mark heap-type of efficient, the safe nuclear reactor of forth generation, with " full ceramics " type coated particle
Fuel sphere is fuel element, using graphite as moderator and core structural material, using helium as cooling agent, is had good solid
There is security.
In the Shandong Huaneng Group Shidao Bay nuclear power station built, total installed capacity amount is 10,000,000 KW, wherein high temperature gas cooled reactor 4,000,000 in China
KW, this also indicates forth generation high temperature gas cooled reactor formally into commercialization.
High temperature gas cooled reactor nuclear fuel element production method is：Fuel uranium after carborundum coats (1mm or so) uniformly disperses
In graphite matrix, " graphite nodule " of diameter 60mm is made, is known as nuclear fuel element.
Graphite substrate material is mainly bonded by graphous graphite powder and natural graphite powder by phenolic aldehyde data, is fired in core
Expect in element, weight accounting is one of core material during nuclear fuel element is manufactured up to more than 90%.
Due to having very harsh condition, native graphite prepared by previous methods into any material in nuclear reactor
Powder can not meet the requirement of nuclear reactor, therefore, how research and develop a kind of natural graphite powder preparation side suitable for high temperature gas cooled reactor
Method becomes people's urgent problem to be solved.
The content of the invention
A kind of preparation side of high temperature gas cooled reactor nuclear fuel element natural graphite powder is provided it is an object of the invention to open
Method and graphite powder.
Technical solution provided by the invention, specifically, a kind of system of high temperature gas cooled reactor nuclear fuel element natural graphite powder
Preparation Method, which is characterized in that include the following steps：
1) it is milled：Crystalline flake graphite is put into Air Grinder and carries out broken milling, obtains powder, wherein, the powder
Average grain diameter is 30~40 μm；
2) shaping and classification processing：The powder is put into shaping device, removes burr water chestnut, shaping 12~15 minutes
Afterwards, by cyclone classified, the powder of removal grain size >=160 μm and grain size less than 5 μm obtains uniform particle sizes' powder, wherein, by weight
Gauge, the powder content that the size distribution of uniform particle sizes' powder is 160 μm of grain size ＜ is 100%, the powder that 32 μm of grain size ＜
Body content is 75~85%；
3) high temperature purification：Uniform particle sizes' powder is put into crucible, after sealed processing, is put into high temperature purification stove
Heating purification is carried out, when the furnace temperature of the high temperature purification stove reaches 2000 DEG C, chlorine is passed through into the high temperature purification stove, when
When the furnace temperature of the high temperature purification stove reaches 2450 DEG C, freon is passed through into the high temperature purification stove, when the high temperature purification
After the furnace temperature of stove reaches 2700 DEG C, when high-temperature process 24~36 is small, graphite powder finished product is made.
It is preferred that in the step 1) crystalline flake graphite volatile matter content ≯ 0.3%, real density >=2.24g/cm3, moisture content contains
＜ 0.3%, content of ashes ＜ 0.5%, fixed carbon content >=99% are measured, grain size is 100~200 μm.
Further preferably, the intake of chlorine is in the step 3)：30~35kg is passed through in epigranular powder per ton
Chlorine.
Further preferably, the intake of freon is in the step 3)：It is passed through 15 in epigranular powder per ton~
The freon of 20kg.
The present invention also provides a kind of high temperature gas cooled reactor nuclear fuel element natural graphite powders, which is characterized in that the stone
Ink powder is prepared according to any one above-mentioned preparation method, wherein, the average grain diameter of the graphite is 30~40 μm, grain size point
Cloth is less than 160 μm of contents 100% for grain size, grain size is less than 32 μm of contents 75~85%, and total boron equivalent ＜ 1ppm, water content≤
0.05%th, total ash ＜ 50ppm, specific surface are 5~6m2/ g, real density ≮ 2.24g/cm3, apparent density >=0.50g/cm3。
The preparation method of high temperature gas cooled reactor nuclear fuel element natural graphite powder provided by the invention, be milled successively,
Shaping and classification processing and high temperature purification step, wherein, it is milled, ground using Air Grinder being milled in step
Powder average grain diameter carried out shaping and classification processing step again for 30~40 μm, after the step that is milled, remove the burr of powder
Water chestnut makes the shape of powder all approach circular or ellipse, has then carried out cyclone classified, eliminates larger particles and micro-
Fine grained, so entire powder granularity are distributed more uniform, apparent density bigger, be filled in high temperature purification step chlorine and
On the one hand freon, the injection of two kinds of gas reduce the total ash of product, product total ash are made to be less than 50ppm, improves product
Corrosion resistance and radiation resistance performance on the other hand for absorbing boron element, make total boron equivalent be less than 1ppm, due to boron element
Neutron can be largely absorbed in nuclear reactor, reaction chain is caused to stop, therefore to reduce total boron equivalent in graphite, process is above-mentioned
Graphite powder after step process, when carrying out nuclear fuel element engineer testing using it, since graphite powder is all circular or oval
Shape, and granule size is reasonably distributed, the nuclear fuel element suppressed, and inside will not form hole because of bridging phenomenon,
The density of fuel particle is big, and intensity is high, and stability is good, and the service life in reactor is long.
Description of the drawings
Attached drawing herein is merged in specification and forms the part of this specification, shows the implementation for meeting the present invention
Example, and the principle for explaining the present invention together with specification.
It in order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
There is attached drawing needed in technology description to be briefly described, it should be apparent that, for those of ordinary skill in the art
Speech, without having to pay creative labor, can also be obtained according to these attached drawings other attached drawings.
Fig. 1 is the preparation that the present invention discloses a kind of high temperature gas cooled reactor nuclear fuel element natural graphite powder that embodiment provides
The scanning electron microscope (SEM) photograph of crystalline flake graphite before being milled in method in step 1)；
Fig. 2 is the preparation that the present invention discloses a kind of high temperature gas cooled reactor nuclear fuel element natural graphite powder that embodiment provides
In method in step 2) before shaping powder scanning electron microscope (SEM) photograph；
Fig. 3 is the preparation that the present invention discloses a kind of high temperature gas cooled reactor nuclear fuel element natural graphite powder that embodiment provides
In method in step 2) after shaping powder scanning electron microscope (SEM) photograph.
Specific embodiment
With reference to specific embodiment, the present invention is further described in detail, but is not limited to this hair
Bright protection domain.
When carrying out nuclear fuel element engineer testing to solve the natural graphite powder prepared using conventional method in the past, exist
It cracks in fuel element roasting process, compression strength is inadequate, and corrosion resistance is poor, and the problems such as wearing no resistance, the present embodiment provides
A kind of preparation method of high temperature gas cooled reactor nuclear fuel element natural graphite powder, specific preparation process are as follows：
1) it is milled：Crystalline flake graphite is put into Air Grinder and carries out broken milling, obtains powder, wherein, the powder
Average grain diameter is 30~40 μm；
2) shaping and classification processing：The powder is put into shaping device, removes burr water chestnut, shaping 12~15 minutes
Afterwards, by cyclone classified, the powder of removal grain size >=160 μm and grain size less than 5 μm obtains uniform particle sizes' powder, wherein, by weight
Gauge, the powder content that the size distribution of uniform particle sizes' powder is 160 μm of grain size ＜ is 100%, the powder that 32 μm of grain size ＜
Body content is 75~85%；
3) high temperature purification：Uniform particle sizes' powder is put into crucible, after sealed processing, is put into high temperature purification stove
Heating purification is carried out, when the furnace temperature of the high temperature purification stove reaches 2000 DEG C, chlorine is passed through into the high temperature purification stove, when
When the furnace temperature of the high temperature purification stove reaches 2450 DEG C, freon is passed through into the high temperature purification stove, when the high temperature purification
After the furnace temperature of stove reaches 2700 DEG C, when high-temperature process 24~36 is small, graphite powder finished product is made.
Wherein, in the milling process of step 1), broken milling is carried out using Air Grinder, the broken of powder can be improved
Degree reduces the average grain diameter of powder, reduces participating in for impurity, then matching step 2) in shaping and classification processing, by powder
Burr water chestnut in body removes, and makes powder rounded or oval, wherein, it is before the crystalline flake graphite and shaping before milling and whole
The scanning electron microscope (SEM) photograph of powder can be then cyclone classified by the powder progress after shaping again respectively referring to Fig. 1, Fig. 2 and Fig. 3 after shape,
Remove big grain size powder and small particle powder, improve the uniformity of entire powder granularity distribution, wherein grain size is less than 160 μm of powder
Body content is 100%, and powder content of the grain size less than 32 μm is 75~80%, increases apparent density, is carrying out nuclear fuel element
During engineer testing, hole will not be formed because of bridging phenomenon inside the nuclear fuel element suppressed, the density of fuel particle is big,
Intensity is high, and stability is good, and the service life in reactor is long.
And during the high temperature purification of step 3), chlorine is passed through when furnace temperature reaches 2000 DEG C, reaches 2450 DEG C in furnace temperature
When be passed through freon, wherein, freon is passed through main function in total boron equivalent in graphite powder is reduced.
It is excellent in the raw material selection of crystalline flake graphite in order to improve graphite powder end properties obtained in the present embodiment
Choosing, volatile matter content ≯ 0.3% of crystalline flake graphite, real density >=2.24g/cm3, water content ＜ 0.3%, content of ashes ＜
0.5%th, fixed carbon content >=99%, grain size are 100~200 μm.Wherein, real density is the guarantee of graphite powder quality, graphite powder
Real density limiting value be 2.265g/cm3, i.e. degree of graphitization 100%, this is can not be attainable, therefore in the present embodiment
Real density is selected to be more than or equal to 2.24 1 higher indexs；Ash content and fixed carbon, be in order to ensure later-period purification handle, because
Lower for ash content, fixed carbon is higher, and impurity content is fewer, and post-processing is easier；And granularity is milled mainly for facilitating, granularity
Too thin, too slightly, distribution is too wide, and later stage milling intractability can increase.
The intake of chlorine is in step 3)：The chlorine of 30~35kg is passed through in epigranular powder per ton；Freon
Intake is：The freon of 15~20kg is passed through in epigranular powder per ton.Wherein, the effect of chlorine and freon is：
1st, the total ash of product is reduced, product total ash is made to be less than 50ppm, improves the corrosion resistance of product and radiation resistance performance；
2nd, boron element is absorbed, total boron equivalent is made to be less than 1ppm, because boron element can largely absorb neutron in nuclear reactor, causes to react
Chain stops, therefore to reduce total boron equivalent in graphite.
Present embodiment provides a kind of high temperature gas cooled reactor nuclear fuel element natural graphite powder, which is according to upper
Any one preparation method is stated to be prepared, wherein, the average grain diameter of the graphite is 30~40 μm, and particle diameter distribution is small for grain size
It is less than 32 μm of contents 75~85% in 160 μm of contents 100%, grain size, it is total boron equivalent ＜ 1ppm, water content≤0.05%, total
Ash content ＜ 50ppm, specific surface are 5~6m2/ g, real density ≮ 2.24g/cm3, apparent density be >=0.50g/cm3。
In above example, if not special indicate, the content is weight content.
It is compared with specific embodiment and comparative example, the present invention is explained below closer.
Embodiment 1：
A kind of preparation method of high temperature gas cooled reactor nuclear fuel element natural graphite powder, specific preparation process are as follows：
1) it is milled：Crystalline flake graphite is put into Air Grinder and carries out broken milling, obtains powder, wherein, the powder
Average grain diameter is 30~40 μm, wherein, volatile matter content ≯ 0.3% of crystalline flake graphite, real density >=2.24g/cm3, moisture content contains
＜ 0.3%, content of ashes ＜ 0.5%, fixed carbon content >=99% are measured, grain size is 100~200 μm；
2) shaping and classification processing：Powder is put into shaping device, removes burr water chestnut, after shaping 12~15 minutes,
By cyclone classified, the powder of removal grain size >=160 μm and grain size less than 5 μm obtains uniform particle sizes' powder, wherein, by weight
Meter, the powder content that the size distribution of uniform particle sizes' powder is 160 μm of grain size ＜ is 100%, grain in uniform particle sizes' powder
The powder content that 32 μm of footpath ＜ is 75~85%；
3) high temperature purification：Uniform particle sizes' powder is put into graphite crucible, after sealed processing, is put into high temperature purification stove
Heating purification is carried out, when the furnace temperature of high temperature purification stove reaches 2000 DEG C, chlorine is passed through into high temperature purification stove, is passed through to be every
The chlorine of 30~35kg is passed through in ton epigranular powder, when the furnace temperature of high temperature purification stove reaches 2450 DEG C, to high temperature purification
Freon is passed through in stove, intake is that the freon of 15~20kg is passed through in epigranular powder per ton, when high temperature purification stove
Furnace temperature reach 2700 DEG C after, when high-temperature process 24~36 is small, graphite powder finished product is made.
Comparative example 1
This comparative example and embodiment 1 the difference is that：In the milling step of step 1), by the average grain diameter of powder
Control is at 25~29 μm, while diameter of particle is distributed as the powder content of 32 μm of grain size ＜ after shaping and classification processing in step 2)
For 90~95%, high temperature purification step is consistent with embodiment 1.
Comparative example 2
This comparative example difference from Example 1 is：The shaping in step 2) and classification processing, others mill are not carried out
Powder and high temperature purification step are consistent.
Comparative example 3
This comparative example and embodiment 1 the difference is that：High temperature purification step in step 3) in purification process not
Chlorine and freon are passed through, is directly warming up to 2700 DEG C or so, then cooling obtains product, others milling and shaping and divides
Grade processing step is consistent.
Embodiment 2
Graphite powder in embodiment 1, comparative example 1, comparative example 2 and comparative example 3 is subjected to performance detection, is specifically shown in Table 1.
Table 1：
| Sequence number | Analysis project | Implement 1 | Comparison 1 | Comparison 2 | Comparison 3 |
| 1 | Laser particle size D50 | 34μm | 28μm | 38μm | 36μm |
| 2 | Total boron equivalent | 0.4ppm | 0.5ppm | 0.4ppm | 78ppm |
| 3 | Moisture content | 0.05% | 0.04% | 0.06% | 0.05% |
| 4 | Total ash | 28ppm | 32ppm | 40ppm | 480ppm |
| 5 | Mechanical picker ＜ 160 | 100% | 100% | 99% | 100% |
| 6 | 32 μ of mechanical picker ＜ | 81% | 92% | 80% | 77% |
| 7 | Specific surface | 5.2m2/g | 5.8m2/g | 8.3m2/g | 5.3m2/g |
| 8 | Real density | 2.25g/cm3 | 2.24g/cm3 | 2.25g/cm3 | 2.23g/cm3 |
| 9 | Apparent density | 0.52g/cm3 | 0.49g/cm3 | 0.31g/cm3 | 0.51g/cm3 |
Wherein, font-weight part represents Indexes Abnormality in table 1, because reducing or changing in native graphite powder, preparation method thereof
After becoming a preparation process, changing occurs in the performance indicator of natural graphite powder.
Embodiment 3
Respectively using the natural graphite powder in embodiment 1, comparative example 1, comparative example 2, comparative example 3, according to nuclear fuel element
Production method, adding in identical graphous graphite powder and phenolic resin, (graphous graphite powder and phenolic resin can reach the pure grade of core
Not), by mediating, it is granulated, dry, milling and homogenization obtain producing the matrix powder of nuclear fuel pellet, be eventually adding uranium combustion
Expect that particle carries out ball press technique detection, finally the nuclear fuel element produced is detected, specific testing result is shown in Table 2.
Table 2
| Sequence number | Analysis project | Implement 1 | Comparison 1 | Comparison 2 | Comparison 3 |
| 1 | Density (g/cm3)≥1.70 | 1.75 | 1.70 | 1.64 | 1.73 |
| 2 | Thermal conductivity factor (1000 DEG C) (W/ (mk)) >=24 | 33 | 30 | 19 | 21 |
| 3 | Total ash (μ g/g)≤50 | 26 | 29 | 45 | 400 |
| 4 | Boron equivalent (μ g/g)≤1.3 | 0.5 | 0.6 | 0.5 | 68 |
| 5 | Lithium content (μ g/g)≤0.05 | 0.03 | 0.02 | 0.04 | 0.39 |
| 7 | Wear rate (mg/ (ball h))≤6.0 | 3.0 | 3.1 | 7.2 | 6.8 |
| 8 | Crushing strength (kN) (>=20) | 22 | 17 | 13 | 20 |
| 9 | Falling sphere intensity (4m, ball bed) (>=50 times) | 100 | 88 | 30 | 70 |
| 10 | Thermal expansion anisotropic≤1.3 | 1.15 | 1.28 | 1.70 | 1.50 |
Wherein, font-weight part represents Indexes Abnormality in table 2, because reducing or changing in native graphite powder, preparation method thereof
After becoming a preparation process, the nuclear fuel element performance indicator of production is caused to occur changing, do not meet high temperature gas-cooled core combustion
Expect the requirement of element.
Those skilled in the art will readily occur to the present invention its after considering specification and putting into practice invention disclosed herein
Its embodiment.This application is intended to cover the present invention any variations, uses, or adaptations, these modifications, purposes or
Person's adaptive change follows the general principle of the present invention and including undocumented common knowledge in the art of the invention
Or conventional techniques.Description and embodiments are considered only as illustratively, and true scope and spirit of the invention are by following
Claim is pointed out.
Claims (5)
1. a kind of preparation method of high temperature gas cooled reactor nuclear fuel element natural graphite powder, which is characterized in that include the following steps：
1) it is milled：Crystalline flake graphite is put into Air Grinder and carries out broken milling, obtains powder, wherein, the powder is averaged
Grain size is 30~40 μm；
2) shaping and classification processing：The powder is put into shaping device, removes burr corner angle, after shaping 12~15 minutes,
By cyclone classified, the powder of removal grain size >=160 μm and grain size less than 5 μm obtains uniform particle sizes' powder, wherein, by weight
Meter, the powder content that the size distribution of uniform particle sizes' powder is 160 μm of grain size ＜ is 100%, the powder that 32 μm of grain size ＜
Content is 75~85%；
3) high temperature purification：Uniform particle sizes' powder is put into crucible, after sealed processing, is put into high temperature purification stove and carries out
Heating purification, when the furnace temperature of the high temperature purification stove reaches 2000 DEG C, is passed through chlorine, when described into the high temperature purification stove
When the furnace temperature of high temperature purification stove reaches 2450 DEG C, freon is passed through into the high temperature purification stove, when the high temperature purification stove
After furnace temperature reaches 2700 DEG C, when high-temperature process 24~36 is small, graphite powder finished product is made.
2. the preparation method of high temperature gas cooled reactor nuclear fuel element natural graphite powder according to claim 1, which is characterized in that
Volatile matter content ≯ 0.3% of crystalline flake graphite in the step 1), real density >=2.24g/cm3, moisture ＜ 0.3%, ash
Divide content ＜ 0.5%, fixed carbon content >=99%, grain size is 100~200 μm.
3. the preparation method of high temperature gas cooled reactor nuclear fuel element natural graphite powder according to claim 1, which is characterized in that
The intake of chlorine is in the step 3)：The chlorine of 30~35kg is passed through in epigranular powder per ton.
4. the preparation method of high temperature gas cooled reactor nuclear fuel element natural graphite powder according to claim 1, which is characterized in that
The intake of freon is in the step 3)：The freon of 15~20kg is passed through in epigranular powder per ton.
5. a kind of high temperature gas cooled reactor nuclear fuel element natural graphite powder, which is characterized in that the graphite powder is according to aforesaid right
It is required that any one preparation method is prepared in 1~4, wherein, the average grain diameter of the graphite is 30~40 μm, particle diameter distribution
For grain size be less than 160 μm of contents 100%, grain size be less than 32 μm of contents 75~85%, total boron equivalent ＜ 1ppm, moisture≤
0.05%th, total ash ＜ 50ppm, specific surface are 5~6m2/ g, real density ≮ 2.24g/cm3, apparent density >=0.50g/cm3。
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| CN201610420471.7A CN106006622B (en) | 2016-06-13 | 2016-06-13 | The preparation method and graphite powder of high temperature gas cooled reactor nuclear fuel element natural graphite powder |
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| CN201610420471.7A CN106006622B (en) | 2016-06-13 | 2016-06-13 | The preparation method and graphite powder of high temperature gas cooled reactor nuclear fuel element natural graphite powder |
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| CN106006622B true CN106006622B (en) | 2018-05-25 |
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| CN107935595A (en) * | 2017-11-22 | 2018-04-20 | 永安市鼎丰碳素科技有限公司 | A kind of preparation method of Htgr Graphite brick |
| CN109835893A (en) * | 2017-11-25 | 2019-06-04 | 甘肃金土新能源材料科技有限公司 | The reprocessing of byproduct graphite powder in a kind of production of silicon carbide utilizes method |
| CN113511896A (en) * | 2020-04-09 | 2021-10-19 | 清华大学 | Nuclear fuel matrix graphite powder, nuclear fuel graphite matrix material and preparation method |
| CN113800511B (en) * | 2020-06-11 | 2023-12-29 | 清华大学 | Natural graphite powder for nuclear reactor fuel element and preparation method thereof |
| CN112201377B (en) * | 2020-09-29 | 2022-07-19 | 内蒙古金彩矿业有限公司 | Shaping system and shaping method of natural graphite powder for high-temperature gas-cooled reactor nuclear fuel element |
| CN113307265A (en) * | 2021-06-21 | 2021-08-27 | 永安市鼎丰碳素科技有限公司 | High-performance microcrystalline graphite powder material for high-temperature gas cooled reactor and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102126721A (en) * | 2011-04-27 | 2011-07-20 | 深圳市贝特瑞新能源材料股份有限公司 | Purification and graphitization method of graphite material |
| CN104401982A (en) * | 2014-11-13 | 2015-03-11 | 东莞市翔丰华电池材料有限公司 | Nuclear graphite material preparation method |
| CN105347337A (en) * | 2015-12-07 | 2016-02-24 | 湖南顶立科技有限公司 | Method for high-temperature purification of natural graphite by utilizing freon |
-
2016
- 2016-06-13 CN CN201610420471.7A patent/CN106006622B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102126721A (en) * | 2011-04-27 | 2011-07-20 | 深圳市贝特瑞新能源材料股份有限公司 | Purification and graphitization method of graphite material |
| CN104401982A (en) * | 2014-11-13 | 2015-03-11 | 东莞市翔丰华电池材料有限公司 | Nuclear graphite material preparation method |
| CN105347337A (en) * | 2015-12-07 | 2016-02-24 | 湖南顶立科技有限公司 | Method for high-temperature purification of natural graphite by utilizing freon |
Non-Patent Citations (1)
| Title |
|---|
| 石墨在高纯氦中的高温氧化研究;白新德 等;《原子能科学技术》;19970131;第31卷(第1期);84页 1.1 国产石墨的生产工艺 部分 * |
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