CN109396965A - Surface Multi-scale model tungsten material and preparation method thereof - Google Patents

Surface Multi-scale model tungsten material and preparation method thereof Download PDF

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CN109396965A
CN109396965A CN201811339712.0A CN201811339712A CN109396965A CN 109396965 A CN109396965 A CN 109396965A CN 201811339712 A CN201811339712 A CN 201811339712A CN 109396965 A CN109396965 A CN 109396965A
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layer
scale model
tungsten
micron
preparation
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CN109396965B (en
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蒋燕
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Panzhihua University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B24GRINDING; POLISHING
    • B24BMACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B1/00Processes of grinding or polishing; Use of auxiliary equipment in connection with such processes
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C27/00Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
    • C22C27/04Alloys based on tungsten or molybdenum

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Powder Metallurgy (AREA)

Abstract

The present invention relates to the preparation methods of a kind of surface Multi-scale model tungsten material and its material, belong to field of metal surface treatment technology.The surface texture of surface Multi-scale model tungsten material of the invention is to being provided with gradient layer between matrix, the crystallite dimension of the gradient layer changes in gradient, gradient layer from the surface texture to matrix is followed successively by nanometer layer, sub-micron layer, micron layer, the nanometer layer, sub-micron layer, micron layer crystallite dimension be respectively nanoscale, submicron order and micron order.The multiple dimensioned layer tungsten material in surface of the invention, phenomena such as being well combined, do not have sharp interface, micro-crack, delamination do not occur between each scale layer.The present invention is simple, quickly, and is suitable for bulk sample and prepares.

Description

Surface Multi-scale model tungsten material and preparation method thereof
Technical field
The present invention relates to the preparation methods of a kind of surface Multi-scale model tungsten material and its material, belong at metal surface Manage technical field.
Background technique
Service Environment of the fusion reactor towards plasma source components is extremely harsh, it is desirable that material therein can be for a long time Damage effect caused by high heat load and strong irradiation is resisted, to guarantee the long-term stable operation of fusion reactor.Tungsten is that fusing point is highest Metal material, and there is high heat conductance, low sputtering raste, it is considered to be it is most potential to can be applied to towards plasma source components One of material.But the maximum deficiency of tungsten is that have apparent brittleness at room temperature (even rolling state business level tungsten, ductile-brittle transiton temperature Spend DBTT between 200 DEG C -300 DEG C), radiation embrittlement, thermic load cracking the defects of, significantly limit it as the first wall material The practical application of material.
In order to improve tungsten above shortcomings, scholars have carried out with tungsten alloy, tungsten/tungsten alloy plastic deformation processing Tungsten toughness is improved with the approach based on tungsten Surface Nanocrystalline.The principle of these methods is all to induce the crystal grain refinement of tungsten strong Change.Alloying is generally used in combination with plastic deformation, main by adding second phase nano particle such as oxide carbide etc. more It dissipates tungsten basal body and prepares fine grain tungsten alloy, and combine subsequent rolling process, achieve the effect that alloy densification, refinement and strengthen.Liu Auspicious, Xie Zhuoming etc. disclosed in patent CN104388789B " a kind of nanostructure tungsten-carbonization zircaloy and preparation method thereof " And Xie Zhuoming etc. is in paper " Extraordinary high ductility/strength of the interface Designed bulk W-ZrC alloy plate at relatively low temperature ", " Scientific Reports " addition nano-zirconium carbide is reported in 5 (2015) 16014 refines tungsten basal body crystal grain adequately, it obtains a large amount of Crystal boundary/phase boundary, to make alloy that there is more excellent obdurability and thermal-shock resistance.But shortcoming is to sacrifice the heat of pure tungsten Conductance, the phase boundary in W-ZrC alloy also enhance the scattering process to electronics while increasing mechanical property, thermal conductivity is compared Pure tungsten is decreased obviously.Liu Rui etc. is improved mentioned component, and a kind of " potassium carbonization is disclosed in patent CN108149103A Zirconium codope tungsten alloy and preparation method thereof " further improves the power of tungsten by the collective effect of nanometer potassium bubble and zirconium carbide Performance is learned, thermal conductivity is not characterized.But it can speculate that presence will make alloy thermal conductivity into one to potassium bubble jointly with ceramic nanoparticles Step decline.
High thermal conductivity is just conducive to remove the heat being deposited on the first wall in time, can be while improving mechanical property Tungsten is not lost to have great importance from the thermal conductivity of height yet.Under most of Service Environments, construction instability starts from surface more, For this purpose, the research of pure tungsten surface self-nanocrystallinzation receives the concern of researchers, because it has the advantage that 1) nano surface tungsten is brilliant Grain can reduce the ductile-brittle transition temperature towards plasma dignity tungsten, improve heat shock resistance and anti-radiation performance;2) surface Zi Na Riceization can reduce the difficulty of blocky tungsten processing;3) tungsten surface self-nanocrystallinzation remains the high heat conductance of tungsten.Although material surface It is more from the method for nanosizing, such as surface mechanical treatment process and unequilibrium thermodynamics method, but tungsten metal surface is directed to from nanometer Change also in research and trial, because tungsten is the highest metal of fusing point and has big brittleness.What Guo Hongyan was delivered “Nanostructured laminar tungsten alloy with improved ductility by surface Mechanical attrition treatment ", in " Scientific Reports " 7 (2017) 1351 article, it was recently reported that Surface is formd by high-frequency high-speed bullet constant impingement tungsten surface using the mechanical grinding techniques in the mechanical treatment process of surface It is nanocrystalline and crystallite dimension through-thickness change of gradient to receive micro- Multi-scale model.It is worth mentioning that from focused ion beam From the point of view of the Multi-scale model section of cutting, occur multiple layering interfaces in gradient-structure layer, integrality is insufficient.Layering is touched with high energy The effect of hitting is related, and tungsten is bcc metals and has larger brittleness, can not lead under the effect of the strong collision of surface High-velocity Projectiles It crosses quickly plastic deformation and reaches sustained release stress effect, stress is difficult to transmit the internal formation crackle of cause in tungsten.The method is mainly fitted Together in the preferable metal and alloy materials of the plasticity such as copper, iron, nickel, titanium, to tungsten material processing, there is also more deficiencies.
Therefore, in order to meet the requirement towards plasma facing materials, the surface for also needing development to have high quality is more Scale layer tungsten material and process for treating surface.
Summary of the invention
The invention solves first technical problem be to provide a kind of multiple dimensioned layer tungsten material in the surface with high quality.
In order to solve the first technical problem mentioned above, the surface texture of Multi-scale model tungsten material in surface of the present invention is to base Gradient layer is provided between body tissue, the crystallite dimension of the gradient layer changes in gradient, from the surface texture to matrix group The gradient layer knitted is followed successively by nanometer layer, sub-micron layer, micron layer, the crystallite dimension point of the nanometer layer, sub-micron layer, micron layer It Wei not nanoscale, submicron order and micron order;It is preferred that 60~100nm of the nanometer layer crystallite dimension;Sub-micron layer crystal particle size 0.1~1 μm;1~5 μm of micron layer crystallite dimension.
Preferably, the total layer of the gradient layer is with a thickness of 5~60 microns.
Preferably, 0.5~5 μm of the nanometer layer, 1~10 μm of sub-micron thickness;3~35 μm of thickness of micron.
Preferably, the preparation method of the material includes: with abrading-ball under 200~500 DEG C of constant temperature in tungsten block surface unlubricated friction 10 Surface Multi-scale model tungsten block is made in~60min.
Preferably, the abrading-ball is aluminium oxide ball.
Preferably, the normal pressure of the unlubricated friction and friction linear velocity are respectively 10~50N, 0.1~0.6m/s.
Preferably, the preparation method of the material further include: sanding and polishing is carried out to tungsten block surface before unlubricated friction, acetone is gone Oil, ultrasonic cleaning, drying.
The invention solves second technical problem be to provide the preparation side of above-mentioned surface Multi-scale model tungsten material Method.
To solve second technical problem of the invention, the preparation side of Multi-scale model tungsten material in surface of the present invention Method includes:
Surface Multi-scale model tungsten block is made in tungsten block surface 10~60min of unlubricated friction with abrading-ball under 200~500 DEG C of constant temperature; The abrading-ball is preferably aluminium oxide ball.
Preferably, the normal pressure of the unlubricated friction and friction linear velocity are respectively 10~50N, 0.1~0.6m/s.
Preferably, the preparation method of the material further include: sanding and polishing is carried out to tungsten block surface before unlubricated friction, acetone is gone Oil, ultrasonic cleaning, drying.
The utility model has the advantages that
The multiple dimensioned layer tungsten material in surface prepared by the present invention, surface texture to changing in gradient between matrix, Crystallite dimension increases to sub-micron by nanometer from table to interior, then arrives micron.The total thickness degree of gradient layer can reach in a short time several Ten microns.Phenomena such as being well combined between each scale layer, not having sharp interface, micro-crack, delamination do not occur.
The preparation side for the surface Multi-scale model tungsten material that a kind of scale provided by the invention is continuous and Coating combination is excellent Method, used dry friction technology can be stablized, accurately adjust the normal pressure applied on the surface of the material, so that material uniform force And it is destructive smaller.The technology can also adjust contact linear velocity, reaches tungsten block under pressure and pulling force effect and slowly deforms Effect.In addition, hot environment plays the role of destressing of annealing to material, so that deformation layer, without peeling, Coating combination is good.
The present invention is simple, quickly, and is suitable for bulk sample and prepares.
Detailed description of the invention
Fig. 1 is the Cross Section Morphology prepared by the present invention with Multi-scale model tungsten material;Total about 50 μm of thickness;
I nanometer layer of region amplifies pattern in Fig. 2 Fig. 1;About 5 μm of nanometer layer;
Region II sub-micron layer amplifies pattern in Fig. 3 Fig. 1;About 10 μm of sub-micron thickness;
Region III micron refinement layer amplifies pattern in Fig. 4 Fig. 1;About 35 μm of thickness of micron.
Specific embodiment
In order to solve the first technical problem mentioned above, the surface texture of Multi-scale model tungsten material in surface of the present invention is to base Gradient layer is provided between body tissue, the crystallite dimension of the gradient layer changes in gradient, from the surface texture to matrix group The gradient layer knitted is followed successively by nanometer layer, sub-micron layer, micron layer, the crystallite dimension point of the nanometer layer, sub-micron layer, micron layer It Wei not nanoscale, submicron order and micron order;It is preferred that 60~100nm of the nanometer layer crystallite dimension;Sub-micron layer crystal particle size 0.1~1 μm;1~5 μm of micron layer crystallite dimension.
Preferably, the total layer of the gradient layer is with a thickness of 5~60 microns.
Preferably, 0.5~5 μm of the nanometer layer, 1~10 μm of sub-micron thickness;3~35 μm of thickness of micron.
Preferably, the preparation method of the material includes: with abrading-ball under 200~500 DEG C of constant temperature in tungsten block surface unlubricated friction 10 Surface Multi-scale model tungsten block is made in~60min.
Preferably, the abrading-ball is aluminium oxide ball.
Preferably, the normal pressure of the dry grinding and friction linear velocity are respectively 10~50N, 0.1~0.6m/s.
Preferably, the preparation method of the material further include: sanding and polishing is carried out to tungsten block surface before dry grinding, acetone is gone Oil, ultrasonic cleaning, drying.
To solve second technical problem of the invention, the preparation side of Multi-scale model tungsten material in surface of the present invention Method includes:
Surface Multi-scale model tungsten block is made in tungsten block surface 10~60min of unlubricated friction with abrading-ball under 200~500 DEG C of constant temperature; The abrading-ball is preferably aluminium oxide ball.
Preferably, the normal pressure of the unlubricated friction and friction linear velocity are respectively 10~50N, 0.1~0.6m/s.
Preferably, the preparation method of the material further include: sanding and polishing is carried out to tungsten block surface before unlubricated friction, acetone is gone Oil, ultrasonic cleaning, drying.
Embodiment 1
The specific steps of the surface Multi-scale model tungsten material preparation of total 50 microns of thickness are as follows:
Step 1: state tungsten block P400 will be rolled, 800,1500,2000 carborundum paper is successively polished surface, then used The diamond paste of polishing cloth and W2.5, W1 and W0.5 are to its fine polishing.The tungsten remained on surface after polishing is had with acetone Machine object previous cleaning, it is smooth clean to surface to place into ultrasonic device cleaning, finally takes out tungsten block dried for standby.
Step 2: the tungsten block handled well in step 1 being placed in the sample room of high-temperature friction testing machine, fixes and guarantees table Face is flushed with horizontal plane.Sample room temperature is risen to 500 DEG C, 150 DEG C/min of heating rate.It grinds pearl and uses aluminium oxide ball, just Pressure and friction linear velocity are respectively set to 20N, 0.6m/s.It rubs 50 minutes in the above conditions, obtains the multiple dimensioned layer in surface Tungsten material, Cross Section Morphology are detailed in Fig. 1, Fig. 2, Fig. 3 and Fig. 4.
It can be seen that about 50 μm of the total thickness of gradient layer of surface Multi-scale model tungsten material of the invention by Fig. 1;By scheming 2 can be seen that about 5 μm of nanometer layer, 60~100nm of nanometer layer crystallite dimension;About 10 μm of sub-micron thickness as seen from Figure 3;It is sub- 0.1~1 μm of micron layer crystallite dimension;About 35 μm of micron thickness as seen from Figure 4;1~5 μm of micron layer crystallite dimension.
The multiple dimensioned layer tungsten material in surface prepared by the present invention, surface texture can be seen that as Fig. 1, Fig. 2, Fig. 3 and Fig. 4 To changing in gradient between matrix, crystallite dimension increases to sub-micron by nanometer from table to interior, then arrives micron.Gradient layer is total Thickness degree can reach tens microns in a short time.It is well combined between each scale layer, does not have sharp interface, fine fisssure does not occur Phenomena such as line, delamination.

Claims (10)

1. surface Multi-scale model tungsten material, which is characterized in that the surface texture of the surface Multi-scale model tungsten material to base Gradient layer is provided between body tissue, the crystallite dimension of the gradient layer changes in gradient, from the surface texture to matrix group The gradient layer knitted is followed successively by nanometer layer, sub-micron layer, micron layer, the crystallite dimension point of the nanometer layer, sub-micron layer, micron layer It Wei not nanoscale, submicron order and micron order;It is preferred that 60~100nm of the nanometer layer crystallite dimension;Sub-micron layer crystal particle size 0.1~1 μm;1~5 μm of micron layer crystallite dimension.
2. Multi-scale model tungsten material in surface according to claim 1, which is characterized in that the total layer of gradient layer with a thickness of 5~60 microns.
3. Multi-scale model tungsten material in surface according to claim 1 or 2, which is characterized in that the nanometer thickness 0.5~ 5 μm, 1~10 μm of sub-micron thickness;3~35 μm of thickness of micron.
4. described in any item surface Multi-scale model tungsten materials according to claim 1~3, which is characterized in that the material Preparation method includes: that surface Multi-scale model is made in tungsten block surface 10~60min of unlubricated friction with abrading-ball under 200~500 DEG C of constant temperature Tungsten block.
5. Multi-scale model tungsten material in surface according to claim 4, which is characterized in that the abrading-ball is aluminium oxide circle Pearl.
6. Multi-scale model tungsten material in surface according to claim 4 or 5, which is characterized in that the normal pressure of the unlubricated friction It is respectively 10~50N, 0.1~0.6m/s with friction linear velocity.
7. Multi-scale model tungsten material in surface according to any one of claim 4 to 6, which is characterized in that the material Preparation method further include: sanding and polishing is carried out to tungsten block surface before unlubricated friction, acetone deoils, is cleaned by ultrasonic, dries.
8. the preparation method of surface Multi-scale model tungsten material, which is characterized in that the preparation method of the material includes: 200~ Surface Multi-scale model tungsten block is made in tungsten block surface 10~60min of unlubricated friction with abrading-ball under 500 DEG C of constant temperature;The abrading-ball is preferred For aluminium oxide ball.
9. the preparation method of Multi-scale model tungsten material in surface according to claim 8, which is characterized in that the unlubricated friction Normal pressure and friction linear velocity are respectively 10~50N, 0.1~0.6m/s.
10. surface Multi-scale model tungsten material according to claim 8 or claim 9, which is characterized in that the preparation side of the material Method further include: sanding and polishing is carried out to tungsten block surface before unlubricated friction, acetone deoils, is cleaned by ultrasonic, dries.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110346271A (en) * 2019-07-22 2019-10-18 南京理工大学 A method of radiation resistance attacking material is screened using gradient-structure
CN112226662A (en) * 2020-10-21 2021-01-15 广州大学 Double-nanostructure tungsten alloy with good high-temperature stability and preparation method and application thereof
CN114480935A (en) * 2022-01-20 2022-05-13 广东工业大学 Tungsten-based alloy with grain size having gradient effect and preparation method thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101240370A (en) * 2007-02-09 2008-08-13 中国科学院金属研究所 Metal material surface nano preparation method
CN101353720A (en) * 2007-07-23 2009-01-28 宝山钢铁股份有限公司 Manufacturing method of metallic plate having superfine crystal continuous gradient tissue and metallic plate

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101240370A (en) * 2007-02-09 2008-08-13 中国科学院金属研究所 Metal material surface nano preparation method
CN101353720A (en) * 2007-07-23 2009-01-28 宝山钢铁股份有限公司 Manufacturing method of metallic plate having superfine crystal continuous gradient tissue and metallic plate

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110346271A (en) * 2019-07-22 2019-10-18 南京理工大学 A method of radiation resistance attacking material is screened using gradient-structure
CN110346271B (en) * 2019-07-22 2021-09-17 南京理工大学 Method for screening radiation damage resistant material by using gradient structure
CN112226662A (en) * 2020-10-21 2021-01-15 广州大学 Double-nanostructure tungsten alloy with good high-temperature stability and preparation method and application thereof
CN114480935A (en) * 2022-01-20 2022-05-13 广东工业大学 Tungsten-based alloy with grain size having gradient effect and preparation method thereof
CN114480935B (en) * 2022-01-20 2022-11-29 广东工业大学 Tungsten-based alloy with grain size having gradient effect and preparation method thereof

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