CN109396965B - Tungsten material with surface multi-scale structure and preparation method thereof - Google Patents
Tungsten material with surface multi-scale structure and preparation method thereof Download PDFInfo
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- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 title claims abstract description 81
- 229910052721 tungsten Inorganic materials 0.000 title claims abstract description 81
- 239000010937 tungsten Substances 0.000 title claims abstract description 81
- 239000000463 material Substances 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000002052 molecular layer Substances 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 12
- 239000011159 matrix material Substances 0.000 claims abstract description 11
- 230000008859 change Effects 0.000 claims abstract description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 14
- 238000000227 grinding Methods 0.000 claims description 14
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 7
- 238000009837 dry grinding Methods 0.000 claims description 7
- 239000011324 bead Substances 0.000 claims description 5
- 229910052751 metal Inorganic materials 0.000 abstract description 6
- 239000002184 metal Substances 0.000 abstract description 6
- 238000004381 surface treatment Methods 0.000 abstract description 3
- 239000010410 layer Substances 0.000 description 47
- 239000000956 alloy Substances 0.000 description 9
- 229910045601 alloy Inorganic materials 0.000 description 8
- 230000000694 effects Effects 0.000 description 8
- 229910026551 ZrC Inorganic materials 0.000 description 7
- 238000007709 nanocrystallization Methods 0.000 description 6
- 230000007547 defect Effects 0.000 description 4
- 229910001080 W alloy Inorganic materials 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000004927 fusion Effects 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- OTCHGXYCWNXDOA-UHFFFAOYSA-N [C].[Zr] Chemical compound [C].[Zr] OTCHGXYCWNXDOA-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 238000005275 alloying Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- SGGPVBOWEPPPEH-UHFFFAOYSA-N [K].[Zr] Chemical compound [K].[Zr] SGGPVBOWEPPPEH-UHFFFAOYSA-N 0.000 description 1
- DBIMSKIDWWYXJV-UHFFFAOYSA-L [dibutyl(trifluoromethylsulfonyloxy)stannyl] trifluoromethanesulfonate Chemical compound CCCC[Sn](CCCC)(OS(=O)(=O)C(F)(F)F)OS(=O)(=O)C(F)(F)F DBIMSKIDWWYXJV-UHFFFAOYSA-L 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000009531 guhong Substances 0.000 description 1
- 230000003116 impacting effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000010884 ion-beam technique Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- OJYBUGUSFDKJEX-UHFFFAOYSA-N tungsten zirconium Chemical compound [Zr].[W].[W] OJYBUGUSFDKJEX-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B1/00—Processes of grinding or polishing; Use of auxiliary equipment in connection with such processes
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/04—Alloys 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 invention relates to a tungsten material with a surface multi-scale structure and a preparation method of the material, belonging to the technical field of metal surface treatment. The gradient layer is arranged between the surface tissue and the matrix tissue of the tungsten material with the surface multi-scale structure, the grain size of the gradient layer is in gradient change, the gradient layer from the surface tissue to the matrix tissue sequentially comprises a nano layer, a sub-micron layer and a micro layer, and the grain sizes of the nano layer, the sub-micron layer and the micro layer are respectively nano, sub-micron and micron. The surface multi-scale layer tungsten material has good combination among all scale layers, has no obvious interface, and does not generate phenomena of microcrack, peeling and the like. The method is simple, rapid and suitable for preparing large samples.
Description
Technical Field
The invention relates to a tungsten material with a surface multi-scale structure and a preparation method of the material, belonging to the technical field of metal surface treatment.
Background
The service environment of the fusion reactor facing to the plasma body part is extremely harsh, and the materials in the fusion reactor can resist the damage effect caused by high thermal load and strong irradiation for a long time so as to ensure the long-term stable work of the fusion reactor. Tungsten is the highest melting point metal material and has high thermal conductivity, low sputtering rate, and is considered to be one of the most potential materials that can be applied to plasma-facing components. However, the biggest defects of tungsten are obvious defects of room temperature brittleness (even rolling state commercial grade tungsten, the ductile-brittle transition temperature DBTT is between 200 and 300 ℃), irradiation embrittlement, thermal load cracking and the like, and the practical application of the tungsten as the first wall material is greatly limited.
In order to overcome the above-mentioned disadvantages of tungsten, researchers have developed approaches to improve the toughness of tungsten, mainly by alloying tungsten, plastic deformation processing of tungsten/tungsten alloy, and nanocrystallization of tungsten surface. The principle of these methods is to induce grain refinement strengthening of tungsten. Alloying is generally combined with plastic deformation for use, and the fine-grained tungsten alloy is mainly prepared by adding second-phase nano particles such as oxide carbide and other dispersed tungsten matrixes, and is combined with subsequent rolling treatment to achieve the effects of alloy densification, refinement and strengthening. Liu Rui, Xizhu Ming et al in patent CN104388789B disclose "a nanometer structure tungsten-zirconium carbide alloy and its preparation method" and Xizhu Ming et al in the article "improvement high performance/strength of the interfacial designed bulk W-ZrC alloy plate at a relative low temperature" and "scientific reports 5(2015)16014 reported that adding nanometer zirconium carbide makes tungsten matrix crystal grains fully refined, obtains a large amount of grain boundaries/phase boundaries, thereby making the alloy have more excellent obdurability and thermal shock resistance. But the defects are that the heat conductivity of pure tungsten is sacrificed, the phase boundary in the W-ZrC alloy increases the mechanical property and enhances the scattering effect on electrons, and the heat conductivity of the W-ZrC alloy is obviously reduced compared with that of the pure tungsten. Liurui and the like improve the components, and a patent CN108149103A discloses 'a potassium zirconium carbide co-doped tungsten alloy and a preparation method thereof', the mechanical property of tungsten is further improved through the combined action of nano potassium bubbles and zirconium carbide, and the thermal conductivity is not characterized. It is surmised that the presence of potassium bubbles in combination with the ceramic nanoparticles will further reduce the thermal conductivity of the alloy.
The high thermal conductivity is beneficial to timely removing the heat deposited on the first wall, and the high thermal conductivity of tungsten is not lost while the mechanical property is improved, so that the method has important significance. In most service environments, material instability begins to occur on the surface, and for this reason, the self-nanocrystallization research of the pure tungsten surface is concerned by researchers, and has the following advantages: 1) the surface nano tungsten crystal grains can reduce the ductile-brittle transition temperature of the tungsten facing the plasma surface and improve the thermal shock resistance and the irradiation resistance; 2) the difficulty of processing the blocky tungsten can be reduced by surface self-nanocrystallization; 3) the self-nanocrystallization of the tungsten surface preserves the high thermal conductivity of tungsten. Although there are many methods for the self-nanocrystallization of the surface of a material, such as surface mechanical treatment and non-equilibrium thermodynamic method, research and attempts have been made for the self-nanocrystallization of the surface of tungsten metal, because tungsten is the highest melting metal and has great brittleness. In "Nanostructured less structured alloy with improved properties by surface mechanical attachment" article, "Scientific Reports" 7(2017)1351 published by guhong swallow, a nano-micro multi-scale structure is reported in which surface nanocrystals are formed by continuously impacting a tungsten surface with high-frequency high-speed projectiles to change the grain size in a gradient manner in the thickness direction by using a mechanical grinding technique in a surface mechanical treatment method. It is worth proposing that from the multi-scale structural section cut by the focused ion beam, a plurality of layered interfaces appear in the gradient structural layer, and the integrity is insufficient. The layering is related to the high-energy collision effect, the tungsten is body-centered cubic metal and has larger brittleness, the slow-release stress effect cannot be achieved through rapid plastic deformation under the strong collision effect of the surface high-speed projectile, and the stress in the tungsten is difficult to transfer to cause cracks to be formed inside. The method is mainly suitable for metals and alloy materials with good plasticity, such as copper, iron, nickel, titanium and the like, and has more defects in tungsten material treatment.
Therefore, in order to meet the requirements of the first wall material for plasma, the development of a surface multi-scale layer tungsten material with high quality and a surface treatment technology are required.
Disclosure of Invention
The first technical problem to be solved by the invention is to provide a surface multi-scale layer tungsten material with high quality.
In order to solve the first technical problem, a gradient layer is arranged between the surface tissue and the matrix tissue of the tungsten material with the surface multi-scale structure, the grain size of the gradient layer is in gradient change, the gradient layer from the surface tissue to the matrix tissue is a nano layer, a sub-micron layer and a micro layer in sequence, and the grain sizes of the nano layer, the sub-micron layer and the micro layer are respectively nano, sub-micron and micron; preferably, the grain size of the nano-layer is 60-100 nm; the grain size of the submicron layer is 0.1-1 μm; the grain size of the micron layer is 1 to 5 μm.
Preferably, the total thickness of the gradient layer is 5-60 microns.
Preferably, the nano layer is 0.5-5 μm, and the sub-micron layer is 1-10 μm thick; the thickness of the micron layer is 3-35 μm.
Preferably, the preparation method of the material comprises the following steps: and (3) carrying out dry friction on the surface of the tungsten block for 10-60 min by using a grinding ball at a constant temperature of 200-500 ℃ to prepare the tungsten block with the surface multi-scale structure.
Preferably, the grinding balls are alumina balls.
Preferably, the positive pressure of dry friction and the linear speed of friction are respectively 10-50N and 0.1-0.6 m/s.
Preferably, the preparation method of the material further comprises the following steps: before dry-grinding, the surface of the tungsten block is polished, deoiled by acetone, ultrasonically cleaned and dried.
The second technical problem to be solved by the invention is to provide a preparation method of the tungsten material with the surface multi-scale structure.
In order to solve the second technical problem, the preparation method of the surface multi-scale structure tungsten material comprises the following steps:
carrying out dry friction on the surface of the tungsten block for 10-60 min by using a grinding ball at a constant temperature of 200-500 ℃ to prepare the tungsten block with the surface multi-scale structure; the grinding balls are preferably alumina beads.
Preferably, the positive pressure of dry friction and the linear speed of friction are respectively 10-50N and 0.1-0.6 m/s.
Preferably, the preparation method of the material further comprises the following steps: before dry-grinding, the surface of the tungsten block is polished, deoiled by acetone, ultrasonically cleaned and dried.
Has the advantages that:
the surface multi-scale layer tungsten material prepared by the invention has gradient change from the surface tissue to the matrix tissue, and the grain size is increased from nanometer to submicron and then micron from the surface to the inside. The total layer thickness of the gradient layer can reach tens of microns in a short time. The scale layers are well combined, no obvious interface exists, and phenomena such as microcracks, peeling and the like do not occur.
According to the preparation method of the surface multi-scale structure tungsten material with continuous scale and excellent interlayer combination, the adopted dry friction technology can stably and accurately adjust the positive pressure applied to the surface of the material, so that the material is uniformly stressed and has small destructiveness. The technology can also adjust the contact linear velocity, so that the tungsten block can achieve the effect of slow deformation under the action of pressure and tension. In addition, the high-temperature environment has the annealing and stress-removing effects on the material, so that the deformation layer is free of stripping phenomenon, and the interlayer bonding is good.
The method is simple, rapid and suitable for preparing large samples.
Drawings
FIG. 1 is a cross-sectional view of a tungsten material with a multi-scale structure prepared by the present invention; the total layer thickness is about 50 μm;
FIG. 2 is an enlarged view of the nanolayer of region I of FIG. 1; nanolayer about 5 μm;
FIG. 3 is an enlarged view of the submicron layer in region II of FIG. 1; the sub-micron layer is about 10 μm thick;
FIG. 4 is an enlarged view of the zone III micron refinement layer of FIG. 1; the microlayers are about 35 μm thick.
Detailed Description
In order to solve the first technical problem, a gradient layer is arranged between the surface tissue and the matrix tissue of the tungsten material with the surface multi-scale structure, the grain size of the gradient layer is in gradient change, the gradient layer from the surface tissue to the matrix tissue is a nano layer, a sub-micron layer and a micro layer in sequence, and the grain sizes of the nano layer, the sub-micron layer and the micro layer are respectively nano, sub-micron and micron; preferably, the grain size of the nano-layer is 60-100 nm; the grain size of the submicron layer is 0.1-1 μm; the grain size of the micron layer is 1 to 5 μm.
Preferably, the total thickness of the gradient layer is 5-60 microns.
Preferably, the nano layer is 0.5-5 μm, and the sub-micron layer is 1-10 μm thick; the thickness of the micron layer is 3-35 μm.
Preferably, the preparation method of the material comprises the following steps: and (3) carrying out dry friction on the surface of the tungsten block for 10-60 min by using a grinding ball at a constant temperature of 200-500 ℃ to prepare the tungsten block with the surface multi-scale structure.
Preferably, the grinding balls are alumina balls.
Preferably, the positive pressure and the linear friction speed of the dry grinding are respectively 10-50N and 0.1-0.6 m/s.
Preferably, the preparation method of the material further comprises the following steps: before dry grinding, the surface of the tungsten block is polished, deoiled by acetone, ultrasonically cleaned and dried.
In order to solve the second technical problem, the preparation method of the surface multi-scale structure tungsten material comprises the following steps:
carrying out dry friction on the surface of the tungsten block for 10-60 min by using a grinding ball at a constant temperature of 200-500 ℃ to prepare the tungsten block with the surface multi-scale structure; the grinding balls are preferably alumina beads.
Preferably, the positive pressure of dry friction and the linear speed of friction are respectively 10-50N and 0.1-0.6 m/s.
Preferably, the preparation method of the material further comprises the following steps: before dry-grinding, the surface of the tungsten block is polished, deoiled by acetone, ultrasonically cleaned and dried.
Example 1
The preparation method of the surface multi-scale structure tungsten material with the total layer thickness of 50 micrometers comprises the following specific steps:
step 1: the rolled tungsten block was sequentially polished on its surface with silicon carbide sandpaper of P400, 800, 1500, 2000, and then finely polished with a polishing cloth and diamond abrasive pastes of W2.5, W1, and W0.5. Primarily washing organic matters remained on the surface of the polished tungsten by using acetone, then putting the tungsten into an ultrasonic device for cleaning until the surface is smooth and clean, and finally taking out the tungsten block for drying for later use.
Step 2: and (3) placing the tungsten block processed in the step (1) in a sample chamber of a high-temperature friction tester, and fixing and ensuring that the surface is flush with the horizontal plane. The sample chamber temperature was raised to 500 ℃ at a rate of 150 ℃/min. The grinding beads are alumina beads, and the positive pressure and the friction linear velocity are respectively set to be 20N and 0.6 m/s. Rubbing for 50 minutes under the above conditions to obtain the surface multi-scale layer tungsten material, the cross-sectional morphology of which is detailed in fig. 1, fig. 2, fig. 3 and fig. 4.
From FIG. 1, it can be seen that the total layer thickness of the gradient layer of the tungsten material of the surface multi-scale structure of the invention is about 50 μm; FIG. 2 shows that the nano-layer is about 5 μm, and the grain size of the nano-layer is 60-100 nm; from FIG. 3 it can be seen that the sub-micron layer is about 10 μm thick; the grain size of the submicron layer is 0.1-1 μm; from FIG. 4 it can be seen that the microlayers are about 35 μm thick; the grain size of the micron layer is 1 to 5 μm.
It can be seen from fig. 1, fig. 2, fig. 3 and fig. 4 that the surface multi-scale layer tungsten material prepared by the present invention has gradient change from the surface tissue to the matrix tissue, and the grain size increases from nanometer to submicron and then to micrometer from surface to interior. The total layer thickness of the gradient layer can reach tens of microns in a short time. The scale layers are well combined, no obvious interface exists, and phenomena such as microcracks, peeling and the like do not occur.
Claims (8)
1. The surface multi-scale structure tungsten material is characterized in that a gradient layer is arranged between the surface tissue and the matrix tissue of the surface multi-scale structure tungsten material, the grain size of the gradient layer is in gradient change, the gradient layer from the surface tissue to the matrix tissue is a nano layer, a sub-micron layer and a micron layer in sequence, and the grain sizes of the nano layer, the sub-micron layer and the micron layer are respectively nano, sub-micron and micron; the grain size of the nano-layer is 60-100 nm; the grain size of the submicron layer is 0.1-1 μm; the grain size of the micron layer is 1-5 mu m;
the preparation method of the material comprises the following steps: carrying out dry friction on the surface of the tungsten block for 10-60 min by using a grinding ball at a constant temperature of 200-500 ℃ to prepare the tungsten block with the surface multi-scale structure;
the positive pressure of dry friction and the linear speed of friction are respectively 10-50N and 0.1-0.6 m/s.
2. The surface multi-scale structure tungsten material according to claim 1, wherein the total layer thickness of the gradient layer is 5-60 microns.
3. The surface multi-scale structure tungsten material according to claim 1 or 2, wherein the nano layer is 0.5-5 μm thick, and the sub-micron layer is 1-10 μm thick; the thickness of the micron layer is 3-35 μm.
4. The surface multi-scale structure tungsten material according to claim 1, wherein the grinding balls are alumina beads.
5. The surface multi-scale structure tungsten material according to claim 1, wherein the preparation method of the material further comprises: before dry-grinding, the surface of the tungsten block is polished, deoiled by acetone, ultrasonically cleaned and dried.
6. The preparation method of the tungsten material with the surface multi-scale structure is characterized by comprising the following steps: carrying out dry friction on the surface of the tungsten block for 10-60 min by using a grinding ball at a constant temperature of 200-500 ℃ to prepare the tungsten block with the surface multi-scale structure;
the positive pressure of dry friction and the linear speed of friction are respectively 10-50N and 0.1-0.6 m/s.
7. The method for preparing the surface multi-scale structure tungsten material according to claim 6, wherein the grinding balls are alumina balls.
8. The method for preparing the surface multi-scale structure tungsten material according to claim 6 or 7, wherein the method for preparing the material further comprises the following steps: before dry-grinding, the surface of the tungsten block is polished, deoiled by acetone, ultrasonically cleaned and dried.
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Effective date of registration: 20240529 Address after: 230000 B-1015, wo Yuan Garden, 81 Ganquan Road, Shushan District, Hefei, Anhui. Patentee after: HEFEI MINGLONG ELECTRONIC TECHNOLOGY Co.,Ltd. Country or region after: China Address before: 617000 Airport Road, East District, Panzhihua, Sichuan Province, No. 10 Patentee before: PANZHIHUA University Country or region before: China |