CN102312186B - Method for improving bonding strength of vacuum plasma spraying tungsten coating - Google Patents
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Abstract
The invention belongs to the field of coating materials and particularly relates to a method for improving the bonding strength of a vacuum plasma spraying tungsten coating. In the method, a copper-molybdenum (Cu-Mo) compound coating is used as an intermediate layer between a W coating and a copper alloy base material, and the intermediate layer is 50-200mum thick. By utilizing the method provided by the invention, the bonding strength between the prepared W coating and the copper alloy base material can reach at least 40MPa through controlling technological parameters, and simultaneously, the coating containing the intermediate layer has the characteristics of uniform structure, high thermal conductivity and simple technological preparation process.
Description
Technical field
The invention belongs to coated material field, be specifically related to a kind of method that improves bonding strength of vacuum plasma spraying tungsten coating.
Background technology
Tungsten is a kind of Rare Metals Materials of infusibility, has the feature such as physicals and stable chemical nature of high-melting-point, high boiling point, high rigidity, low thermal expansivity.Because of its special physics and chemistry performance, tungsten is widely used in the fields such as electronics, metallurgy, oil, space flight.Along with the development of fusion research, also become one of key issue of fusion research for the material of fusion facility.The material wherein directly contacting with plasma body is called as plasma facing material (Plasma-facing material, PFM), need to directly bear the multiple harsh effects such as high heat-flux, high energy particle irradiation, machinery and thermal stresses corrosion.
Tungsten material has high-melting-point, high thermal conductance, high physical sputtering threshold value and without premium propertiess such as chemical sputterings, be considered to most promising plasma facing material [G.Janeschiz, P.Barabaschi, G.Federici, The requirements of a next step large steady state tokamak, Nuclear Fusion, 2000 (40) 1197-1221.].But tungsten material exists the shortcomings such as poor processability, mechanical strength are not high, it is subject to certain restrictions in engineering application.Preparing tungsten coating take copper alloy heat sink material as base material on its surface, is the effective scheme addressing this problem.
The preparation method of tungsten coating mainly contains chemical vapour deposition (Chemical vapor deposition, CVD), physical vapor deposition (Physical vapor deposition, PVD) and plasma spraying (Plasma spraying, PS) etc.Compare CVD and PVD method, the advantage such as plasma spraying technology has can prepare thick coating (being greater than 0.5mm), be applicable to big area manufacture, economy is good, the coating of preparation also has the features such as thickness is controlled, void content is lower simultaneously.Therefore, plasma spray process is considered to the most promising tungsten coating preparation method [J.
p.Chr á ska, J.Linke, Thermal spray coating for fusion applications-review, Journal of Thermal Spray Technology, 2007 (16) 64-83.].
Preparing tungsten coating take copper alloy heat sink material as matrix has the requirement of two aspects, and the one, the thermal conductivity of coating is high, is that the combination of coating and body material is good on the other hand.Adopt vacuum plasma spray technology, pass through process optimization, the coating's air hole ratio of preparation is low, and avoid the oxidative phenomena in atmospheric environment spraying process, foreign matter content is low, there is higher thermal conductivity [Y.Niu, X.Zheng, H.Ji, C.Ding, J.Chen, Y.Yahiro, N.Yoshida, Characterization of Thick Vacuum Plasma Sprayed Tungsten Coatings on Water-cooled Copper Alloy Substrate, NIFS Proceedings2009 (76) 123-127.].But there is notable difference in the thermal expansivity between tungsten coating and copper alloy base material.Coefficient of thermal expansion mismatch between coating and base material, causes thermal stresses in spraying process to be concentrated in the two interface, affects the combination of coating and base material.Someone adopts Cu-W gradient transitional lay, and (Cu is respectively 1:1 with W opaque amount ratio, 1:2, 1:3) prepare vacuum plasma spraying tungsten coating at copper alloy surface, improve the bonding properties of tungsten coating and copper alloy base material, can reach 40MPa[Deyang Hu, Xuebin Zheng, Yaran Niu, Heng Ji, Fali Chong, Junling Chen, Effect of oxidation behavior on the mechanical and thermal properties of plasma sprayed tungsten coatings.Journal of Thermal Spray Technology, 17 (2008): 377-384.].Just can reach positive effect but the method need to be prepared multilayer transition layer, complex technical process, is easy to cause the foreign matter content of coating to increase.Meanwhile, the density of tungsten and the density variation of copper are remarkable, the more difficult control of spraying parameter, and prepared Cu-W interlayer structure is inhomogeneous, and bonding properties is stable not.
Summary of the invention
The object of the invention is to overcome the defect of prior art, a kind of method that improves bonding strength of vacuum plasma spraying tungsten coating is provided.
The present invention adopts following technical scheme to solve the problems of the technologies described above:
A kind of method that improves bonding strength of vacuum plasma spraying tungsten coating, it is characterized in that, the method adopts Cu-Mo composite interlayer between tungsten coating and copper alloy base material, after described Cu-Mo composite interlayer refers to copper powder and molybdenum powder is mixed in proportion, the coating forming at copper alloy substrate surface through vacuum plasma spray, described tungsten coating refers to the coating that tungsten powder is formed on Cu-Mo composite interlayer surface through vacuum plasma spray, the thickness of described Cu-Mo composite interlayer is 50-200 micron, the thickness of described tungsten coating is 200-1000 micron, the particle diameter of described copper powder is 20-100 μ m, the particle diameter of described molybdenum powder is 10-80 μ m, the particle diameter of described tungsten powder is 10-70 μ m, in the total mass of described Cu-Mo composite interlayer, the mass percent of described copper is 10%-50%, the mass percent of described molybdenum is 50%-90%.
Preferably, the described method containing raising bonding strength of vacuum plasma spraying tungsten coating comprises the steps:
1) copper powder and molybdenum powder mix after preparing burden in proportion;
2) while spraying, by copper alloy base material clean, the pre-treatment such as sandblast, adopting vacuum plasma spray method to prepare a layer thickness is the Cu-Mo compound coating of 50～200 microns, and then spraying a layer thickness is the tungsten coating of 200～1000 microns, can obtain the tungsten coating that contains Cu-Mo composite interlayer.
Preferably, in step 1), the particle diameter of described copper powder is 20～100 μ m, and the particle diameter of described molybdenum powder is 10～80 μ m, and the particle diameter of described tungsten powder is 10～70 μ m.
Preferably, step 2) in, the plasma spraying processing parameter of described Cu-Mo compound coating is: the flow of plasma gas Ar is 30～50slpm(standard liter/min), plasma gas H
2flow be 6～15slpm, spray power is 30～50kW, spray pressure is 100～400mbar, the flow of powder carrier gas Ar is 2～7slpm, spray distance is 150～350mm, powder feeding rate is 8～35gmin
-1.
Preferably, step 2) in, the plasma spraying processing parameter of described tungsten coating is: the flow of plasma gas Ar is 30～50slpm(standard liter/min), plasma gas H
2flow be 6～15slpm, spray power is 35～60kW, spray pressure is 100～900mbar, the flow of powder carrier gas Ar is 2～8slpm, spray distance is 150～350mm, powder feeding rate is 5～35gmin
-1.
The following several respects of principle reference of the present invention:
1, the thermal linear expansion coefficient of molybdenum is between tungsten and copper alloy, more approaching with tungsten.In Fig. 1, show the comparison [Y.S.Touloukian of molybdenum, tungsten, copper three kinds of material thermal linear expansion coefficients, R.K.Kirby, R.E.Taylor, P.D.Desai, Thermophysical properties of mater, Vol.12:thermal expansion-metallic elements and alloys, IFI/Plenum, New York, 1975.].Adopt Cu-Mo compound coating as middle layer, can change by the component proportion of design Cu and Mo element the thermal linear expansion coefficient of Cu-Mo compound coating, relax Coefficient of Thermal Expansion mismatch problem between tungsten coating and copper alloy base material, reduce thermal stresses and concentrate, improve the bonding strength of coating.
2, the thermal conductivity of molybdenum is higher, very approaching with the thermal conductivity of tungsten, Fig. 2 has shown thermal conductivity variation with temperature [Y.S.Touloukian, R.W.Powell, the C.Y.Ho of molybdenum, tungsten, three kinds of materials of copper, P.G.Klemens, Thermophysical properties of matter, Vol.1:thermal conductivity-metallic elements and alloys, IFI/Plenum, New York, 1970.].Adopt Cu-Mo compound coating to there is good thermal conductivity as middle layer, be conducive to scattering and disappearing of heat flux, reduce concentrating of thermal stresses.
3, the density of molybdenum and copper alloy are more approaching, and Fig. 3 has shown [Chinese material engineering grand ceremony editorial committee, the grand ceremony of Chinese material engineering, the 4th and the 5th volume, Chemical Industry Press, Beijing, 2006.] of density ratio of molybdenum, tungsten, three kinds of materials of copper.This is conducive to the control of spraying parameter, and middle layer component and the microstructure of preparation are comparatively even.
4, molybdenum and tungsten, all belongs to periodic table of elements VI subgroup element, has good chemical compatibility, for the combination improving between tungsten coating and copper alloy base material provides assurance.
Schematic diagram shown in Fig. 4 is design of the present invention.Before spraying, the copper powder of definite composition and molybdenum powder are mixed, for subsequent use.When spraying, by copper alloy base material clean, the pre-treatment such as sandblast, adopt vacuum plasma spray method to prepare one deck Cu-Mo compound coating, and then carry out the spraying of tungsten coating, can obtain the tungsten coating that contains Cu-Mo composite interlayer.
The invention provides a kind of method that improves vacuum plasma spray tungsten (W) anchoring strength of coating.Utilize method provided by the invention, can make by the control of processing parameter more than bonding strength between W coating and the copper alloy base material of preparation reaches 40MPa, contain the coating in middle layer simultaneously and have that even structure, thermal conductivity are high, the simple feature of technique preparation process.
Accompanying drawing explanation
Fig. 1 is molybdenum, tungsten, three kinds of material thermal linear expansion coefficient variation with temperature of copper.
Fig. 2 is the thermal conductivity variation with temperature of molybdenum, tungsten, three kinds of materials of copper.
Fig. 3 be molybdenum, tungsten, three kinds of materials of copper density ratio.
Fig. 4 is the tungsten coating schematic diagram that contains Cu-Mo composite interlayer.
Fig. 5 be embodiment 1 prepared containing the tungsten coating bonding strength of mass ratio 30%Cu-70%Mo composite interlayer: in figure, left side square frame is the bonding strength value containing the tungsten coating in middle layer not, and right side square frame is the bonding strength value of the tungsten coating that contains 30%Cu-70%Mo composite interlayer.
Fig. 6 be embodiment 2 prepared containing the tungsten coating bonding strength of mass ratio 50%Cu-50%Mo composite interlayer: in figure, left side square frame is the bonding strength value containing the tungsten coating in middle layer not, and right side square frame is the bonding strength value of the tungsten coating that contains 50%Cu-50%Mo composite interlayer.
Embodiment
Further describe technical scheme of the present invention below by specific embodiment.Should be understood that these embodiment are only not used in and limit the scope of the invention for the present invention is described.
Further illustrate feature of the present invention and effect below by embodiment.Limit absolutely not the present invention.
Embodiment 1: adopting particle diameter is the molybdenum powder of 30-60 μ m and the copper powder of 10-70 μ m, is that 30%:70% mixes, as middle layer spray powders by copper powder and molybdenum powder mass ratio.Adopting particle diameter is that the tungsten powder of 5-50 μ m is as tungsten coating spraying powder.Using the copper alloy through sandblasting, alcohol ultrasonic cleaning as body material.After the vacuum tightness of vacuum chamber is down to below 0.1mbar, fill shielding gas Ar gas to certain pressure.Under the spraying parameter shown in table 2, adopt the vacuum plasma spray system of Sulzer Metco company of Switzerland first Cu-Mo compound coating to be sprayed to copper alloy substrate surface, and then spraying tungsten coating.For effect more of the present invention, prepared the tungsten coating that does not contain middle layer simultaneously.Application ASTMC-633 method has been measured the bonding strength of coating, the results are shown in Figure 5.The thickness of described Cu-Mo composite interlayer is 120 microns, and the thickness of described tungsten coating is 300 microns.As seen from Figure 5, in the situation that has 30%Cu-70%Mo composite interlayer, the average bonding strength of tungsten coating and copper alloy increases to 42MPa from 34MPa, and increase rate is 23.5%.
Table 2 vacuum plasma spray processing parameter
| Processing parameter | Cu-Mo composite interlayer | Tungsten coating |
| Plasma gas Ar, (slpm) | 35 | 40 |
| Plasma gas H 2，（slpm） | 9 | 13 |
| Spray power kW | 32 | 50 |
| |
100 | 900 |
| Powder carrier gas Ar slpm | 2 | 6 |
| |
350 | 150 |
| Powder feeding rate gmin -1 | 30 | 25 |
Embodiment 2: adopting particle diameter is the molybdenum powder of 30-60 μ m and the copper powder of 10-70 μ m, is that 50%:50% mixes, as middle layer spray powders by copper powder and molybdenum powder mass ratio.Adopting particle diameter is that the tungsten powder of 5-50 μ m is as tungsten coating spraying powder.Adopt the spray parameters identical with embodiment 1, prepare tungsten coating at copper alloy substrate surface.The thickness of described Cu-Mo composite interlayer is 80 microns, and the thickness of described tungsten coating is 300 microns.The bonding strength of coating is shown in Fig. 6.Adopt as seen from Figure 6 50%Cu-50%Mo composite interlayer, the bonding strength of tungsten coating is 40MPa.
Embodiment 3: adopting particle diameter is the molybdenum powder of 30-60 μ m and the copper powder of 10-70 μ m, is that 40%:60% mixes, as middle layer spray powders by copper powder and molybdenum powder mass ratio.Adopting particle diameter is that the tungsten powder of 5-50 μ m is as tungsten coating spraying powder.
Adopt following spray parameters, prepare tungsten coating at copper alloy substrate surface.
The plasma spraying processing parameter of Cu-Mo compound coating is: the flow of plasma gas Ar is 40slpm(standard liter/min), plasma gas H
2flow be 7slpm, spray power is 38kW, spray pressure is 400mbar, the flow of powder carrier gas Ar is 5slpm, spray distance is 250mm, powder feeding rate is 30gmin
-1.
The plasma spraying processing parameter of tungsten coating is: the flow of plasma gas Ar is 35slpm(standard liter/min), plasma gas H
2flow be 8slpm, spray power is 50kW, spray pressure is 100mbar, the flow of powder carrier gas Ar is 2slpm, spray distance is 350mm, powder feeding rate is 20gmin
-1.
The thickness of described Cu-Mo composite interlayer is 150 μ m, and the thickness of described tungsten coating is 320 μ m.Adopt 40%Cu-60%Mo composite interlayer, the bonding strength of tungsten coating is 43MPa.
Embodiment 4: adopting particle diameter is the molybdenum powder of 30-60 μ m and the copper powder of 10-70 μ m, is that 10%:90% mixes, as middle layer spray powders by copper powder and molybdenum powder mass ratio.Adopting particle diameter is that the tungsten powder of 5-50 μ m is as tungsten coating spraying powder.
Adopt following spray parameters, prepare tungsten coating at copper alloy substrate surface.
The plasma spraying processing parameter of Cu-Mo compound coating is: the flow of plasma gas Ar is 28slpm(standard liter/min), plasma gas H
2flow be 8slpm, spray power is 30kW, spray pressure is 100mbar, the flow of powder carrier gas Ar is 2slpm, spray distance is 350mm, powder feeding rate is 20gmin
-1.
The plasma spraying processing parameter of tungsten coating is: the flow of plasma gas Ar is 40slpm(standard liter/min), plasma gas H
2flow be 10slpm, spray power is 40kW, spray pressure is 400mbar, the flow of powder carrier gas Ar is 6slpm, spray distance is 250mm, powder feeding rate is 30gmin
-1.
The thickness of described Cu-Mo composite interlayer is 80 μ m, and the thickness of described tungsten coating is 200 μ m.Adopt 10%Cu-90%Mo composite interlayer, the bonding strength of tungsten coating is 41MPa.
Claims (4)
1. one kind is improved the method for bonding strength of vacuum plasma spraying tungsten coating, it is characterized in that, the method adopts Cu-Mo composite interlayer between tungsten coating and copper alloy base material, after described Cu-Mo composite interlayer refers to copper powder and molybdenum powder is mixed in proportion, the coating forming at copper alloy substrate surface through vacuum plasma spray, described tungsten coating refers to the coating that tungsten powder is formed on Cu-Mo composite interlayer surface through vacuum plasma spray, the thickness of described Cu-Mo composite interlayer is 50-200 micron, the thickness of described tungsten coating is 200-1000 micron, the particle diameter of described copper powder is 20-100 μ m, the particle diameter of described molybdenum powder is 10-80 μ m, the particle diameter of described tungsten powder is 10-70 μ m, in the total mass of described Cu-Mo composite interlayer, the mass percent of described copper is 10%-50%, the mass percent of described molybdenum is 50%-90%.
2. the method that improves as described in claim 1 bonding strength of vacuum plasma spraying tungsten coating, is characterized in that, comprises the steps:
1) copper powder and molybdenum powder mix after preparing burden in proportion;
2) while spraying, by copper alloy base material clean, sandblast pretreatment, adopt vacuum plasma spray method to prepare the Cu-Mo compound coating that a layer thickness is 50-200 micron, and then spraying a layer thickness be the tungsten coating of 200-1000 micron, can obtain the tungsten coating that contains Cu-Mo composite interlayer.
3. improve as described in claim 2 the method for bonding strength of vacuum plasma spraying tungsten coating, it is characterized in that, step 2) in, the plasma spraying processing parameter of described Cu-Mo compound coating is: the flow of plasma gas Ar is 30-50slpm, and the flow of plasma gas H2 is 6-15slpm, and spray power is 30-50kW, spray pressure is 100-400mbar, the flow of powder carrier gas Ar is 2-7slpm, and spray distance is 150-350mm, and powder feeding rate is 8-35gmin
-1.
4. improve as described in claim 2 the method for bonding strength of vacuum plasma spraying tungsten coating, it is characterized in that, step 2) in, the plasma spraying processing parameter of described tungsten coating is: the flow of plasma gas Ar is 30-50slpm, plasma gas H
2flow be 6-15slpm, spray power is 35-60kW, spray pressure is 100-900mbar, the flow of powder carrier gas Ar is 2-8slpm, spray distance is 150-350mm, powder feeding rate is 5-35gmin
-1.
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| CN103352222B (en) * | 2013-06-24 | 2016-03-02 | 核工业西南物理研究院 | A kind of preparation method of the carbon-base tungsten coating for tokamak device |
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| JP昭60-203436A 1985.10.15 |
| 不同界面对等离子喷涂钨结合强度的影响;宋书香等;《稀有金属材料与工程》;20071031;第36卷(第10期);1811页右栏倒数第11行至1812页左栏第7行，表1 * |
| 宋书香等.不同界面对等离子喷涂钨结合强度的影响.《稀有金属材料与工程》.2007,第36卷(第10期),1811页右栏倒数第11行至1812页左栏第7行，表1. |
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