CN103320735B - Continuous silicon plating process of molybdenum and alloy thereof - Google Patents
Continuous silicon plating process of molybdenum and alloy thereof Download PDFInfo
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- CN103320735B CN103320735B CN201310226315.3A CN201310226315A CN103320735B CN 103320735 B CN103320735 B CN 103320735B CN 201310226315 A CN201310226315 A CN 201310226315A CN 103320735 B CN103320735 B CN 103320735B
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Abstract
The invention relates to a continuous silicon plating process of molybdenum and alloy thereof. The invention belongs to the technical field of metal-based composite material continuous production. The continuous silicon plating process of molybdenum and alloy thereof comprises the steps of washing, preheating, continuous silicon plating, annealing and alloying, and plated sample cooling. With the process, continuous silicon plating can be carried out upon molybdenum and alloy thereof, such that a molybdenum-based composite material can be produced. The processing target includes pure molybdenum materials, molybdenum-niobium alloy materials, tungsten-molybdenum alloy materials, chromium-molybdenum alloy materials, nickel-molybdenum alloy materials, silicon-molybdenum alloy materials, and the like. With the method, the molybdenum-based composite material with compact and uniform plated layer, regular and smooth surface, corrosion resistance, and high-and-low-temperature-oxidation resistance can be continuously prepared. The types of the composite material comprise corrosion-resistant and antioxidant metal-based composite materials such as Mo-MoSi2/Si, Mo-Nb-MoSi2/NbSi2/Si, Mo-W-MoSi2/WSi2/Si, Mo-Cr-MoSi2/CrSi2, Mo-Ni-MoSi2/NiSi2/Si, and the like. With the process, production process is simplified, production cost is reduced, product quality is improved, and production efficiency is effectively improved.
Description
Technical field
The invention belongs to the continuous seepage technical field of metal-base composites, in particular, provide a kind of continuous plating silicon technology of Mo and Mo alloys.
Background technology
Mo and Mo alloys obtains quick application at electronics, metallurgy, nuclear industry, aviation and space field, is widely used as the fields such as the emtting electrode in the thermionic reactor of space, guided missile jet pipe, satellite rocket thruster, engine blade and high temperature electrode.But Mo and Mo alloys is at high temperature very easily oxidized and generates high-volatile MoO
3, finally cause component to damage, cause Mo and Mo alloys can not be on active service for a long time in oxidizing atmosphere.At present, the preparation method of domestic and international Mo and Mo alloys coating mainly contains plasma spraying process, chemical Vapor deposition process (CVD), laser cladding and fused salt electrodip process etc.Adopt above-mentioned several method to prepare molybdenum-base composite material and mostly there is the defects such as hole, cavity and crackle, mechanical property and high-temperature oxidation resistance are all relative poor, and the work-ing life of material is short; Secondly, there is processing condition complexity in aforesaid method, production cost is high, easily produces toxic gas, contaminate environment, can not realize the shortcomings such as serialization industrial production.At present, the research for the continuous plating silicon production molybdenum-base composite material of Mo and Mo alloys have not been reported.
Summary of the invention
The object of the present invention is to provide a kind of continuous plating silicon technology of Mo and Mo alloys, handling object is Mo and Mo alloys, mainly comprises pure Mo, molybdenum niobium alloy material, miramint material, chrome molybdenum Materials science, nickel-molybdenum alloy material, silicon molybdenum alloy material etc.
The present invention adopts the continuous plating silicon technology of cleaning-preheating-plate continuously silicon-annealed alloy-plating sample cooling, can plate silicon continuously to Mo and Mo alloys and produce molybdenum-base composite material, handling object mainly comprises pure Mo, molybdenum niobium alloy material, miramint material, chrome molybdenum material, nickel-molybdenum alloy material, silicon molybdenum alloy material etc.Can continuously produce possess that plated layer compact is even, rule of surface is smooth, the molybdenum-base composite material of corrosion-resistant, anti-high and low-temp oxidation, the type of matrix material comprises Mo-MoSi
2/ Si, Mo-Nb-MoSi
2/ NbSi
2/ Si, Mo-W-MoSi
2/ WSi
2/ Si, Mo-Cr-MoSi
2/ CrSi
2, Mo-Ni-MoSi
2/ NiSi
2corrosion-resistant, the oxidation resistant metal-base composites such as/Si, material shape can be the Mo and Mo alloys material of sheet material, wire rod, tubing and complicated shape.Achieve the suitability for industrialized production of the continuous plating silicon composite of Mo and Mo alloys, simplify production technique, reduce production cost, improve quality product, effectively enhance productivity.Processing step is as follows:
(1) Mo and Mo alloys material uncoiling, pinch, align: by the uncoiling of Mo and Mo alloys material Abrollhaspel, align after pinching, make its rule of surface, smooth.
(2) weld, clean: welding adopts CO
2gasshielded welding machine welds, and welding wire can choose different gas shield welding wires according to the difference of Mo and Mo alloys material; Cleaning is removed the ROLLING OIL of material surface and impurity, and cleaning equipment is bedroom electrolytic cleaning, and cleaning equipment comprises alkali spray tank, electrolytic cleaning tank, alkali are scrubbed, hot water rinse tank and induction furnace drying system.Scavenging solution is concentration is 2 ~ 3%, the caustic soda (NaOH) of temperature about 50 DEG C ~ 70 DEG C.
(3) preheating; Mo and Mo alloys material is preheating to 250 DEG C ~ 350 DEG C in argon shield induction preheating oven, and temperature survey infrared thermometer is measured.Preheating section furnace shell adopts the thick carbon steel furnace shell of 6mm, and refractory materials adopts the thick ceramic fiber of 150mm, and liner adopts 2mm304 stainless steel lined, and furnace bottom is 200mm ceramic fiber.
(4) silicon liquid preparation: purity is that the polysilicon of 7N is heated to 1450 ~ 1500 DEG C by the large-scale vacuum induction adopting American I A company to produce, and process furnace atmosphere is argon atmosphere.
(5) silicon-air knife process is plated continuously: Mo and Mo alloys is sent into silicon groove in argon atmosphere; carry out silicon layer and be coated with plating; coating temperature is at 1450 ~ 1500 DEG C; and the coating weight of Mo and Mo alloys material surface is controlled by air knife, air knife adopts coating weight automated closed-loop to control and artificial vernier control.
(6) annealed alloy: Mo and Mo alloys plating piece is sent into the annealed alloy process carrying out processing condition in vacuum controlled atmosphere annealing furnace, annealing temperature is 1000 ~ 1400 DEG C, and annealing time is 1 ~ 3 hour, and high temperature annealing atmosphere is argon atmosphere.By controlling control thickness of coating that annealing temperature and annealing time can be strict and coating material composition.
(7) plating piece cooling: the plating piece after coating is carried out argon gas and spray cooling and shrend cooling.First spray cooling with argon gas and plating piece is cooled to 150 ~ 250 DEG C, then carry out being cooled to 50 DEG C ~ 80 DEG C entering watch-quench tank.Drying plating piece adopts Electric heating to dry plating piece, and bake out temperature controls at 60 ~ 120 DEG C.Then carry out plating piece inspection, namely an X-ray thickness of coating tester is set after watch-quench tank, feedback thickness of coating, according to feedback data adjustment air knife parameter, better control thickness of coating.
(8) polishing, aligning: polishing aligning carries out polishing with polishing machine after plating piece being gone out cooling tower, and align in withdrawal straightening machine, straight to ensure the polishing of plating piece.
(9) oven dry is batched: adopt Electric heating to dry plating piece, bake out temperature controls at 60 ~ 120 DEG C, and rear detection to be dried shows quality and batches with mandrel sleeve pipe cantilevered reeling machine.
In aforesaid method, Mo and Mo alloys material is after the process of a series of continuous plating silicon, and just can obtain corrosion-resistant, oxidation resistant molybdenum-base composite material, the type of matrix material comprises Mo-MoSi
2/ Si, Mo-Nb-MoSi
2/ NbSi
2/ Si, Mo-W-MoSi
2/ WSi
2/ Si, Mo-Cr-MoSi
2/ CrSi
2, Mo-Ni-MoSi
2/ NiSi
2the multiple molybdenum-base composite material such as/Si.
Compared with existing technological method, tool of the present invention has the following advantages:
1. the invention has the advantages that the continuous plating silicon process that can be used for multiple Mo and Mo alloys, handling object mainly comprises pure Mo, molybdenum niobium alloy material, miramint material, chrome molybdenum Materials science, nickel-molybdenum alloy material, silicon molybdenum alloy material etc.
2. can continuously produce possess that plated layer compact is even, rule of surface is smooth, the molybdenum-base composite material of corrosion-resistant, anti-high and low-temp oxidation, the type of matrix material comprises Mo-MoSi
2/ Si, Mo-Nb-MoSi
2/ NbSi
2/ Si, Mo-W-MoSi
2/ WSi
2/ Si, Mo-Cr-MoSi
2/ CrSi
2, Mo-Ni-MoSi
2/ NiSi
2corrosion-resistant, the oxidation resistant metal-base composites such as/Si.
3. produced molybdenum-base composite material has good comprehensive mechanical property, has corrosion-resistant, anti-high and low-temp oxidation etc.
Advantage, can meet the particular requirement of electronics, metallurgy, nuclear industry, boats and ships, aviation and space field preferably.
4. body material shape can be the Mo and Mo alloys material of sheet material, wire rod, tubing and complicated shape.Achieving the suitability for industrialized production of the continuous plating silicon composite of Mo and Mo alloys, simplify production technique, reduce production cost, improve quality product, effectively enhance productivity, is a kind of continuous plating silicon novel process of Mo and Mo alloys of energy-conserving and environment-protective.
Accompanying drawing explanation
The continuous plating silicon technological process of production of the Mo and Mo alloys of Fig. 1 involved by the inventive method.
The continuous plating silicon silicon groove structure of the Mo and Mo alloys of Fig. 2 involved by the inventive method, structure comprises: air knife 1, process furnace 2, stabilizing roller 3, sinking roller 4, silicon liquid 5, molybdenum plate 6.
The Mo-MoSi that Fig. 3 is plating silicon temperature when being 1460 DEG C
2/ Si matrix material photo.
The Mo-MoSi that Fig. 4 is plating silicon temperature when being 1490 DEG C
2/ Si matrix material photo.
The Mo-MoSi that Fig. 5 is plating silicon temperature when being 1520 DEG C
2/ Si matrix material photo.
The Mo-MoSi that Fig. 6 is plating silicon temperature when being 1460 DEG C
2/ Si composite material surface SEM photo.
The Mo-MoSi that Fig. 7 is plating silicon temperature when being 1490 DEG C
2/ Si composite material surface SEM photo.
The Mo-MoSi that Fig. 8 is plating silicon temperature when being 1520 DEG C
2/ Si composite material surface SEM photo.
Fig. 9 is Mo-MoSi
2silicon molybdenum content distribution plan on/Si composite deposit section.
Figure 10 is Mo-MoSi
2the EDS figure on/Si composite deposit surface
Figure 11 is for being Mo-MoSi
2the XRD figure on/Si composite deposit surface
Embodiment
With embodiment, the inventive method is described below.It should be understood that these embodiments are only used for further illustrating embodiment of the present invention, instead of for limiting the present invention.
Embodiment 1:
By many crowdes of 2mm × 200mm × 10000mm metal molybdenum plate Abrollhaspel uncoiling, align after pinching, make its rule of surface, smooth.Adopt CO
2gasshielded welding machine welding molybdenum plate, and to send into bedroom electrolytic cleaning tank concentration be 2%, the caustic soda (NaOH) of temperature about 60 DEG C scrubs molybdenum plate, removes ROLLING OIL and the impurity of material surface, with hot water rinsing molybdenum plate, and dries with electrical heater.Metal molybdenum plate is preheating to 300 DEG C in argon shield preheating oven, and temperature survey infrared thermometer is measured.Molybdenum plate is sent in argon atmosphere in polysilicon bath trough after preheating terminates and start to plate silicon continuously; the polysilicon solution of silicon liquid to be purity be 7N; plating silicon temperature is 1450 DEG C; the plating silicon time is 15 minutes; plating silicon atmosphere is argon atmosphere; and the coating weight on molybdenum plate surface is controlled by air knife, air knife adopts coating weight automated closed-loop to control and artificial vernier control.After coating terminates, molybdenum plate plating piece is sent in vacuum annealing furnace the annealed alloy process carrying out 1000 DEG C, annealing time is 3 hours, and high temperature annealing atmosphere is argon atmosphere.By controlling control thickness of coating that annealing temperature and annealing time can be strict and coating material composition.Anneal terminate rear to plating piece carry out argon gas spray cooling and shrend cooling.First spraying cooling with argon gas is cooled to lower than 200 DEG C by plating piece, then carries out being cooled to about 50 DEG C entering watch-quench tank.Cooling terminates rear X-ray thickness of coating tester, feedback thickness of coating, according to feedback data adjustment air knife parameter, better controls thickness of coating.Finally carry out polishing aligning to molybdenum plate plating piece, adopt Electric heating to dry plating piece, bake out temperature controls at 70 DEG C, detects and shows quality and batch with mandrel sleeve pipe cantilevered reeling machine, successfully prepared the Mo-MoSi that thickness of coating is 30 μm after drying
2/ Si matrix material.
Embodiment 2:
By many crowdes of 2mm × 200mm × 10000mm Mo-3Nb alloy sheets Abrollhaspel uncoiling, align after pinching, make its rule of surface, smooth.Adopt CO
2gasshielded welding machine welding Mo-3Nb alloy sheets, and to send into bedroom electrolytic cleaning tank concentration be 2%, the caustic soda (NaOH) of temperature about 60 DEG C scrubs molybdenum plate, removes ROLLING OIL and the impurity of material surface, with hot water rinsing molybdenum plate, and dries with electrical heater.Mo-3Nb alloy sheets protected in preheating oven at argon gas and be preheating to 300 DEG C, temperature survey infrared thermometer is measured.Molybdenum plate is sent in argon atmosphere in polysilicon bath trough after preheating terminates and start to plate silicon continuously; the polysilicon solution of silicon liquid to be purity be 7N; plating silicon temperature is 1475 DEG C; the plating silicon time is 20 minutes; plating silicon atmosphere is argon atmosphere; and by the coating weight on air knife control Mo-3Nb alloy sheets surface, air knife adopts coating weight automated closed-loop to control and artificial vernier control.After coating terminates, molybdenum plate plating piece is sent in vacuum annealing furnace the annealed alloy process carrying out 1200 DEG C, annealing time is 2 hours, and high temperature annealing atmosphere is argon atmosphere.By controlling control thickness of coating that annealing temperature and annealing time can be strict and coating material composition.Anneal terminate rear to plating piece carry out argon gas spray cooling and shrend cooling.First spraying cooling with argon gas is cooled to lower than 200 DEG C by plating piece, then carries out being cooled to about 50 DEG C entering watch-quench tank.Cooling terminates rear X-ray thickness of coating tester, feedback thickness of coating, according to feedback data adjustment air knife parameter, better controls thickness of coating.Finally carry out polishing aligning to molybdenum plate plating piece, adopt Electric heating to dry plating piece, bake out temperature controls at 90 DEG C, detects and shows quality and batch with mandrel sleeve pipe cantilevered reeling machine, successfully prepared the Mo-Nb-MoSi that thickness of coating is 60 μm after drying
2/ NbSi
2/ Si matrix material.
Embodiment 3:
By the Mo-30W alloy sheets Abrollhaspel uncoiling of many crowdes of 2mm × 100mm × 1000mm, align after pinching, make its rule of surface, smooth.Sending into bedroom electrolytic cleaning tank concentration is 2%, and the caustic soda (NaOH) of temperature about 60 DEG C scrubs Mo-30W alloy sheets, removes ROLLING OIL and the impurity of material surface, with hot water rinsing molybdenum plate, and dries with electrical heater.Mo-30W alloy sheets is preheating to 300 DEG C in argon shield preheating oven, and temperature survey infrared thermometer is measured.Molybdenum plate is sent in argon atmosphere in polysilicon bath trough after preheating terminates and start to plate silicon continuously; the polysilicon solution of silicon liquid to be purity be 7N; plating silicon temperature is 1500 DEG C; the plating silicon time is 25 minutes; plating silicon atmosphere is argon atmosphere; and by the coating weight on air knife control Mo-30W alloy sheets surface, air knife adopts coating weight automated closed-loop to control and artificial vernier control.After coating terminates, molybdenum plate plating piece is sent in vacuum annealing furnace the annealed alloy process carrying out 1400 DEG C, annealing time is 1 hour, and high temperature annealing atmosphere is argon atmosphere.By controlling control thickness of coating that annealing temperature and annealing time can be strict and coating material composition.Anneal terminate rear to plating piece carry out argon gas spray cooling and shrend cooling.First spraying cooling with argon gas is cooled to lower than 200 DEG C by plating piece, then carries out being cooled to about 50 DEG C entering watch-quench tank.Cooling terminates rear X-ray thickness of coating tester, feedback thickness of coating, according to feedback data adjustment air knife parameter, better controls thickness of coating.Finally carry out polishing aligning to molybdenum plate plating piece, adopt Electric heating to dry plating piece, bake out temperature controls at 110 DEG C, detects and shows quality and batch with mandrel sleeve pipe cantilevered reeling machine, successfully prepared the Mo-W-MoSi that thickness of coating is 60 μm after drying
2/ WSi
2/ Si matrix material.
Claims (3)
1. a continuous plating silicon technology for Mo and Mo alloys, is characterized in that: handling object is Mo and Mo alloys; Processing step is as follows:
(1) Mo and Mo alloys material uncoiling, pinch, align: by the uncoiling of Mo and Mo alloys material Abrollhaspel, align after pinching, make its rule of surface, smooth;
(2) weld, clean: welding adopts CO
2gasshielded welding machine welds;
(3) preheating; Mo and Mo alloys material is preheating to 250 DEG C ~ 350 DEG C in argon shield induction preheating oven;
(4) silicon liquid preparation: purity is that the polysilicon of 7N is heated to 1450 ~ 1500 DEG C by employing large-scale vacuum induction heater, and process furnace atmosphere is argon atmosphere;
(5) silicon-air knife process is plated continuously: Mo and Mo alloys is sent into silicon groove in argon atmosphere, carry out silicon layer and be coated with plating, coating temperature is at 1450 ~ 1500 DEG C, and the coating weight of Mo and Mo alloys material surface is controlled by air knife, air knife adopts coating weight automated closed-loop to control and artificial vernier control;
(6) annealed alloy: sent in vacuum controlled atmosphere annealing furnace by Mo and Mo alloys plating piece and carry out, annealing temperature is 1000 ~ 1400 DEG C, and annealing time is 1 ~ 3 hour, and annealing atmosphere is argon atmosphere;
(7) plating piece cooling: the plating piece after coating is carried out argon gas and spray cooling and shrend cooling; First spray cooling with argon gas and plating piece is cooled to 150 ~ 250 DEG C, and then immerse watch-quench tank and carry out being cooled to 50 DEG C ~ 80 DEG C;
(8) polishing, aligning: polishing aligning carries out polishing with polishing machine after plating piece being gone out cooling tower, and align in withdrawal straightening machine, straight to ensure the polishing of plating piece;
(9) oven dry is batched: adopt Electric heating to dry plating piece, bake out temperature controls at 60 ~ 120 DEG C, and rear detection surface quality to be dried is also batched with mandrel sleeve pipe cantilevered reeling machine.
2. technique according to claim 1, is characterized in that, described Mo and Mo alloys comprises pure Mo, molybdenum niobium alloy material, miramint material, chrome molybdenum material, nickel-molybdenum alloy material, silicon molybdenum alloy material.
3. technique according to claim 1, it is characterized in that, cleaning in step (2) is removed the ROLLING OIL of material surface and impurity, cleaning equipment is horizontal electrolytic cleaning, and cleaning equipment comprises alkali spray tank, electrolytic cleaning tank, alkali are scrubbed, hot water rinse tank and induction furnace are dried; Scavenging solution is concentration is 2 ~ 3%, the caustic soda of temperature 50 C ~ 70 DEG C.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3192065A (en) * | 1962-06-01 | 1965-06-29 | North American Aviation Inc | Method of forming molybdenum silicide coating on molybdenum |
| US5389454A (en) * | 1992-12-21 | 1995-02-14 | Praxair S.T. Technology, Inc. | Silicide coating having good resistance to molten metals |
| CN101704310A (en) * | 2009-11-17 | 2010-05-12 | 河北理工大学 | Mo-Mo+Si+Al functionally graded material and preparation method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01287950A (en) * | 1988-05-13 | 1989-11-20 | Seiko Epson Corp | Semiconductor device and manufacture thereof |
-
2013
- 2013-06-07 CN CN201310226315.3A patent/CN103320735B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3192065A (en) * | 1962-06-01 | 1965-06-29 | North American Aviation Inc | Method of forming molybdenum silicide coating on molybdenum |
| US5389454A (en) * | 1992-12-21 | 1995-02-14 | Praxair S.T. Technology, Inc. | Silicide coating having good resistance to molten metals |
| CN101704310A (en) * | 2009-11-17 | 2010-05-12 | 河北理工大学 | Mo-Mo+Si+Al functionally graded material and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| JP平1-287950A 1989.11.20 * |
| Progress in Research on Mo-MoSi2 Functionally Gradient Material;Yingyi Zhang et al;《Advanced Materials Research》;20110604;第287-290卷;第636-641页 * |
| 渗硅制备Mo-MoSi2梯度材料层的特性;李运刚;《稀有金属材料与工程》;20081130;第37卷(第11期);第1992-1995页 * |
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