CN103320735A - 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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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 production technical field of metal-base composites, the continuous plating silicon technology of a kind of molybdenum and alloy thereof particularly is provided.
Background technology
Molybdenum and alloy thereof have obtained quick application at electronics, metallurgy, nuclear industry, aviation and space field, are widely used as the fields such as emtting electrode, guided missile jet pipe, satellite rocket thruster, engine blade and high temperature electrode in the thermionic reactor of space.But, molybdenum and alloy thereof at high temperature very easily oxidation generate high-volatile MoO
3, finally cause member to damage, cause molybdenum and alloy thereof not to be on active service in the oxidizing atmosphere midium or long term.At present, the preparation method of molybdenum and alloy coat thereof mainly contains plasma spraying process, chemical Vapor deposition process (CVD), laser cladding and fused salt electrodip process etc. both at home and abroad.Adopt above-mentioned several method to prepare molybdenum-base composite material and mostly have defectives such as hole, cavity and crackle, mechanical property is all relative relatively poor with high-temperature oxidation resistance, and the work-ing life of material is short; Secondly, there is the processing condition complexity in aforesaid method,, the production cost height is easy to generate toxic gas, and contaminate environment can not realize shortcomings such as serialization industrial production.At present, the research of producing molybdenum-base composite material at the continuous plating silicon of molybdenum and alloy thereof yet there are no report.
Summary of the invention
The object of the present invention is to provide the continuous plating silicon technology of a kind of molybdenum and alloy thereof, processing mainly comprises pure Mo, molybdenum niobium alloy material, miramint material, chrome molybdenum Materials science, nickel-molybdenum alloy material, silicon molybdenum alloy material etc. to liking molybdenum and alloy thereof.
The present invention adopts the continuous plating silicon technology of cleaning-preheating-plate continuously silicon-annealed alloyization-plating sample cooling, can plate silicon production molybdenum-base composite material continuously to molybdenum and alloy thereof, handle object and mainly comprise pure Mo, molybdenum niobium alloy material, miramint material, chrome molybdenum material, nickel-molybdenum alloy material, silicon molybdenum alloy material etc.Can continuously produce and possess that coating is fine and close evenly, rule of surface is smooth, corrosion-resistant, the molybdenum-base composite material of 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, oxidation resistant metal-base composites such as/Si, material shape can be molybdenum and the alloy materials thereof of sheet material, wire rod, tubing and complicated shape.Realized the suitability for industrialized production of the continuous plating silicon composite of molybdenum and alloy thereof, simplified production technique, reduced production cost, improved quality product, effectively enhanced productivity.Processing step is as follows:
(1) uncoiling of molybdenum and alloy material thereof, pinches, aligns: molybdenum and alloy material thereof with the Abrollhaspel uncoiling, align, are made its rule of surface, smooth after pinching.
(2) welding, cleaning: CO is adopted in welding
2The gasshielded welding machine welding, welding wire can be chosen different gas shield welding wires according to the difference of molybdenum and alloy material thereof; Cleaning is with the ROLLING OIL of material surface and contaminant removal, and cleaning equipment is the bedroom electrolytic cleaning, and cleaning equipment comprises that alkali spray tank, electrolytic cleaning tank, alkali are scrubbed, hot water rinse tank and induction furnace drying system.Scavenging solution is that concentration is 2～3%, the caustic soda (NaOH) that temperature is about 50 ℃～70 ℃.
(3) preheating; Molybdenum and alloy material thereof are preheating to 250 ℃～350 ℃ in argon shield induction preheating oven, temperature survey is measured with infrared thermometer.The 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 the 2mm304 stainless steel lined, and furnace bottom is the 200mm ceramic fiber.
(4) silicon liquid preparation: adopting large-scale vacuum induction that American I A company produces is that the polysilicon of 7N is heated to 1450～1500 ℃ with purity, and process furnace atmosphere is argon shield atmosphere.
(5) plating silicon-air knife continuously handles: molybdenum and alloy thereof are sent into the silicon groove in argon shield atmosphere; carrying out the silicon layer coating handles; the coating temperature is at 1450～1500 ℃; and control the coating weight on molybdenum and alloy material surface thereof by air knife, air knife adopts the control of coating weight automated closed-loop and artificial fine setting control.
(6) annealed alloyization: molybdenum and alloy plating piece thereof are sent into the annealed alloy processing of carrying out processing condition in the vacuum controlled atmosphere annealing furnace, and annealing temperature is 1000～1400 ℃, and annealing time is 1～3 hour, and high temperature annealing atmosphere is argon shield atmosphere.By controlling control thickness of coating and the coating material composition that annealing temperature and annealing time can be strict.
(7) plating piece cooling: the plating piece behind the coating is carried out argon gas shower cooling and shrend cooling.At first with the argon gas shower cooling plating piece is cooled to 150～250 ℃, is cooled to 50 ℃～80 ℃ entering watch-quench tank then.The oven dry plating piece adopts Electric heating oven dry plating piece, and bake out temperature is controlled at 60～120 ℃.Carry out the plating piece inspection then, an X ray thickness of coating tester namely is set in the watch-quench tank back, the feedback thickness of coating is adjusted the air knife parameter according to feedback data, better controls thickness of coating.
(8) polishing, aligning: the polishing aligning is to carry out polishing with the light complete machine after plating piece is gone out cooling tower, and aligns in the straightening machine, and is straight with the polishing that guarantees plating piece.
(9) oven dry is batched: adopt Electric heating oven dry plating piece, bake out temperature control at 60～120 ℃, waits to dry the back and detects and show that quality also batches with mandrel sleeve pipe cantilevered reeling machine.
In the aforesaid method, molybdenum and alloy material thereof just can obtain corrosion-resistant, oxidation resistant molybdenum-base composite material after a series of continuous plating silicon are handled, and 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
2Multiple molybdenum-base composite material such as/Si.
Compare with existing technological method, the present invention has following advantage:
1. the invention has the advantages that the continuous plating silicon processing that can be used for multiple molybdenum and alloy thereof, handle object and mainly comprise 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 and possess that coating is fine and close evenly, rule of surface is smooth, corrosion-resistant, the molybdenum-base composite material of 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, oxidation resistant metal-base composites such as/Si.
3. the molybdenum-base composite material of producing has good comprehensive mechanical properties, has corrosion-resistant, anti-high and low-temp oxidation etc.
Advantage can satisfy the particular requirement of electronics, metallurgy, nuclear industry, boats and ships, aviation and space field preferably.
4. the body material shape can be molybdenum and the alloy material thereof of sheet material, wire rod, tubing and complicated shape.Having realized the suitability for industrialized production of the continuous plating silicon composite of molybdenum and alloy thereof, simplified production technique, reduced production cost, improved quality product, effectively enhanced productivity, is a kind of continuous plating silicon novel process of molybdenum and alloy thereof of energy-conserving and environment-protective.
Description of drawings
Fig. 1 is the continuous plating silicon technological process of production of the related molybdenum of the inventive method and alloy thereof.
Fig. 2 is the continuous plating silicon silicon groove structure of the related molybdenum of the inventive method and alloy thereof, and structure comprises: air knife 1, process furnace 2, stablize roller 3, sinking roller 4, silicon liquid 5, molybdenum plate 6.
Mo-MoSi when Fig. 3 is 1460 ℃ for plating silicon temperature
2/ Si matrix material photo.
Mo-MoSi when Fig. 4 is 1490 ℃ for plating silicon temperature
2/ Si matrix material photo.
Mo-MoSi when Fig. 5 is 1520 ℃ for plating silicon temperature
2/ Si matrix material photo.
Mo-MoSi when Fig. 6 is 1460 ℃ for plating silicon temperature
2/ Si composite material surface SEM photo.
Mo-MoSi when Fig. 7 is 1490 ℃ for plating silicon temperature
2/ Si composite material surface SEM photo.
Mo-MoSi when Fig. 8 is 1520 ℃ for plating silicon temperature
2/ Si composite material surface SEM photo.
Fig. 9 is Mo-MoSi
2Silicon molybdenum content distribution figure on the/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 specifying embodiment of the present invention, rather than be used for restriction the present invention.
Embodiment 1:
Many crowdes of 2mm * 200mm * 10000mm metal molybdenum plate with the Abrollhaspel uncoiling, align, is made its rule of surface, smooth after pinching.Adopt CO
2Gasshielded welding machine welding molybdenum plate, and to send into bedroom electrolytic cleaning tank concentration be 2%, the about 60 ℃ caustic soda (NaOH) of temperature is scrubbed molybdenum plate, removes ROLLING OIL and the impurity of material surface, usefulness hot water rinsing molybdenum plate, and dry with electrical heater.The metal molybdenum plate is preheating to 300 ℃ in the argon shield preheating oven, temperature survey is measured with infrared thermometer.After preheating finishes molybdenum plate sent in the polysilicon bath trough beginning plating silicon continuously in argon shield atmosphere; silicon liquid is that purity is the polysilicon solution of 7N; plating silicon temperature is 1450 ℃; the plating silicon time is 15 minutes; plating silicon atmosphere is argon shield atmosphere; and control the coating weight on molybdenum plate surface by air knife, air knife adopts the control of coating weight automated closed-loop and artificial fine setting control.After coating finishes the molybdenum plate plating piece sent into and carry out 1000 ℃ annealed alloy processing in the vacuum annealing furnace, annealing time is 3 hours, and high temperature annealing atmosphere is argon shield atmosphere.By controlling control thickness of coating and the coating material composition that annealing temperature and annealing time can be strict.Anneal finishes the back plating piece is carried out argon gas shower cooling and shrend cooling.At first with the argon gas shower cooling plating piece is cooled to and is lower than 200 ℃, be cooled to about 50 ℃ entering watch-quench tank then.Cooling finishes the back with X ray thickness of coating tester, feeds back thickness of coating, adjusts the air knife parameter according to feedback data, better controls thickness of coating.At last the molybdenum plate plating piece is carried out polishing and align, adopt Electric heating oven dry plating piece, bake out temperature is controlled at 70 ℃, and the detection of oven dry back shows quality and batch with mandrel sleeve pipe cantilevered reeling machine that successfully having prepared thickness of coating is the Mo-MoSi of 30 μ m
2/ Si matrix material.
Embodiment 2:
Many crowdes of 2mm * 200mm * 10000mm Mo-3Nb alloy sheets with the Abrollhaspel uncoiling, align, is made its rule of surface, smooth after pinching.Adopt CO
2Gasshielded welding machine welding Mo-3Nb alloy sheets, and to send into bedroom electrolytic cleaning tank concentration be 2%, the about 60 ℃ caustic soda (NaOH) of temperature is scrubbed molybdenum plate, removes ROLLING OIL and the impurity of material surface, usefulness hot water rinsing molybdenum plate, and dry with electrical heater.The Mo-3Nb alloy sheets is preheating to 300 ℃ in argon gas is protected preheating oven, temperature survey is measured with infrared thermometer.After preheating finishes molybdenum plate sent in the polysilicon bath trough beginning plating silicon continuously in argon shield atmosphere; silicon liquid is that purity is the polysilicon solution of 7N; plating silicon temperature is 1475 ℃; the plating silicon time is 20 minutes; plating silicon atmosphere is argon shield atmosphere; and control the coating weight on Mo-3Nb alloy sheets surface by air knife, air knife adopts the control of coating weight automated closed-loop and artificial fine setting control.After coating finishes the molybdenum plate plating piece sent into and carry out 1200 ℃ annealed alloy processing in the vacuum annealing furnace, annealing time is 2 hours, and high temperature annealing atmosphere is argon shield atmosphere.By controlling control thickness of coating and the coating material composition that annealing temperature and annealing time can be strict.Anneal finishes the back plating piece is carried out argon gas shower cooling and shrend cooling.At first with the argon gas shower cooling plating piece is cooled to and is lower than 200 ℃, be cooled to about 50 ℃ entering watch-quench tank then.Cooling finishes the back with X ray thickness of coating tester, feeds back thickness of coating, adjusts the air knife parameter according to feedback data, better controls thickness of coating.At last the molybdenum plate plating piece is carried out polishing and align, adopt Electric heating oven dry plating piece, bake out temperature is controlled at 90 ℃, and the detection of oven dry back shows quality and batch with mandrel sleeve pipe cantilevered reeling machine that successfully having prepared thickness of coating is the Mo-Nb-MoSi of 60 μ m
2/ NbSi
2/ Si matrix material.
Embodiment 3:
The Mo-30W alloy sheets of many crowdes of 2mm * 100mm * 1000mm with the Abrollhaspel uncoiling, align, is made its rule of surface, smooth after pinching.Sending into bedroom electrolytic cleaning tank concentration is 2%, and the about 60 ℃ caustic soda (NaOH) of temperature is scrubbed the Mo-30W alloy sheets, removes ROLLING OIL and the impurity of material surface, uses hot water rinsing molybdenum plate, and dries with electrical heater.The Mo-30W alloy sheets is preheating to 300 ℃ in the argon shield preheating oven, temperature survey is measured with infrared thermometer.After preheating finishes molybdenum plate sent in the polysilicon bath trough beginning plating silicon continuously in argon shield atmosphere; silicon liquid is that purity is the polysilicon solution of 7N; plating silicon temperature is 1500 ℃; the plating silicon time is 25 minutes; plating silicon atmosphere is argon shield atmosphere; and control the coating weight on Mo-30W alloy sheets surface by air knife, air knife adopts the control of coating weight automated closed-loop and artificial fine setting control.After coating finishes the molybdenum plate plating piece sent into and carry out 1400 ℃ annealed alloy processing in the vacuum annealing furnace, annealing time is 1 hour, and high temperature annealing atmosphere is argon shield atmosphere.By controlling control thickness of coating and the coating material composition that annealing temperature and annealing time can be strict.Anneal finishes the back plating piece is carried out argon gas shower cooling and shrend cooling.At first with the argon gas shower cooling plating piece is cooled to and is lower than 200 ℃, be cooled to about 50 ℃ entering watch-quench tank then.Cooling finishes the back with X ray thickness of coating tester, feeds back thickness of coating, adjusts the air knife parameter according to feedback data, better controls thickness of coating.At last the molybdenum plate plating piece is carried out polishing and align, adopt Electric heating oven dry plating piece, bake out temperature is controlled at 110 ℃, and the detection of oven dry back shows quality and batch with mandrel sleeve pipe cantilevered reeling machine that successfully having prepared thickness of coating is the Mo-W-MoSi of 60 μ m
2/ WSi
2/ Si matrix material.
Claims (4)
1. the continuous plating silicon technology of a molybdenum and alloy thereof is characterized in that: handle to as if molybdenum and alloy thereof; Processing step is as follows:
(1) uncoiling of molybdenum and alloy material thereof, pinches, aligns: molybdenum and alloy material thereof with the Abrollhaspel uncoiling, align, are made its rule of surface, smooth after pinching;
(2) welding, cleaning: CO is adopted in welding
2The gasshielded welding machine welding;
(3) preheating; Molybdenum and alloy material thereof are preheating to 250 ℃～350 ℃ in argon shield induction preheating oven;
(4) silicon liquid preparation: adopting the large-scale vacuum induction is that the polysilicon of 7N is heated to 1450～1500 ℃ with purity, and process furnace atmosphere is argon shield atmosphere;
(5) plating silicon-air knife continuously handles: molybdenum and alloy thereof are sent into the silicon groove in argon shield atmosphere, carrying out the silicon layer coating handles, the coating temperature is at 1450～1500 ℃, and control the coating weight on molybdenum and alloy material surface thereof by air knife, air knife adopts the control of coating weight automated closed-loop and artificial fine setting control;
(6) annealed alloyization: molybdenum and alloy plating piece thereof sent in the vacuum controlled atmosphere annealing furnace carry out, annealing temperature is 1000～1400 ℃, and annealing time is 1～3 hour, and annealing atmosphere is argon shield atmosphere;
(7) plating piece cooling: the plating piece behind the coating is carried out argon gas shower cooling and shrend cooling; At first with the argon gas shower cooling plating piece is cooled to 150～250 ℃, is cooled to 50 ℃～80 ℃ entering watch-quench tank then;
(8) polishing, aligning: the polishing aligning is to carry out polishing with the light complete machine after plating piece is gone out cooling tower, and aligns in the straightening machine, and is straight with the polishing that guarantees plating piece;
(9) oven dry is batched: adopt Electric heating oven dry plating piece, bake out temperature control at 60～120 ℃, waits to dry the back and detects and show that quality also batches with mandrel sleeve pipe cantilevered reeling machine.
2. method according to claim 1 is characterized in that, described molybdenum and alloy thereof comprise pure Mo, molybdenum niobium alloy material, miramint material, chrome molybdenum material, nickel-molybdenum alloy material, silicon molybdenum alloy material.
3. method according to claim 1, it is characterized in that, cleaning in the step (2) is ROLLING OIL and the contaminant removal with material surface, and cleaning equipment is the bedroom electrolytic cleaning, and cleaning equipment comprises that alkali spray tank, electrolytic cleaning tank, alkali are scrubbed, hot water rinse tank and induction furnace oven dry; Scavenging solution is that concentration is 2～3%, the caustic soda that temperature is about 50 ℃～70 ℃.
4. method according to claim 1, it is characterized in that induction preheating oven preheating section furnace shell adopts the thick carbon steel furnace shell of 6mm in the step (3), refractory materials adopts the thick ceramic fiber of 150mm, liner adopts the 2mm304 stainless steel lined, and furnace bottom is the 200mm ceramic fiber.
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Citations (4)
| 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 |
| JPH01287950A (en) * | 1988-05-13 | 1989-11-20 | Seiko Epson Corp | Semiconductor device and manufacture thereof |
| 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 |
-
2013
- 2013-06-07 CN CN201310226315.3A patent/CN103320735B/en active Active
Patent Citations (4)
| 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 |
| JPH01287950A (en) * | 1988-05-13 | 1989-11-20 | Seiko Epson Corp | Semiconductor device and manufacture thereof |
| 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 (2)
| Title |
|---|
| YINGYI ZHANG ET AL: "Progress in Research on Mo-MoSi2 Functionally Gradient Material", 《ADVANCED MATERIALS RESEARCH》 * |
| 李运刚: "渗硅制备Mo-MoSi2梯度材料层的特性", 《稀有金属材料与工程》 * |
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